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Preparation method of carbodiimide modified isocyanate with low color number and high stability

A carbodiimide and diisocyanate technology, applied in the field of isocyanates, can solve the problems of poor stability, unsatisfactory product color number, poor product color number, etc., and achieves the effect of simple method, convenient industrial application, and improved stability

Pending Publication Date: 2021-03-30
WANHUA CHEMICAL (NINGBO) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1789241A discloses the use of alkylating reagents such as triflates to terminate the reaction, and the stability can be achieved by increasing the molar equivalent ratio of the terminator and the catalyst, but the product color number is not ideal
[0008] In summary, the existing isocyanate liquefaction methods generally have the problems of poor product color and poor stability

Method used

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  • Preparation method of carbodiimide modified isocyanate with low color number and high stability
  • Preparation method of carbodiimide modified isocyanate with low color number and high stability
  • Preparation method of carbodiimide modified isocyanate with low color number and high stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1000g diphenylmethane diisocyanate in N 2 Heating to 50°C while stirring under protection, adding 1.0ppm of 1-methyl-3-methyl-3-phosphole-1-oxide (based on the total weight of isocyanate monomers), and rapidly heating to 110°C, after reacting for 5 hours, reverse 500g of diphenylmethane diisocyanate, rapidly cool the temperature down to 60°C, stir for 30 minutes, add 3.0ppm of methyl oxalyl chloride (based on the total weight of the reaction solution) for aging, and after aging for 4 hours, test the CDI When the content is 0.5%, 5.0ppm terminator trifluoromethanesulfonic anhydride is added to obtain the final product.

Embodiment 2

[0047] 1000g diphenylmethane diisocyanate in N 2 Heating to 50°C while stirring under protection, adding 1.0ppm of 1-methyl-3-methyl-3-phosphole-1-oxide (based on the total weight of isocyanate monomers), and rapidly heating to 110°C, after reacting for 5 hours, reverse diphenylmethane diisocyanate 500g, cool the temperature down to 60°C, stir for 30min, add 5.0ppm methyl oxalyl chloride for aging, after aging for 2h, test that the CDI content is 1.0%, add 5.0 ppm terminator trifluoromethanesulfonic anhydride to obtain the final product.

Embodiment 3

[0049] 1000g diphenylmethane diisocyanate in N 2 Heating to 50°C while stirring under protection, adding 3.0ppm of 1-phenyl-2-phosphene-1-oxide, mixing and rapidly heating to 110°C, reacting for 8 hours and then reversed 500g of diphenylmethane diisocyanate, Rapidly cool the temperature down to 60°C, stir for 30 minutes, add 8.0ppm of methyl oxalyl chloride for aging, and after aging for 2 hours, when the CDI content is 1.0%, add 7.5ppm of terminator trifluoromethanesulfonic anhydride to obtain the final product.

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Abstract

The invention relates to a preparation method of carbodiimide modified isocyanate with low color number and high stability. The method comprises the following steps: S1, carrying out a carbodiimide reaction on an isocyanate monomer to obtain a reaction solution containing carbodiimide (CDI) and / or uretonimine (UTI) groups; S2, carrying out curing reaction to reduce the CDI content in the reactionliquid, and controlling the CDI content to be 0.5-4.0%; and S3, adding a terminating agent to terminate the carbodiimide reaction. The modified isocyanate prepared by the method has the characteristics of normal-temperature liquid state, normal-temperature and high-temperature storage stability and low color number.

Description

technical field [0001] The invention belongs to the field of isocyanate, in particular to a preparation method of carbodiimide modified isocyanate with low color number and high stability. Background technique [0002] Diisocyanate is one of the main raw materials of polyurethane, and it is a clear and transparent liquid when melted. However, pure isocyanate is solid at room temperature and has poor stability during storage and transportation, which brings inconvenience to operation and storage. Carbodiimide-modified isocyanate is liquid at room temperature, easy to use, and has been favored by the majority of users. Carbodiimide-modified isocyanate, under the action of a high-efficiency catalyst, isocyanate is heated to cause polycondensation reaction to form a modified product containing carbodiimide structure. Carbodiimide group can be formed by addition reaction with isocyanate Uretonimine group, through this method, the isocyanate contains carbodiimide (CDI) and ureto...

Claims

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Application Information

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IPC IPC(8): C07C263/18C07C265/14
CPCC07C263/18C07C265/14
Inventor 陈盟王文博夏以禄肖应鹏朱梦雅包金鹏徐丹张宏科
Owner WANHUA CHEMICAL (NINGBO) CO LTD
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