Method for synthesizing alpha-tetralone by gas solid phase reaction

A tetralone, gas-solid phase technology, applied in chemical instruments and methods, preparation of heterocyclic compounds, molecular sieve catalysts, etc., can solve problems such as difficult to recycle, unrecoverable, large amount of catalyst, etc., to improve production efficiency Effect

Inactive Publication Date: 2010-01-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] (5) Benzene and 1,4-butyrolactone are synthesized under the action of anhydrous aluminum trichloride (C.E.Olson, A.R.Bader, Org.Synth., 1963,4,898), wherein as a catalyst, anhydrous trichloro The molar amount of aluminum chloride is generally 3-5 times that of lactone, which cannot be recovered after the reaction, and a large amount of acidic wastewater will be generated in the post-treatment process
[0010] In the above-mentioned (2)-(5) methods, liquid acid is required as a catalyst, and the amount of catalyst is large and it is difficult to recycle and use. The post-treatment of the product requires a large amount of water to wash, and the discharge of a large amount of acidic wastewater cannot be avoided.
In addition, the raw materials of methods (1) (3) (4) are not easy to obtain, and the application may be greatly restricted

Method used

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  • Method for synthesizing alpha-tetralone by gas solid phase reaction
  • Method for synthesizing alpha-tetralone by gas solid phase reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 2.2g of H-ZSM5 (Si / Al=150) (20-40 mesh) catalyst was charged into a quartz tube fixed-bed reactor with an inner diameter of 8mm and a length of 280mm, and passed N at 380°C. 2 (20ml / min) after treatment for 2h, the temperature was lowered to 240°C and kept at a constant temperature. The mixture of benzene and γ-butyrolactone (volume ratio 19 / 1) was injected with a micro injection pump at a constant flow rate (2.75mL / h, LHSV=1.1h) -1 ) into the vaporization chamber (280°C), followed by N 2 into the catalyst bed, N 2 Flow rate 20ml / min. The product condensed at the outlet of the reaction tube was collected every 20 minutes, and the content of γ-butyrolactone and α-tetralone in the product was analyzed by gas chromatography (chromatographic column: 5% FFAP / AW DMCS (60-80 mesh) )), the conversion of butyrolactone and the yield of α-tetralone were calculated. The average conversion of γ-butyrolactone was 46.5%, and the average molar yield of α-tetralone was 29.6%. The r...

Embodiment 2～4

[0027] Under other conditions and the same conditions as Example 1, the mixed solution of benzene and γ-butyrolactone (volume ratio 15 / 1), using H-Beta (S / Al=12.5) and SAPO-11 molecular sieve as catalysts, The results of the reactions under different reaction temperature, liquid space velocity and reaction time conditions are listed in Table 1 (2-4), respectively.

Embodiment 5～8

[0029] Under the same conditions as in Example 1, the mixed solution of benzene and γ-butyrolactone (volume ratio 25 / 1) was used as H-ZSM5 with different Si / Al ratios (50, 25, 19, 12.5) respectively. Catalyst at a reaction temperature of 240°C and a liquid space velocity of 1.1h -1 and the results of the reaction for 2-4 hours are listed in Table 1 (5-8), respectively.

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Abstract

The invention relates to a method for synthesizing alpha-tetralone by gas solid phase reaction. Benzene and gamma-butyrolactone are taken as raw materials; a molecular sieve is taken as a catalyst; the alpha-tetralone is continuously synthesized in a fixed bed reactor by the gas solid phase reaction; the reaction temperature is 210-300 DEG C; the reaction is carried out under the condition that the liquid space velocity is 1-6.0 h<-1>; the average conversion rate of gamma-butyrolactone is 25-79%; and the average mole yield of alpha-tetralone is 5-40%. The catalyst which is devitalized can be reproduced through oxygenation ignition to recover the catalyst performance. The method for synthesizing alpha-tetralone has the characteristics of avoiding the problems of not reusing the catalyst and discharging a great amount of acidic waste water. A serialization synthetic process is beneficial to automation production and production efficiency and enhances the production efficiency.

Description

Technical field: [0001] The invention relates to a method for synthesizing α-tetralone, which takes benzene and γ-butyrolactone as raw materials, and after gasification, under the action of a solid molecular sieve catalyst, the α-tetralone is continuously and flownly synthesized Methods. Background technique: [0002] α-Tetralone (α-tetralone, also known as tetralone), is a yellow liquid, soluble in benzene and ethanol, insoluble in chloroform, relative density 1.096 (25 / 4 ℃), melting point 5-6 °C, the boiling point is 255 °C. Refractive index 1.5675-1.5695. [0003] α-Tetralone is an important intermediate in pharmaceutical synthesis, mainly used in products such as norethindrone-ethinyl estradiol methyl ether tablets (a contraceptive), antidepressant Sertraline, and insecticide carbaryl (Petrochemical, 2004, Vol. 13, No. 1, P34; Japan Chemical Week, 2004, 45 (2286)), it can also be used as a solvent, plastic softener, etc. [0004] At present, the synthetic methods of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/67C07C45/59B01J29/85B01J29/70B01J29/40B01J37/30B01J37/08B01J38/12
CPCY02P20/584
Inventor 毛建新王存进罗云郑小明
Owner ZHEJIANG UNIV
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