CN106120346A - A kind of preparation method of polyester-imides modified amino silicon oil fabric softeners - Google Patents
A kind of preparation method of polyester-imides modified amino silicon oil fabric softeners Download PDFInfo
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- CN106120346A CN106120346A CN201610553248.XA CN201610553248A CN106120346A CN 106120346 A CN106120346 A CN 106120346A CN 201610553248 A CN201610553248 A CN 201610553248A CN 106120346 A CN106120346 A CN 106120346A
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- polyester
- imides
- silicon oil
- performed polymer
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- 239000003921 oil Substances 0.000 title claims abstract description 112
- 229920003055 poly(ester-imide) Polymers 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002979 fabric softener Substances 0.000 title claims abstract description 19
- OBFQBDOLCADBTP-UHFFFAOYSA-N aminosilicon Chemical class [Si]N OBFQBDOLCADBTP-UHFFFAOYSA-N 0.000 title claims abstract description 13
- -1 amido silicon Chemical compound 0.000 claims abstract description 49
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 46
- 239000010703 silicon Substances 0.000 claims abstract description 46
- 229920000642 polymer Polymers 0.000 claims abstract description 42
- 229920001577 copolymer Polymers 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 102000004190 Enzymes Human genes 0.000 claims abstract description 14
- 108090000790 Enzymes Proteins 0.000 claims abstract description 14
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229910021529 ammonia Inorganic materials 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000004952 Polyamide Substances 0.000 claims description 9
- 229920002647 polyamide Polymers 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 239000004367 Lipase Substances 0.000 claims description 7
- 102000004882 Lipase Human genes 0.000 claims description 7
- 108090001060 Lipase Proteins 0.000 claims description 7
- 108091005804 Peptidases Proteins 0.000 claims description 7
- 239000004365 Protease Substances 0.000 claims description 7
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 7
- 235000019421 lipase Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000004744 fabric Substances 0.000 abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 19
- 239000008367 deionised water Substances 0.000 abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 abstract description 13
- 239000004902 Softening Agent Substances 0.000 abstract description 10
- 238000004383 yellowing Methods 0.000 abstract description 7
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000001804 emulsifying effect Effects 0.000 abstract description 4
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 abstract description 4
- 150000001412 amines Chemical class 0.000 abstract description 3
- 235000009392 Vitis Nutrition 0.000 abstract description 2
- 241000219095 Vitis Species 0.000 abstract description 2
- 125000000217 alkyl group Chemical group 0.000 abstract description 2
- 150000002170 ethers Chemical class 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000835 fiber Substances 0.000 description 8
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 210000002268 wool Anatomy 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 125000003368 amide group Chemical group 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 150000002466 imines Chemical class 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- LDDMACCNBZAMSG-BDVNFPICSA-N (2r,3r,4s,5r)-3,4,5,6-tetrahydroxy-2-(methylamino)hexanal Chemical compound CN[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO LDDMACCNBZAMSG-BDVNFPICSA-N 0.000 description 1
- 206010016322 Feeling abnormal Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229920013822 aminosilicone Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- ZHDTXTDHBRADLM-UHFFFAOYSA-N hydron;2,3,4,5-tetrahydropyridin-6-amine;chloride Chemical compound Cl.NC1=NCCCC1 ZHDTXTDHBRADLM-UHFFFAOYSA-N 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 108010062085 ligninase Proteins 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/452—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing sequences
- C08G77/455—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing sequences containing polyamide, polyesteramide or polyimide sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to the preparation method of a kind of polyester-imides modified amino silicon oil fabric softeners, belong to softening agent preparing technical field.The present invention is first with octamethylcy-clotetrasiloxane as body, carry out polymerisation in bulk and obtain amido silicon oil performed polymer, then 4 are used, 4 diaminodiphenyl ethers and pyromellitic acid anhydride carry out reaction and obtain polyamic acid, generation polyester-imides performed polymer is reacted again by alkyl Fructus Vitis viniferae amine and polyamic acid, then amido silicon oil performed polymer and polyester-imides prepolymer reaction are obtained polyester-imides amido silicon oil copolymer, the enzyme of various function is added again in copolymer, optimize the performance of copolymer, it is eventually adding deionized water and carries out emulsifying, obtain a kind of polyester-imides modified amino silicon oil fabric softeners.Fabric softener prepared by the present invention can make fabric sofetening, and pliability improves 17～19%, and guarantees not have yellowing phenomenon on fabric.
