Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method for polyurethane prepolymer

A polyurethane prepolymer, polyisocyanate technology, applied in the direction of polyurea/polyurethane adhesive, sustainable manufacturing/processing, adhesive type, etc., can solve the problem of unstable polyurethane prepolymer, low production efficiency, irritation, etc. Great odor and other problems, to achieve the effect of reducing viscosity, low fog value and good stability

Active Publication Date: 2020-07-03
HUBEI HUITIAN NEW MATERIALS STOCK CO LTD +2
View PDF10 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) The reaction temperature is generally controlled at 70°C to 95°C, and the reaction time is 2 to 5 hours. The reaction is terminated by adding a polymerization inhibitor. It generally takes 2 hours or more to cool down to 50°C. When it is scaled up to industrial production, the reaction system has a volume of tons of tons, 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method for polyurethane prepolymer
  • Preparation method for polyurethane prepolymer
  • Preparation method for polyurethane prepolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Prepolymer Ⅰ: Add 24.5 parts of polyether diol Tdiol-2000 (molecular weight 2000), 40.2 parts of polyether triol F3128 (molecular weight 6000), and 11.144 parts of diisooctyl phthalate into a dry three-necked flask , 0.01 part of toluenesulfonyl isocyanate, stirred and mixed in vacuum at 50℃~55℃ for 20min, wherein the vacuum degree ≤-0.09MPa. Nitrogen pressure relief, where the nitrogen purity is ≥95%, add 13 parts of diphenylmethane-4,4'-diisocyanate and 0.002 parts of dibutyltin dilaurate to the reaction mixture, and the addition is controlled within 5 minutes, vacuum Stir and heat up, wherein the heating rate is 10°C / 10min, the vacuum degree is ≤-0.09MPa, and at a temperature of 65°C±2°C, after 1.5 hours of reaction, the NCO reaches the preset target ≤2.95%, and the heating and heat preservation equipment is turned off. Nitrogen pressure relief, wherein the nitrogen purity is ≥95%, add 11.144 parts of di-isooctyl phthalate to the reaction mixture at room temperature,...

Embodiment 2

[0037] Prepolymer II, add 22 parts of polyether diol Tdiol-3000 (molecular weight 3000), 48.5 parts of polyether triol GEP-330N (molecular weight 5000), 5.5 parts of diisophthalic acid in a dry three-necked flask Octyl ester, 0.01 part of toluenesulfonyl isocyanate, stirred and mixed under vacuum at 50℃~55℃ for 20min, wherein the degree of vacuum is ≤-0.09MPa. Nitrogen pressure relief, wherein the nitrogen purity is ≥ 95%, add 13 parts of diphenylmethane-4,4'-diisocyanate and 0.002 parts of dibutyltin dilaurate to the reaction mixture, the addition is controlled within 5 minutes, and vacuum stirring Heating, where the heating rate is 10°C / 10min, the vacuum degree is ≤-0.09MPa, and the temperature is 65°C±2°C, react for 1.5 hours, and the NCO reaches the preset target ≤2.85%, turn off the heating and heat preservation equipment. Nitrogen pressure relief, wherein the nitrogen purity is ≥95%, add 11 parts of di-isooctyl phthalate to the reaction mixture at room temperature, stir ...

Embodiment 3

[0040]Prepolymer III: Add 26.7 parts of polyether diol Tdiol-2000 (molecular weight 2000), 42.8 parts of polyether triol F3135 (molecular weight 5000), and 5 parts of diisooctyl phthalate into a dry three-necked flask The mixture with dioctyl terephthalate (V:V=1:1), 0.03 parts of toluenesulfonyl isocyanate, stirred and mixed in vacuum at 50℃~55℃ for 20min, wherein the vacuum degree≤-0.09MPa. Nitrogen pressure relief, wherein the nitrogen purity is ≥ 95%, 10.467 parts of hexamethylene diisocyanate and 0.003 parts of dibutyltin diacetate are respectively added to the first reaction mixture, the addition is controlled within 5 minutes, and the temperature is raised under vacuum stirring, wherein the heating rate is 10°C / 10min, vacuum degree ≤-0.09MPa, at 65°C±2°C, after 1.5 hours of reaction, NCO reaches the preset target ≤3.56%, turn off the heating and heat preservation equipment. Nitrogen pressure relief, where the nitrogen purity is ≥95%, add 15 parts of a mixture of di-octy...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a polyurethane adhesive and a preparation method for a polyurethane prepolymer of the polyurethane adhesive. The preparation method for the polyurethane prepolymer provided bythe invention uses raw materials with specific parts by weight and comprises the following steps: S1, mixing polyether polyol, a first diluent, a water absorbent, polyisocyanate and a catalyst, carrying out reaction under a vacuum condition until NCO reaches a preset target, and stopping heating; and S2, adding a diluent under a room temperature condition into the mixture obtained in the step S1,and carrying out stirring under a vacuum condition; wherein the ratio of the first diluent used in the step S1 to the first diluent used in the step S2 is 1: (1-3). According to the invention, one part of the diluent in the adhesive component is used for synthesizing the prepolymer for the first time; and the diluent is added step by step to instantaneously reduce the temperature of a reaction system to terminate the reaction, so the polyurethane prepolymer with high stability is obtained. The method provided by the invention is high in production efficiency and good in environmental protection property.

Description

technical field [0001] The invention specifically relates to a preparation method of a polyurethane adhesive and a polyurethane prepolymer thereof. Background technique [0002] The one-component polyurethane adhesive is mainly composed of isocyanate (NCO) group-terminated polyurethane prepolymer, filler, diluent, catalyst, etc., the main component of which is polyurethane prepolymer, which is a monomeric polyol A polymer substance initially polymerized with polyisocyanate. The existing polyurethane prepolymer and its synthesis technology generally have the following problems: [0003] (1) The reaction temperature is generally controlled at 70°C to 95°C, and the reaction time is 2 to 5 hours. The reaction is terminated by adding a polymerization inhibitor. It generally takes 2 hours or more to cool down to 50°C. When it is scaled up to industrial production, the reaction system has a volume of tons of tons, and the cooling process will be longer. The entire production proc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products