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WO1998052993A1 - Matiere polymere contenant du bore presentant une structure fonctionnelle de protection et sa preparation - Google Patents

Matiere polymere contenant du bore presentant une structure fonctionnelle de protection et sa preparation Download PDF

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Publication number
WO1998052993A1
WO1998052993A1 PCT/CN1998/000072 CN9800072W WO9852993A1 WO 1998052993 A1 WO1998052993 A1 WO 1998052993A1 CN 9800072 W CN9800072 W CN 9800072W WO 9852993 A1 WO9852993 A1 WO 9852993A1
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WO
WIPO (PCT)
Prior art keywords
group
boron
organic
metal
parts
Prior art date
Application number
PCT/CN1998/000072
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English (en)
Chinese (zh)
Inventor
Shenggang Zhou
Original Assignee
Shenzhen House Safety Investment Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from CN 97112075 external-priority patent/CN1199748A/zh
Priority claimed from CN 97112073 external-priority patent/CN1199747A/zh
Application filed by Shenzhen House Safety Investment Co., Ltd. filed Critical Shenzhen House Safety Investment Co., Ltd.
Priority to AU73301/98A priority Critical patent/AU7330198A/en
Publication of WO1998052993A1 publication Critical patent/WO1998052993A1/fr

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G79/00Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
    • C08G79/08Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing boron

Definitions

  • the invention relates to a boron polymer material with an adaptive protective function structure and a preparation method thereof, and in particular, to a protective function with high-temperature insulation, high-temperature oxidation resistance, fire retardancy, radiation absorption, nuclear radiation shielding, and high-energy beam impact resistance.
  • Structural materials and methods of making them The so-called “adaptiveness” refers to a continuous physical and chemical comprehensive reaction with a protective effect caused by environmental conditions, especially temperature changes, and the protective response has a dynamic corresponding property; the so-called “protective functional structure” refers to the elements of the structure on the one hand The proportion and element structure are reasonable. On the other hand, it is required that the structure does not collapse instantaneously under the action of high temperature or high temperature kinetic energy, but has a directional transition from one adaptive structure to another adaptive structure. Part of the transformation is reversible.
  • thermos flask The heat insulation is not adiabatic--Only the structure of the thermos flask is within a very narrow range of temperature difference of 300'C-600'C. It has adiabatic effect; 5. The commercial cost of the price / performance ratio is high, and it cannot meet the growing social needs.
  • Harmful elements containing halogen, sulfur, phosphorus, and heavy metals-High-temperature thermal decomposition is likely to produce toxic asphyxiating gases or substances that are likely to pollute the environment.
  • Patent documents include US85-4504611, US85-4506036, US5179048, US4910173, US93-5272237, JP91-289338, and other halogen-containing elements; JP91-305218, tebupine 7-278267, and other phosphorus-containing elements; JP87-130782 contains lead.
  • the core element boron of the flame retardant should not directly form a molecular structure with elements other than C, 0, N, otherwise it is not conducive to high temperature oxidation resistance or to form a stable protective structure under high temperature conditions.
  • US5179048 Such as patent document: US5179048.
  • US85-450461 1 uses non-boron-based molecular structures such as cyclooctyl hexachlorocyclopentane and polyamines, which is not conducive to the formation of anti-oxidation reactions at high temperatures, and its high chlorine content also easily releases harmful gases; 'US93- 5272237 adopts the molecular structure of acetylene carboboron-siloxamidine. Since the boron group is on a branched chain, there is no better high temperature application effect.
  • W095-11272 contains aldehyde toxicants and the above-mentioned literature (has been pointed out) synthetic materials containing halogen, phosphorus and heavy metal elements are easy to harm the environment and production personnel during the production process.
  • Ping 7-27826 does not contain halogen, it contains harmful flame retardants such as phosphoric acid in its synthesis, and can generate toxic phosphoric acid vapor and other harmful gases in high heat, which pollutes the environment.
  • US75-3891621 is a glucopyranoside-containing boropolymer and its derivative, in which the alkylboronyl group is in an important position in the structure between sugar alcohols.
  • the reactants due to improper selection of the raw material reactants, that is, the reactants contribute to the biological elements ⁇ : 0 ⁇ 4: 1, the hydrogen element easily burns and generates heat at high temperatures, and the production preparation method is not optimized, that is, the orientation of the structured water is not increased in the reaction preparation method.
  • Process reaction so there are many deficiencies in the technical system-in addition to the previous analysis, there is also a very low structural water content (about 36%), and no functional structure is formed. Therefore, high temperature insulation, resistance to high energy beam impact and radiation Poor performance such as shielding.
  • JP87-38874 uses a water-soluble polycondensation preparation method.
  • the main raw materials are also inorganic borides, such as boric acid.
  • the shortcomings are mainly reflected in the choice of reactants to be fluorinated hydrocarbon groups or chloride compounds.
  • the former generates a large amount of heat at high temperatures, which is not conducive to it. Fire and flame retardant, the latter chloride is liable to produce harmful gases or pollution components in the fire.
  • the disadvantage of the method is also that the directional process reaction of structured water is not added in the preparation method. No better protection.
  • thermal decomposition of functional materials and adaptive reaction changes are used to achieve the goal of higher thermal conductivity and lower thermal conductivity.
  • the thermal conductivity between 700-3600 ° C is smaller than traditional thermal insulation materials 2- 4 orders of magnitude;
  • the present invention also provides a protective material having the following characteristics:
  • thermonuclear firefighting which can absorb thermal neutrons while also losing nuclear energy-control and block the ongoing of thermonuclear accidents
  • High-energy impact resistance the impact resistance of high-energy beams such as lasers exceeds any existing materials
  • the commercial cost is suitable, and it can be mass-produced and easy to be widely used.
  • the present invention forms an organic boron polymer with a protective functional structure by using inorganic boride and organic matter or sugars, so that it can be used under adaptive dynamic (thermal reaction / thermal decomposition) conditions
  • organic functional materials are used to achieve high-precision and cost-effective comprehensive protection purposes.
