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Manufacturing method of alkyl benzene solvent and its application

A technology of alkylbenzene and solvent, which is applied in the field of preparation of alkylbenzene solvent, can solve the problems of isobutylene storage, inconvenient transportation, low chemical stability of solvent, low purity of alkylbenzene solvent, etc., and achieve shortened reaction time, High reactant selectivity and environmental friendliness

Inactive Publication Date: 2006-08-30
彭光辉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its main disadvantages are: (1) olefins are used as alkylating agents, using traditional catalysts such as sulfuric acid, aluminum trichloride or other Lewis acids, which is highly dangerous, and the utilization rate of isobutylene is not high and recovery is difficult; (2) isobutylene is prone to occur. (3) The raw material isobutylene is inconvenient to store and transport; (4) The purity of the obtained alkylbenzene solvent is not high, contains unsaturated groups, and the chemical stability of the solvent is not high
[0006] After retrieval, the research on the alkylation of aromatics is mainly concentrated in the two main fields of benzene alkylation to ethylbenzene and benzene alkylation to cumene, and there are few researches on the alkylation of p-xylene and ethylbenzene at home and abroad. to report

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  • Manufacturing method of alkyl benzene solvent and its application

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Experimental program
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Embodiment 1

[0029] (1) raw material: o-xylene 160Kg, purity is 99%, water content is 20ppm;

[0030] 140Kg of tert-butyl chloride, the purity is 99%, and the water content is 300ppm;

[0031] Catalyst: 1.65Kg of triethylamine hydrochloride, 3.3Kg of anhydrous aluminum trichloride.

[0032] (2) Preparation process

[0033] Put 160Kg of o-xylene, 3.3Kg of anhydrous aluminum trichloride, and 1.65Kg of triethylamine hydrochloride into the reaction kettle in turn, start stirring, add 140Kg of tert-butyl chloride, control the temperature at 20°C, and stir at constant temperature for 4 Hour. Follow up and analyze with gas chromatography according to the conventional method, stop stirring when reaching the end of the reaction, and separate the catalyst in the lower layer for future use. The reaction solution was washed with alkali and water according to the conventional method, and after the treatment, it was distilled under reduced pressure, and the fraction at 138-140°C was...

Embodiment 2

[0039] (1) Raw material: ethylbenzene 167.4Kg, purity is 95%, water content is 100ppm;

[0040] Tert-butyl chloride 94.4Kg, purity 99%, water content 1000ppm;

[0041] Catalyst: 0.48Kg of tetrabutylammonium bromide, 0.83Kg of anhydrous aluminum trichloride.

[0042] (2) Preparation process

[0043] Add 167.4Kg of ethylbenzene, 0.83Kg of anhydrous aluminum trichloride, and 0.48Kg of tetrabutylammonium bromide into the reaction kettle in turn, start stirring, add 94.4Kg of tert-butyl chloride, control the temperature at 0°C, and stir at a constant temperature for 5 Hours. Follow up the analysis with gas chromatography according to the conventional method, and stop stirring at the end of the reaction. The reaction solution was washed with alkali and water according to the conventional method, and after the treatment, it was distilled under reduced pressure, and the fraction at 138-140°C was collected at 10Kpa to obtain 150Kg of alkylbenzene solvent with a pur...

Embodiment 3

[0045] Raw materials: m-xylene 106.5Kg, purity 99.5%, water content 30ppm; tert-butyl chloride 144.6Kg, purity 97%, water content 100ppm; catalyst: cetyltrimethylammonium bromide 23.4Kg, no Aluminum trichloride water 26.8Kg.

[0046] Reaction temperature is 5 ℃, all the other are the same as embodiment 1.

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Abstract

The present invention relates to a preparation method of alkyl benzene solvent. It is made up by adopting tert-butyl chloride or tert.-butyl alcohol and dimethylbenzene or ethylbenzene through a certain reaction process. Its reaction temperature is 0-50 deg.C, reaction pressure is normal pressure, the mole ratio of tert.-butyl chloride or tert.-butyl alcohol and dimethylbenzene or ethylbenzene is 1.5-1-1:1.5, the catalyst dose is 0.5-20% of solvent weight. The catalyst is an ion liquid catalyst or one of anhydrous aluminium trichloride, anhydrous iron trichloride, sulfuric acid and hydrofluoric acid. The invented alkyl benzene solvent purity is 98%-100%, boiling range is 200-215 deg.C and relative density is 0.86-0.88. It can be used for synthesis of phthalocyanine copper.

Description

technical field [0001] The invention relates to a method for preparing an alkylbenzene solvent, in particular to a method for preparing an alkylbenzene solvent and its application in the synthesis of copper phthalocyanine. Background technique [0002] The solvent method is the main method for the synthesis of copper phthalocyanine, and the solvent commonly used in my country is trichlorobenzene. However, due to the partial condensation of trichlorobenzene under the action of high temperature and copper catalyst, a small amount of strong carcinogenic polychlorinated biphenyls (PCBs) will be generated. At present, developed countries such as Western Europe, the United States, and Japan have clearly stipulated that the content of PCBs should be limited. , Therefore, the trichlorobenzene preparation process is difficult to survive. [0003] The common solvents used to replace trichlorobenzene are: nitrobenzene, dodecylbenzene, kerosene, methylbenzene, dichlorobenzene, diisopro...

Claims

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Application Information

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IPC IPC(8): C07C2/00C07C15/02C07F1/08C09B47/06
Inventor 彭光辉王兴堂郭荣章
Owner 彭光辉
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