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Method for preparing aliphatic polyisocyanurate by using microreactor

An isocyanurate and microreactor technology, applied in organic chemistry and other directions, can solve the problems of high product viscosity, many catalysts and additives, and difficult to control the reaction process.

Active Publication Date: 2010-08-18
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the yellowing resistance of the trimer in the product placement is obviously better than that of biuret and other adduct products, but in the process of preparing the trimer, there are the following problems: the catalyst is easy to remain, which affects the later application ; The obtained adduct is easy to turn yellow, which affects the performance of the later product; the product obtained from the trimer has a high viscosity, which affects the construction performance
The main problem of the trimerization reaction is that the reaction heat is too large, it is difficult to control the reaction process, and there are too many additional catalysts and additives. Undesirable by-products, and in the post-processing process, these trace components cannot be eliminated, thereby affecting the application properties of the final trimer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Use nitrogen to remove a small amount of air and water vapor from the HDI monomer, add 0.01 g / min of catalyst (the mass ratio of DABCOTMR to tert-butanol is 4:6) and 100 g / min of HDI monomer into the pre-set to 40 ° C In the microreactor with an inner diameter of 0.1mm and a length of 10cm manufactured by Wanhua Polyurethane Company, the number of microchannels is 250, the reaction pressure is 0.2bar, and the residence time of the reaction raw materials in the reactor is about 3 minutes, 30 minutes Stop the continuous catalyst and monomer feeding, and detect NCO and viscosity at the sampling point provided; the reaction solution enters a 5-liter reactor equipped with a stirrer, nitrogen inlet, and automatic temperature control system. The temperature of the reactor is increased to 30°C, and the reaction temperature of the second reactor is increased to 50°C depending on the exothermic reaction in the microreactor, and the reaction is carried out in the second reactor for...

Embodiment 2

[0032] Use nitrogen to remove a small amount of air and water vapor from the HDI monomer, add 0.01 g / min of catalyst (the mass ratio of DABCOTMR to tert-butanol is 1:1) and 100 g / min of HDI monomer into the preset temperature of 40 ° C In a microreactor with an inner diameter of 0.1 mm and a length of 15 cm manufactured by Wanhua Polyurethane Company, the number of microchannels is 250, the reaction pressure is 0.2 bar, and the residence time of the reaction raw materials in the microreactor is about 5 minutes. Stop the continuous catalyst and monomer feeding after 10 minutes, and detect NCO and viscosity at the sampling point provided; the reaction solution then enters a 5-liter reactor equipped with a stirrer, nitrogen inlet, and automatic temperature control system. Raise the temperature of the reactor to 30°C, rely on the exothermic reaction in the microreactor to increase the reaction temperature of the second reactor to 50°C, and react in the second reactor for 0.5 hours ...

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Abstract

The invention discloses a method for preparing aliphatic polyisocyanurate by using a microreactor, which comprises the following steps: adding isocyanurate and a catalyst compound system formed by quaternary ammonium salt and inert alcohol solvent to enable the isocyanurate to generate a polymerization reaction; then feeding a formed material flow into a dynamic reactor for continuously carrying out a polymerization reaction; and enabling reaction solution obtained by the reaction to pass through a second-stage evaporator to obtain a polyisocyanurate product. The method can well control the reactivity of the catalyst, so that a trimerization reaction of the isocyanurate is finished under a mild condition to obtain a tripolymer product with excessively-high quality.

Description

technical field [0001] The invention relates to a preparation method of aliphatic isocyanate trimer, specifically, a method for preparing aliphatic polyisocyanurate through a microreactor. Background technique [0002] Microreactor is a kind of fluid flow channel manufactured by micromachining technology. It is a chemical reactor with a characteristic scale within hundreds of microns. In the early 1980s, Tuckerman and Pease first proposed the concept of "microchannel radiator". Successfully solved the "thermal barrier" problem faced by large-scale and ultra-large-scale integrated circuits. In the early 1990s, microreactors began to be applied in the chemical industry. Due to their good application characteristics, the concept of microchemical technology quickly aroused the strong interest and attention of experts in the chemical industry. The use of microreactors in the chemical industry is essentially a continuous flow pipeline reactor, which includes mixers, heat exchange...

Claims

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Application Information

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IPC IPC(8): C07D251/34
Inventor 孙中平尚永华华卫琦王玉启尹明辉王海影石滨李建峰隋宝华宋锦宏王勇
Owner WANHUA CHEM GRP CO LTD
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