Catalyst for reaction of isocyanate and sulfydryl and preparation method of catalyst

A technology of isocyanate and catalyst, which is applied in the field of catalyst and its preparation for catalyzing the reaction between isocyanate and mercapto group, and can solve problems such as high activity, affecting product viscosity and structural regularity, and inability to prepare clean odor products

Active Publication Date: 2020-10-30
武汉长盈鑫科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the very low reactivity of isocyanate and mercapto groups, the typical reaction between isophorone diisocyanate and 3-mercaptopropyltrimethoxysilane usually needs to be catalyzed by dibutyltin dilaurate at 80°C. Over hours (Yu Zongping, Qiu Fengxian, Ding Hailin, et al. Synthesis and properties of UV-curable mercaptoacrylate[J]. Information Recording Materials, 2015, v.16; No.85(06):14-17.)
However, isocyanate and hydroxyl usually only need 2-4 hours to complete the reaction under the same reaction conditions. Too long reaction time will affect production efficiency, and long-term reaction at high temperature will cause more side reactions between moisture and isocyanate , affecting product performance
It has been reported in the literature that triethylamine has better reactivity to isocyanate and mercapto as a catalyst. In the actual preparation of urethane acrylate, it is found that the odor of triethylamine is very large, and the residual odor is difficult to remove. It is impossible to prepare clean odor products, and three Ethylamine has poor selectivity to the reaction between isocyanate and hydroxyl, and has high activity in catalyzing the side reaction between isocyanate and moisture
In the system that needs to catalyze the reaction between isocyanate and hydroxyl group and the reaction between isocyanate and mercapto group at the same time, triethylamine will cause more side reactions of isocyanate and water reaction, which will affect the viscosity and structural regularity of the product, which is not good for performance

Method used

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  • Catalyst for reaction of isocyanate and sulfydryl and preparation method of catalyst
  • Catalyst for reaction of isocyanate and sulfydryl and preparation method of catalyst
  • Catalyst for reaction of isocyanate and sulfydryl and preparation method of catalyst

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Effect test

Embodiment 1

[0024] A kind of preparation method for the catalyst of isocyanate and mercapto reaction, the steps are as follows:

[0025] S1-1: Add 480g of 3-mercaptopropyltriethoxysilane and 351.03g of dibutyltin diacetate into the reactor, stir evenly, heat to 90°C, and maintain the reaction for 4 hours;

[0026] S1-2: Keep the reaction temperature at 90°C and then connect the condenser tube to vacuumize the system so that the vacuum degree is kept below -0.1MPa, and remove the acetic acid generated by the reaction until there is no low boiling material dripping from the condenser tube;

[0027] S1-3: Keep the reaction temperature at 120°C and continue vacuuming for 2 hours, remove the excess mercaptosiloxane, stop the reaction and discharge the product, and the product obtained is a catalyst for the reaction between isocyanate and mercapto group (marked as catalyst CC- 01, the structure is shown in Formula 1, where R is -OCH 2 CH 3 ), the state is a light yellow transparent liquid, wi...

Embodiment 2

[0029] A kind of preparation method for the catalyst of reaction of isocyanate and mercapto group, the steps are as follows:

[0030] S1-1: Add 400g of 3-mercaptopropyltrimethoxysilane and 351.03g of dibutyltin diacetate into the reactor, stir evenly, heat to 85°C, and maintain the reaction for 5 hours;

[0031] S1-2: Keep the reaction temperature at 85°C and then connect the condenser tube to vacuumize the system so that the vacuum degree is kept below -0.1MPa, and remove the acetic acid generated by the reaction until there is no low boiling material dripping from the condenser tube;

[0032] S1-3: Keep the reaction temperature at 110°C and continue vacuuming for 2.5 hours, remove the excess mercaptosiloxane, stop the reaction and discharge the product, and the product obtained is a catalyst for the reaction between isocyanate and mercapto group (marked as catalyst CC- 02, the structure is shown in Formula 1, where R is -OCH 3 ), the state is a light yellow transparent liqu...

Embodiment 3

[0034] A kind of preparation method for the catalyst of reaction of isocyanate and mercapto group, the steps are as follows:

[0035] S1-1: Add 240g of 3-mercaptopropyltriethoxysilane, 200g of 3-mercaptopropyltrimethoxysilane and 351.03g of dibutyltin diacetate into the reactor, stir evenly, heat to 88°C, and maintain React for 4 hours;

[0036] S1-2: Keep the reaction temperature at 88°C and then connect the condenser tube to vacuumize the system so that the vacuum degree is kept below -0.1MPa, and remove the acetic acid generated by the reaction until there is no low boiling material dripping from the condenser tube;

[0037] S1-3: Keep the reaction temperature at 115°C and continue vacuuming for 2.5 hours, remove the excess mercaptosiloxane, stop the reaction and discharge the product, and the product obtained is a catalyst for the reaction between isocyanate and mercapto group (marked as catalyst CC- 03, the structure is shown in Formula 1, and R is -OCH respectively 2 C...

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PUM

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Abstract

The invention discloses a catalyst for reaction of isocyanate and sulfydryl. The catalyst is prepared by reaction of mercaptosilane and dibutyltin diacetate, has quite high reaction activity for reaction of isocyanate and sulfydryl, is quite high in final conversion rate, solves the problem of reaction of isocyanate and sulfydryl, and provides more technical methods for introduction of sulfydryl-containing materials into polyurethane materials.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a catalyst capable of efficiently catalyzing the reaction between isocyanate and mercapto groups and a preparation method thereof. Background technique [0002] Isocyanate and mercapto group can react to produce thiourethane. Compared with traditional polyurethane structure, this special polyurethane structure has better low temperature flexibility and better adhesion characteristics. However, due to the very low reactivity of isocyanate and mercapto groups, the typical reaction between isophorone diisocyanate and 3-mercaptopropyltrimethoxysilane usually needs to be catalyzed by dibutyltin dilaurate at 80°C. More than hours (Yu Zongping, Qiu Fengxian, Ding Hailin, et al. Synthesis and properties of UV-curable mercaptoacrylate [J]. Information Recording Materials, 2015, v.16; No.85(06):14-17.). However, isocyanate and hydroxyl usually only need 2-4 hours to complete the react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22B01J31/12C07C333/04C08G18/24
CPCB01J31/122B01J2231/4294C07C333/04C07F7/226C08G18/242
Inventor 黄星余晓梦崔丽云万欢桂振东皮亚斌高旭
Owner 武汉长盈鑫科技有限公司
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