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Water soluble polyurethane associative thickener, and inverse polymerization method and use thereof

An associative polyurethane and reverse-phase polymerization technology, applied in the field of materials, can solve the problems of low product production and storage stability, dark color of polyurethane associative thickener, and many side reaction products, so as to achieve stability Sexuality, low cost, and simple method

Active Publication Date: 2011-06-22
GUANGZHOU SHINE POLYMER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Because the isocyanate group (NCO) of organic monoisocyanate or diisocyanate has reactivity to water and active hydrogen, therefore, in order to avoid the generation of by-products, before carrying out polymerization reaction, usually by vacuum drying dehydration method in the prior art, will The water in the raw material is removed, and the bulk polymerization reaction is carried out. The obtained product is usually a waxy solid, which is very inconvenient in application. It needs to be dissolved with a solvent and a co-solvent before it can be added to the latex paint, etc. in thickened products
In addition, the existing reverse-phase polymerization method has many side reaction products, and the obtained polyurethane associative thickener has darker color, high reaction viscosity, difficulty in mass and heat transfer, difficulty in increasing molecular weight and achieving effective thickening branched structure , product production and storage stability is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Add 60 parts by mass of PEG6000 and 30 parts by mass of ethyl acetate into a flask with a stirring device, mix well, and dehydrate at 77° C. for 1 hour using an oil-water separator.

[0039] (2) Cool down to 60°C and fill with nitrogen, add 2.52 parts by mass of HDI, react at 60°C for 4.5 hours, then add 0.93 parts by mass of lauryl alcohol, react at 60°C for 5 hours, and finally add 0.22 parts by mass of TMP for reaction. The reaction was terminated after detection of no free isocyanate groups.

[0040] (3) Next, add 255 parts by mass of deionized water to the product solution obtained in step (2), raise the temperature to 98°C to azeotrope, remove the organic solvent through the oil-water separator, replenish the lost water, and cool to room temperature to obtain the solid content 20% water soluble polyurethane associative thickener.

[0041] In this example, the molar ratio of NCO to OH is 1:1, the molar ratio of PEG6000 to lauryl alcohol is 1:0.5, and the molar...

Embodiment 2

[0043] (1) Add 80 parts by mass of PEG8000 and 160 parts by mass of acetone into a flask with a stirring device, mix well, and dehydrate at 57° C. for 5 hours using an oil-water separator.

[0044] (2) Cool down to 50°C and fill with nitrogen, add 3.02 parts by mass of HDI, react at 60°C for 4.5 hours, then add 1.49 parts by mass of lauryl alcohol, react at 50°C for 5 hours, and finally add 0.36 parts by mass of TMP for reaction. The reaction was terminated after detection of no free isocyanate groups.

[0045] (3) Next, add 85 parts by mass of deionized water to the product solution obtained in step (2), heat up to 98° C. to azeotrope, remove the organic solvent through the oil-water separator, replenish the lost water, and cool to room temperature to obtain a solid content of 50 % water-soluble polyurethane associative thickener.

[0046]In this example, the molar ratio of NCO to OH is 1:1, the molar ratio of PEG8000 to lauryl alcohol is 1:0.8, and the molar ratio of TMP to...

Embodiment 3

[0048] (1) Add 100 parts by mass of PEG10000 and 100 parts by mass of methyl ethyl ketone into a flask with a stirring device, mix well, and dehydrate at 80° C. for 5 hours using an oil-water separator.

[0049] (2) Cool down to 75°C and fill with nitrogen, add 3.48 parts by mass of TDI, react at 75°C for 1 hour, then add 2.7 parts by mass of stearyl alcohol, react at 75°C for 1 hour, and finally add 0.34 parts by mass of pentaerythritol for reaction, The reaction was terminated when no free isocyanate groups were detected by infrared chromatography.

[0050] (3) Next, add 320 parts by mass of deionized water to the product solution obtained in step (2), heat up to 95°C to azeotrope, remove the organic solvent through the oil-water separator, replenish the lost water, and cool to room temperature to obtain the solid content 25% water soluble polyurethane associative thickener.

[0051] In this example, the molar ratio of NCO to OH is 1:1, the molar ratio of PEG10000 to steary...

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Abstract

The invention discloses a water soluble polyurethane associative thickener, and an inverse polymerization method and use thereof. The method comprises: dehydrating polyethylene glycol by using an organic solvent with a boiling point below 110 DEG C; adding diisocyanate in the protection of an inert gas to perform a reaction; adding fatty alcohol of which the chain is 8 to 22 carbon atoms long as a capping agent for further reaction; adding polyol containing at least three hydroxys as a chain extender to perform an reaction till there are no free isocyanate groups; and adding water, and removing the organic solvent by an azeotropic process to obtain the water soluble polyurethane associative thickener which is white, transparent and sticky fluid. The dehydration temperature of water soluble associative polyurethane is low, so the side reactions are inhibited effectively; and reaction is performed in the organic solvent and catalyst is not required, so cost is reduced and the hydrolysis side reaction of the product due to the catalyst is avoided. Because the polyol is used as a chain extender, the thickener of the invention has a branch structure and high thickening performance.

Description

technical field [0001] The invention relates to a thickener, in particular to a water-soluble associative polyurethane thickener and its reverse-phase polymerization method and application, belonging to the field of materials. Background technique [0002] Polyurethane associative thickener is a kind of thickener developed in the 1980s, which is a water-soluble oligomer containing hydrophobic groups. Traditional polyurethane associative thickener molecules are generally obtained by direct addition of organic monoisocyanate and polyether, or by reacting polyether with a certain molecular weight and excess diisocyanate first, and then blocked by organic amines or alcohols. It is a linear structure with lipophilic end groups at both ends and a long-chain hydrophilic group in the middle. The thickening principle of polyurethane associative thickener is: lipophilic end groups associate to form micelles, and the association of micelles forms a network structure, that is, the coup...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/32B01F17/52A61K8/87C09K23/52
Inventor 石建伟李向涛周亮杨全文杜纯丽
Owner GUANGZHOU SHINE POLYMER TECH
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