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Catalyst of solid acid in use for preparing isobutene, and preparation method

A solid acid catalyst, isobutylene technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry and other directions, can solve the problems of high reaction temperature, expensive additional costs, difficult operation, etc., to achieve high methanol selectivity, equipment The effect of high utilization and low energy consumption

Inactive Publication Date: 2007-02-21
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Though raising reaction temperature is conducive to the raising of MTBE cracking conversion rate, also be conducive to the generation of side reaction simultaneously, cause the loss of product isobutylene as isobutene dimerization; methanol into the initial etherification reaction system; the hydration of water and isobutene produced during the formation of dimethyl ether also causes the product to suffer loss, and the formation of by-product tert-butanol increases the cost of separation and purification of the product, etc.
The higher reaction temperature also brings difficulties to the operation and increases energy consumption
The above-mentioned catalyst has a high conversion rate for MTBE cracking, but a large amount of water vapor and other inert substances need to be added during the reaction, and the recovery rate and equipment utilization rate of methanol and isobutene are greatly reduced, which makes the process complicated and leads to expensive additional cost
The disadvantage of the ion exchange resin catalyst is that the high temperature resistance is poor. When the reaction temperature is too high, the sulfonic acid group in it is easy to fall off. Due to the limitation of the reaction temperature, the conversion rate of the reaction is low.
The Achilles' heel of the sulfate system catalyst is that under the reaction conditions, the sulfate will gradually decompose, which will cause corrosion of equipment and decrease of catalyst activity.

Method used

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  • Catalyst of solid acid in use for preparing isobutene, and preparation method
  • Catalyst of solid acid in use for preparing isobutene, and preparation method
  • Catalyst of solid acid in use for preparing isobutene, and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 20 grams of γ-alumina was added to 50 ml of 5% Ti(SO 4 ) 2 In aqueous solution, let it stand overnight. After filtering, soak in 30ml of 15% ammonia by weight for 0.5 hours, filter off the ammonia, wash in deionized water until the pH is 8.5, and dry the filter cake in an oven at 130°C for 5 hours.

[0048] Then the product was impregnated with 50ml of 2N sulfuric acid solution at room temperature for 3 hours, filtered by suction, dried in an oven at 150°C for 3 hours, and roasted at 800°C to obtain SO 4 ＝ / TiO 2 / Al 2 o 3 .

[0049] then SO 4 / TiO 2 / Al 2 o 3 Join in 50ml weight concentration and be 10% ammonium chloride aqueous solution, filter, dry, in 800 ℃ roasting 8 hours, namely obtain the Cl of the present invention - / SO 4 ＝ / TiO 2 / Al 2 o 3 low temperature catalyst.

[0050] Put 20 grams of catalyst into a micro-fixed-bed reactor with a diameter of Φ2cm, feed methyl tert-butyl ether with a micro pump, and control the liquid space velocity to 2...

Embodiment 2

[0052] 20 grams of γ-alumina was added to 40 ml of 8% Ti(SO 4 ) 2 , let stand overnight. After filtering, soak in 40ml of 25% ammonia by weight for 0.5 hours, filter off the ammonia, wash in deionized water until the pH is 8.5, and dry the filter cake in an oven at 130°C for 5 hours.

[0053] Then the product was impregnated with 40ml of 1N sulfuric acid solution at room temperature for 4 hours, filtered by suction, dried in an oven at 110°C for 3 hours, and roasted at 800°C to obtain SO 4 / TiO 2 / Al 2 o 3 . then SO 4 / TiO 2 / Al 2 o 3 Add it into 40ml of 8% ammonium fluoride aqueous solution, filter, dry, and roast at 300°C for 3 hours to obtain the F - / SO 4 ＝ / TiO 2 / Al 2 o 3 low temperature catalyst.

[0054] Put 20 grams of catalyst into a micro-fixed-bed reactor with a diameter of Φ2cm, feed methyl tert-butyl ether with a micro pump, and control the liquid space velocity to 2.5h -1 , the reaction temperature is 150°C, the conversion rate of MTBE is 97%, t...

Embodiment 3

[0056] 20 grams of γ-alumina was added to 60 ml of 10% Ti(SO 4 ) 2 , let stand overnight. After filtering, soak in 40ml of 20% ammonia by weight for 1 hour, filter off the ammonia, wash in deionized water until the pH is 8.5, and dry the filter cake in an oven at 130°C for 5 hours.

[0057] Then the product was impregnated with 60ml of 1.5N sulfuric acid solution at room temperature for 3 hours, filtered by suction, dried in an oven at 130°C for 3 hours, and roasted at 800°C to obtain SO 4 / TiO 2 / Al 2 o 3 .

[0058] then SO 4 / TiO 2 / Al 2 o 3 Be added into 60ml weight concentration and be in the ammonium bromide aqueous solution of 12%, filter, dry, roast at 600 ℃ for 5 hours, promptly obtain the B of the present invention - / SO 4 / TiO 2 / Al 2 o 3 low temperature catalyst.

[0059] Put 20g of catalyst into a miniature fixed-bed reactor with a diameter of Φ2cm, feed methyl tert-butyl ether with a micropump, and control the liquid space velocity to 2.5h -1 , the...

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Abstract

A solid acid catalyst for preparing isobutene from methyl tert-butylether by low-temp cracking reaction with high selectivity and output rate contains Al2O3 (20-90 Wt %), TiO2 (0.1-20), 'SO4' radical (0.5-50) and halogen (0.5-20). Its preparing process is also disclosed.

Description

technical field [0001] The invention relates to a solid acid catalyst for preparing isobutene and a preparation method thereof, in particular to a solid acid catalyst for preparing isobutene by methyl tert-butyl ether cracking reaction. Background technique [0002] Isobutylene is an important chemical raw material. When it is used to synthesize butyl rubber, polyisobutylene, methacrylate and other chemical products, its purity requirements are quite high, requiring a large number of complicated separation processes or acid extraction, adsorption separation, etc. be realized. [0003] Due to the many downstream products of isobutene, the demand for isobutene is very large, and the market competitiveness is also very fierce. It mainly comes from the C4 fraction in steam cracking and catalytic cracking products. [0004] The traditional processes for industrial production of isobutene include sulfuric acid extraction, molecular sieve adsorption, direct hydration, catalytic cr...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J27/02B01J27/08B01J21/04B01J21/06C07C11/09C07C4/00
Inventor 王筠松金仙丽卢冠忠郭杨龙郭耘张志刚王艳芹刘晓晖
Owner EAST CHINA UNIV OF SCI & TECH