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 pro

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

Example Embodiment

[0044] Example one

[0045] Styrene, divinylbenzene and curing agent are uniformly mixed according to a certain mass ratio and then added to the reactor for pre-polymerization. Then the temperature is raised to continue polymerization to obtain a resin prepolymer, and then the resin prepolymer is passed through the same volume of dichloromethane Ethane solvent cooking, sulfonation with 98% sulfuric acid, and washing with pure water to obtain the catalyst carrier; add 200ml catalyst carrier and 200ml deionized water into the container, and then add 45mlPd 2+ The ternary solution of palladium nitrate-nitric acid-water with a concentration of 0.2-0.5mol / L performs ion exchange, and the H in the solution + The concentration is 0.3mol / L, the exchange time is 30min, then the mixture is stirred, the waste liquid is filtered, washed with deionized water to neutrality, and dried at 50℃ for 2h to obtain a resin-based catalyst with different palladium content. The specific catalyst numbers a...

Example Embodiment

[0049] Example two

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

[0051] Table 4 Comparison of MIBK synthesis with 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. In Table 4, examples 1 and 2 are the composition of low-temperature catalytic reaction products, and examples 3 and 4 are high-temperature reaction 4. The product composition was tested after months.

[0055] From Table 4, almost all epoxy isobutane is converted to isobutyraldehyde during the low temperature reaction. Isobutyraldehyde is a light component, and ...

Example Embodiment

[0056] Example three

[0057] The industrial by-product waste liquid acetone mixture is passed through a fixed-bed reactor. The catalyst adopts catalysts 1-4 and is made into spherical particles 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 volume 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 Reaction conditions and results for the synthesis of MIBK

[0059]

[0060] From Table 5: Acetone can be used to catalyze the synthesis of MIBK products in one step, the acetone conversion rate is moderate, and MIBK selectivity is high; all epoxy isobutane in the raw materials is converted to isobutanol; a slight increase in isopropanol content indicates a small amount of acetone catalytic synthesis It is isopropanol; me...

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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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