  • the object of the present invention is to overcome the shortcomings in the prior art, and to provide a material with a protective function structure having adaptive dynamic characteristics and a preparation method thereof.
  • the object of the present invention is achieved by providing a boron polymer material with a protective function structure.
  • the material has a main structure with a boron group or a boroxy group as the center and an organic active group, and has Structured and bound water with a total weight of 50-80%;
  • the organic active group is selected from the group consisting of a hydroxyl group, an aldehyde group, a ketone group, and a carboxyl group;
  • the bound water refers to free water naturally adsorbed when the material is generated and water molecules in various forms in the reaction filling;
  • the structured water refers to all H and 0 elements constituting the functional structure of the material, and the content ratio is 1.6: 1-2.5: 1.
  • a material provided by the present invention is that the main structure composed of a boron group or a boronoxy group and an organic active group contains one or more of the following structural units:
  • Sc is a glycosyl
  • R, R, and R 2 are an oxygen-containing organic group or an alkane group
  • M is a base or other inorganic root.
  • the main structure of the above materials may further contain one or more of auxiliaries, modifiers, and fillers to form a marginal functional structure having the following general formula:
  • MC is a stabilizing group of a modifier or stabilizer
  • the auxiliary agent is selected from one or two selected from the group consisting of sodium hydroxide, potassium hydroxide, ammonia, silica, and non-toxic organic acids;
  • the modifier is selected from the group consisting of alkaline earth metal hydroxides, fourth-cycle metal oxides, fourth-cycle metal hydroxides, antimony and tin compounds, ammonia or alkali metal silicates, ammonia or alkali metal carbonates, One or two of the group consisting of ammonia or alkali metal organic acid salt, gum arabic, and active silica;
  • the filler is selected from alumina, aluminum hydroxide, aluminum compounds, titanium oxide, titanium hydroxide, magnesium double oxide, calcium hydroxide, poorly soluble silicates and carbonates, silicon powder, boron powder, and carbides. , Insoluble carbohydrates, natural adhesives, one or more of the group consisting of halogen / sulfur / phosphorus-free synthetic resins and their adhesives.
  • Another material provided by the present invention is that the main structure composed of a boron group or a boronoxy group and an organic active group contains one or more of the following structural units:
  • R, R, and R 2 are the same or different oxygen-containing organic groups
  • M is a base or an inorganic root.
  • the main structure of the above materials may further contain one or more of auxiliaries, modifiers, and fillers to form a marginal functional structure having the following general formula:
  • MC is a stabilizing group of a modifier or stabilizer
  • the auxiliary agent is selected from the group consisting of metal organic catalyst, silicon oxide, boron oxide, alkali metal hydroxide, and alkali.
  • metal organic catalyst silicon oxide, boron oxide, alkali metal hydroxide, and alkali.
  • earth metal oxide shrinkage agent one or more of the group consisting of earth metal oxide shrinkage agent, alkaline earth metal silicide powder, carbon powder, semiconductor elementary ultrafine particles, resin ion adsorbent, amphoteric metal oxide, amino acid and other pH buffer adjusters
  • the modifier is selected from the group consisting of metal oxides, metal hydroxides, carbonates, silicas, silicates, volatile non-toxic or slightly toxic alcohols and ester solvents, active groups containing metal elements, elemental carbon, stable metals
  • the filler is any inorganic or organic substance which does not directly react with boron-based or ammonia solution, alcohols, alkali metal alcoholates, aliphatic carboxylic acids and derivatives thereof, and alcohol amines.
  • the invention further provides a method for preparing a boron polymer material with an adaptive protective function structure, which is a reaction of a substance having a hydroxyl group, an aldehyde group or a ketone group with an inorganic boride to produce a compound having a boron group or a boronoxy group as
  • the center and the organic active group constitute a main structure, and have structured water and bound water which account for 50-80% of the total weight of the material;
  • the bound water refers to free water naturally adsorbed when the material is generated and water molecules in various forms in the reaction filling;
  • the structured water refers to all H and 0 elements in the material, and the content ratio is close to 1.6: 1-2.5: 1;
  • the inorganic boride is selected from one or more of metal boride, boron oxide, boric acid and its salts, metaborate, tetra / pentaborate, and perborate.
  • the present invention also provides the above-mentioned boron polymer material with a protective function structure in the preparation of a) 200.
  • C-5000 'C Application in high energy beam impact resistant products The product may be an engineering structural material or a decorative material.
  • the substance having a hydroxyl group, an aldehyde group or a keto group is selected from the group consisting of monosaccharides, disaccharides, trisaccharides, polysaccharides, sugar acids and their metal salts, ammonium sugar acids, water-soluble cellulose and their salts, and sugars ( Class) composed of organic cellulose
  • an inorganic boride containing no halogen, sulfur, phosphorus, and arsenic and the saccharides and derivatives are derived. React with each other to form a sugar-boron copolymer having one or more of the aforementioned functional structures (al)-(alO).
  • the functional structure is to ensure as much structural water content as possible, so carbohydrates are selected as the main reactants-water-soluble substances are one of the reactants that make up the functional structure, and water-insoluble substances are used as fillers.
  • carbohydrates are selected as the main reactants-water-soluble substances are one of the reactants that make up the functional structure, and water-insoluble substances are used as fillers.
  • water-insoluble substances are used as fillers.
  • the inorganic boride is selected (acid / base / salt) water-soluble boride;
  • Alcohol or an aqueous solution containing 0.1-50% alcohol and derivatives is an intermediate reactant of the present invention, wherein the alcohol One or more selected from the group consisting of ethanol, ethylene glycol, glycerol, pentaerythritol, sorbitol and the like; non-toxic polyols are preferred (preferable range should be less than the aforementioned range).
  • the inorganic boride is selected from one or more of the group consisting of metal boride, boron oxide, boric acid (salt), metaborate, tetra / pentaborate, and perborate; preferably, boride Aluminium (zinc / sodium / magnesium), boron oxide, boric acid, sodium (potassium) borate, sodium metaborate (potassium), (aqueous) sodium tetraborate (potassium), ammonium pentaborate, sodium perborate Or more.
