Method of preparing gamma-butyrolactone and/or 1,4-butanediol using chromium less catalyst

A technology of catalyst and butyrolactone, which is applied in chemical instruments and methods, preparation of hydroxy compounds, preparation of organic compounds, etc., can solve the problems of increasing the difficulty of manufacturing process, increasing equipment investment, production personnel and environmental hazards, etc., and achieve improvement Production efficiency, reduction of washing times, cost saving effects

Inactive Publication Date: 2004-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mitsubishi Chemical Corporation has developed a method for producing γ-butyrolactone from maleic anhydride liquid-phase hydrogenation, but this method needs to be reacted under high-pressure 100atm conditions, which increases the difficulty of the manufacturing process, and some also need to use Pa , Rh, Ru and other precious metals
[0005] Above-mentioned each prior art has characteristic respectively, but its shortcoming is: the catalyzer in the open technology that has contains the Cr component with strong toxicity, serious pollution, has caused great harm to production personnel and environment, in order to eliminate Cr pollution, must A large amount of money has been invested in the protection and treatment of production personnel. Even so, the pollution caused by Cr cannot be completely solved. In addition, the waste catalyst containing Cr cannot be recycled
Other technologies require high-pressure or two-stage hydrogenation process, which significantly increases equipment investment. At the same time, the activity of the catalyst is low. When the reaction temperature is 260°C-280°C, the liquid hourly space velocity is only 0.2-0.3hr -1

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 52.2g Cu(NO 3 ) 2 .3H 2 O, 91g 50% Mn(NO) 2 .Aqueous solution, 122gAl(NO 3 ) 3 .9H 2 O, dissolved in 500ml deionized water to make solution A. Na2CO3 (23mol) was made into solution B. Put 200ml of deionized water in a 1000ml beaker, add the two solutions of A and B into the beaker at the same time under stirring, control the dripping speed of A and B, keep the pH at 5.5±0.5, age for 1 hour after titration, then filter, and pass through 6 times Wash with water, collect the precipitate, dry at 120°C for 3 hours, and roast at 750°C for 2 hours to obtain catalyst A: CuMn 0.9 Al 1.5 o 4.2 .

Embodiment 2

[0022] 35.5g Cu(NO 3 ) 2 .3H 2 O (Beijing Chemical Plant, chemically pure), 48.9g 50% Mn (NO) 2 .Aqueous solution (Beijing Chemical Plant, chemically pure), 10.7g Al(NO 3 ) 3 .9H 2 O (Beijing Chemical Plant, chemically pure), be dissolved in 500ml deionized water, add dropwise ammoniacal liquor (23% by weight, Beijing Chemical Plant, chemically pure) under stirring, aging 1 hour when the solution pH is 6.5 ± 0.5, then Filter, wash once with water to collect the precipitate, dry at 200°C for 2 hours, and roast at 500°C for 2 hours to obtain catalyst B: CuMn 0.46 Al 0.2 o 1.76

Embodiment 3

[0024] 52.2g Cu(NO 3 ) 2 .3H 2 O, 5.6g 50% Mn(NO) 2 .Aqueous solution, 74.9gAl(NO 3 ) 3 .9H 2 O, dissolved in 500ml deionized water to make solution A. Na 2 CO 3 (23% by weight) was prepared as solution B. Put 200ml of deionized water in a 1000ml beaker, add the two solutions of A and B into the beaker at the same time under stirring, control the dissolution rate of A and B, keep the pH at 9±0.5, age for 1 hour after titration, then filter, and pass through 6 times Wash with water, collect the precipitate, dry at 120°C for 2 hours, and roast at 600°C for 2 hours to obtain catalyst C: CuMn 0.07 Al 0.9 o 2.42 .

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Abstract

A process for preparing gamma-butyrolactone and/or 1,4-butanediol by use of Cr-free catalyst includes making the the dialkyl maleate and/or dialkyl succinate in contact with hydrocatalyst, reacting at 170-300 deg.c and 0.1-15 hr under 0.1-7 Mpa, and collecting products. Said hydrocatalyst is CuMnaAlbOc, where a=0.01-1.5, b=0.1-2 and c is number of necessary oxygen atoms. Its advantage is controllable ratio between both products.

Description

technical field [0001] The invention relates to a method for preparing gamma-butyrolactone and / or 1,4-butanediol by gas-phase catalytic hydrogenation. technical background [0002] γ-butyrolactone is a synthetic butyric acid compound, polyvinylpyrrolidone, vitamin B 1 An intermediate of Naofukang, a suitable solvent for acrylate and styrene polymers, and a useful ingredient in paint detergents and textile auxiliaries. [0003] Usually γ-butyrolactone is obtained by dehydrogenating 1,4-butanediol as a raw material, but 1,4-butanediol is generally more expensive. 4 With the development of oxidation technology to prepare maleic anhydride, hydrogenation of maleic anhydride as raw material to prepare γ-butyrolactone has been developed rapidly. Mitsubishi Chemical Corporation has developed a method for producing γ-butyrolactone from maleic anhydride liquid-phase hydrogenation, but this method needs to be reacted under high-pressure 100atm conditions, which increases the difficul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/147C07C31/20C07D307/58
Inventor 王海京张建国高国强
Owner CHINA PETROLEUM & CHEM CORP
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