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The preparation method of 3-chloromethyl-3-ethyl oxetane

A technology of oxetane and chloromethyl, applied in the field of preparation of 3-chloromethyl-3-ethyl oxetane, can solve the problem of high preparation cost, reduce preparation cost and improve utilization rate , the effect of efficient use

Active Publication Date: 2022-04-22
CHANGZHOU TRONLY NEW ELECTRONICS MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The main purpose of the present invention is to provide a preparation method of 3-chloromethyl-3-ethyl oxetane, to solve the problem of high preparation cost in the existing preparation method of oxetane monomers

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0014] As described in the background technique, the existing preparation method of oxetane monomer has the problem of high preparation cost. In order to solve the above technical problems, the present application provides an industrial 3-chloromethyl-3-ethyl oxetane compound preparation method, the preparation method comprising: the molten trimethylolpropane into the hydrogen chloride gas for chlorination reaction, to obtain a mixture system containing monochlorolate and dichlorolate, hydrogen chloride gas per hour through weight of trimethylolpropane input weight of 2 ‰ ~ 13 ‰; rectification separation of the above mixture system to obtain dichloro intermediates and monochloros containing mother liquor The above-mentioned dichloroser intermediates are cyclic reaction, to obtain the 3-chloromethyl-3-ethyl oxetane product; the mother liquor containing monochlorolate is directly applied to the next batch of reactions to replace trimethylolpropane in a medium amount, and the hydroge...

Embodiment 1

[0027] The reactor is put into trimethylolpropane 1340Kg, adipic acid 100Kg, heated to 80 °C, after trimethylolpropane melting, turn on stirring, increase the temperature and control the internal temperature in the reactor at 130 °C, begin to pass into hydrogen chloride gas, hydrogen chloride gas ventilation is controlled at 13Kg / h (9.7 ‰), reaction under atmospheric pressure 58h, gas chromatography (GC) control, monochlorose conversion rate of 35%, dichlorose conversion rate of 61%, end of the reaction.

[0028] By distilling the dichlorobiate by the distillation column, where the control vacuum is 8mmHg, the temperature is 140 °C, the fraction below 95 °C is collected, and the dichlorogenate is obtained 940Kg, the purity is 97%, and the yield is 92%; the remaining mother liquor 725Kg is directly applied to the next batch of production, and the utilization rate of hydrogen chloride in the process is 77%.

[0029] The reactor was put into 1740Kg of dichlorolate, crown ether 2.2Kg,...

Embodiment 2

[0031] The reactor is put into the distillation remaining mother liquor in Example 1 725Kg, and then put into trimethylolpropane 615Kg, heated to 80 ° C, after the trimethylolpropane melts to open the stirring, increase the temperature control internal temperature at 130 ° C, begin to pass into hydrogen chloride gas, hydrogen chloride gas ventilation amount controlled at 13Kg / h (9.7 ‰), atmospheric pressure reaction, reaction 58h, GC central control, monochlorose conversion 34%, dichloros conversion rate of 60%, end of the reaction.

[0032] By distilling dichlorolate by distillation column, controlling vacuum 8mmHg at a temperature of 140 °C, collecting fractions below 95 °C to obtain dichlorohydrogen 925Kg, purity 97%, yield 91%; the remaining mother liquor 745Kg is directly applied to the next batch of production, and the utilization rate of hydrogen chloride in the process is 77%.

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Abstract

The invention provides a preparation method of 3-chloromethyl-3-ethyloxetane. The preparation method comprises: feeding hydrogen chloride gas into molten trimethylolpropane for chlorination reaction to obtain a mixture system containing monochloride and dichloride, and the weight of hydrogen chloride gas per hour is trimethylolpropane Put in 2‰~13‰ of the total weight; rectify and separate the above mixture system to obtain the dichloride intermediate and the mother liquor containing monochloride; the above dichloride intermediate undergoes a ring closure reaction to obtain 3-chloromethyl-3 ‑Ethyl oxetane product; the mother liquor containing monochloride is directly applied to the chlorination reaction of the next batch of reactions. By limiting the ventilation rate of hydrogen chloride, the utilization rate of hydrogen chloride is improved; the dichloride produced by the reaction can continue to react to produce products, and the residual mother liquor is used as the raw material of the chlorination reaction again, so as to realize the efficient utilization of hydrogen chloride and trimethylolpropane. Reduce preparation costs.

Description

Technical field [0001] The present invention relates to the field of organic synthesis, in particular, to a method for preparing 3-chloromethyl-3-ethyloxyxabutane. Background [0002] Oxetane monomer is one of the key components in the current formulation of cationic systems, with excellent application performance and huge market prospects. 3-Chloromethyl-3-ethyloxetane in the preparation of oxetane monomers It is the most important intermediate, and it is also an indispensable factor to solve the problem of the cost of oxetane monomers. 3-Chloromethyl-3-ethyloxyxabutane conventional production methods need to use highly toxic sulfonates, with the increasingly stringent requirements of environmental protection, the original production methods are difficult to ensure normal production, and operating costs increase sharply, resulting in declining production capacity. At present, there is a hydrogen chloride process to replace the original sulfonate process to prepare 3-chlorometh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/06
CPCC07D305/06
Inventor 钱晓春翁云峰马丽君胡春青衡京
Owner CHANGZHOU TRONLY NEW ELECTRONICS MATERIALS