  • Carbohydrates and their derivatives are selected from the group consisting of monosaccharides, disaccharides, trisaccharides, polysaccharides, sugar acids and their metal salts, sugar acid ammonium salts, water-soluble cellulose and their salts, and sugar (class) organic derivatives.
  • One or two of the group preferably a group consisting of monosaccharides, disaccharides, trisaccharides, hydrolysable polysaccharides such as starch, gluconic acid and its sodium (zinc) salts, hydroxycellulose and CMC, sugar esters One or two.
  • the auxiliary is selected from one or two of the group consisting of sodium hydroxide (potassium hydroxide), ammonia, silica, and non-toxic organic acids; preferably, sodium hydroxide, ammonia, sodium silicate, lactic acid, and synthetic fatty acids , Oxalic acid, acetic acid.
  • the modifier is selected from the group consisting of alkaline earth metal hydroxides, fourth-cycle metal (hydrogen) oxides, antimony and tin compounds, ammonia or alkali metal silicic acid (carbonic acid / organic acid) salts, gum arabic, and active silica.
  • alkaline earth metal hydroxides fourth-cycle metal (hydrogen) oxides, antimony and tin compounds, ammonia or alkali metal silicic acid (carbonic acid / organic acid) salts, gum arabic, and active silica.
  • One or two of the group preferably made of calcium hydroxide (magnesium hydroxide), (hydrogen) titanium oxide (zinc / copper / manganese), ammonium antimonate (sodium / bell), sodium stannate, sodium silicate, carbonic acid
  • (hydro) ammonium weak base salts of organic acids, gum arabic, fumed silica, and white carbon black.
  • the filler is selected from (hydro) alumina, aluminum compounds, (hydro) titanium oxide, magnesium (calcium) hydroxide, poorly soluble silicates and carbonates, silicon powder, boron powder, carbides, insoluble carbohydrates
  • Natural adhesives one or more of the group consisting of halogen / sulfur / phosphorus-free synthetic resins and their adhesives; preferably composed of (hydrogen) aluminum oxide, aluminum powder, aluminum silicate, (hydrogen) oxidation Titanium, magnesium hydroxide, quartz sand, calcium carbonate, magnesium trisilicate, silicon powder, boron powder, activated carbon powder, carbon fiber, sawdust, natural rubber, epoxy resin and its curing agent, unsaturated polyester, silicone One or more of a group consisting of a polymer and an acrylic resin.
  • boron (oxygen) Can be combined with a single polyhydroxy sugar molecule, or can be copolymerized with two or three sugar molecules; in contrast, a single sugar can be combined with a single boron (oxy) group, or with two or three to six boron ( Oxygen) group.
  • the latter copolymerization group is mainly selected as the main functional structure in terms of the amount of raw materials and the reaction method.
  • auxiliaries can be added to the intermediate reaction solution.
  • the (al)-(alO) group contains sugar aldehyde group and ketone group, so the functional structure at this time is still unstable. Further technical treatment; or stand for several days at room temperature, naturally grow (micro) crystals to form the basic product of protective function structure; or add modifiers or fillers (should use the waste heat), in a multi-component mixed solution Formation of complex synthetic reactions-(addition reactions on aldehydes and ketone groups), esterification reactions, cross-linking reactions, etc.
  • (al l) (al2) (al3) Derivatives of (al l) (al2) (al3), where MC-/ MC is a stabilizing group of a modifier or filler, including metal (oxide) powder that absorbs radiation.
  • (Al l)-(al3) Form a product with a protective function structure that has the physical and chemical characteristics of a family or department and the same heterogeneous appearance effect, (al l) is a metastable structure; (al2) is a free structure; (al3) is Random structure.
  • the polysaccharide is not easily soluble in water, it is first hydrolyzed (the acid or alkali auxiliary agent can be used), and then the following reaction is performed.
  • the C1-C2 technical solution can be measured in the following optimized ranges:
  • the water or alcohol is both a reaction mediator and a reactant.
  • the main reaction methods include two kinds of hydrolysis reaction, displacement reaction / ion exchange reaction, esterification reaction, coupling reaction, polycondensation reaction and cross-linking reaction. Multiple coexisting methods.
  • arbitrary synthesis and mixing methods that do not affect the (al)-(al0) functional structure skeleton are used.
  • the boride is subjected to a series of copolymerization reactions; or d) the copolymerization reaction is performed under the above-mentioned waste heat conditions at normal pressure.
  • Can be added during the above a)-d) reaction Alternatively, no alkaline or acidic additives are added; and during or after the above a) to d) reaction, modifiers and fillers may or may not be added.
  • the intermediary reactant is selected from water or an aqueous solution containing 0.1 to 50% of an alcohol-based alcohol derivative in an amount of 30 to 230 parts by weight; 10 to 200 parts by weight of boride 3 ⁇ 41; 1 to 100 parts by weight of sugar And its derivatives; 0-50 parts by weight of auxiliaries; 0-100 parts by weight of modifiers; 0-300 parts by weight of fillers.
  • the intermediate reactant is selected from 30 to 180 parts by weight of water or 50 to 230 parts by weight of an aqueous solution containing 1 to 35% of a polyol and a derivative thereof;
  • 50 to 150 parts by weight Part of boride said boride is selected from alkali-soluble or acid-soluble non-heavy metal boride, boron oxide, boric acid, sodium (potassium) borate, sodium metaborate (potassium), (aqueous) sodium tetraborate (potassium), five One or two of ammonium borate and sodium perborate;
  • auxiliary agent selected from sodium hydroxide, ammonium
  • the intermediary reactant described in a) is selected from 50 to 120 parts by weight of water or 60 to 200 parts by weight of a non-toxic or slightly toxic alcohol aqueous solution containing 2 to 30%, wherein the alcohol may be ethanol, ethyl Glycols, glycerol, pentaerythritol, sorbitol, etc .; b) 30-120 parts by weight of boride selected from aluminum boride (zinc / sodium / magnesium), boron oxide, boric acid, sodium borate, sodium tetraborate pentahydrate, borax, One or two of ammonium pentaborate and sodium perborate; c) 5-60 parts by weight of sugars and derivatives thereof, selected from disaccharides, trisaccharides, starch, sodium gluconate (zinc), CMC, hydroxymethyl One or two of (ethyl / propyl) -based cellulose and sugar esters; d) 0-30 parts by weight of
  • MC ' is a high-temperature residue of MC, n + m water loses a lot of heat, and at the same time, it forms a microporous high temperature resistant (2000 -C-3000' C) protective structure.
