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A kind of method for preparing m-xylylene diisocyanate

A technology of m-xylylene diisocyanate and m-xylylene diurethane, which is applied in the field of compound preparation, can solve the problem of low yield of 1,6-hexamethylene diisocyanate, high price of ionic liquid, The product yield is not high, and the effect of easy industrialization and automation, low cost and easy separation is achieved

Active Publication Date: 2021-03-19
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN101195590A discloses a method for preparing 1,6-hexamethylene diisocyanate by liquid-phase pyrolysis of methyl hexamethylene dicarbamate. The ionic liquid is used as the reaction solvent and the supported metal oxide is used as the catalyst. The main method of the method is It is characterized by mild reaction conditions, clean, green, and low volatility, but the ionic liquid is expensive and difficult to remove in the later stage, and the yield of 1,6-hexamethylene diisocyanate prepared by it is not high
Using this material as a catalyst has the advantages of easy separation from the reaction solution and reusability, but the catalyst is easily deactivated, and the yield of the prepared product is not high
[0009] CN105143177A discloses a method for producing xylylene diisocyanate. After the product xylylene diisocyanate is separated from alcohols and solvents, the solvent is directly taken out and mixed with fresh xylylene diaminocarbonate for recycling. In this way, the residual xylylene diisocyanate in the solvent is polymerized and accumulated in the solvent, causing the solvent to deteriorate easily and cannot be used normally, and the yield of the product is not high

Method used

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  • A kind of method for preparing m-xylylene diisocyanate
  • A kind of method for preparing m-xylylene diisocyanate

Examples

Experimental program
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Effect test

Embodiment 1-29

[0037] The present embodiment prepares m-xylylene diisocyanate, and its preparation method comprises the steps:

[0038] Adopt 1000mL reactor as thermal decomposition reactor, and x g ethyl m-xylylene dicarbamate, yg solvent A, z g catalyst B are added to reactor, seal reactor, start stirring, control pressure is a MPa, temperature is b°C, and a thermal decomposition reaction is carried out under cmL / min nitrogen purging for t min to obtain the m-xylylene diisocyanate.

[0039] In the preparation method of embodiment 1-29, the concrete numerical value of each parameter and the conversion ratio of raw material xylylene diurethane (XDC), the yield of m-xylylene diisocyanate (XDI) are as table 1 and Table 2 shows.

Embodiment 30

[0041] The present embodiment carries out enlarged preparation m-xylylene diisocyanate, and its preparation method comprises the following steps:

[0042] A 100L reactor was used as a thermal decomposition reactor, and 6.5Kg of ethyl m-xylylenedicarbamate, 58.5Kg of o-dichlorobenzene, and 0.65Kg of zinc oxide were added to the reactor, and the reactor was sealed, stirred, and the pressure was controlled. The temperature is 0.75MPa, the temperature is 270°C, and the thermal decomposition reaction is carried out under 50L / min nitrogen purging for 120min to obtain the m-xylylene diisocyanate.

[0043] The yield of m-xylylene diisocyanate (XDI) prepared in Examples 1-30 and the conversion rate of the raw material m-xylylene diurethane (XDB) are shown in Table 1 and Table 2.

[0044] Table 1

[0045]

[0046] Table 2

[0047]

[0048] According to the data of Table 1 and Table 2, it can be known that: comparative example 1 and embodiment 21-25, the mass percent concentratio...

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Abstract

The invention relates to a method used for preparing m-xylylene diisocyanate. The method comprises following steps: m-xylylene diamino ethyl formate is dissolved in an organic solvent, under protective gas purging, thermal decomposition reaction is carried out so as to obtain the m-xylylene diisocyanate. The preparation technology is simple and convenient, is friendly to the environment, is low incost, and is capable of realizing amplification production; the adopted reaction solvent can be recycled; and the product yield is high.

Description

technical field [0001] The invention relates to the field of compound preparation, and relates to a method for preparing m-xylylene diisocyanate. Background technique [0002] The special isocyanate m-xylylene diisocyanate (XDI) has both aromatic and aliphatic structures, and a methylene group is introduced between the benzene ring and the isocyanate group, so that the polyurethane products made from it have no yellowing Therefore, it is mainly used in various anti-yellowing coatings, high-grade polyurethane elastomers, polyurethane leather, and high-grade polyurethane ophthalmic lenses. At present, XDI, as a relatively large isocyanate, has considerable demand in both the international market and the domestic market. [0003] The traditional production process of XDI is to use m-xylylenediamine (XDA) phosgenation to form salt at low temperature. XDA first reacts with dry hydrogen chloride or carbon dioxide to form salt, and then reacts with gaseous phosgene at an appropria...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C263/04C07C265/08
CPCC07C263/04C07C265/08
Inventor 王利国李会泉陈家强曹妍贺鹏周俊雅
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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