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Production process for biphenylnitrile type liquid crystal material

A technology of liquid crystal material and production process, which is applied in the field of production process of biphenyl nitrile liquid crystal material, can solve problems such as limited supply of catalyst market, unsatisfactory resistivity, unqualified product color, etc., and achieve easy industrialized mass production, The effect of less by-products and easy handling

Inactive Publication Date: 2012-09-19
HANGZHOU CHEMORGANIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature has also reported the coupling reaction of Grignard reagents prepared by some alk(oxy)-based brominated biphenyls with p-bromoxynil under the catalysis of palladium acetate or nickel phosphorus ligands to prepare liquid crystal materials of this type of biphenylnitrile [WO 9730970 , CN101671271A], the actual scale-up experiments of these process methods show that there are many by-products, and the obtained products still need high-vacuum sublimation and column chromatography for purification, or the color and luster of the resulting products are unqualified, and the resistivity does not meet the requirements, or the catalyst market supply is limited or the price expensive etc.

Method used

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  • Production process for biphenylnitrile type liquid crystal material
  • Production process for biphenylnitrile type liquid crystal material

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Under the protection of nitrogen, put 10 mmoles of iodine, 10 moles of metal magnesium chips and 5 liters of anhydrous tetrahydrofuran into the reaction kettle in turn, heat and keep the reaction temperature of tetrahydrofuran reflux, drop 10 moles of 4-n-butylchlorobenzene Add in the above-mentioned reaction kettle, dropwise time is 12 hours, continue reflux reaction 2 hours after dropwise addition and make the tetrahydrofuran solution of corresponding 4-n-butanyl phenylmagnesium chloride Grignard reagent; Then put the above-mentioned Grignard reagent The tetrahydrofuran solution was dripped into a reaction kettle containing 0.5 moles of manganese dichloride, 10 moles of 4-bromoxynil and 5 liters of anhydrous tetrahydrofuran under the protection of nitrogen. The dropping temperature was 0°C, and the dropping time was 8 hours. After the addition is complete, continue the heat preservation reaction for 2 hours to end the reaction, filter and recover the metal salt, carry ...

Embodiment 2

[0022] Under the protection of nitrogen, put 15 mmoles of iodine, 10 moles of magnesium metal chips and 5 liters of anhydrous tetrahydrofuran into the reaction kettle in turn, heat and keep the reaction temperature of tetrahydrofuran reflux, add 9.8 moles of 4-ethylbromobenzene dropwise In the above-mentioned reaction kettle, the dropwise addition time is 4 hours, and after the dropwise addition, the reflux reaction is continued for 3 hours to obtain a tetrahydrofuran solution of the corresponding 4-ethylphenylmagnesium bromide Grignard reagent; then the above-mentioned Grignard reagent The tetrahydrofuran solution was dripped into a reaction kettle containing 0.5 moles of 1,1'-bis(diphenylphosphino)ferrocene nickel chloride, 10.5 moles of 4-bromoxynil and 5 liters of anhydrous tetrahydrofuran under nitrogen protection. The adding temperature is -10°C, the dropping time is 4 hours, and the reaction is continued for 2 hours after the dropping is completed, the metal salt is reco...

Embodiment 3

[0024] Under the protection of nitrogen, put 10 mmoles of iodine, 10 moles of magnesium metal chips and 5 liters of anhydrous tetrahydrofuran into the reaction kettle in turn, heat and keep the reaction temperature of tetrahydrofuran reflux, and drop 9.9 moles of 4-n-octylbromobenzene Add in the above-mentioned reaction kettle, dropwise time is 5 hours, continue reflux reaction for 3 hours after dropwise addition and make the tetrahydrofuran solution of corresponding 4-n-octylphenylmagnesium bromide Grignard reagent; Then put the above-mentioned Grignard The tetrahydrofuran solution of the reagent was dropped into a reaction kettle containing 0.5 moles of 1,1'-bis(diphenylphosphino)ferrocenepalladium chloride, 10 moles of 4-bromobenzonitrile and 5 liters of anhydrous tetrahydrofuran under nitrogen protection. , the dropping temperature is 5°C, the dropping time is 6 hours, after the dropping is completed, the insulation reaction is continued for 2 hours to end the reaction, the...

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Abstract

The invention discloses a production process for a biphenylnitrile type liquid crystal material. The production process comprises the following steps: firstly, reacting 4-N-alkyl halogenated benzene or 4-N-alkoxy halogenated benzene and metal magnesium powder in tetrahydrofuran under the protection of nitrogen gas to obtain a corresponding tetrahydrofuran solution of a Grignard reagent; secondly, dropping the tetrahydrofuran solution of the Grignard reagent into the tetrahydrofuran mixed solution containing a coupling reaction catalyst and 4-halogen-substitued cyanophenyl; after the reaction is ended, filtering and recovering metal salts; distilling to recover the solvent; carrying out rectification under vacuum and clay bleaching; and respectively recrystalizing with normal heptane and ethanol as solvent to obtain the biphenylnitrile type liquid crystal material. The production process disclosed by the invention has the advantages of low-priced and easily-accessible raw material, simple reaction, high yield, favorable quality of products, low production cost and the like, and is suitable for industrial production of biphenylnitrile type liquid crystal products.

Description

technical field [0001] The invention relates to a preparation process of a liquid crystal material, in particular to a production process of a biphenylnitrile type liquid crystal material. Background technique [0002] Liquid crystal is a mesomorphic substance with liquid fluidity and crystal anisotropy. Its application scope includes various types of displays and light valves, as well as medical diagnosis, gas chromatography, field strength detection, spectral analysis and environmental monitoring. In some small or portable devices such as mobile phones and laptop computers, liquid crystal displays have been in an absolute monopoly. The emergence of liquid crystal flat-panel color TV has made a breakthrough in the application of liquid crystal display. Due to the outstanding advantages of liquid crystal displays such as lightness, thinness, low power consumption and easy matching with integrated circuits, their application range is constantly expanding. Liquid crystal dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K19/12
Inventor 林旭锋石磊任炼军王俊
Owner HANGZHOU CHEMORGANIC
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