Description
Technical field
The present invention relates to the preparation method of a kind of polyester-imides modified amino silicon oil fabric softeners, belong to softening agent system
Standby technical field.
Background technology
Fabric softener can make fabric have the medicament of soft feeling after drying in washing.Mainly there are three classes, i.e. on-surface-active
Agent, surfactant and surfactant and the mixture of non-surface-active agent.One type and three classes such as silicone oil, mineral
Oil, fatty alcohol, fatty acid, fatty amine, neutral fat etc., because being insoluble in water, must be dissolved in during use in other solvents, the most not
With.Use at present is the most surfactant-based such as softening agent EST, softening agent i--IC', softening agent M5-20, softening agent PEN
Deng.
Polydimethylsiloxane is the fabric softener that a kind of performance is the most superior, due to its good molecular flexibility and
Abundant methyl content, so that form methyl cover layer at fiber surface, thus the sound friction reduced between fiber is
Number, reaches good soft effect.But owing to it is the most firm and fiber forms adhesion, simply by a limited number of models
De Huali and hydrogen bond are combined with fiber, simultaneously as intramolecular does not has crosslinkable group so cannot be individually at fiber surface
Film forming, fastness is poor.And with amido silicon oil as representative, due to the existence of amino, under mildly acidic conditions, amino can be with cation
Changing, produce and can form the most firmly being bonded of being combined of electrostatic attraction by negative charge group on fiber, fastness is better than ordinary silicon
Oil, and due to the effect of this electrostatic attraction so that have the more methyl can be outside, so series products has super softness
Effect, is the organosilicon product that softness is best in the market.But amino silicone also has its shortcoming, due in amino
Nitrogen-atoms cloud density is higher, so easy and absorbing light electronics generation photochemical reaction, thus it is existing to produce so-called xanthochromia
As, and amido silicon oil is also difficult to emulsifying, the shortcoming that easy breakdown of emulsion forms the hydrophilic differences such as oil mark on fabric.
Summary of the invention
The technical problem to be solved: for poor using amido silicon oil as hydrophilic during fabric softener, Yi Fan
Huang, amido silicon oil is difficult to emulsifying, easy breakdown of emulsion, and forms the shortcomings such as oil mark on fabric, it is provided that with prestox ring four silica
Alkane is body, carries out polymerisation in bulk and obtains amido silicon oil performed polymer, then uses 4,4-diaminodiphenyl ether and Pyromellitic Acid
Dianhydride carries out reaction and obtains polyamic acid, then reacts generation polyester-imides performed polymer by alkyl Fructus Vitis viniferae amine and polyamic acid,
Then amido silicon oil performed polymer and polyester-imides prepolymer reaction are obtained polyester-imides amido silicon oil copolymer, then to altogether
Polymers adds the enzyme of various function, optimizes the performance of copolymer, be eventually adding deionized water and carry out emulsifying, obtain a kind of polyamides
The method of the ester modified amino silicon oil fabric softeners of imines, the present invention introduces imide in amido silicon oil and hands over as physics
The hard segment of connection, has been simultaneously introduced N-methyl-D-glucosamine as hydrophilic segment, has solved amino-silicone oil softening agent and be easily generated Huang