  • This microporous has good vacuum insulation performance. -The higher the temperature, the better this performance. The combined contribution of both contributes to the good performance of high-temperature insulation.
  • 800 'C-1500' C its thermal conductivity is 2 to 3 orders of magnitude lower than the prior art; 1500 'C-3500' C is 3 to 4 orders of magnitude lower.
  • the thermal decomposition and heat dissipation of the material of the present invention can be directly performed below 2000 ° C-3000 'C.
  • the high water-containing material of the present invention can dissipate a large amount of heat, and can produce it in> 800 1; (al4)
  • the stable structure of the inorganic boron polymer in the formula Both the H, OH, and M components before thermal decomposition and the inorganic polymer components after thermal decomposition can absorb a large number of thermal neutrons and block the thermonuclear reaction. This double-effect contribution is better than specialty cement, and it is also superior to expensive carbon boron fibers.
  • the material of the invention contains relatively high combined water and structured water, so when it encounters high-energy beam impacts above 2500 'C-10000' C, water vapor will form hundreds to tens of thousands of dynamic atmospheric pressure-shock waves to block High energy beam strike for a long time. Such blocking performance is difficult to compare with any protective material in the prior art.
  • the adaptability of the protective material of the present invention can be applied to a wide range of wide-ranging protection fields. Therefore, it is superior to the existing protective flame retardant technology.
  • many carbohydrates such as wood and fiberboard
  • the existing technology only solves the problem of flame retardancy, and the material of the present invention surpasses the flame retardancy of existing materials in a continuous fire.
  • Performance On the one hand, dig 56% of "fire-fighting water” (about 56% of carbohydrate-containing structured water) with the help of a high-temperature environment; on the other hand, make the carbonized part not only difficult to burn, but also block its harmful gas generation.
  • the fireproof and flame retardant materials of the invention can be used in the temperature range of 350'C-5000'C.
  • the present invention solves the problem of the poor comprehensive effect of static technology in the prior art, which only highlights one characteristic but loses other characteristics.
  • an aldehyde group or a ketone group is selected from the group consisting of oils and fats, aliphatic compounds and their derivatives, organic polymers in natural plants and animals, such as vegetable fats, gums, animal oils and their salts, and synthetic resins
  • the inorganic boride is in the presence of the intermediate reactant hydroxyorganic substance and its derivative or aliphatic hydroxy acid and its derivative or alcohol amine or chlorine It reacts with organic compounds that do not contain halogen, sulfur, phosphorus, and arsenic to form a copolymer with a boron group or a boronoxy group as the functional structure.
  • the copolymer is one of the following units (bl)-(b7) or A variety of organic copolymers.
  • the present invention uses a boron group or a borooxy group as the core and an organic group as a bond to form a protective function structure of a macromolecule. Therefore, organic matter and boride are the main materials of choice.
  • each reactant is mainly composed of C, H, 0, Si, B, Na, N and other elements, and other alkali metals, alkaline earth metals, fourth-cycle transition metal elements and aluminum, germanium, antimony, etc. auxiliary.
  • the reactants of the present invention are classified as follows:
  • A3-1 Inorganic boride includes metal boride, boron oxide, boric acid and its salts, sodium perborate (potassium) and other perborate, metaborate, ice-free tetra / pentaborate, sodium borohydride (Potassium);
  • A3-2 Organic matter includes oils and fats, alicyclic compounds and their derivatives, organic polymers and salts of natural plants and animals, and (oxygen) synthetic resins;
  • A3-3 intermediary reactants include ammonia solution, alcohols, alkali metal alcoholates, aliphatic carboxylic acids and their ester derivatives, non-toxic or slightly less toxic alcohol amines;
  • A3-4 Auxiliaries include: metal organic catalyst / or silicon oxide, boron oxide, alkali metal hydroxide, alkaline earth metal oxide shrinking agent / or silicide powder, carbon powder, semiconductor element ultrafine particles, adsorption resin ion adsorbent / Or pH buffer regulators such as amphoteric metal oxides and amino acids;
  • A3-5 modifiers include metal (hydroxide) oxides, carbonates, silicas, silicates, volatile non-toxic or slightly toxic alcohols and ester solvents, active groups containing metal elements, elemental carbon, and stable metals Powder, natural organic matter and its binder, synthetic resin and its binder, ultraviolet absorber;
  • A3-6 fillers include any inorganic or organic materials that are relatively inexpensive and inert (that is, they do not react directly with boron groups or intermediaries).
  • the inorganic boride can easily form a boron group or a boronoxy group as a main structure or a key structure of an organic boron polymer with a large number of organic molecules in a hydroxy compound solution.
  • the organic substance is a hydroxy compound or a hydroxy derivative (such as an ester)
  • an organic boride having a boron group or a boronoxy group as a core structure and capable of crystal growth can be formed.
  • the crystal formation conditions and growth The condition can be controlled by a variety of additives, such as base, acid and so on.
  • a free solution of hydroxyl small and medium molecules (molecular weight of 2000) containing anhydrous or little free water is used.
  • the free liquid is both the medium and the reactant in the reaction, so as to realize the protective functional structure of the boride and organic matter to form a macromolecule (basic Mission).
  • the present invention adopts a reaction technology circuit that promotes the polymerization of organic substances with a boryloxy / boron group as the center.
  • a copolymerization reaction method and an auxiliary agent that are beneficial to molecular weight increase The present invention is suitable for use.
  • the present invention also considers adding other additives or fillers. '
  • B2 in the reaction synthesis method of the present invention, a substitution / ion exchange reaction, an esterification / ester exchange reaction, a crosslinking reaction, a coupling reaction, a polycondensation reaction and Synthetic method mainly based on copolymerization and supplemented by other reactions such as catalytic reaction.
  • A3-2 determines the reactants in the organic matter of A3-2 and select the corresponding organic intermediary reactants.
  • One or more of the intermediary reactants can be selected in A3-3.
  • A3-2 determines the epoxy resins
  • A3-3 should choose the corresponding alcohol amines
  • H and 0 element ratios of organics should be fully considered in this choice.
  • A3-1 Inorganic boride forms the initial organic boron active group:
  • D, D, and D 2 are the same or different organic macromolecular groups.
  • A3-5 modifiers can be added to the above copolymers to cross-link, homogenize, and so on. This process can be integrated in Structure with marginal protective function formed on the copolymer group
  • [] is any one or two or more block groups in the structural formula (bl)-(b7), and MC is an A3-4 modifier group or the following filler molecular component.
  • A3-3 intermediate reactants choose one or more of A3-3 intermediate reactants to take 50-200 parts by weight, preferably in the range of 20-100 parts by weight;
  • C9-2 A3-1 one or more inorganic borides are taken in an amount of 10-120 parts by weight and blended / melted with the above amount, preferably in a range of 20-100 parts by weight;
  • C9-4 A3-4 additives take one or two parts of 0-50 parts by weight;
  • C9-5 A3-5 modifier takes one to a plurality of 0-100 parts by weight, preferably one or two 5-80 parts by weight;
  • C9-6 A3-6 filler takes one or two total 0-300 parts by weight, less 5-230 parts; C9-7 soaking takes 50 'C-270 V according to the characteristics of the copolymerization reaction, the pressure is the reaction It is advisable that the material does not vaporize.
  • the protective functional material of the present invention can be made with any applicable amount according to the actual protection needs.
  • a catalyst In the preparation of the above-mentioned organic boron polymer having a protective function, a catalyst, a shrinkage promoter, an ion adsorbent, and a pH buffer adjuster may be used to generate the derivative, and the main reaction thereof is a substitution reaction or an ion exchange reaction, and a cross-linking reaction. Coupling reaction, copolymerization reaction and mixing method without chemical change and cross-bonding fusion method.
  • the organic boron polymer having a protective functional structure of the present invention is prepared using the following components: a) 10-120 parts by weight of an inorganic boron polymer; b) 50-200 parts by weight of an intermediate reactant; c) an organic substance 5-200 parts by weight; d) additives 0-150 parts by weight; e) modifiers 0-100 parts by weight; f) fillers 0-300 parts by weight.
  • a boride selected from the group consisting of aluminum boride (zinc / titanium / magnesium), boron oxide, alkali (earth) metal borate, alkali (earth) metal metaboric acid
  • a boride selected from the group consisting of aluminum boride (zinc / titanium / magnesium), boron oxide, alkali (earth) metal borate, alkali (earth) metal metaboric acid
  • intermediate reactants selected from ammonia , Liquid alcohol, sodium (potassium) ethoxide (di),.
  • fatty acids above 2 esters above C 3 and C 2 -C 6 alcohol amines
  • organic matter selected from polymer fats, non-toxic or low-toxic alicyclic compounds And one or two of its derivatives, alginic acid, rosin, gelatin, oxygen-containing synthetic resin and its binder
  • the auxiliary is selected from one of tetrabutyl titanate and aluminum isopropylate 0-S parts by weight, or one of sodium hydroxide, silicon oxide, boron oxide, and calcium oxide, 0-30 parts by weight, or white carbon black, activated white clay, activated carbon powder, silicon ultrafine particles, acrylic resin One is from 0 to 30 parts by weight, or one of alumina powder and aminoacetic acid is from 0 to 30 parts by weight; wherein a + b + c + (d) is used to synthesize a prepolymer product at any ratio specified or re- With or without adding e) 5 to 80 parts by weight
  • the protective functional material of the present invention is suitable for comprehensive protection in multiple fields and multiple uses, and has the following superior performance and good effects than the existing static protective materials:
  • the boron group or boron carbon / boron oxycarbon group in the functional structure has a high temperature anti-oxidation catalytic ability above 700 'C-1500' C. Experiments have shown that this anti-oxidation ability is still apparent under the high heat of 3000 'C-4500' C in the air.
  • the formed water vapor on the one hand loses a large amount of energy, and on the other hand, the (M l) -type inorganic component formed by coking / carbonization absorbs thermal neutrons to prevent the thermonuclear reaction from continuing.
  • the nuclear shielding material in the modifier also has a certain ability to absorb and protect-comprehensively, when the energy of the thermonuclear reaction increases and the neutron proliferation is less than the loss and absorption value, it will be blocked, which can achieve the purpose of nuclear fire protection.
  • the functional structure of the material encounters a high-energy beam impact above 1800 'C-4000' C, such as a laser beam (up to 10,000 degrees to 100 million degrees), the rapid evaporation of structured water forms a few hundred to several tens. Ten thousand atmospheric high-pressure dynamic air cushions caused a sharp decrease in high-energy impact forces in the direction of high-energy transmission gradients.
  • materials such as the carbonized layer of organic matter absorb a small part of the energy transmitted through and vaporize, and form an internal high-pressure layer.
  • the internal high-pressure layer such as - ⁇ -0-C
  • the formation of complex high-temperature resistant materials As a result, the functional protective material has better resistance to high-energy impact than steel, ceramics, and the like. Experiments have shown that this performance is several times to several tens of times higher than that of hard steel in the high heat of oxyhydrogen flames, and the higher the temperature, the better its performance.
  • the organic boron polymer material provided by the present invention with dynamic adaptive protection function has comprehensive advantages that are incomparable with the products of the prior art.
  • US93-5272237 is suitable for making changes between 600'C-1000'C, and the present invention is suitable for making changes above 500'C-2000'C
  • US85-4504611, Ping 7-41611 and Ping 7-278267 are best to achieve V-0 flame retardancy
  • the organic boron polymer material of the present invention is preferably non-flammable above 1000 'C-2000' C--by the method of the present invention
  • the flame retardancy of the material can be self-extinguished within ⁇ 3-5 seconds, while the average of flat 7-4161 1 embodiment is 12.8 seconds.
  • the total components of the present invention do not contain halogen, sulfur, phosphorus, arsenic, heavy metals and radioactive elements that are toxic or pollute the environment.
  • the present invention has good environmental benefits throughout the process.
  • the present invention utilizes adaptive changes in the organic protective function structure in the material to correspond to various changes in the external environment; Allergies change.
  • the former has a limitless protective performance, and the latter has only a certain amount of static indicators and protective performance.
  • the experimental research on the two types of boron polymers shows that (1) the protective material with functional structure provided by the present invention has crystals grown in the main functional structure of dendritic (three-dimensional) and various snowflake-shaped ( Most of the planes), crystalline composite materials with marginal functional structures are mostly skin-like, cream-like, shrinking hilly, and solid and oily without obvious appearance characteristics; (2) Burning quality after 800-1200 'C The loss method determines that the protective material with a functional structure of the present invention contains 50%-80% of the structured water and the combined water according to different reaction conditions, and the combined water and structured water of the present invention for high-temperature protection is generally Less than 36%; (3) The product of the present invention is 200%.
  • 600 'C-750' C is tan for a long time (the performance of boride containing).
  • the layer is flammable, indicating the formation of high-molecular boron carbide;
  • the crystal of the present invention contains a large amount of structured water and crystalline water, and a variety of raw materials containing ionic bond compounds such as borax in each proportion of the material do indeed produce a polymerization reaction-each ionic group
  • the agglomerates together form an integral part of the product of the invention.
  • Aqueous solution reaction adopts temperature controlled conditions of 80 ° C-95 ° C, and organic polymerization reaction adopts reaction method containing alcohol or ester as carrier;
  • B C ⁇ 1 is generally required in boron polymers.
  • B C> 1, the content of structured water and bound water should be ⁇ 50%;
  • reaction residue is used as a filler for the application material.
  • preheat 70-80 'C cast for insulation shirt wall use For energy-saving applications in high-temperature metallurgy, preheat 70-80 'C cast for insulation shirt wall use; b. If used on metal structures, 5-15 parts by weight of epoxy resin and its curing agent can be added; c For applications such as building fire doors, it can be added with 10-30 parts by weight of resin adhesive to make boards or directly attached to metal walls.
  • a metal protective layer such as aluminum profile
  • silicone oil As a metal protective layer (such as aluminum profile), add 5-15 parts by weight of silicone oil and 5-10 parts by weight of epoxy resin or polyurethane adhesive, mechanical coating or manual coating, 80 'C-230 ° C baking dry.
  • a-b can be used for insulation applications above 2000 'C-3000' C and its comprehensive application of high temperature protection in about 5-100 minutes.
  • adding an appropriate amount of aluminum powder, silicon powder, boron powder, or a small amount of activated carbon powder filler is suitable for the requirements of radiation absorption and shielding.
  • Example 1 -3 basic products adding 900 'C-1500' C residues of the present invention burning in the air, that is, a complex solid mixture containing NB and CB (high molecular) as the main component 10-30 parts by weight as a filler, That can be used as ointment-like core shielding filling material.
  • This product is mainly used for high energy impact resistance below 10000 'C and other comprehensive protection. Above 10000 'C, its breakdown resistance is also better than steel. Experiments have shown that oxygen-hydrogen torch cutting at about 3500' C proves that its breakdown resistance is about 20 times that of carbon steel.
  • Example 6 100 parts by weight of the base maturation solution of Example 6 were mixed with 50 parts by weight of magnesium trisilicate using the residual heat, and then 30 parts of ultrafine aluminum silicate was added into the 30-60 ° C residual heat, mixed and ground, and then Compression molding, natural drying for finished products.
  • the hard solid material made of this material has a resistance to 3500 'C hydrogen-oxygen flame torch strikes as in Example 6. About 1.5 times, which is 30 times that of ordinary steel.
  • a method for preparing an alcohol solvent at normal pressure and normal temperature is used to prepare a heat-insulating, fire-retardant and flame-retardant transparent coating of an organosilicon functional structure copolymer.
  • the weight ratio take 35 parts of boron oxide powder and mix in 120 parts of ethanol (content> 96%), and then mix with 50 parts of silicone glass resin and 5-15 parts of non-toxic solid alcohol (such as pentaerythritol cross-linking agent). That is to obtain a transparent fire-resistant coating.
  • 1 to 2 parts of an alkali metal compound such as sodium borate, 1 to 5 parts of an antimony oxide or an alkali metal antimonate flame retardant modifier can also be added. In this case, the fire and flame retardant effect on 5-15mm thick wood boards has reached the national standard B1.
  • an epoxy resin functional copolymer is prepared by esterification, and is mainly used as a fire-resistant and radiation-resistant coating for rubber, plastic, wood, and metal.
  • the weight ratio take 30 parts of boric acid, dissolve in 100 parts of glyceryl ether, and add 30 to 50 parts of glycidyl ester epoxy resin.
  • the coating According to the color requirements of the coating, add an appropriate amount (such as 30-50 parts) of stable metals or metal oxides and carbon substances to the copolymer, such as silver-white aluminum powder, white titanium oxide powder, yellow iron oxide, and black Activated carbon powder and so on.
  • the coating is cured by irradiation or baking during use. The experiment proves that this coating adheres to the protected article with a thickness of 0.1-1mm, which not only has the shielding effect on ⁇ , ⁇ and ⁇ , but also has a good high temperature fire protection effect below 3500 'C.
  • This embodiment is prepared by copolymerization to prepare an epoxy functional structural engineering material, which is used as an adiabatic, fireproof and radiation resistant engineering material.
  • a method for copolymerizing with fiber articles is used to prepare materials that are specially used for immersion in wood, polymer fiber materials, or composite microporous materials to play the role of oxidation resistance, flame retardancy, and radiation protection.
  • the weight ratio take 50 parts of sodium perborate and dissolve in 150 parts of organic acid.
  • it can also be dissolved in a homogeneous solution of 150 parts of isopropanolamine and 30 glycerol. Then, the article is immersed in this solution for infiltration treatment.
  • the processing time is generally measured in hours according to the volume and surface area of the article, and then taken out at 70'C-130'C for about 1-2 hours. This treatment method is suitable for fire and flame retardant applications below 1500 'C.
  • High-molecular multi-functional structural materials or coatings are specially used for long-term thermal insulation and radiation shielding.
  • hydrophobic silica filler or fumed silica in an amount of 10% and 50 parts of the silicone resin to form 100 parts of the semi-finished product with a high temperature resistance copolymer.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)
  • Paints Or Removers (AREA)

Abstract

L'invention concerne une matière polymère borée présentant une structure fonctionnelle auto-adaptative et sa préparation. Ladite matière a un centre boryle ou boroxy constituant la structure principale conjointement avec un groupe actif organique, l'eau de constitution et l'eau combinée représentant 50 à 80 % de la masse totale de ladite matière. Ce groupe actif organique appartient à l'ensemble des groupes hydroxy, aldéhyde, cétone et carboxyle. L'eau combinée précitée est en fait, lors de la production de ladite matière, de l'eau naturelle libre adsorbée et différentes molécules d'eau morphologique d'une matière de charge réactive. Par eau de constitution on entend tous les éléments H et O formant ladite structure fonctionnelle, dont le rapport de dosage est d'environ 2:1. La matière, faisant l'objet de cette invention, peut être utilisée comme isolation thermique haute température, comme anti-oxydant haute température, comme matière ignifuge, comme matière d'absorption de rayonnements, comme matière de protection contre les radiations nucléaires et de protection contre l'impact de faisceaux haute énergie.
PCT/CN1998/000072 1997-05-19 1998-05-14 Matiere polymere contenant du bore presentant une structure fonctionnelle de protection et sa preparation WO1998052993A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU73301/98A AU7330198A (en) 1997-05-19 1998-05-14 Boron-containing polymer material having protective functional structure and itspreparation

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN97112075.7 1997-05-19
CN 97112075 CN1199748A (zh) 1997-05-19 1997-05-19 具有防护功能结构的糖硼聚物及其制备方法和产品用途
CN 97112073 CN1199747A (zh) 1997-05-19 1997-05-19 具有防护功能结构的有机硼聚物及其制备方法和产品用途
CN97112073.0 1997-05-19

Publications (1)

Publication Number Publication Date
WO1998052993A1 true WO1998052993A1 (fr) 1998-11-26

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WO (1) WO1998052993A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7033526B2 (en) 2001-08-24 2006-04-25 National Starch And Chemical Investment Holding Corporation Fire retardant foam and gel compositions
US20150248941A1 (en) * 2011-05-09 2015-09-03 U.S.A. As Represented By The Administrator Of The National Aeronautics And Space Administration Radiation shielding materials containing hydrogen, boron and nitrogen
US11633636B2 (en) 2017-12-02 2023-04-25 Mighty Fire Breaker Llc Wireless neighborhood wildfire defense system network supporting proactive protection of life and property in a neighborhood through GPS-tracking and mapping of environmentally-clean anti-fire (AF) chemical liquid spray applied to the property before wild fires reach the neighborhood
US11826592B2 (en) 2018-01-09 2023-11-28 Mighty Fire Breaker Llc Process of forming strategic chemical-type wildfire breaks on ground surfaces to proactively prevent fire ignition and flame spread, and reduce the production of smoke in the presence of a wild fire
US11865390B2 (en) 2017-12-03 2024-01-09 Mighty Fire Breaker Llc Environmentally-clean water-based fire inhibiting biochemical compositions, and methods of and apparatus for applying the same to protect property against wildfire
US11865394B2 (en) 2017-12-03 2024-01-09 Mighty Fire Breaker Llc Environmentally-clean biodegradable water-based concentrates for producing fire inhibiting and fire extinguishing liquids for fighting class A and class B fires
US11911643B2 (en) 2021-02-04 2024-02-27 Mighty Fire Breaker Llc Environmentally-clean fire inhibiting and extinguishing compositions and products for sorbing flammable liquids while inhibiting ignition and extinguishing fire
US12168152B2 (en) 2021-02-04 2024-12-17 Mighty Fire Breaker Llc Remotely-triggered wildfire defense system for automatically spraying environmentally-clean water-based liquid fire inhibitor to proactively form thin fire-inhibiting alkali metal salt crystalline coatings on sprayed combustible surfaces prior to wildfire

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3891621A (en) * 1972-05-23 1975-06-24 Us Agriculture Carbohydrate-boron alkoxide compounds
US5226481A (en) * 1992-03-04 1993-07-13 Bj Services Company Method for increasing the stability of water-based fracturing fluids
EP0594363A1 (fr) * 1992-10-20 1994-04-27 Halliburton Company Fluide de fracturation réticulé au borate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3891621A (en) * 1972-05-23 1975-06-24 Us Agriculture Carbohydrate-boron alkoxide compounds
US5226481A (en) * 1992-03-04 1993-07-13 Bj Services Company Method for increasing the stability of water-based fracturing fluids
EP0594363A1 (fr) * 1992-10-20 1994-04-27 Halliburton Company Fluide de fracturation réticulé au borate

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US7033526B2 (en) 2001-08-24 2006-04-25 National Starch And Chemical Investment Holding Corporation Fire retardant foam and gel compositions
US20150248941A1 (en) * 2011-05-09 2015-09-03 U.S.A. As Represented By The Administrator Of The National Aeronautics And Space Administration Radiation shielding materials containing hydrogen, boron and nitrogen
US11794044B2 (en) 2017-12-02 2023-10-24 Mighty Fire Breaker Llc Method of proactively forming and maintaining GPS-tracked and mapped environmentally-clean chemical firebreaks and fire protection zones that inhibit fire ignition and flame spread in the presence of wild fire
