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Method for continuously synthesizing hexamethylene diisocyanate tripolymer

A technology of hexamethylene diisocyanate and trimer, which is applied in the field of continuous synthesis of hexamethylene diisocyanate trimer, can solve the problem of low quality of HDI trimer finished product, low catalytic efficiency of catalyst and technological process. Complex problems, to achieve the effect of easy industrialization, saving raw material costs, and simple process

Pending Publication Date: 2022-07-01
NINGXIA RUITAI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of the synthesis method of HDI trimer, such as low catalytic efficiency of catalyst, complex process flow, high consumption of raw materials, and low quality of finished HDI trimer, the application provides a continuous synthesis of hexamethylene diisocyanate trimer The overall method has the advantages of high catalytic efficiency, simple process, low consumption of polymerization inhibitor, high quality of finished product, and easy engineering implementation, including the following steps:

Method used

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  • Method for continuously synthesizing hexamethylene diisocyanate tripolymer
  • Method for continuously synthesizing hexamethylene diisocyanate tripolymer
  • Method for continuously synthesizing hexamethylene diisocyanate tripolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Under the catalysis of catalyst, hexamethylene diisocyanate is continuously synthesized to obtain hexamethylene diisocyanate (Hexamethylene Diisocyanate, HDI) trimer, and the reaction equation is such as figure 2 shown.

[0034] Process such as image 3 shown. The spherical silica particles containing the solid catalyst are filled into the tubular reactor to form a particle bed as a catalyst, wherein the aspect ratio of the tubular reactor is 5 to 20:1, and the diameter of the spherical particles containing the solid catalyst is 4 ~10mm, the porosity of the particle bed is 0.3~0.5, the volume ratio of the particle bed to the tubular reactor is 0.7~0.9, the solid catalyst is a kind of carboxylate and alkoxide, preferably potassium acetate, calcium acetate, propylene Potassium acetate, sodium acetate, cobalt acetate, zirconium ethoxide, titanium ethoxide, potassium ethoxide, calcium ethoxide.

[0035]The hexamethylene diisocyanate (HDI) preheated to 30~150℃ and nitrog...

Embodiment 2

[0038] The mesoporous silica supported potassium acetate was used as the catalyst, and the diameter of the catalyst particles was 5 mm. The height-diameter ratio of the tubular reactor is selected to be 10, the void ratio of the particle bed is 0.4, and the volume ratio of the particle bed to the tubular reactor is 0.85.

[0039] The internal temperature of the tubular reactor was 80°C. The HDI was preheated to 80°C for the feed, and the amount of nitrogen introduced per minute was 0.6 times the void volume of the tubular reactor. The reaction residence time was controlled to be 5h. The conversion rate of HDI is 60%, and the crude product of HDI trimer overflows to the transition tank.

[0040] Add dibutyl phosphate 0.0003 times the mass of the overflow material to the transition tank every hour. The synthetic liquid in the transition tank was passed through a thin film evaporator and a molecular distiller successively, and the temperature of the thin film evaporator was co...

Embodiment 3

[0043] The mesoporous silica supported calcium ethoxide was used as the catalyst, and the diameter of the catalyst particles was 5 mm. The height-diameter ratio of the tubular reactor is selected to be 10, the void ratio of the particle bed is 0.4, and the volume ratio of the particle bed to the tubular reactor is 0.85.

[0044] The internal temperature of the tubular reactor was 80°C. The HDI was preheated to 80°C for the feed, and the amount of nitrogen introduced per minute was 0.6 times the void volume of the tubular reactor. The reaction residence time was controlled to be 5h. The conversion rate of HDI is 60%, and the crude product of HDI trimer overflows to the transition tank.

[0045] Add dibutyl phosphate 0.0003 times the mass of the overflow material to the transition tank every hour. The synthetic liquid in the transition tank was passed through a thin film evaporator and a molecular distiller successively, and the temperature of the thin film evaporator was con...

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Abstract

The invention discloses a method for continuously synthesizing a hexamethylene diisocyanate tripolymer. The method comprises the following steps: preheating hexamethylene diisocyanate (hereinafter referred to as HDI), enabling the preheated hexamethylene diisocyanate to flow through a tubular reactor containing solid catalyst particles, controlling the temperature, and introducing nitrogen to promote a polymerization reaction of materials; when the HDI conversion rate reaches a specified value, HDI is continuously added into the reactor, and meanwhile, synthetic liquid overflows out. And adding a small amount of polymerization inhibitor into the synthetic liquid, and sequentially passing through a film evaporator and a molecular distiller to obtain an HDI tripolymer finished product. According to the method, the HDI tripolymer is synthesized by taking the catalyst as a stationary phase and the HDI material flow as a continuous phase, so that the separation of the catalyst and the HDI tripolymer material flow is facilitated. Meanwhile, further polymerization of HDI can be prevented only by adding a small amount of polymerization inhibitor, and the raw material cost of the polymerization inhibitor is saved. The method has the advantages of simple process, high catalytic efficiency and easiness in industrial implementation.

Description

technical field [0001] The present application relates to the field of fine chemicals, in particular to a method for continuous synthesis of hexamethylene diisocyanate trimer. Background technique [0002] Hexamethylene diisocyanate (HDI) trimer is a polyisocyanate curing agent formed by self-polymerization of HDI under the action of a catalyst. It has the advantages of low volatility, low toxicity and high functionality. Therefore, it is widely used as a curing crosslinking agent. Polyurethane coatings and adhesives. The theoretical functionality of the HDI trimer is 3, and the mass fraction of isocyanate is 25%. Due to the selectivity of the catalyst and the limitation of the reaction conditions, the HDI trimer product usually prepared by the method is a mixture of multiple components. More than 3, the mass fraction of isocyanate groups is less than 25%. [0003] In the technical aspect of preparing HDI trimer, the difficulty is to find an efficient catalyst for trimeriz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/30
CPCC07D251/30
Inventor 刘勇朱斌张金财摆永明党大徽赵芙蓉
Owner NINGXIA RUITAI TECH
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