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CN101921372B - Preparation method of cosolvent by compounding concrete admixture - Google Patents

Preparation method of cosolvent by compounding concrete admixture Download PDF

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Publication number
CN101921372B
CN101921372B CN2010102598948A CN201010259894A CN101921372B CN 101921372 B CN101921372 B CN 101921372B CN 2010102598948 A CN2010102598948 A CN 2010102598948A CN 201010259894 A CN201010259894 A CN 201010259894A CN 101921372 B CN101921372 B CN 101921372B
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China
Prior art keywords
kinds
reaction
cosolvent
water
preparation
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Expired - Fee Related
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CN2010102598948A
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Chinese (zh)
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CN101921372A (en
Inventor
陈国忠
陈炜
徐大勇
彭振华
宋树贵
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Jiangsu TMS Concrete Admixture Co Ltd
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Jiangsu TMS Concrete Admixture Co Ltd
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Abstract

The invention discloses a preparation method of a cosolvent by compounding a concrete admixture, comprising the following steps of: (1) esterification reaction: mixing methyl-terminated polyethylene glycol containing 5-20 percent of cyclopropane in the mol ratio with methacrylic acid or acrylic acid with the mol ratio of 1:(2.5-10) and reacting at the temperature of 105-125DEG C for 3-6 hours; (2) polymerization reaction: adding water in the prepared carboxylate for diluting, adding an initiator the addition quantity of which is 2-13 percent of the mass of total reactants and reacting at the temperature of 70-90DEG C for 2.5-6 hours; (3) neutralization reaction: adding alkali in the substances and adjusting the pH value to be 5-7 to obtain a high polymer cosolvent; and (4) adding the neutralized water-soluble high polymer cosolvent in a polycarboxylic acid superplastic agent. After the cosolvent is added according a certain proportion, the solution is not demixed; and the preparation process is simpler and the reaction conditions are easy to control.

