Method for preparing hexamethylbenzene by using cardanol and methanol as raw materials

A technology for hexamethylbenzene and cardanol, which is applied in the field of preparing hexamethylbenzene, can solve the problems of high requirements on reaction conditions, waste of raw materials and high energy consumption, and achieves the effects of low price, mild process conditions and excellent performance

Active Publication Date: 2017-11-07
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production method not only requires high reaction conditions and high energy consumption, but also has a low yield, wastes raw materials and produces a large amount of three wastes

Method used

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  • Method for preparing hexamethylbenzene by using cardanol and methanol as raw materials
  • Method for preparing hexamethylbenzene by using cardanol and methanol as raw materials
  • Method for preparing hexamethylbenzene by using cardanol and methanol as raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of hexamethylbenzene from cardanol and methanol:

[0042] (1) Add 5g of 20-40 mesh granular solid catalyst in the reaction tube, place it in a tubular heating furnace, heat it to 300°C, feed nitrogen, and the pressure is normal pressure;

[0043] (2) Cardanol and methanol are mixed at a volume ratio of 1:1 and then pumped into the nitrogen flow through the material, and the mixed gas-liquid material enters the fixed-bed catalytic reactor, and reacts at a temperature of 300 ° C to generate hexamethylbenzene;

[0044] (3) The above-mentioned crude product hexamethylbenzene is recrystallized, and the solvent used for recrystallization purification is dichloromethane and benzene to obtain the finished product of hexamethylbenzene, and its target selectivity (mass ratio of hexamethylbenzene in the crystallization product) ) was 27.9%; product (crystal product) yield was 82.3%.

Embodiment 2

[0046] Preparation of hexamethylbenzene from cardanol and methanol:

[0047] (1) Add 5g of 20-40 mesh granular solid catalyst into the reaction tube, place it in a tubular heating furnace, heat it to 350°C, feed nitrogen, and the pressure is normal pressure;

[0048] (2) Cardanol and methanol are mixed at a volume ratio of 1:1 and then pumped into the nitrogen stream through the material, and the mixed gas-liquid material enters the fixed-bed catalytic reactor, and reacts at a temperature of 350 ° C to generate hexamethylbenzene;

[0049] (3) Recrystallize the above-mentioned crude product hexamethylbenzene, and the solvents used for recrystallization and purification are dichloromethane and benzene to obtain finished hexamethylbenzene with a target selectivity of 96.1% and a product yield of 80.7%.

Embodiment 3

[0051] Preparation of hexamethylbenzene from cardanol and methanol:

[0052] (1) Add 5g of 20-40 mesh granular solid catalyst into the reaction tube, place it in a tubular heating furnace, heat it to 400°C, feed nitrogen, and the pressure is normal pressure;

[0053] (2) Cardanol and methanol are mixed at a volume ratio of 1:1 and then pumped into the nitrogen stream through the material, and the mixed gas-liquid material enters the fixed-bed catalytic reactor, and reacts at a temperature of 400 ° C to generate hexamethylbenzene;

[0054] (3) Recrystallize the crude product of hexamethylbenzene to obtain the finished product of hexamethylbenzene. The solvents used for recrystallization and purification are dichloromethane and benzene, and the target selectivity is 98.9%; the product yield is 73.6%.

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Abstract

The present invention relates to a method for preparing hexamethylbenzene by using cardanol and methanol as raw materials. The method comprises: B, introducing nitrogen gas into a fixed bed reactor filled with a catalyst; and C, feeding the mixed solution of cardanol and methanol into the nitrogen gas flow, mixing, making the formed gas-liquid mixture enter the fixed bed reactor filled with the catalyst, and carrying out a reaction to generate the hexamethylbenzene, wherein a volume ratio of cardanol to methanol is 5:1-1:5. According to the present invention, the used raw material cardanol has advantages of regeneration, low price, excellent performance, rich source and the like; the hexamethylbenzene obtained through the production process has high selectivity, wherein the selectivity can achieve 98.9%, and the product yield can achieve 82.3%; the generated by-product and the generated three-wastes are less; the production process and the operation are simple, and the method can be achieved only with the one-step reaction; and the reaction conditions are mild, the pressure is the normal pressure, and the great advantages are provided in the economy and the safety.

Description

technical field [0001] The invention belongs to the field of industrial catalysis, and in particular relates to a method for preparing hexamethylbenzene by using cardanol and methanol as raw materials. Background technique [0002] Hexamethylbenzene, colorless flaky crystal. The melting point is 166-167°C (165.5°C), the boiling point is 265°C, and the relative density is 1.0630 (25 / 4°C). It is easily soluble in ethanol and benzene, soluble in ether, acetone and acetic acid, and insoluble in water. It has important applications in the field of fine chemicals. Due to the special symmetry and stability of hexamethylbenzene, it is often used as an internal standard substance in analytical chemistry, such as the determination of the magic angle in physics and the determination of pollutants in atmospheric aerosols. Hexamethylbenzene can form complexes with many metal compounds, and is an important ligand for research and development of catalysts. For example, cyclopentadiene hex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C1/20C07C15/02
CPCC07C1/20C07C2521/04C07C15/02
Inventor 方云明王晨曦陈必强孟达
Owner BEIJING UNIV OF CHEM TECH
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