Flexible liquid crystal intermediate trans p-alkyl dicyclohexyl methanol benzene and preparation method thereof

A flexible liquid crystal and dicyclohexyl technology, which is applied in the field of liquid crystal raw material preparation, can solve the problems affecting the use of alkylbenzene dicyclohexyl carbinol, low purity of alkyl benzene dicyclohexyl carbinol, and difficulty in purification, so as to improve the service life and eliminate acetic acid. Generate and reduce the effect of equipment cost

Inactive Publication Date: 2014-06-25
SHIJIAZHUANG CROWN DISPLAY MATERIAL
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the trans-p-alkylbenzenebicyclohexylmethanol prepared by the existing preparation method has low purity and contains by-product acetic acid, and further purification is very difficult, which seriously affects the application of trans-p-alkylbenzenebicyclohexylcarbinol in the field of liquid crystals. use

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method for a flexible liquid crystal intermediate trans-para-alkylbenzene bicyclohexylmethanol, comprising the following steps:

[0029] The following parts are parts by weight;

[0030] A. Feeding: Add 200g of trans-formaldehyde and 1000g of tetrahydrofuran into the reaction vessel and stir, add 400g of absolute ethanol after dissolving, and then cool down in an ice-salt bath; the raw materials used in the ice-salt bath include 400g of sodium chloride and 300g of NH4CNS .

[0031] B. Dropping: use the dropping liquid prepared by 70g of potassium borohydride and 600g of distilled water to add dropwise to the solution prepared in step A; the temperature of the dropping process is controlled at 23°C to 24°C.

[0032] C. Stirring: remove the ice-salt bath, and stir at room temperature for 2 hours.

[0033] D. Neutralization: Use 2500g of distilled water and 200g of concentrated hydrochloric acid to prepare a neutralization solution, add the solution prepare...

Embodiment 2

[0041] A preparation method for a flexible liquid crystal intermediate trans-para-alkylbenzene bicyclohexylmethanol, comprising the following steps:

[0042] The following parts are parts by weight;

[0043] A. Feeding: Add 400g of trans-formaldehyde and 2000g of tetrahydrofuran into the reaction vessel to stir, add 700g of absolute ethanol after dissolving, and then cool down in an ice-salt bath; the raw materials used in the ice-salt bath include 350 parts of CaCl2 6H2O and 650 parts of NH4CNS.

[0044] B. Dropping: use the dropping liquid prepared by 150g of potassium borohydride and 1000g of distilled water to add dropwise to the solution prepared in step A; the temperature of the dropping process is controlled at 20°C to 21°C.

[0045] C. Stirring: remove the ice-salt bath, and stir at room temperature for 4 hours.

[0046] D. Neutralization: Use 3500g of distilled water and 300g of concentrated hydrochloric acid to prepare a neutralization solution, add the solution pr...

Embodiment 3

[0054] A preparation method for a flexible liquid crystal intermediate trans-para-alkylbenzene bicyclohexylmethanol, comprising the following steps:

[0055] The following parts are parts by weight;

[0056] A. Feeding: Add 372g of trans-formaldehyde and 1780g of tetrahydrofuran into the reaction vessel to stir, add 632g of absolute ethanol after dissolving, and then cool down in an ice-salt bath; the raw materials used in the ice-salt bath include 300 parts of CaCl2 6H2O and 550 parts NH4CNS.

[0057]B. Dropping: use the dropping liquid prepared by 100g of potassium borohydride and 800g of distilled water to add dropwise to the solution prepared in step A; the temperature of the dropping process is controlled below 20°C.

[0058] C. Stirring: remove the ice-salt bath, and stir for 3 hours at room temperature.

[0059] D. Neutralization: Use 3000g of distilled water and 243g of concentrated hydrochloric acid to prepare a neutralization solution, add the solution prepared in ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for preparing a flexible liquid crystal intermediate trans p-alkyl dicyclohexyl methanol benzene. The method includes the following steps: A, mixing transformaldehyde, tetrahydrofuran and absolute ethyl alcohol, and cooling by using ice-salt bath; B, dripping by using a potassium borohydride solution; C, removing the ice-salt bath, and stirring at room temperature; D, adding a hydrochloric acid solution for neutralizing; E, adding dichloromethane for layering; F, extracting the separated water layer by using dichloromethane; G, washing the extraction liquid by using a sodium carbonate solution, and then drying the same by using anhydrous sodium sulfate; H, normal pressure distilling; I, adding petroleum ether for solution, and then cooling to crystallize; and J, carrying out suction filtering and purifying the crystal to obtain a white crystal finished product. By adopting the method, the defects of the prior art are solved, the purity of the finished product of flexible liquid crystal intermediate trans p-alkyl dicyclohexyl methanol benzene is improved, and the generation of acetic acid is avoided. In addition, the invention further provides trans p-alkyl dicyclohexyl methanol benzene prepared by the method.

Description

technical field [0001] The invention relates to the technical field of preparation of liquid crystal raw materials, in particular to a flexible liquid crystal intermediate trans-para-alkylbenzenebicyclohexylmethanol and a preparation method thereof. Background technique [0002] With the popularization of liquid crystal technology, more and more liquid crystal materials are used in various display devices. As a liquid crystal material with good electrical properties, miscibility, and large optical anisotropy, the flexible liquid crystal intermediate trans-p-alkylbenzenebicyclohexylmethanol is one of the preferred raw materials for liquid crystal products. However, the trans-p-alkylbenzenebicyclohexylmethanol prepared by the existing preparation method has low purity and contains by-product acetic acid, and further purification is very difficult, which seriously affects the application of trans-p-alkylbenzenebicyclohexylcarbinol in the field of liquid crystals. use. Conten...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/34C07C29/09C07C29/14C07C29/00
CPCC07C29/38C07C33/34C07C2601/14
Inventor 聂文超杨树华王华玉古春雷
Owner SHIJIAZHUANG CROWN DISPLAY MATERIAL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap