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Process for preparing 2, 3-dimethylpyridine

A lutidine and 3PO4·3H2O technology, applied in 2 fields, can solve the problems of low yield of nitrile ethyl butanone, short catalyst life, difficult regeneration, etc., and achieve low raw material cost, high production efficiency and low equipment requirements Effect

Inactive Publication Date: 2009-02-11
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Method 1, using formaldehyde, acetaldehyde and butanone as raw materials for gas-phase catalytic synthesis (EP0131887), the reaction catalyst of this method is ZSM-5 molecular sieve, and the yield is only 10%; method 2, using butanone and acrylonitrile as raw materials , with the solution of ethylene glycol and potassium hydroxide as a liquid-phase catalyst, first react to generate cyanoethyl butanone, and then use Pd / Al2O3 as a catalyst to form a ring, (Chemical Journal of Universities, 1984, 5 (4): 499 ), the yield of nitrile ethyl butanone is extremely low in this method, and the main product is dinitrile ethyl butanone; method three, is to be raw material with propenol, butanone and ammonia, with Cd 3 (PO 4 ) 2 Catalyst gas-phase catalytic synthesis, (J.Pharm.Soc.Japan, 1955,75:1496), the yield is also relatively low, only 24%, the main by-products are 3-methylpyridine and 2-ethylpyridine, and the catalyst short lifespan, difficult to regenerate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1) Weigh 100g of activated clay and bake it at 300°C for 12 hours, then pour it into a 1000mL flask with 2.8g of basic alumina after cooling, then add 36.8g of palladium chloride solid and 350mL of distilled water, stir to obtain the mixture, weigh 18.5g (NH 4 ) 3 PO 4 ·3H 2 O crystals were dissolved in 100mL distilled water, slowly dropped into the flask containing the mixture under stirring, stirred for 30min, filtered with suction, and the filter cake was washed with 4×200mL distilled water, dried and formed, then calcined at 400°C for 12 hour to obtain composite catalyst;

[0016] 2) Put the composite catalyst into a fixed-bed reactor, measure 1026mL (15mol) propenol and 1338mL (15mol) butanone respectively and pour them into a clean container, shake and mix evenly, and feed the mixture of propenol and butanone into the fixed-bed reactor Mixed liquid and ammonia gas, the speed of ammonia gas is 300mL / min, the speed of mixed liquid is 0.3mL / min, the temperature i...

Embodiment 2

[0020] 1) Weigh 82.3g of activated clay and bake it at 450°C for 10 hours, then pour it into a 1000mL flask with 7.4g of basic silicon oxide after cooling, then add 27.6g of rhodium chloride solid and 350mL of distilled water, stir to obtain the mixture, weigh Take 18.5g (NH 4 ) 3 PO 4 ·3H 2 O crystals were dissolved in 100mL distilled water, slowly dropped into the flask containing the mixture under stirring, stirred for 30min, filtered with suction, and the filter cake was washed with 4×200mL distilled water, dried and formed, and then roasted at 525°C for 10 hour to obtain composite catalyst;

[0021] 2) Put the composite catalyst into a fixed-bed reactor, measure 1026mL (15mol) propenol and 1338mL (15mol) butanone respectively and pour them into a clean container, shake and mix evenly, and feed the mixture of propenol and butanone into the fixed-bed reactor Mixed liquid and ammonia gas, the speed of ammonia gas is 150mL / min, the speed of mixed liquid is 0.2mL / min, the ...

Embodiment 3

[0025] 1) Weigh 64.8g of activated clay and bake it at 600°C for 8 hours, then pour it into a 1000mL flask with 13.8g of basic alumina after cooling, then add 18.6g of cadmium chloride solid and 350mL of distilled water, stir to obtain the mixture, weigh Take 18.5g (NH 4 ) 3 PO 4 ·3H 2 O crystals were dissolved in 100mL distilled water, slowly dropped into the flask containing the mixture under stirring, stirred for 30min, filtered with suction, and the filter cake was washed with 4×200mL distilled water, dried and formed, and then calcined at 650°C for 8 The composite catalyst was obtained within hours.

[0026] 2) Put the composite catalyst into a fixed-bed reactor, measure 1026mL (15mol) propenol and 1338mL (15mol) butanone respectively and pour them into a clean container, shake and mix evenly, and feed the mixture of propenol and butanone into the fixed-bed reactor Mixed liquid and ammonia gas, the speed of ammonia gas is 50mL / min, the speed of mixed liquid is 0.1mL / m...

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PUM

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Abstract

The invention discloses a preparingmethod of 2, 3-dimethylpyridine, which comprises the following steps: preparing the composition with ammonium phosphate and fifth periodical transition metal chloride with acid adjusting agent as catalyst; making allyl alcohol, methyl ethyl ketone and ammonia gas as raw material; reacting in the catalytic reactor of solid bed at 250-400 Deg C; proceeding ringing reaction to obtain rough product; washing the rough product through saturated sodium chloride; removing water layer; rectifying to obtain the product.

Description

technical field [0001] The invention relates to a preparation method of 2,3-lutidine. Background technique [0002] 2,3-lutidine is an intermediate for preparing H+ / K+-ATPase inhibitors lansoprazole and rabeprazole for treating peptic ulcer. Existing 2, the preparation method of 3-lutidine mainly contains following several kinds: [0003] Method 1, using formaldehyde, acetaldehyde and butanone as raw materials for gas-phase catalytic synthesis (EP0131887), the reaction catalyst of this method is ZSM-5 molecular sieve, and the yield is only 10%; method 2, using butanone and acrylonitrile as raw materials , with the solution of ethylene glycol and potassium hydroxide as a liquid-phase catalyst, first react to generate cyanoethyl butanone, and then use Pd / Al2O3 as a catalyst to form a ring, (Chemical Journal of Universities, 1984, 5 (4): 499 ), the yield of nitrile ethyl butanone is extremely low in this method, and the main product is dinitrile ethyl butanone; method three, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/12C07D213/06
Inventor 戴立言王晓钟陈英奇叶玮
Owner ZHEJIANG UNIV