Cash as, easy breakdown of emulsion forms the problem of oil mark on fabric, improve the softness of fabric, and the mold protease added has
Being beneficial to the loose of fabric fibre, the pliability of reinforced fabric and richness, lipase can decompose the oils and fats on fabric fibre, make
Oils and fats is dissolved in water, and ligninase can suppress Yellowing to produce, and has discoloration.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) weigh 10～20g octamethylcy-clotetrasiloxanes and join in 100mL there-necked flask, flask is placed in oil bath, to burning
After being passed through nitrogen 10～20min with 1～2L/min flow velocity in Ping, controlling oil bath temperature is 80～90 DEG C, then adds 1 in beaker
～3mL mass concentration is 10% tetramethoxy Ammonia, isothermal reaction 2～3h, obtain amido silicon oil performed polymer, standby；
(2) measuring 40～50mL4,4-diaminodiphenyl ether joins in 250mL there-necked flask, is placed in oil bath by flask, to
Being passed through nitrogen 10～20min with 1～2L/min flow velocity in flask, controlling oil bath temperature is 80～90 DEG C, adds successively in flask
Entering 40～50mL pyromellitic acid anhydrides, 1～3mL mass concentration is 10% tetramethoxy Ammonia, isothermal reaction 3～
4h, obtains polyamic acid performed polymer；
(3) in above-mentioned polyamide acid performed polymer, it is sequentially added into 3～5gN-methyl-D-glucosamine, 5～10mL0.1mol/L salt
Acid, controlling oil bath temperature is 65～75 DEG C, stirring reaction 3～4h, adds 0.1mol/L sodium hydroxide solution and adjust in reactant liquor
Joint pH to 7.0～7.2, obtains polyester-imides performed polymer；
(4) the polyester-imides performed polymer of above-mentioned preparation is joined in 250mL there-necked flask, then by ammonia standby for step (1)
Base silicone oil performed polymer adds in flask, carries out oil bath heating, and controlling oil bath temperature is 85～95 DEG C, stirring reaction 8～10h,
To polyester-imides amido silicon oil copolymer；
(5) in above-mentioned polyester-imides amido silicon oil copolymer, it is sequentially added into 0.1～0.3g mold protease, 0.1～0.3g
Lipase, 0.1～0.3g lignoenzyme, stirring mixing 20～30min, obtain the polyester-imides amido silicon oil containing multiple enzyme
Copolymer, then in the polyester-imides amido silicon oil copolymer containing multiple enzyme, add 300～400mL deionized waters, stir 2
～3h, obtain a kind of polyester-imides modified amino silicon oil fabric softeners.
The application process of the present invention: after superfine wool fabric is cleaned 2～3 times with deionized water, be placed in beaker, and to
Adding in deionized water in beaker, not have fabric 2～3cm to be advisable, and to control water temperature be 40～45 DEG C, then adds in beaker
Fabric quality 30～the polyester-imides modified amino silicon oil fabric softeners of 40% above-mentioned preparation, by magnetic stirrer 20
～after 30min, take out fabric, dehydration, being placed in temperature is to dry in 80～85 DEG C of baking ovens, can become finished product.After testing, this one-tenth
Product are soft, smooth, and do not have yellowing and oil spot phenomenon.
The present invention is compared with additive method, and Advantageous Effects is:
(1) fabric softener prepared by the present invention can make fabric sofetening, and pliability improves 17～19%, and guarantees on fabric not
There will be yellowing phenomenon；
(2) preparation process of the present invention is simple, required low cost.