US11697039B2 (en) 2017-12-02 2023-07-11 Mighty Fire Breaker Llc Wireless communication network, GPS-tracked back-pack spraying systems and command center configured for proactively spraying environmentally-safe anti-fire chemical liquid on property surfaces to inhibit fire ignition and flame spread in the presence of wild fire
US11642555B2 (en) 2017-12-02 2023-05-09 Mighty Fire Breaker Llc Wireless wildfire defense system network for proactively defending homes and neighborhoods against wild fires by spraying environmentally-clean anti-fire chemical liquid on property and buildings and forming GPS-tracked and mapped chemical fire breaks about the property
US11654314B2 (en) 2017-12-02 2023-05-23 Mighty Fire Breaker Llc Method of managing the proactive spraying of environment ally-clean anti-fire chemical liquid on GPS-specified property surfaces so as to inhibit fire ignition and flame spread in the presence of wild fire
US11654313B2 (en) 2017-12-02 2023-05-23 Mighty Fire Breaker Llc Wireless communication network, GPS-tracked ground-based spraying tanker vehicles and command center configured for proactively spraying environmentally-safe anti-fire chemical liquid on property surfaces to inhibit fire ignition and flame spread in the presence of wild fire
US11697040B2 (en) 2017-12-02 2023-07-11 Mighty Fire Breaker Llc Wild fire defense system network using a command center, spraying systems and mobile computing systems configured to proactively defend homes and neighborhoods against threat of wild fire by spraying environmentally-safe anti-fire chemical liquid on property surfaces before presence of wild fire
US11697041B2 (en) 2017-12-02 2023-07-11 Mighty Fire Breaker Llc Method of proactively defending combustible property against fire ignition and flame spread in the presence of wild fire
US12364885B2 (en) 2017-12-02 2025-07-22 Mighty Fire Breaker Llc System for proactively forming and maintaining GPS-tracked and mapped environmentally-clean chemical fire protection zones over the property surfaces of a neighborhood of homes so as to inhibit fire ignition and flame spread in the presence of wild fire
US11707639B2 (en) 2017-12-02 2023-07-25 Mighty Fire Breaker Llc Wireless communication network, GPS-tracked mobile spraying systems, and a command system configured for proactively spraying environmentally-safe anti-fire chemical liquid on combustible property surfaces to protect property against fire ignition and flame spread in the presence of wild fire
US12364886B2 (en) 2017-12-02 2025-07-22 Mighty Fire Breaker Llc Neighborhood of homes provided with a system installed for proactively forming and maintaining environmentally-clean chemical fire protection zones over the property and ground surfaces of the neighborhood
US11638844B2 (en) 2017-12-02 2023-05-02 Mighty Fire Breaker Llc Method of proactively protecting property from wild fire by spraying environmentally-clean anti-fire chemical liquid on property surfaces prior to wild fire arrival using remote sensing and GPS-tracking and mapping enabled spraying
US11633636B2 (en) 2017-12-02 2023-04-25 Mighty Fire Breaker Llc Wireless neighborhood wildfire defense system network supporting proactive protection of life and property in a neighborhood through GPS-tracking and mapping of environmentally-clean anti-fire (AF) chemical liquid spray applied to the property before wild fires reach the neighborhood
US11730987B2 (en) 2017-12-02 2023-08-22 Mighty Fire Breaker Llc GPS tracking and mapping wildfire defense system network for proactively defending homes and neighborhoods against threat of wild fire by spraying environmentally-safe anti-fire chemical liquid on property surfaces to inhibit fire ignition and flame spread in the presence of wild fire
US11865394B2 (en) 2017-12-03 2024-01-09 Mighty Fire Breaker Llc Environmentally-clean biodegradable water-based concentrates for producing fire inhibiting and fire extinguishing liquids for fighting class A and class B fires
US11865390B2 (en) 2017-12-03 2024-01-09 Mighty Fire Breaker Llc Environmentally-clean water-based fire inhibiting biochemical compositions, and methods of and apparatus for applying the same to protect property against wildfire
US11826592B2 (en) 2018-01-09 2023-11-28 Mighty Fire Breaker Llc Process of forming strategic chemical-type wildfire breaks on ground surfaces to proactively prevent fire ignition and flame spread, and reduce the production of smoke in the presence of a wild fire
US12251587B2 (en) 2018-01-09 2025-03-18 Mighty Fire Breaker Llc Ground-based vehicle for making and applying a fire and smoke inhibiting slurry composition on ground surfaces before the arrival of wildfire
US12208296B2 (en) 2021-02-04 2025-01-28 Mighty Fire Breaker Llc Wildfire defense spraying process for automatically spraying environmentally-clean water-based liquid fire inhibitor over combustible property surfaces to form thin fire-inhibiting potassium salt crystalline coatings thereon before presence of wildfire
US12214233B2 (en) 2021-02-04 2025-02-04 Mighty Fire Breaker Llc Wildfire defense spraying system for spraying environmentally-clean water-based liquid fire inhibitor to proactively form thin fire-inhibiting potassium salt crystalline coatings on sprayed property surfaces prior to the presence of wildfire
US12226661B2 (en) 2021-02-04 2025-02-18 Might Fire Breaker Llc Wildfire defense spraying system for spraying environmentally-clean water-based liquid fire inhibitor to proactively form thin fire-inhibiting alkali metal salt crystalline coatings on sprayed property surfaces prior to the presence of wildfire
US12168152B2 (en) 2021-02-04 2024-12-17 Mighty Fire Breaker Llc Remotely-triggered wildfire defense system for automatically spraying environmentally-clean water-based liquid fire inhibitor to proactively form thin fire-inhibiting alkali metal salt crystalline coatings on sprayed combustible surfaces prior to wildfire
US11911643B2 (en) 2021-02-04 2024-02-27 Mighty Fire Breaker Llc Environmentally-clean fire inhibiting and extinguishing compositions and products for sorbing flammable liquids while inhibiting ignition and extinguishing fire

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