Method of preparing gamma butyrolactone and tetrahydropyrane from 1,4-butanediol

A technology of tetrahydrofuran and butanediol, which is applied in the direction of organic chemistry, can solve the problems of Cr component production personnel and environmental hazards, high catalyst manufacturing cost, and increased operation difficulty, and achieves low price, reduced power consumption, and good selectivity Effect

Inactive Publication Date: 2006-11-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main shortcomings of the above technology: 1) although the catalysts used have higher activity and selectivity, some contain noble metals, and some contain highly toxic and polluting Cr components, and the use of noble metals makes the catalyst cost high, while the Cr components Distributed to production personnel and the environment have caused great harm
The catalysts described in these patents all support two or more noble metal elements on the activated carbon carrier, and the total content of noble metals is relatively high, generally greater than 5% of the total mass of the catalyst, making the catalyst manufacturing cost higher; and using these more Precious metal catalysts must be under very high pressure conditions, generally higher than 15.0MPa, in order to obtain a good yield of tetrahydrofuran, high pressure operation not only increases the equipment investment but also increases the difficulty of operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Catalyst preparation: 52.2g Cu(NO 3 ) 2 .3H 2 O, 44.0g Al(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. Add A to B so that the final pH value is 9±0.5, age for 1 hour after titration, then filter, wash with water 5 times, collect the precipitate, dry at 120°C for 2 hours, and roast at 750°C for 2 hours to obtain catalyst A: CuAl 0.49 o 1.7 .

[0024] Catalyst pre-reduction: Take 3.2g of catalyst A with a particle size of 26-40 mesh and put it into a tubular reactor made of stainless steel with an inner diameter of 8mm. Hydrogen, reduced for 20 hours.

[0025] Catalytic dehydrogenation reaction: the reaction conditions are temperature 230±3°C, hydrogen / alcohol molar ratio 2:1, system pressure 0.1MPa, 1,4-butanediol liquid phase space velocity 8h -1 . The reaction product was determined by FID using a gas chromatograph with packed column PEG20000. The conversion rate of 1,4-buta...

Embodiment 2

[0027] Catalyst preparation: 35.5g Cu(NO 3 ) 2 .3H 2 O, 5.9gAl(NO3 ) 3 .9H 2 O, dissolved in 500ml deionized water, then added 1.3g TiO 2 , to make suspension A. Na 2 CO 3 (23mol%) to make solution B. Add solution B to A. Keep the final pH at 8±0.5, age for 1 hour after titration, then filter, wash with water 5 times, collect the precipitate, dry at 120°C for 12 hours, and roast at 750°C for 3 hours to obtain catalyst B: CuAl 0.1 Ti 0.1 o 1.4 .

[0028] Catalyst B was pre-reduced and reacted in the manner of Example 1. The difference is that the reaction conditions are temperature 230±3°C, the hydrogen / alcohol molar ratio is 9:1, the system pressure is adjusted to 0.1MPa, and the liquid phase space velocity of 1,4-butanediol is 6h-1,1.4-butanediol The conversion rate is 99.7w%, and the selectivity of γ-butyrolactone is 53.9w%. The tetrahydrofuran selectivity is 44.9w%.

Embodiment 3

[0030] Catalyst preparation: 35.5g Cu(NO 3 ) 2 .3H 2 O, 83.9gAl(NO 3 ) 3 .9H 2 O, dissolved in 500ml deionized water, then added 11.9g TiO 2 , made suspension A. Na 2 CO 3 (23mol%) to make solution B. Add B and A to a 2000ml beaker at the same time. Keep the pH at 5.5±0.5. After adding the materials, age for 1 hour, then filter, wash with water for 3 times, collect the precipitate, dry at 120°C for 12 hours, and roast at 500°C for 3 hours to obtain catalyst C: CuAl 1.5 TiO 5.52 .

[0031] Catalyst C was pre-reduced and reacted in the manner of Example 1. The difference is that the reaction conditions are temperature 230±3°C, the hydrogen / alcohol molar ratio is 1.7:1, the system pressure is adjusted to 0.5MPa, and the liquid phase space velocity of 1,4-butanediol is 6h -1 , 1. The conversion rate of 4-butanediol is 99.6w%, the selectivity of γ-butyrolactone is 55.9w%, and the selectivity of tetrahydrofuran is 42w%.

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Abstract

A process for preparing gamma-butyrolactone and tetrahydrofuran from 1,4-butanediol features that in H2 atmosphere the 1,4-butanediol is in contact with the catalyst CuTiaAlbOc at 170-300 deg.C under 0.1-1 MPa, where a=0-1.5, b=0.04-2, c is the number of oxygen atoms. Said catalyst has high activity and selectivity.

Description

technical field [0001] The invention relates to a method for preparing gamma-butyrolactone and tetrahydrofuran in one step from 1,4-butanediol. technical background [0002] γ-butyrolactone is an important organic chemical product. It is an intermediate in the synthesis of butyric acid compounds, polyvinylpyrrolidone, methionine, vitamin B1 and brain rehabilitation. It is a suitable solvent for acrylate and styrene polymers. Can be used as a useful ingredient in paint cleaners and textile auxiliaries. [0003] Known methods for preparing gamma-butyrolactone are mainly divided into two classes, one is the gas-phase hydrogenation of maleic anhydride or its ester to prepare gamma-butyrolactone, such as US 4,584,419; US 3,853,922; US 3,829,448; CN 1034541A stated. The other is the catalytic dehydrogenation of 1,4-butanediol to γ-butyrolactone, and the relevant technologies in this regard will be described below. [0004] 1, 4-butanediol catalytic dehydrogenation system gamma-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/08C07D307/58
Inventor 王海京高国强
Owner CHINA PETROLEUM & CHEM CORP
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