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Isobutylene refining kettle residue treating method

A processing method and technology for isobutene, applied in chemical instruments and methods, hydrocarbon purification/separation, chemical/physical processes, etc., can solve the problems of high operating temperature, low economic value, recovery of isobutene, etc. Green chemical industry, the effect of reducing pollution discharge

Active Publication Date: 2019-06-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the characteristics of the raw material, the crude isobutene after the cracking of tert-butanol produced by propylene oxide contains water, methanol, acetone, tert-butanol, methyl tert-butyl ether, isopropyl tert-butyl ether, isobutyl tert-butyl ether Butyl ether, diisobutene and other impurities, the refined residue contains the above impurities and a small amount of isobutene, wherein the ether and alcohol that can regenerate isobutene account for 60-90wt% of the residue, due to the composition of the residue It is very complicated, there are many kinds of binary or multiple azeotropes, it is difficult to recover tert-butanol by refining, and directly returning to the main reactor will cause the accumulation of various impurities in the reaction system, reducing the reaction efficiency; recycling by extraction It will cause an increase in the proportion of wastewater, and the accumulation of water-soluble impurities such as methanol and acetone in the main reactor will reduce the selectivity of the reaction; therefore, incineration is mostly used to recover energy at present, and the economic value is extremely low.
[0005] Patent CN105712818A proposes to use a modified alumina catalyst, a mixture of methyl tert-butyl ether and tert-butanol to prepare isobutene by catalytic cracking in the gas phase method. It is relatively high, and it is also easy to produce carbon deposits during the reaction, and the raw material used in this method is only a mixture of methyl tert-butyl ether and tert-butanol, and isobutene is refined by cracking tert-butanol produced by propylene oxide. The components in the still residue are far more complex than the patent, therefore, this method is not applicable
[0006] At present, there is no suitable method to recover isobutene from the crude isobutene refining residue of propylene oxide by-product tert-butanol cracking

Method used

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  • Isobutylene refining kettle residue treating method
  • Isobutylene refining kettle residue treating method
  • Isobutylene refining kettle residue treating method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 290g Co(NO 3 ) 2 6(H 2 O) (1mol) and 19.3g quinoline (0.15mol) and 224.3g terephthalic acid (1.35mol) were dissolved in 1L of water, mixed evenly and then transferred to a 2L reactor at 230°C for 60h at a constant temperature, and the obtained precipitate was dissolved in 0.8L nitromethane, and add 0.3molH 2 SO 4 and 0.4molTf 2 O, stirred at 30°C for 1h, cooled the reaction liquid to -10°C to precipitate precipitates, filtered the precipitates, washed them with water and acetone in turn, and then roasted at 280°C for 6h to obtain the catalyst substrate, extruded into 3mm*5mm Particulate matter, whose composition is 37.5 wt% Co 2 o 3 , 50.8wt% terephthalic acid, 11.7wt% sulfoquinoline.

[0049] Load the catalyst into a Ф40cm fixed-bed reactor with an operating pressure of 0.9MPa, a temperature of 135°C, and a space velocity of 2.3h for isobutylene refining residue -1 , the lysate is flashed at 0.3MPa, and the crude isobutene compressed liquid obtained after the c...

Embodiment 2

[0053] 287g Mn(NO 3 ) 2 6(H 2 O) (1mol) and 19.8g of pyridine (0.25mol), 273.9g of terephthalic acid (1.65mol) were dissolved in 1L of water, mixed evenly and then transferred to a 2L reactor at a constant temperature of 180°C for 90h, and the obtained precipitate was dissolved in 1.0 L nitromethane, and add 0.4molH 2 SO 4 and 0.5molTf 2 O, stirred at 35°C for 1.6h, cooled the reaction solution to -25°C to precipitate precipitates, filtered the precipitates, washed them with water and acetone in turn, and then roasted at 240°C for 8h to obtain a catalyst matrix, extruded into 3mm*5mm particulate matter, whose composition is 20.6wt% MnO 2 , 65.1wt% terephthalic acid, 14.3wt% pyridine sulfonate.

[0054] Load the catalyst into a Ф40cm fixed-bed reactor with an operating pressure of 1.4MPa, a temperature of 160°C, and a space velocity of 0.8h -1 , the cracked reaction solution is flashed at 0.5MPa, and the non-condensable gas at the top of the flash column is compressed to...

Embodiment 3

[0058] 288gFe(NO 3 ) 2 6(H 2 O) (1mol) and 6.8g of imidazole (0.1mol), 133.2.g of 1,3,5-benzenetricarboxylic acid (0.8mol) were dissolved in 1L of water, mixed evenly and then transferred to a 2L reaction kettle at 230°C for 60h. The resulting precipitate was dissolved in 0.8L nitromethane, and 0.2molH 2 SO 4 and 0.3molTf 2 O, Stir at 40°C for 1h, cool the reaction solution to -15°C to precipitate precipitates, filter the precipitates, wash with water and acetone in turn, and then roast at 300°C for 4h to obtain a catalyst substrate, extruded into 3mm*5mm Particulate matter, whose composition is 44.7 wt% Fe 2 o 3 , 47.0wt% 1,3,5-benzenetricarboxylic acid, 8.3wt% sulfoimidazole.

[0059] Load the catalyst into a Ф40cm fixed-bed reactor with an operating pressure of 1.2MPa, a temperature of 145°C, and a space velocity of 1.5h -1 , the cracked reaction solution was flashed at 0.2MPa, and the non-condensable gas at the top of the flash column was compressed to obtain a cru...

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Abstract

The invention provides an isobutylene refining kettle residue treating method, wherein isobutylene refining kettle residue is cracked under the action of a solid acid catalyst, and the cracking liquidis subjected to flash evaporation, extraction, refining and other operations to remove isobutylene having a purity of more than 99.8 wt%. According to the present invention, through the comprehensiveutilization of isobutylene refining kettle residue, the isobutylene refining kettle residue is converted into isobutylene so as to be further recovered, such that the utilization rate of resources isincreased, the energy saving and consumption reducing is further achieved in the production, the production cost is reduced, the production environment is improved, and the environmental pollution isreduced.

Description

technical field [0001] The invention relates to a method for treating isobutene refining residue, in particular to a method for recovering useful components therefrom, and more specifically to a method for recovering isobutene from crude isobutene refining residue cracked by propylene oxide by-product tert-butanol. Background technique [0002] Isobutylene is an important chemical raw material, which is used to synthesize polyisobutylene rubber, butyl rubber, and the main monomer of isoprene. It is also widely used as medicine, pesticide, antioxidant, synthetic high-grade lubricating oil, gasoline additive and other Raw materials for fine chemical products. [0003] At present, isobutene mainly comes from the separation of C4 fractions in refining and chemical enterprises or the dehydration of tert-butanol by-product of propylene oxide. , isomerization, co-oxidation, etc., among which tert-butanol dehydration is the most simple and effective method to obtain high-purity iso...

Claims

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Application Information

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IPC IPC(8): C07C7/00C07C7/17C07C7/04C07C7/10C07C11/09B01J31/22
Inventor 王中华何岩袁帅刘振峰吕艳红曹善键黎源
Owner WANHUA CHEM GRP CO LTD
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