Detailed description of the invention
First weigh 10～20g octamethylcy-clotetrasiloxanes to join in 100mL there-necked flask, flask is placed in oil bath
In, after being passed through nitrogen 10～20min with 1～2L/min flow velocity in flask, controlling oil bath temperature is 80～90 DEG C, then to beaker
Middle addition 1～3mL mass concentration is 10% tetramethoxy Ammonia, and isothermal reaction 2～3h obtains amido silicon oil pre-polymerization
Body, standby；Measuring 40～50mL4 again, 4-diaminodiphenyl ether joins in 250mL there-necked flask, is placed in oil bath by flask,
Being passed through nitrogen 10～20min with 1～2L/min flow velocity in flask, controlling oil bath temperature is 80～90 DEG C, in flask successively
Adding 40～50mL pyromellitic acid anhydrides, 1～3mL mass concentration is 10% tetramethoxy Ammonia, isothermal reaction 3
～4h, obtain polyamic acid performed polymer；Then in above-mentioned polyamide acid performed polymer, it is sequentially added into 3～5gN-methyl D-glucose
Amine, 5～10mL0.1mol/L hydrochloric acid, controlling oil bath temperature is 65～75 DEG C, stirring reaction 3～4h, adds in reactant liquor
0.1mol/L sodium hydroxide solution regulation pH to 7.0～7.2, obtains polyester-imides performed polymer；Again by the polyamides of above-mentioned preparation
Imines ester performed polymer joins in 250mL there-necked flask, then is added in flask by the amido silicon oil performed polymer of preparation, carries out oil bath
Heating, controlling oil bath temperature is 85～95 DEG C, stirring reaction 8～10h, obtains polyester-imides amido silicon oil copolymer；Finally
Be sequentially added in above-mentioned polyester-imides amido silicon oil copolymer 0.1～0.3g mold protease, 0.1～0.3g lipase,
0.1～0.3g lignoenzyme, stirring mixing 20～30min, obtain the polyester-imides amido silicon oil copolymer containing multiple enzyme,
In the polyester-imides amido silicon oil copolymer containing multiple enzyme, add 300～400mL deionized waters again, stir 2～3h,
To a kind of polyester-imides modified amino silicon oil fabric softeners.
Example 1
First weigh 20g octamethylcy-clotetrasiloxane and join in 100mL there-necked flask, flask is placed in oil bath, to flask
In be passed through nitrogen 20min with 2L/min flow velocity after, control oil bath temperature be 90 DEG C, then in beaker add 3mL mass concentration be
10% tetramethoxy Ammonia, isothermal reaction 3h, obtain amido silicon oil performed polymer, standby；Measure 50mL4,4-diamino again
Yl diphenyl ether joins in 250mL there-necked flask, is placed in oil bath by flask, is passed through nitrogen with 2L/min flow velocity in flask
20min, controlling oil bath temperature is 90 DEG C, is sequentially added into 50mL pyromellitic acid anhydride, 3mL mass concentration is 10% in flask
Tetramethoxy Ammonia, isothermal reaction 4h, obtain polyamic acid performed polymer；Then in above-mentioned polyamide acid performed polymer
Being sequentially added into 5gN-methyl-D-glucosamine, 10mL0.1mol/L hydrochloric acid, controlling oil bath temperature is 75 DEG C, and stirring reaction 4h, to instead
Answer and liquid adds 0.1mol/L sodium hydroxide solution regulation pH to 7.2, obtain polyester-imides performed polymer；Again by above-mentioned preparation
Polyester-imides performed polymer joins in 250mL there-necked flask, then is added in flask by the amido silicon oil performed polymer of preparation, carries out
Oil bath is heated, and controlling oil bath temperature is 95 DEG C, stirring reaction 10h, obtains polyester-imides amido silicon oil copolymer；The most upwards
State and polyester-imides amido silicon oil copolymer is sequentially added into 0.3g mold protease, 0.3g lipase, 0.3g lignoenzyme, stir
Mix mixing 30min, obtain the polyester-imides amido silicon oil copolymer containing multiple enzyme, then to the polyimides containing multiple enzyme
Ester amido silicon oil copolymer adds 400mL deionized water, stirs 3h, obtain a kind of polyester-imides modified amino silicon oil fabric
Softening agent.
After superfine wool fabric is cleaned 3 times with deionized water, it is placed in beaker, and in beaker, adds deionized water
In, not have fabric 3cm to be advisable, and to control water temperature be 45 DEG C, then adds the poly-of the above-mentioned preparation of fabric quality 30% in beaker
Imide ester modified amino silicon oil fabric softeners, after magnetic stirrer 30min, takes out fabric, dehydration, is placed in temperature
Degree is to dry in 85 DEG C of baking ovens, can finished product.After testing, this finished product is soft, smooth, and does not haves yellowing and oil mark is existing
As.