Description

The preparation method who is used for the solubility promoter of compounding concrete admixture
Technical field
The present invention relates to a kind of preparation method of cement water reducing agent, particularly added the method for the not stratified efficient cement water reducing agent of the composite preparation of poly carboxylic acid parent of use different molecular structures of solubility promoter.
Background technology
At present, polycarboxylic acid polymer has obtained promoting and widespread use as efficient cement water reducing agent; Because the needs of function have had a mind to adjust the oxyethane in the side chain and the ratio of propylene oxide in the poly carboxylic acid molecular structure, perhaps since with a kind of molecular structure owing to the difference of the polymerization degree; Two kinds or two or more such water-soluble polymer solutions are after mixing is composite, when concentration reaches certain value; System can be divided into two immiscible phases by nature; Two all contain moisture mutually, constitute double-aqueous phase system, cause the unsettled defective of product.The present invention selects a kind of tensio-active agent according to the poly carboxylic acid of different HLB values, and the solution system is divided into immiscible biphase problem naturally.
Summary of the invention
The composite admixture of concrete provides compounding polycarboxylic acid with different molecular structures and does not produce stratified method in the object of the invention solution actual production.
The present invention is used for the preparation method of the solubility promoter of compounding concrete admixture, and the solution system is divided into immiscible biphase problem naturally, carries out according to the following step:
(1) esterification: will contain with the molar ratio computing is the terminal methyl polyoxyethylene glycol of 5%-20% Trimetylene; Wherein the molecular weight of terminal methyl polyoxyethylene glycol is 300-6000; With mol ratio is 1: methylacrylic acid or the vinylformic acid of 2.5-10 mix; Under nitrogen protection and catalyzer, reaction is 3-6 hour under 105-125 ℃ temperature; Wherein said catalyzer is sodium pyrosulfate, toluene sulfonic acide or the vitriol oil, perhaps the mixture of two of above-mentioned arbitrary proportion kinds or three kinds;
(2) polyreaction: with the carboxylate of above-mentioned preparation; Add the entry dilution, making its concentration is 30-50%, and adding total reactant is the initiator of 2-13% in mass; Reaction is 2.5-6 hour under 70-90 ℃ temperature; Initiated polymerization becomes water-soluble high-molecular substance, and wherein said initiator is Potassium Persulphate, ammonium persulphate, ydrogen peroxide 50 or Sodium Persulfate, perhaps the mixture of any two kinds or three kinds of above-mentioned substance or four kinds;
(3) neutralization reaction: in above-mentioned substance, add alkali, adjustment pH value promptly obtains the polymeric retention aid solvent at 5-7; Wherein said alkali is sodium hydroxide, Pottasium Hydroxide, calcium hydroxide or yellow soda ash, or their any two kinds and two or more mixtures;
(4) the water-soluble polymer solubility promoter after the above-mentioned neutralization of adding in polycarboxylate water-reducer, the ratio of adding is the 2-20% of solid mass ratio.
Advantage of the present invention: the characteristics of the solubility promoter of method for preparing in the water reducer aqua after ethers and lipid are composite, add a certain proportion of solubility promoter; Solution is not stratified, and, this high molecular polymer solubility promoter and parent; In concrete uses, has same performance; The preparation process is fairly simple, and reaction conditions is easy to control.
Further set forth the present invention through instance below, but be not limited to the present invention.
Embodiment
Embodiment one:
It is 1500 terminal methyl Liquid Macrogol gram, vinylformic acid 65 grams that reaction flask adds the molecular weight contain 3% propylene oxide (mol ratio); Add 20 milliliters of benzene; Fed nitrogen 20 minutes; Under nitrogen protection, add composite catalyst (wherein composite catalyst is that p-methyl benzenesulfonic acid and sodium pyrosulfate mass ratio are 1: 1 mixture) 20g, 115-120 ℃ of reaction 6 hours.Add dilution water, be added dropwise in 90 ℃ the water 3 hours time simultaneously with the ammonium persulfate aqueous solution.Dropping finishes, and is warming up to 95 ℃ of reactions 1 hour, is cooled to 50 ℃, adds liquid caustic soda, and the adjustment pH value is 5-7.Obtain solid content and be 23% water-soluble polymer solubility promoter.
Double-aqueous phase system: lipid polycarboxylate water-reducer 20 grams, ethers poly carboxylic acid 20 grams, polynary carbohydrate 2 grams, water 58 grams.
The system solution that does not add solubility promoter after 24 hours, obvious layering occurs.
Add the solution of 3 gram solubility promoters, do not have the generation of demixing phenomenon.
Embodiment two:
Reaction flask adds and to contain 10% propylene oxide (mol ratio), molecular weight is 600 terminal methyl Liquid Macrogol gram, TEB 3K 200 grams; Fed nitrogen 20 minutes; Under nitrogen protection; Add composite catalyst (wherein composite catalyst is that p-methyl benzenesulfonic acid and sulfuric acid mass ratio are 1: 1 mixture) 20g, 110 ℃ of fractionator reactions 6 hours.Add dilution water and a certain proportion of ferrous sulfate, dripped ydrogen peroxide 50 5 hours down at 75-80 ℃.Dropwise, be warming up to 85 ℃ of reactions 1 hour, be cooled to 50 ℃, add liquid caustic soda, the adjustment pH value is 5-7.Obtain solid content and be 45% water-soluble polymer solubility promoter.
Double-aqueous phase system: lipid polycarboxylate water-reducer 40 grams, ethers poly carboxylic acid 40 grams, polynary carbohydrate 3 grams, water 17.
The system solution that does not add solubility promoter after 24 hours, obvious layering occurs.
Add the solution of 2 gram solubility promoters, do not have the generation of demixing phenomenon.
Embodiment three:
Reaction flask adds and to contain 4% propylene oxide (mol ratio), molecular weight is 800 terminal methyl Liquid Macrogol gram, methylacrylic acid 140 grams; Fed nitrogen 20 minutes; Under nitrogen protection; Add composite catalyst (wherein composite catalyst is that sodium pyrosulfate and sulfuric acid mass ratio are 1: 1 mixture) 20g, 120-125 ℃ of reaction 6 hours.Add dilution water and a certain proportion of Thiovanic acid, dripped sodium persulfate aqueous solution 3 hours down at 75-80 ℃.Sodium persulfate aqueous solution finishes, and is warming up to 85 ℃ of reactions 1 hour, is cooled to 50 ℃, adds liquid caustic soda, and the adjustment pH value is 5-7.Obtain solid content and be 40% water-soluble polymer solubility promoter.
Double-aqueous phase system: lipid polycarboxylate water-reducer 25 grams, ethers poly carboxylic acid 15 grams, polynary carbohydrate 3 grams, water 57.
The system solution that does not add solubility promoter after 24 hours, obvious layering occurs.
Add the solution of 8 gram solubility promoters, do not have the generation of demixing phenomenon.

