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Method for preparing biuret polyisocyanates

A technology for polyisocyanates and diisocyanates is applied in the field of preparing biuret polyisocyanates, which can solve the problems of energy waste, poor adjustability and high product viscosity, and achieve the effects of improving operation safety, avoiding energy consumption and reducing product viscosity.

Active Publication Date: 2016-06-01
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, in the water method preparation, due to the wide average residence time of the reaction liquid in the conventional full-mixed tank reactor, the product viscosity is high; during the reaction process, the raw materials need to be preheated and added to the reactor, and the circulation is introduced during the reaction process. Water cooling removes the heat of reaction to maintain the reaction temperature of the system, and the energy consumption is high;
[0006] Chinese patent CN95113103.6-Preparation method of biuret-containing polyisocyanate discloses a method for preparing biuret in a batch tank reactor. The raw material isocyanate and catalyst are preheated to 130°C, and then water in a finely dispersed form is introduced. After the reaction reaches the set conversion rate, the reaction is stopped, and the monomer is separated to obtain qualified products; the process adopts batch reaction, and the process belongs to the total mixed flow reaction, the residence time distribution is wide, and the product viscosity is high; the raw materials need to be preheated before the reaction, and the reaction Process raw materials need to be fed into circulating water to remove reaction heat, resulting in waste of energy
This method uses multiple reactors connected in series and reacts in the form of water vapor. Although the residence time distribution is partially reduced, the adjustability is poor, the reaction temperature is too high, the product viscosity is high, and the chroma is high.

Method used

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  • Method for preparing biuret polyisocyanates
  • Method for preparing biuret polyisocyanates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Prepare the mixed solution of hexamethylene diisocyanate and catalyst diethyl phosphate and piperazine, the temperature is 25 ℃, wherein the consumption of diethyl phosphate and piperazine is 0.6wt% based on hexamethylene diisocyanate, wherein phosphoric acid The mass ratio of diethyl ester and piperazine is 5:1, and the mixed solution is continuously pumped into the built-in heat exchanger 6 with a flow rate of 110kg / h, and then preheated by the built-in heat exchanger 6 to obtain preheated isocyanate Raw material 2, the reaction temperature in the bubble column reactor is 130°C, the mass ratio of water vapor and nitrogen is 1:1, the flow rate is 3.6kg / h, the temperature of the water vapor and nitrogen mixer is 165°C; the circulating reaction solution 5 The ratio of raw material liquid (raw material isocyanate and catalyst mixed raw material 1 or preheated isocyanate raw material 2) is 10:1, and the average residence time of the reaction liquid in the bubble column reac...

Embodiment 2

[0058] Prepare a mixed solution of hexamethylene diisocyanate and catalyst diethyl phosphate and triethylene diamine at a temperature of 25°C, wherein the amount of diethyl phosphate and triethylene diamine is 1 wt% of the mass of hexamethylene diisocyanate , wherein the mass ratio of diethyl phosphate and triethylenediamine is 9:1, the mixed solution is continuously pumped into the built-in heat exchanger 6, the flow rate is 110kg / h, and then preheated by the built-in heat exchanger 6 to obtain For the preheated isocyanate raw material 2, the reaction temperature in the bubble column reactor is 110°C, the mass ratio of water vapor to nitrogen is 1:1, the flow rate is 3.6kg / h, and the temperature of the water vapor and nitrogen mixer is 105°C ; The ratio of circulating reaction liquid 5 to raw material liquid (raw material isocyanate and catalyst mixed raw material 1 or preheated isocyanate raw material 2) is 2:1, and the average residence time of the reaction liquid in the bub...

Embodiment 3

[0060] Prepare a mixed solution of hexamethylene diisocyanate and catalyst diethyl phosphate and imidazole at a temperature of 25°C, wherein the amount of diethyl phosphate and imidazole is 1.05wt% of the mass of hexamethylene diisocyanate, wherein diethyl phosphate The mass ratio of ester and imidazole is 20:1, and the mixed solution is continuously pumped into the built-in heat exchanger 6 with a flow rate of 110kg / h, and then the preheated isocyanate raw material 2 is obtained after being preheated by the built-in heat exchanger 6, The reaction temperature in the bubble column reactor is 100°C, the mass ratio of water vapor and nitrogen is 1:1, the flow rate is 3.6kg / h, the temperature of the water vapor and nitrogen mixer is 100°C; the circulating reaction liquid 5 and the raw material liquid (The ratio of raw material isocyanate and catalyst mixed raw material 1 or preheated isocyanate raw material 2) is 1:5, the average residence time of the reaction liquid in the bubble ...

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Abstract

The invention discloses a method for continuously preparing biuret polyisocyanates. Isocyanate is subjected with water vapor in a bubble tower under the effect of a catalyst. A reaction solution passes through an evaporator and the unreacted isocyanate monomer is separated out to obtain the biuret polyisocyanates. By compounding the catalysis effect of the catalyst and adjusting the average residence time of the bubble tower, the product chromaticity and viscosity can be effectively lowered; a special built-in heat exchanger is utilized for preheating a reaction raw material, reaction temperature control and energy integration are achieved, and energy consumption is lowered.

Description

technical field [0001] The invention relates to a method for preparing biuret polyisocyanate, in particular to a method for preparing biuret polyisocyanate by reacting diisocyanate and water vapor in a bubble tower under the action of a catalyst. Background technique [0002] Biuret polyisocyanate is widely used in the production of coatings, adhesives, sealants, waterproofing agents, foams, elastomers, fiber treatment agents, etc. Patent document DE1101394B published in 1958 has disclosed a method for preparing aliphatic polyisocyanate having a biuret structure. The review paper The Synthesis of Aliphatic Polyisocyanates Containing Biuret, isocyanurate oruret dione backbones for use in coatings (for the synthesis of aliphatic polyisocyanates containing biuret, isocyanurate or uretdione backbone for coatings, J.prakt.Chem, 336, 1994, 185-200) discloses further possible preparation methods and discusses the advantages and disadvantages of these particular methods. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/62C07C273/18B01J31/02
CPCC07C273/1872B01J31/0235B01J31/0258B01J35/19C07C275/62
Inventor 石滨尚永华李海军王彪胡展黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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