Method for preparing amino-terminated polyurethane

A technology of amino-terminated polyurethane and hydroxyl-terminated polyurethane, which is applied in the field of preparation of active amino-terminated functional compounds, and can solve problems such as poor fatigue resistance, heat resistance and impact resistance, affecting the performance of amino-terminated polyurethane, and difficulty in guaranteeing the performance of sprayed products, etc. , to achieve low cost, reduce production risk, and inhibit the generation of cross-linked structure

Inactive Publication Date: 2012-05-02
JIANGSU LANLING POLYMER MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, amino-terminated polyurethanes on the market are usually prepared by reacting isocyanate-terminated polyurethane prepolymers with highly reactive diamines. Because the reaction rate of isocyanate reacts with amino groups to form urea bonds is extremely fast, and the two reactants are Two or four functionalities, so the risk of gel polymerization in production is extremely high. It is necessary to protect the primary ammonia by adding acetone, that is, to prepare amino-terminated polyurethane by chemical protection method. Due to the inevitable energy loss when removing the solvent acetone The consumption increases, and the residual solvent will affect the performance of amino-terminated polyurethane to some extent
[0003] In recent years, spray-coated polyurea elastomers have been developed on a large scale due to their excellent performance, but the spray-coated polyurea elastomers widely used in China still have some performance defects, the main reason is that pure polyurea products are expensive
Spraying polyurethane / urea is widely used in the market. Since the polyurea system is doped with polyurethane, the reaction mechanism of polyurethane is quite different from that of polyurea. Urea bonds are easier to form than ester bonds, resulting in system compatibility. The performance of sprayed products is difficult to guarantee, so the polyurea products on the market are fake, and the quality is uneven
Similarly, epoxy resin has been widely used in aerospace, machinery, chemical industry, construction and other fields due to its excellent comprehensive performance. Therefore, the modification of epoxy resin has always been a hot topic in the research field.

Method used

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  • Method for preparing amino-terminated polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Step 1: Add 10 mol of propylene oxide homopolyether diol with a molecular weight of 400 into the reactor, vacuum dehydrate at 90-100°C for 1-2 hours, take samples to measure the moisture content, when the moisture content is less than 0.08%, Stop dehydration, cool to 70-75°C and maintain at this temperature range, add organic bismuth BiCAT catalyst, add 10mol MDI dropwise while stirring, continue to keep warm for 3 hours after the dropwise addition, and obtain hydroxyl-terminated polyurethane with an average molecular weight of 1050.

[0018] The second step: Slowly add the hydroxyl-terminated polyurethane obtained in the first step into another kettle equipped with 20mol IPDI and organic bismuth BiCAT catalyst under rapid stirring, and react for 3 hours to obtain an isocyanate-terminated polyurethane with an average molecular weight of 1495.

[0019] The third step: lower the temperature to below 30°C, under the condition of rapid stirring, slowly add the product obtain...

Embodiment 2

[0021] Step 1: Add 10 mol of ethylene oxide homopolyether diol with a molecular weight of 1000 into the reaction kettle, vacuum dehydrate at 90-100°C for 1-2 hours, take samples to measure the moisture content, when the moisture content is less than 0.08% , stop dehydration, cool to 70-75°C and maintain at this temperature range, add an organotin catalyst, add 10mol MDI dropwise while stirring, continue to keep warm for 3 hours after the dropwise addition, and obtain a hydroxyl-terminated polyurethane with an average molecular weight of 2250.

[0022] The second step: Slowly add the hydroxyl-terminated polyurethane obtained in the first step into another kettle equipped with 20 mol of IPDI and organic bismuth BiCAT catalyst under rapid stirring, and react for 3 hours to obtain an isocyanate-terminated polyurethane with an average molecular weight of 2695.

[0023] The third step: lower the temperature to below 30°C, under the condition of rapid stirring, slowly add the product ...

Embodiment 3

[0025] Step 1: Add 10 mol of ethylene oxide / propylene oxide copolyether diol with a molecular weight of 2000 into the reaction kettle, vacuum dehydrate at 90-100°C for 1-2 hours, take samples to measure the moisture content, when the moisture content is less than 0.08%, stop dehydration, cool to 70-75°C and maintain at this temperature range, add organotin and organobismuth BiCAT in a mass ratio of 1:1 composition, add 10mol HDI dropwise while stirring, continue to Insulated for 3 hours to obtain a hydroxyl-terminated polyurethane with an average molecular weight of 4250.

[0026] The second step: Slowly add the hydroxyl-terminated polyurethane obtained in the first step into another kettle equipped with 20 mol of IPDI and organic bismuth BiCAT catalyst under rapid stirring, and react for 3 hours to obtain an isocyanate-terminated polyurethane with an average molecular weight of 4695.

[0027] The third step: lower the temperature to below 30°C, under the condition of rapid st...

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Abstract

The invention relates to the technical field of preparation of active amino-terminated functional compounds, in particular to a method for preparing amino-terminated polyurethane by using a steric hindrance protection method. The method concretely comprises the following steps: respectively selecting isophorone diisocyanate and isophorone diisocyanate which have similar functional groups and different reactive activities as blocking modification raw materials; realizing a reaction rate gradient through steric hindrance protection; and directly functioning amino at two ends of a main structure to prepare the amino-terminated polyurethane. The amino-terminated polyurethane is directly and efficiently prepared through the steric hindrance protection method, thus, the defect that isocyanic acid rapidly reacts with the amino is avoided, the reaction process has a certain speed gradient, the generation of a crosslinking structure is inhibited, the production risk and the production energy consumption are remarkably reduced, and the product performance and the production efficiency are increased.

Description

technical field [0001] The invention relates to the technical field of preparation of active amino-terminated functional compounds, in particular to a method for preparing amino-terminated polyurethane by a steric hindrance protection method. Background technique [0002] At present, amino-terminated polyurethanes on the market are usually prepared by reacting isocyanate-terminated polyurethane prepolymers with highly reactive diamines. Because the reaction rate of isocyanate reacts with amino groups to form urea bonds is extremely fast, and the two reactants are Two or four functionalities, so the risk of gel polymerization in production is extremely high. It is necessary to protect the primary ammonia by adding acetone, that is, to prepare amino-terminated polyurethane by chemical protection method. Due to the inevitable energy loss when removing the solvent acetone The consumption increases, and the residual solvent will affect the performance of amino-terminated polyuret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/42C08G18/32C08G18/10C08G18/75C09D175/12
Inventor 高新田马金刘棋陈建刚庄建林王桂银
Owner JIANGSU LANLING POLYMER MATERIAL CO LTD
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