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Method for preparing high-purity methyl isobutyl ketone from industrial by-product acetone waste liquid

A technology of methyl isobutyl ketone and industrial by-products, which is applied in the field of preparing high-purity methyl isobutyl ketone from industrial by-product waste liquid acetone, which can solve the disadvantages of separation and purification of MIBK products and recycling of acetone, shortened catalyst life, and the use of Low temperature and other issues to achieve the effect of enhancing product competitiveness, improving product selectivity, and avoiding waste of raw materials

Active Publication Date: 2014-07-23
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (1) The selectivity of the catalyst is low, and too many by-products affect the purity of the product
Published patents CN1488617, CN101765577, CN102744061, etc. all use metal composite catalysts to prepare MIBK, the selectivity of MIBK is between 40% and 70%, the side reaction is excessively condensed or there is no selective hydrogenation, too many by-products are very important for the separation and purification of MIBK products and the recycling of acetone is very unfavorable
At the same time, low product selectivity leads to complex production process, high operating costs, and conversion of raw materials into more by-products, which is not conducive to the economic benefits of enterprises.
[0008] (2) The operating temperature of the catalyst used in the existing catalytic synthesis of MIBK technology is too low, generally below 110°C. When the temperature is too high, the life of the catalyst is severely shortened, but too low temperature is not good for the conversion of impurities in the by-product acetone

Method used

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  • Method for preparing high-purity methyl isobutyl ketone from industrial by-product acetone waste liquid
  • Method for preparing high-purity methyl isobutyl ketone from industrial by-product acetone waste liquid
  • Method for preparing high-purity methyl isobutyl ketone from industrial by-product acetone waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Mix styrene, divinylbenzene and curing agent evenly according to a certain mass ratio, then add them into the reactor for prepolymerization, and then continue to polymerize at elevated temperature to obtain a resin prepolymer, and then pass the resin prepolymer through the same volume of dichloro Cook with ethane solvent, sulfonate with 98% sulfuric acid, and wash with pure water to obtain the catalyst carrier; add 200ml of catalyst carrier and 200ml of deionized water into the container, and then add 45ml of Pd 2+ The concentration is 0.2-0.5mol / L palladium nitrate-nitric acid-water ternary solution for ion exchange, the H in the solution + The concentration is 0.3mol / L, the exchange time is 30min, and then stirred, the waste liquid is filtered out, washed with deionized water until neutral, and dried at 50°C for 2h to obtain resin-based catalysts with different palladium contents. The specific catalyst labels and process conditions are listed in Table 3.

[0046] Tab...

Embodiment 2

[0050] The Rohm and Haas macroporous ion exchange resin Amb-36 was used to load 0.7wt% palladium, and the catalyst preparation method of Example 1 was used to prepare catalyst-5, which was used for comparison with the catalyst of the present invention. Catalyst-1 and Catalyst-5 were used to synthesize MIBK respectively, and the process parameters are shown in Table 4.

[0051] Table 4 Comparison of MIBK Synthesis by Different Catalysts at Low Temperature and High Temperature

[0052]

[0053]

[0054] Note: Ethers include diisopropyl ether, di-tert-butyl ether, methyl isobutyl ether, methyl tert-butyl ether, etc. Examples 1 and 2 in Table 4 are low-temperature catalytic reaction product compositions, and examples 3 and 4 are high-temperature reaction 4 The composition of the product was checked after one month.

[0055] Drawn from table 4: epoxy isobutane is almost all converted into isobutyraldehyde during low temperature reaction, isobutyraldehyde is a light component...

Embodiment 3

[0057] Pass the industrial by-product waste liquid acetone mixture through the fixed-bed reactor, use catalyst 1-4 as the catalyst and make spherical particles with a diameter of Ф0.3-1.3mm. The inner diameter of the reactor is Ф20mm, and a multi-stage heating insulation system is adopted; the catalyst filling capacity is 100ml; the by-product acetone mixture and hydrogen flow through the catalyst bed in parallel. The liquid samples were collected for analysis, and the specific reaction conditions and results are listed in Table 3.

[0058] Table 5 The reaction conditions and results of synthesizing MIBK

[0059]

[0060] Drawn from Table 5: acetone can catalyze the synthesis of MIBK product in one step, the conversion rate of acetone is moderate, and the selectivity of MIBK is higher; In the raw material, isobutylene oxide is all converted into isobutanol; the slightly increased content of isopropanol shows that a small amount of acetone catalyzes the synthesis It is isop...

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Abstract

The invention discloses a method for preparing high-purity methyl isobutyl ketone from an industrial by-product acetone waste liquid. According to the method, industrial byproduct acetone waste liquid, which contains more impurities and is difficult to separate, and hydrogen directly pass through a fixed bed tubular reactor filled with a heterogeneous catalyst, thereby converting acetone and difficultly separated impurities into MIBK and substances which are easily separated from the product; the reaction products are purified by distillation to obtain high-purity methyl isobutyl ketone. By virtue of the technology disclosed by the invention, a problem of a complex separation of acetone from impurities is solved, the cost for separating raw materials and the acetone circulation cost are greatly reduced, and the economical benefits of the device are greatly improved by converting the by-product acetone waste liquid into an MIBK product with high added value.

Description

technical field [0001] The invention relates to a method for preparing high-purity methyl isobutyl ketone (MIBK) from industrial by-product waste liquid acetone. technical background [0002] The by-product waste liquid acetone of industrial co-production equipment (such as acetone waste liquid produced by petrochemical plant) is not utilized, and a large amount of reaction waste liquid is produced every year. The main composition and content of this waste liquid are shown in Table a: [0003] The main composition and content of table a by-product acetone mixed solution [0004] name Content, wt% water 0.78～0.80 Methanol 2.78～3.07 Acetone 70.0～99.5 Isopropanol 0.01～0.03 Isobutylene oxide 6.20～7.28 tert-butanol 1.55～1.78 Isobutane 3.30～3.83 Propylene oxide 0～0.01 tert-butyl formate 0.01～0.02 Di-tert-butyl peroxide 0～0.01 [0005] As can be seen...

Claims

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Application Information

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IPC IPC(8): C07C49/04C07C45/73
CPCC07C45/73C07C49/04
Inventor 黎源何岩刘军姜庆梅林建平吕艳红董如伟孙安乐王文员玫赵磊孙玉成
Owner WANHUA CHEM GRP
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