CN107602811A - Association thickener manufacturing process - Google Patents

Association thickener manufacturing process Download PDF

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Publication number
CN107602811A
CN107602811A CN201711061398.XA CN201711061398A CN107602811A CN 107602811 A CN107602811 A CN 107602811A CN 201711061398 A CN201711061398 A CN 201711061398A CN 107602811 A CN107602811 A CN 107602811A
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China
Prior art keywords
parts
feed intake
chain
long
hydrophilic
Prior art date
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Withdrawn
Application number
CN201711061398.XA
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Chinese (zh)
Inventor
应建忠
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Yongjia Xincheng Technology Service Co Ltd
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Yongjia Xincheng Technology Service Co Ltd
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Priority to CN201711061398.XA priority Critical patent/CN107602811A/en
Publication of CN107602811A publication Critical patent/CN107602811A/en
Withdrawn legal-status Critical Current

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Abstract

The present invention relates to a kind of association thickener manufacturing process, its reactant includes polyethylene glycol, diisocyanate, solvent, nertralizer, catalyst, antioxidant, double hydroxycarboxylic acid hydrophilic chain extenders, polar aprotic strong solvent, long-chain alkyl alcohol and monoethanolamine;Mainly using the double hydroxycarboxylic acids of hydrophily as chain extender, and carry out chain extension before hydrophobic grouping reacts, form the molecule that end group is isocyano, then reacted with long-chain alkyl alcohol, it is hydrophobic to form last both ends, the long chain of hydrophilic in the middle, the center section of the strand is hydrophilic parts, including polyethylene glycol and double hydroxycarboxylates, strand both ends are the long-chain alkyl alcohol hydrophobic grouping connected by isocyanates root, mixture viscosity is low in preparation process, with good hydrophilic property, thickening effect is good, properties of product are stable, the advantages that preparation technology is simple.

Description

Association thickener manufacturing process
Technical field
The invention belongs to polymeric material field, more particularly to a kind of thickener.
Background technology
Aqueous polyurethane association thickener is typically made up of hydrophobic group, hydrophilic chain and crosslinking agent.Hydrophobic group is typically oil Base, octadecyl, dodecane phenyl, nonyl phenolic group etc., it plays association, is the principal element for determining thickening effect.It is hydrophilic Chain is typically the materials such as Aethoxy Sklerol, can provide chemical stability and viscosity stability.Crosslinking agent refers to diisocyanate or more Isocyanates, usually used is hexamethylene diisocyanate HDI, IPDI IPDI, the hexamethylenes of 4,4'- bis- Dicyclohexylmethane diisocyanate H12MDI etc..Its thickening mechanism is by molecule hydrophobic side and latex particle, surfactant, pigment Associated Deng hydrophobic structure, form space network, when its concentration is higher than critical micelle concentration, form micella;And hydrophilic chain Worked with water molecules hydrogen bond, so as to reach thickening result.Such as the patent CN201210426530.3 " line styles containing hydrophobic side base In the preparation method of aqueous polyurethane thickener ", description can it is a kind of by 40%-60% polyethylene glycol, 10%-30% diisocyanate and 10%-30% end-capping reagents react under catalyst action forms half closed-end structure, then increases molecular weight using small molecule chain extender, Form final aqueous polyurethane thickener.Its shortcoming in course of reaction viscosity it is larger, the performed polymer needs eventually formed It is dried, 20 is pressed after drying:80 add water to stir the thickener to form 20% solid content, and product stability is poor, have impact on thickening Performance.
The content of the invention
The purpose of the present invention is the shortcomings that presence for prior art, there is provided a kind of properties of product are stable, thickening effect is good, Course of reaction viscosity is low, the simple association thickener manufacturing process of preparation technology.
Reactant of the present invention includes polyethylene glycol, diisocyanate, solvent, nertralizer, catalyst, antioxidant, double hydroxyls Yl carboxylic acid hydrophilic chain extender, polar aprotic strong solvent, long-chain alkyl alcohol and monoethanolamine;Mainly use following manufacture work Skill:
1)Feed intake molecular weight 600 953.5 parts of polyethylene glycol enter 2000L stock kettle, be warming up to 1150C, it is small to vacuumize dehydration 0.5 When, reflux condensation mode valve is opened, is passed through nitrogen protection;
2)It is cooled to 800C, under moderate-speed mixer, feed intake 0.2 part of antioxidant, and after stirring, feed intake 200 parts of N- first in order Base pyrrolidones, 252.3 parts of hexamethylene diisocyanates, 1 part of catalyst, insulation reaction 1.0-1.5 hours are to setting isocyanide Acid group value;
3)Feed intake 67 parts of dihydroxypropionic acids, and insulation reaction extremely sets isocyanic acid root in 2 hours;
4)Feed intake 200 parts of DMAs, 135.2 parts of long-chain alkyl alcohols, insulation reaction 1.5-2.0 hours to isocyanic acid Root reaches setting content;
5)Hot water valve is closed, cooling water valve is opened, material is cooled to 500During below C, the 100 parts of ethyl acetates that feed intake be solvent, 45 parts of triethylamines are nertralizer, 3 parts of monoethanolamines, and are sufficiently stirred 30 minutes;
6)Mix slowly down, the 453.5 parts of water that feed intake are diluted, and are stirred;
7)Detect it is qualified after, filter and package.
Compared with the prior art, the invention has the advantages that:The present invention is using the double hydroxycarboxylic acids of hydrophily as chain extension Agent, and chain extension is carried out before hydrophobic grouping reacts, the molecule that end group is isocyano is formed, it is then anti-with long-chain alkyl alcohol Should, forming that last both ends are hydrophobic, long chain of hydrophilic in the middle, the center section of the strand is hydrophilic parts, including Polyethylene glycol and double hydroxycarboxylates, strand both ends are the long-chain alkyl alcohol hydrophobic grouping connected by isocyanates root, are passed through Polyethylene glycol middle element chain after double hydroxycarboxylates strengthen has very strong hydrophily, in polar aprotic strong solvent Under effect, there is association effect well with water and hydrophilic radical, mixture viscosity is low in preparation process, its hydrophily Good, thickening effect is good, and properties of product are stable, and preparation technology is simple.
Embodiment
Reactant in association thickener process for making of the present invention include polyethylene glycol, diisocyanate, solvent, Nertralizer, catalyst, antioxidant, double hydroxycarboxylic acid hydrophilic chain extenders, polar aprotic strong solvent, long-chain alkyl alcohol and one Monoethanolamine;Using following manufacturing process:
1)Feed intake molecular weight 600 953.5 parts of polyethylene glycol enter 2000L stock kettle, be warming up to 1150C, it is small to vacuumize dehydration 0.5 When, reflux condensation mode valve is opened, is passed through nitrogen protection;
2)It is cooled to 800C, under moderate-speed mixer, feed intake 0.2 part of antioxidant, and after stirring, feed intake 200 parts of N- first in order Base pyrrolidones, 252.3 parts of hexamethylene diisocyanates, 1 part of catalyst, insulation reaction 1.0-1.5 hours are to setting isocyanide Acid group value;
3)Feed intake 67 parts of dihydroxypropionic acids, and insulation reaction extremely sets isocyanic acid root in 2 hours;
4)Feed intake 200 parts of DMAs, 135.2 parts of long-chain alkyl alcohols, insulation reaction 1.5-2.0 hours to isocyanic acid Root reaches setting content;
5)Hot water valve is closed, cooling water valve is opened, material is cooled to 500During below C, the 100 parts of ethyl acetates that feed intake be solvent, 45 parts of triethylamines are nertralizer, 3 parts of monoethanolamines, and are sufficiently stirred 30 minutes;
6)Mix slowly down, the 453.5 parts of water that feed intake are diluted, and are stirred;
7)Detect it is qualified after, filter and package.
" part " of the present invention is a unit mass, typically uses 1Kg as a unit mass;Various material compositions Ratio be relative preferred values, various times settings are relative preferred times;The injected volume of each material can be according to reactor capacity Or batch size increases and decreases in proportion.

