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Preparation method of high-purity double-bond liquid crystal monomer

A liquid crystal monomer, high-purity technology, applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve the problems of material waste, insufficient reaction, excessive raw materials, etc., achieve high product purity, reduce by-product formation, and reduce waste liquid The effect of emissions

Inactive Publication Date: 2018-09-21
江苏创拓新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantages of this production method are: the temperature in the reactor is not uniform, and the reaction is not sufficient; in order to ensure the purity of the reaction product, the raw material needs to be excessive, resulting in material waste; at the same time, the purity of the synthesized liquid crystal monomer is not satisfactory

Method used

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  • Preparation method of high-purity double-bond liquid crystal monomer
  • Preparation method of high-purity double-bond liquid crystal monomer
  • Preparation method of high-purity double-bond liquid crystal monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]

[0033] (1) Weigh 236g of a1 in a container, add tetrahydrofuran to dissolve, and determine the final volume as 500mL.

[0034] (2) Add 358g of methyltriphenylphosphine bromide and an appropriate amount of tetrahydrofuran into a 2L glass reactor, under nitrogen protection, add 109.8g of potassium tert-butoxide at 0-5°C under stirring, and stir for 0.5h after the addition, the final volume It is 500mL, and the ylide reagent is prepared under nitrogen protection.

[0035] (3) Two groups of metering pumps are pumped into the microreactor respectively, the flow rate is 0.02mL / min, preheated by the preheating module, and then enter the mixing module for reaction, after mixing and reacting in the mixing module, continue After entering a series of reaction modules, after the reaction is completed, the product flows out from the outlet of the reactor, and then processed after cooling. During the reaction process, the reaction residence time in the microreactor is 90s, and ...

Embodiment 2

[0038]

[0039] (1) Weigh 236kg of a1 in a container, add tetrahydrofuran to dissolve, and determine the final volume as 500L.

[0040] (2) Add 372 kg of ethyltriphenylphosphine bromide and an appropriate amount of tetrahydrofuran into a 1000L tank reactor, under nitrogen protection, add 110 kg of potassium tert-butoxide at 0-5°C under stirring, and stir for 0.5 hours after the addition, the final volume It is 500L, and the ylide reagent is prepared under nitrogen protection.

[0041] (3) Two sets of metering pumps are pumped into the microreactor respectively, and the flow rate is 30L / min. After preheating through the preheating module, it enters the mixing module for reaction. After mixing and reacting in the mixing module, continue to enter the A series of reaction modules, after the reaction is completed, the product flows out from the outlet of the reactor, and then processed after cooling. During the reaction process, the reaction residence time in the microreactor i...

Embodiment 3

[0044]

[0045] (1) Weigh 306g of a3 in a container, add tetrahydrofuran to dissolve, and determine the final volume to be 500mL.

[0046] (2) Add 358g of methyl triphenylphosphine bromide and an appropriate amount of tetrahydrofuran into a 2L glass reactor, under nitrogen protection, add 109.8g of potassium tert-butoxide at 0-5°C under stirring, stir for 0.5h after the addition, and the final volume It is 500mL, and the ylide reagent is prepared under nitrogen protection.

[0047] (3) Two groups of metering pumps are pumped into the microreactor respectively, and the flow rate is 0.04mL / min, which is preheated through the preheating module, and then enters the mixing module for reaction. After mixing and reacting in the mixing module, continue to After a series of reaction modules, after the reaction is completed, the product flows out from the outlet of the reactor, and then processed after cooling. During the reaction process, the reaction residence time in the microrea...

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Abstract

The invention relates to a preparation method of a high-purity double-bond liquid crystal monomer, wherein the monomer is prepared from a carbonyl compound through Ylide reaction, wherein the Ylide reaction is carried out in a micro reactor; the carbonyl compound is a compound of formula I. Compared with conventional reactions, the preparation method that is of continuous mode instead of intermittent mode has the advantages that waste liquid emission and byproduct production are decreased, and product purity is very high, up to 99% and above.

Description

technical field [0001] The invention belongs to the field of liquid crystal materials, and relates to a preparation method of a liquid crystal monomer, in particular to a preparation method of a high-purity double bond-containing liquid crystal monomer. Background technique [0002] With the application of liquid crystal display devices more and more widely, liquid crystal display technology is developing towards high response speed. However, high response speed requires liquid crystal composition to have low viscosity, on this basis, the use of low viscosity liquid crystal monomer becomes the main direction. Among them, the cyclohexane olefin liquid crystal monomer has low viscosity and good physical and chemical properties, which can realize fast response and improve the low-temperature stability of the mixed liquid crystal. [0003] This type of liquid crystal monomer is usually prepared in a conventional reactor, and then the carbonyl compound solution is added dropwise...

Claims

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Application Information

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IPC IPC(8): C09K19/30
CPCC09K19/3003C09K2019/3004C09K2019/301
Inventor 靳灿辉丁兴立孙仲猛谭玉东
Owner 江苏创拓新材料有限公司
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