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Synthesis of amino-base resin-base polyurea polylol

A technology of polyurea polyol and amino resin, which is applied in the field of synthesis of amino resin-based polyurea polyol, can solve the problems of infrequent use of economic benefits, expensive raw materials, increased process costs, etc., and achieve low raw material cost and high acid value Low, less smoke effect

Inactive Publication Date: 2006-08-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When ethylenediamine is used to prepare polyurea polyol, due to the poor solubility of ethylenediamine in polyether, the reaction with isocyanate is too fast, the molecular weight of polyurea increases sharply, and it precipitates out from polyether rapidly, and the obtained polyurea polyol is placed Easy to layer; the preparation of polyurea polyols with hydrazine hydrate will not cause sudden polymerization of polyurea molecules due to the elimination of partial steric effects due to the presence of two methylene groups like ethylenediamine, so it is suitable for polyurea polyols Alcohol preparation, but the price is high and not very economical; piperazine is a cyclized product containing two symmetrical secondary amino groups. When one of the secondary amino groups reacts with isocyanate, the reaction ability of the other secondary amino group has little effect, and the secondary amino group The reaction ability of polyurea is weaker than that of primary amino groups, so it will not cause sudden polymerization of polyurea molecules, which is more suitable for the preparation of polyurea polyols, but its raw materials are more expensive and the post-treatment is more complicated, which increases the process cost. aspect considerations are not often used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Step 1: Add 1mol melamine and 3mol formaldehyde into a four-necked flask, mix and stir, add alkaline reagent sodium hydroxide to adjust the pH value to 7, and add catalyst magnesium carbonate, the amount of magnesium carbonate is 0.2% of the weight of melamine; heat to 60°C , reacted for 0.5 hours to obtain a polymethylol melamine solution; the molar ratio of polymethylol melamine to methanol was 1:10 to add excess methanol, heated to 40°C and continued to react for about 0.5 hours to obtain methoxymethyl Melamine (amino resin) solution.

[0018] Step 2: Add 30g of the above-mentioned amino resin solution (containing 0.042mol of amino resin) and 158g (0.053mol) of polyether polyol (polyether polyol has a hydroxyl value of 56mgKOH / g, a functional group of 3, and a molecular weight of 3000) into a four-necked flask. , the secondary hydroxyl content is 85-100%), stirring and mixing, under the pressure of -0.05Mpa and temperature of 120 ℃, vacuum distillation for 0.5 hours ...

Embodiment 2

[0021] The first step: add 1mol melamine and 3mol formaldehyde in a four-necked flask, mix and stir, add alkaline reagent sodium carbonate to adjust the pH value to 10, and add catalyst magnesium carbonate, the amount of magnesium carbonate is 0.2% of the amount of melamine; heat to 90°C, React for 1.5 hours to obtain a polymethylol melamine solution; add excess methanol according to the molar ratio of polymethylol melamine to methanol at 1:10, heat to 80°C and continue the reaction for about 1 hour to obtain methoxymethyl melamine (amino resin) solution.

[0022] Step 2: Add 30g of the above-mentioned amino resin solution (containing 0.042mol of amino resin) and 99g (0.033mol) of polyether polyol into a four-necked flask (polyether polyol has a hydroxyl value of 56mgKOH / g, a functional group of 3, and a molecular weight of 3000 , secondary hydroxyl content 85-100%), stirring and mixing, under the condition of pressure of -0.08Mpa and temperature of 100°C, vacuum distillation ...

Embodiment 3

[0025] Step 1: Add 1mol melamine and 5mol formaldehyde into a four-neck flask, mix and stir, add alkaline reagent sodium bicarbonate to adjust the pH value to 8, and add catalyst magnesium carbonate, the amount of magnesium carbonate is 0.5% of the weight of melamine; heat to 100°C , reacted for 1 hour to obtain a polymethylol melamine solution; the molar ratio of polymethylol melamine to methanol was 1:15 to add excess methanol, heated to 40 ° C and reacted for about 3 hours to obtain methoxymethyl melamine (amino resin) solution.

[0026]The second step: add 63.6g of the above-mentioned amino resin solution (containing 0.06mol of amino resin) and 99g (0.033mol) of polyether polyol into a four-necked flask (polyether polyol has a hydroxyl value of 56mgKOH / g, a functional group of 3, and a molecular weight of 3000, the secondary hydroxyl content is 85-100%), stirring and mixing, under the condition of pressure of -0.1Mpa and temperature of 100°C, vacuum distillation for 1 hour...

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PUM

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Abstract

Synthesis of amino-resin polyurea polyol is carried out by mixing melamine with methyl aldehyde, agitating, regulating pH value by alkali agent, adding into catalyst, heat reacting to obtain polyhydroxy-methyl-melamine solution, heat reacting the obtained solution with excessive methyl alcohol to obtain amino-resin solution, agitation mixing the obtained amino-resin solution with poly-ether polybasic alcohol with molecular weight 3000, depress distilling to remove small molecule, cooling to lower temperature, adding into paraffin solvent and tertiary amine catalyst, agitating, adding into isocyanate, heat reacting, decompressing and removing residual small molecules to obtain final product. It is simple, cheap, has lower acidity, higher oxygen index and no halogen, phosphor and antimony.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a synthesis method of amino resin-based polyurea polyol. Background technique [0002] Polyurea polyol (PHD) is a branched-chain copolymer formed by the gradual addition reaction of polyisocyanate and polyamine in polyol. It is a high-viscosity, white or beige liquid. Polyurea polyol contains a large amount of polyurea particles containing nitrogen groups, so that the produced polyurethane foam can not only improve the flame retardancy, but also improve the load-bearing capacity of foam plastics. The foam prepared by it can be added without or with very little Only a small amount of flame retardant can achieve a better flame retardant effect, and avoid the migration of part of the flame retardant during the use of the foam, resulting in a decrease in flame retardant performance. In addition, polyurea polyol helps to open the cells when the foam rises t...

Claims

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Application Information

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IPC IPC(8): C08G12/32C08G12/40C08G18/40C08G71/02
Inventor 修玉英王书红罗钟瑜
Owner SOUTH CHINA UNIV OF TECH
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