Claims (1)

  1. A kind of 1. association thickener manufacturing process, it is characterized in that using following processing step:
    1)Feed intake molecular weight 600 953.5 parts of polyethylene glycol enter 2000L stock kettle, be warming up to 1150C, it is small to vacuumize dehydration 0.5 When, reflux condensation mode valve is opened, is passed through nitrogen protection;
    2)It is cooled to 800C, under moderate-speed mixer, feed intake 0.2 part of antioxidant, and after stirring, feed intake 200 parts of N- methyl in order Pyrrolidones, 252.3 parts of hexamethylene diisocyanates, 1 part of catalyst, insulation reaction 1.0-1.5 hours are to setting isocyanic acid Root;
    3)Feed intake 67 parts of dihydroxypropionic acids, and insulation reaction extremely sets isocyanic acid root in 2 hours;
    4)Feed intake 200 parts of DMAs, 135.2 parts of long-chain alkyl alcohols, insulation reaction 1.5-2.0 hours to isocyanic acid Root reaches setting content;
    5)Hot water valve is closed, cooling water valve is opened, material is cooled to 500During below C, the 100 parts of ethyl acetates that feed intake be solvent, 45 parts of triethylamines are nertralizer, 3 parts of monoethanolamines, and are sufficiently stirred 30 minutes;
    6)Mix slowly down, the 453.5 parts of water that feed intake are diluted, and are stirred;
    7)Detect it is qualified after, filter and package.
CN201711061398.XA 2017-11-02 2017-11-02 Association thickener manufacturing process Withdrawn CN107602811A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711061398.XA CN107602811A (en) 2017-11-02 2017-11-02 Association thickener manufacturing process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711061398.XA CN107602811A (en) 2017-11-02 2017-11-02 Association thickener manufacturing process

Publications (1)

Publication Number Publication Date
CN107602811A true CN107602811A (en) 2018-01-19

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711061398.XA Withdrawn CN107602811A (en) 2017-11-02 2017-11-02 Association thickener manufacturing process

Country Status (1)

Country Link
CN (1) CN107602811A (en)

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Application publication date: 20180119