Example 2
First weigh 10g octamethylcy-clotetrasiloxane and join in 100mL there-necked flask, flask is placed in oil bath, to flask
In be passed through nitrogen 10min with 1L/min flow velocity after, control oil bath temperature be 80 DEG C, then in beaker add 1mL mass concentration be
10% tetramethoxy Ammonia, isothermal reaction 2h, obtain amido silicon oil performed polymer, standby；Measure 40mL4,4-diamino again
Yl diphenyl ether joins in 250mL there-necked flask, is placed in oil bath by flask, is passed through nitrogen with 1L/min flow velocity in flask
10min, controlling oil bath temperature is 80 DEG C, is sequentially added into 40mL pyromellitic acid anhydride, 1mL mass concentration is 10% in flask
Tetramethoxy Ammonia, isothermal reaction 3h, obtain polyamic acid performed polymer；Then in above-mentioned polyamide acid performed polymer
Being sequentially added into 3gN-methyl-D-glucosamine, 5mL0.1mol/L hydrochloric acid, controlling oil bath temperature is 65 DEG C, and stirring reaction 3h, to instead
Answer and liquid adds 0.1mol/L sodium hydroxide solution regulation pH to 7.0, obtain polyester-imides performed polymer；Again by above-mentioned preparation
Polyester-imides performed polymer joins in 250mL there-necked flask, then is added in flask by the amido silicon oil performed polymer of preparation, carries out
Oil bath is heated, and controlling oil bath temperature is 85 DEG C, stirring reaction 8h, obtains polyester-imides amido silicon oil copolymer；The most upwards
State and polyester-imides amido silicon oil copolymer is sequentially added into 0.1g mold protease, 0.1g lipase, 0.1g lignoenzyme, stir
Mix mixing 20min, obtain the polyester-imides amido silicon oil copolymer containing multiple enzyme, then to the polyimides containing multiple enzyme
Ester amido silicon oil copolymer adds 300mL deionized water, stirs 2h, obtain a kind of polyester-imides modified amino silicon oil fabric
Softening agent.
After superfine wool fabric is cleaned 2 times with deionized water, it is placed in beaker, and in beaker, adds deionized water
In, not have fabric 2m to be advisable, and to control water temperature be 40 DEG C, then adds the polyamides of the above-mentioned preparation of fabric quality 40% in beaker
The ester modified amino silicon oil fabric softeners of imines, after magnetic stirrer 20min, takes out fabric, dehydration, is placed in temperature
It is that 80 DEG C of baking ovens are dried, can finished product.After testing, this finished product is soft, smooth, and does not haves yellowing and oil mark is existing
As.
Example 3
First weigh 15g octamethylcy-clotetrasiloxane and join in 100mL there-necked flask, flask is placed in oil bath, to flask
In be passed through nitrogen 15min with 1L/min flow velocity after, control oil bath temperature be 85 DEG C, then in beaker add 2mL mass concentration be
10% tetramethoxy Ammonia, isothermal reaction 3h, obtain amido silicon oil performed polymer, standby；Measure 45mL4,4-diamino again
Yl diphenyl ether joins in 250mL there-necked flask, is placed in oil bath by flask, is passed through nitrogen with 1L/min flow velocity in flask
15min, controlling oil bath temperature is 85 DEG C, is sequentially added into 47mL pyromellitic acid anhydride, 2mL mass concentration is 10% in flask
Tetramethoxy Ammonia, isothermal reaction 3h, obtain polyamic acid performed polymer；Then in above-mentioned polyamide acid performed polymer
Being sequentially added into 4gN-methyl-D-glucosamine, 7mL0.1mol/L hydrochloric acid, controlling oil bath temperature is 70 DEG C, and stirring reaction 3h, to instead
Answer and liquid adds 0.1mol/L sodium hydroxide solution regulation pH to 7.1, obtain polyester-imides performed polymer；Again by above-mentioned preparation
Polyester-imides performed polymer joins in 250mL there-necked flask, then is added in flask by the amido silicon oil performed polymer of preparation, carries out
Oil bath is heated, and controlling oil bath temperature is 90 DEG C, stirring reaction 7h, obtains polyester-imides amido silicon oil copolymer；The most upwards
State and polyester-imides amido silicon oil copolymer is sequentially added into 0.2g mold protease, 0.2g lipase, 0.1g lignoenzyme, stir
Mix mixing 25min, obtain the polyester-imides amido silicon oil copolymer containing multiple enzyme, then to the polyimides containing multiple enzyme
Ester amido silicon oil copolymer adds 350mL deionized water, stirs 3h, obtain a kind of polyester-imides modified amino silicon oil fabric
Softening agent.