Claims (1)

1. the preparation method who is used for the solubility promoter of compounding concrete admixture is characterized in that carrying out according to the following step:
(1) esterification: will contain with the molar ratio computing is the terminal methyl polyoxyethylene glycol of 5%-20% propylene oxide; Wherein the molecular weight of terminal methyl polyoxyethylene glycol is 300-6000; With mol ratio is 1: methylacrylic acid or the vinylformic acid of 2.5-10 mix; Under nitrogen protection and catalyzer, reaction is 3-6 hour under 105-125 ℃ temperature; Wherein said catalyzer is sodium pyrosulfate, toluene sulfonic acide or the vitriol oil, perhaps the mixture of two of above-mentioned arbitrary proportion kinds or three kinds;
(2) polyreaction: with the carboxylate of above-mentioned preparation; Add the entry dilution, making its concentration is 30-50%, and adding total reactant is the initiator of 2-13% in mass; Reaction is 2.5-6 hour under 70-90 ℃ temperature; Initiated polymerization becomes water-soluble high-molecular substance, and wherein said initiator is Potassium Persulphate, ammonium persulphate, ydrogen peroxide 50 or Sodium Persulfate, perhaps the mixture of any two kinds or three kinds of above-mentioned substance or four kinds;
(3) neutralization reaction: in above-mentioned substance, add alkali, adjustment pH value promptly obtains the polymeric retention aid solvent at 5-7; Wherein said alkali is sodium hydroxide, Pottasium Hydroxide, calcium hydroxide or yellow soda ash, or their any two kinds and two or more mixtures;
(4) the water-soluble polymer solubility promoter after the above-mentioned neutralization of adding in polycarboxylate water-reducer, the ratio of adding is the 2-20% of solid mass ratio.
CN2010102598948A 2010-08-20 2010-08-20 Preparation method of cosolvent by compounding concrete admixture Expired - Fee Related CN101921372B (en)

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104609761B (en) * 2015-02-13 2016-12-07 重庆欣材混凝土集团股份有限公司 A kind of water reducing agent in series of polyocarboxy acid for concrete regulator and preparation method
CN107573783A (en) * 2017-10-30 2018-01-12 惠州市华昱美实业有限公司 A kind of metallic paint and its preparation technology
CN114522612A (en) * 2022-03-22 2022-05-24 厦门宏发先科新型建材有限公司 Preparation method and equipment of concrete water reducing agent

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1537126A (en) * 2000-12-27 2004-10-13 株式会社日本触媒 Polycarboxylic acid type copolymer, and preparation method and use thereof
CN1667009A (en) * 2005-02-28 2005-09-14 江苏省建筑科学研究院有限公司 A kind of carboxylic acid graft copolymer concrete slump retaining agent

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1537126A (en) * 2000-12-27 2004-10-13 株式会社日本触媒 Polycarboxylic acid type copolymer, and preparation method and use thereof
CN1667009A (en) * 2005-02-28 2005-09-14 江苏省建筑科学研究院有限公司 A kind of carboxylic acid graft copolymer concrete slump retaining agent

Non-Patent Citations (2)

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Title
孙振平等.聚羧酸系减水剂大单体MPEGMA的制备.《建筑材料学报》.2009,第12卷(第1期),101-105. *
李宁等.新型聚羧酸系高效减水剂的合成实验研究.《辽宁化工》.2009,第38卷(第3期),149-152. *

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