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A kind of preparation method of polyurethane prepolymer

A technology of polyurethane prepolymer and polyurethane, applied in the direction of polyurea/polyurethane adhesive, sustainable manufacturing/processing, non-polymer adhesive additives, etc., can solve the problem of unstable polyurethane prepolymer and low production efficiency , prepolymer yellowing and other problems, to achieve the effect of improving compatibility and heating/radiation uniformity, low fog value, and reducing viscosity

Active Publication Date: 2022-06-07
HUBEI HUITIAN NEW MATERIALS STOCK CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) The reaction temperature is generally controlled at 70°C~95°C, and the reaction time is 2~5 hours. The reaction is terminated by adding a polymerization inhibitor. It generally takes 2 hours or more to cool down to 50°C, and when it is scaled up to industrial production, the reaction system has a volume of tons on the level, and the cooling process will be longer. The entire production process takes about 5 to 10 hours, and the production efficiency is not high;
[0004] (2) The addition of small molecules of polymerization inhibitors will easily lead to yellowing of prepolymers, strong irritating odor, high fog value, and environmental protection;
[0005] (3) Polyurethane prepolymers are mainly blocked by isocyanate (NCO) groups, which are easy to react with moisture in the air to produce gels, resulting in very unstable polyurethane prepolymers

Method used

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  • A kind of preparation method of polyurethane prepolymer
  • A kind of preparation method of polyurethane prepolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Prepolymer I.: In a dried three-mouth flask, 24.5 parts of polyetherdiol Tdiol-2000 (molecular weight 2000), 40.2 parts of polyether ternitol F3128 (molecular weight 6000), 11.144 parts diisooctyl phthalate, 0.01 parts of toluene sulfonyl isocyanate, stirred at 50 °C ~ 55 °C vacuum mixed for 20min, wherein the vacuum degree ≤-0.09MPa. Nitrogen pressure relief, wherein the nitrogen purity ≥ 95%, the 13 parts diphenylmethane-4,4'-diisocyanate and 0.002 parts dibutyltin dilaurate were added to the step reaction mixture, the feeding control was controlled within 5 minutes, vacuum stirring heating, wherein the heating rate was 10 °C / 10min, the vacuum degree ≤-0.09MPa, at a temperature of 65 °C ± 2 °C, after the reaction of 1.5 hours, the NCO reached the preset target ≤2.95%, turn off the heating and heat preservation equipment. Nitrogen pressure relief, wherein the nitrogen purity ≥ 95%, the room temperature conditions of 11.144 parts of diisooctyl phthalate added to the reacti...

Embodiment 2

[0037]Prepolymer II., in a dry three-mouth flask added 22 parts of polyether diol Tdiol-3000 (molecular weight 3000), 48.5 parts of polyether ternary alcohol GEP-330N (molecular weight 5000), 5.5 parts diisooctyl phthalate, 0.01 parts of toluene sulfonyl isocyanate, stirred at 50 °C ~ 55 °C vacuum mixed for 20min, wherein the vacuum degree ≤-0.09MPa. Nitrogen pressure relief, wherein the nitrogen purity ≥ 95%, the 13 parts diphenylmethane-4,4'-diisocyanate and 0.002 parts dibutyltin dilaurate were added to the reaction mixture, the feeding was controlled within 5 minutes, vacuum stirring heating, wherein the heating rate was 10 °C / 10min, the vacuum degree was ≤ -0.09MPa, at a temperature of 65 °C ± 2 °C, the reaction was 1.5 hours, the NCO reached the preset target ≤ 2.85%, and the heating and heat preservation equipment was turned off. Nitrogen pressure relief, of which nitrogen purity ≥ 95%, the room temperature conditions of 11 parts of diisooctyl phthalate added to the reactio...

Embodiment 3

[0040]Prepolymer III.: In a dried three-mouth flask, 26.7 parts of polyetherdiol Tdiol-2000 (molecular weight 2000), 42.8 parts of polyether tereth terethyl alcohol F3135 (molecular weight 5000), 5 parts of diisooctyl phthalate and dioctyl terephthalate (V: V = 1: 1) mixture, 0.03 parts of toluene sulfonyl isocyanate, stirred at 50 ° C ~ 55 ° C vacuum mixed for 20min, wherein the vacuum degree ≤-0.09MPa. Nitrogen pressure relief, wherein the nitrogen purity ≥ 95%, the 10.467 parts of hexamethylene diisocyanate, 0.003 parts of dibutyltin diacetate were added to the step reaction mixture, the addition control was controlled within 5 minutes, vacuum stirring heating, wherein the heating rate was 10 °C / 10min, the vacuum degree ≤ -0.09MPa, at a temperature of 65 °C ± 2 °C, after the reaction of 1.5 hours, NCO reached the preset target of 3.56% ≤, turn off the heating and insulation equipment. Nitrogen pressure relief, wherein the nitrogen purity ≥ 95%, the room temperature under the ...

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Abstract

The invention relates to a preparation method of polyurethane adhesive glue and polyurethane prepolymer. The preparation method of polyurethane prepolymer provided by the present invention comprises specific weight parts of raw materials and the following preparation steps: S1, mixing polyether polyol, first diluent, water absorbing agent, polyisocyanate and catalyst, and reacting under vacuum condition Stop heating until the NCO reaches the preset target; S2, add the diluent at room temperature to the mixture obtained in step S1, and stir under vacuum; wherein the ratio of the first diluent used in step S1 and step S2 is 1 : (1-3). The present invention is the first to propose that part of the diluent in the adhesive component is used to synthesize the prepolymer, and the temperature of the reaction system is instantly lowered by adding the diluent step by step to terminate the reaction to obtain a polyurethane prepolymer with high stability. The method of the invention has high production efficiency and good environmental protection.

Description

Technical field [0001] The present invention relates specifically to a polyurethane adhesive and a method for preparing a polyurethane prepolymer thereof. Background [0002] The one-component polyurethane adhesive is mainly composed of polyurethane prepolymers, fillers, diluents, catalysts, etc. of isocyanate group sealing, the main component of which is polyurethane prepolymer, polyurethane prepolymer is a polymer substance formed by the initial polymerization of monomer polyols and polyisocyanates. Existing polyurethane prepolymers and their synthesis techniques generally have the following problems: [0003] (1) The reaction temperature is generally controlled at 70 °C ~ 95 °C, the reaction time is 2 ~ 5 hours, the reaction is terminated by adding a polymer inhibitor, after cooling water cooling, the discharge is stored, for the reaction system of ≥ 20L, the cooling water cooling to 50 °C generally takes 2 hours and more, scaled up to industrial production, the reaction syste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/48C08G18/12C09J175/08C09J11/06
CPCC08G18/4829C08G18/4825C08G18/4812C08G18/12C09J175/08C09J11/06C08K5/435Y02P20/10
Inventor 彭仁贵张虎极刘瑞韩胜利赵勇刚章锋
Owner HUBEI HUITIAN NEW MATERIALS STOCK CO LTD
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