After superfine wool fabric is cleaned 3 times with deionized water, it is placed in beaker, and in beaker, adds deionized water
In, not have fabric 2cm to be advisable, and to control water temperature be 42 DEG C, then adds the poly-of the above-mentioned preparation of fabric quality 35% in beaker
Imide ester modified amino silicon oil fabric softeners, after magnetic stirrer 25min, takes out fabric, dehydration, is placed in temperature
Degree is to dry in 82 DEG C of baking ovens, can finished product.After testing, this finished product is soft, smooth, and does not haves yellowing and oil mark is existing
As.
Claims (1)
1. the preparation method of a polyester-imides modified amino silicon oil fabric softeners, it is characterised in that concrete preparation process
For:
(1) weigh 10～20g octamethylcy-clotetrasiloxanes and join in 100mL there-necked flask, flask is placed in oil bath, to burning
After being passed through nitrogen 10～20min with 1～2L/min flow velocity in Ping, controlling oil bath temperature is 80～90 DEG C, then adds 1 in beaker
～3mL mass concentration is 10% tetramethoxy Ammonia, isothermal reaction 2～3h, obtain amido silicon oil performed polymer, standby；
(2) measuring 40～50mL4,4-diaminodiphenyl ether joins in 250mL there-necked flask, is placed in oil bath by flask, to
Being passed through nitrogen 10～20min with 1～2L/min flow velocity in flask, controlling oil bath temperature is 80～90 DEG C, adds successively in flask
Entering 40～50mL pyromellitic acid anhydrides, 1～3mL mass concentration is 10% tetramethoxy Ammonia, isothermal reaction 3～
4h, obtains polyamic acid performed polymer；
(3) in above-mentioned polyamide acid performed polymer, it is sequentially added into 3～5gN-methyl-D-glucosamine, 5～10mL0.1mol/L salt
Acid, controlling oil bath temperature is 65～75 DEG C, stirring reaction 3～4h, adds 0.1mol/L sodium hydroxide solution and adjust in reactant liquor
Joint pH to 7.0～7.2, obtains polyester-imides performed polymer；
(4) the polyester-imides performed polymer of above-mentioned preparation is joined in 250mL there-necked flask, then by ammonia standby for step (1)
Base silicone oil performed polymer adds in flask, carries out oil bath heating, and controlling oil bath temperature is 85～95 DEG C, stirring reaction 8～10h,
To polyester-imides amido silicon oil copolymer；
(5) in above-mentioned polyester-imides amido silicon oil copolymer, it is sequentially added into 0.1～0.3g mold protease, 0.1～0.3g
Lipase, 0.1～0.3g lignoenzyme, stirring mixing 20～30min, obtain the polyester-imides amido silicon oil containing multiple enzyme
Copolymer, then in the polyester-imides amido silicon oil copolymer containing multiple enzyme, add 300～400mL deionized waters, stir 2
～3h, obtain a kind of polyester-imides modified amino silicon oil fabric softeners.
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Citations (2)
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| CN101446039A (en) * | 2008-12-26 | 2009-06-03 | 东莞市嘉宏纺织助剂有限公司 | Fiber dyeing deepening agent |
| US7713891B1 (en) * | 2007-06-19 | 2010-05-11 | Milliken & Company | Flame resistant fabrics and process for making |
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| US7713891B1 (en) * | 2007-06-19 | 2010-05-11 | Milliken & Company | Flame resistant fabrics and process for making |
| CN101446039A (en) * | 2008-12-26 | 2009-06-03 | 东莞市嘉宏纺织助剂有限公司 | Fiber dyeing deepening agent |
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