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Preparation method of 2-methyl-6-propionyl naphthalene

A technology of propionyl naphthalene and methyl naphthalene, applied in the field of coal chemical industry, can solve the problems of complex process and large investment, and achieve the effects of improving product yield, good shape selectivity, and enhanced synergy.

Pending Publication Date: 2022-03-22
CCTEG CHINA COAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the existing production of 2-methyl-6-propionylnaphthalene has the disadvantages of complicated process and large investment. It is sought to design a catalyst that improves the conversion rate of raw materials, product yield and product purity, thereby improving the existing production process. 2-Methyl-6-propionylnaphthalene has the disadvantages that the process is too complicated and the investment is large

Method used

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  • Preparation method of 2-methyl-6-propionyl naphthalene
  • Preparation method of 2-methyl-6-propionyl naphthalene
  • Preparation method of 2-methyl-6-propionyl naphthalene

Examples

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Effect test

Embodiment 1

[0031] A preparation method of 2-methyl-6-propionyl naphthalene, comprising the steps of:

[0032] Weigh 180g of 2-methylnaphthalene, 326g of propionic anhydride, 350g of modified Hβ zeolite molecular sieve, and 100g of sulfolane into a three-necked flask, one of which is vertically connected to a condenser, one of which is inserted into a thermometer, and one of which is closed with a rubber stopper. Put the three-necked flask containing the raw materials into a metal bath with a stirring function, and carry out the acylation reaction at a speed of 600r / min and a temperature of 190°C. After the reaction has been carried out for 9 hours, stop stirring and keep warm, and wait for the three-necked flask to cool down. , take out a small amount of sample and carry out product analysis with gas chromatography, the transformation rate that analysis can obtain 2-methylnaphthalene: 78.9%. The catalyst was removed after the remaining samples were sucked through a Buchner funnel, and th...

Embodiment 2

[0034] A preparation method of 2-methyl-6-propionyl naphthalene, comprising the steps of:

[0035]Weigh 355g of 2-methylnaphthalene, 660g of propionic anhydride, 700g of modified Hβ zeolite molecular sieve, and 200g of sulfolane into a three-necked flask, one of which is vertically connected to a condenser tube, one of which is inserted into a thermometer, and one of which is closed with a rubber stopper. The flask was placed in a metal bath with a stirring function, and the acylation reaction was carried out at a speed of 600r / min and a temperature of 180°C. After the reaction was carried out for 10 hours, the stirring and heat preservation were stopped. After the three-necked flask was cooled, a small amount of samples were taken out and used for gas phase The product was analyzed by chromatography, and the conversion rate of 2-methylnaphthalene was analyzed to be 82.1%. The catalyst was removed after the remaining samples were sucked through a Buchner funnel, and the filtra...

Embodiment 3

[0037] A preparation method of 2-methyl-6-propionyl naphthalene, comprising the steps of:

[0038] Weigh 710g of 2-methylnaphthalene, 1320g of propionic anhydride, 350g of modified Hβ zeolite molecular sieve, and 200g of sulfolane into a three-necked flask, one of which is vertically connected to a condenser tube, one of which is inserted into a thermometer, and one of which is closed with a rubber stopper. The flask was placed in a metal bath with a stirring function, and the acylation reaction was carried out at a speed of 600r / min and a temperature of 200°C. After the reaction was carried out for 10 hours, the stirring and heat preservation were stopped. The product was analyzed by chromatography, and the conversion rate of 2-methylnaphthalene was analyzed to be 80.2%. The catalyst was removed after the remaining samples were sucked through a Buchner funnel, and the filtrate was distilled under reduced pressure at 180-210°C and 0.4-0.5kPa to obtain crude 2-methyl-6-propiony...

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Abstract

The invention discloses a preparation method of 2-methyl-6-propionyl naphthalene. The method comprises the following steps: (1) preparing a modified H beta zeolite molecular sieve catalyst; (2) preparing 2-methyl-6-propionyl naphthalene; and (3) purification of the 2-methyl-6-propionyl naphthalene. According to the method disclosed by the invention, the modified H beta zeolite molecular sieve is used as the catalyst, so that the Friedel-Crafts acylation reaction is promoted, and the raw material conversion rate, the product yield and the product purity are improved. The conversion rate of the 2-methylnaphthalene can reach about 80.0%, and after purification, the 2-methyl-6-propionyl naphthalene with the yield of 70%-90% and the purity of 91%-93% can be obtained.

Description

technical field [0001] The invention belongs to the technical field of coal chemical industry. Specifically, the invention relates to a preparation method of 2-methyl-6-propionylnaphthalene. Background technique [0002] my country is rich in coal reserves. In today's increasingly tense energy environment, it is of great significance to develop a high value-added route for naphthalene as a measure to increase the comprehensive utilization of heavy components in energy such as coal and petroleum. 2-Methyl-6-propionylnaphthalene is a promising organic chemical raw material, and its biggest use is to synthesize polyester after oxidation. Naphthalene dicarboxylic acid (NDA), the oxidation product of 2-methyl-6-propionylnaphthalene, and polyethylene naphthalate (PEN), obtained by esterification or transesterification of dimethyl naphthalene dicarboxylate and ethylene glycol , is the fastest developed and applied polyester compound containing naphthalene ring in the past ten year...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C45/82C07C45/81C07C49/788B01J29/70
CPCC07C45/46C07C45/82C07C45/81B01J29/7007C07C49/788Y02P20/584
Inventor 毛学锋靳海波张楠李军芳张笑然李恒何广湘杨索和胡发亭赵鹏钟金龙王琦王吉坤黄澎
Owner CCTEG CHINA COAL RES INST
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