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Method for preparing MIBK through industrial by-product low-purity acetone

An industrial by-product and low-purity technology, which is applied in the field of MIBK preparation, can solve the problems of high catalyst use cost, deactivation, side reactions, etc., and achieve the effects of improving product selectivity, prolonging service life, and improving economic benefits

Active Publication Date: 2016-01-13
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, high temperature is also conducive to the occurrence of some side reactions, which reduces the yield of the target product and affects the economics of the device.
At the same time, the long-term experiment of the above process shows that the shedding of the active group of the resin catalyst is an inevitable process. At a high temperature above 130 ° C, the long-term operation of the catalyst still has a certain degree of deactivation.
Coupled with the high cost of catalyst manufacturing, the cost of catalyst use is still high

Method used

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  • Method for preparing MIBK through industrial by-product low-purity acetone
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  • Method for preparing MIBK through industrial by-product low-purity acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation of non-supported copper catalyst Cu-1, Cu-2 and Cu-3 in the protection catalyst used in the second stage process:

[0050] Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 O, Ca(NO 3 ) 2 4H 2 O, Mg(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 9H 2 O was made into solution 1, solution 2 and solution 3 according to the ratio of 9:75:40:15:10:2, 35:55:25:8:15:1, 60:36:26:4:0.61:0.15 respectively , to which Na was slowly added dropwise 2 CO 3 Control the drop rate to keep the pH at 4-6. After the co-precipitation reaction is completed, age at room temperature for 12-24 hours; then vacuum filter to separate the precipitate from the mother liquor, and use a large amount of Rinse the precipitate with deionized water; dry the precipitate at 80-100°C for 8-12 hours, and then 2 Roast at 400°C for 4 hours in the atmosphere; then extrude, and spray the molded catalyst with an ethanol-water solution containing 1% commercial KP-853 water repellent on th...

Embodiment 2

[0053] Preparation of supported copper catalyst Cu-Sn-1, Cu-Sn-2 and Cu-Sn-3 in the protection catalyst used in the second stage process:

[0054] CuCl 2 2H 2 O and SnCl 4 ·5H 2 O was added to the molten stearic acid according to a certain mass ratio, and stirred magnetically at 80-100°C for 6-8 hours. After the dehydration was complete, a certain amount of butyl titanate was added and stirred vigorously for 3-5 hours, and the shell formed a translucent sol. , Dry at 100°C for 4-6 hours, then bake in a muffle furnace at 400°C-500°C for 2-4 hours, and then reduce it under a hydrogen atmosphere at 350-400°C for 4-6 hours.

[0055] According to the above method, m(Cu):m(Sn):m(TiO 2 ) is the catalyst Cu-Sn-1 of 9:11:80, and m(Cu):m(Sn):m(TiO 2 ) is the catalyst Cu-Sn-2 of 25:5:70, and m(Cu):m(Sn):m(TiO 2) is the catalyst Cu-Sn-3 of 39:16:45.

Embodiment 3

[0057] The raw material composition is as shown in Table 1, the catalyst of the first process section is Amberlyst CH-28, the reactor is a fixed-bed reactor, the reaction temperature is 100°C, the reaction pressure is 3MPa, the hydrogen-to-oil ratio (molar ratio) is 0.7, and the air speed is 1h -1 . The catalyst in the second process stage is Ruike D5H5A, the reactor is a continuous stirred tank reactor, the reaction temperature is 125°C, the reaction pressure is 3MPa, the volume of the reactor is 2L, the catalyst dosage is 5g, and the residence time is 30min.

[0058] The reaction products of the first stage process and the second stage process were collected for chromatographic analysis, and the specific results are listed in Table 2.

[0059] The reaction result after the two-stage process of table 2

[0060]

[0061] As can be seen from Table 2: when there is only one stage of technology, the yield of isobutanol is only 9.84%, and most of the isobutane epoxy is conver...

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Abstract

The invention discloses a method for preparing MIBK through industrial by-product low-purity acetone. The method is performed through two segments of technologies. In the first segment of technology, acetone is converted into MIBK and part of impurities under the action of MIBK synthetic catalysts; in the second segment of technology, under the action of protective catalysts, main impurities are converted into products easy to separate and it is guaranteed that acetone is not lost basically. The method can achieve conversion of most part of substances difficult to separate in raw material, products are easy to eliminate through rectification, reaction temperature of a main reaction catalyst bed layer is remarkably lowered, the service life of main catalysts is remarkably prolonged, unexpected side reaction is inhibited, and therefore the product yield and the economical efficiency of a device are further improved. MIBK superior products with the purity being 99.5wt% can be obtained by separating reaction products.

Description

technical field [0001] The invention relates to a method for preparing MIBK (methyl isobutyl ketone), in particular to a method for preparing MIBK by using industrial by-product low-purity acetone, which belongs to the field of organic synthesis. Background technique [0002] Methyl isobutyl ketone (MIBK) is an important organic solvent. It is mainly used as one of the raw materials for the production of rubber antioxidants. It can be used for waxy oil dewaxing of paints and resin coatings. It can also be used as a solvent for the production of tetracycline and penicillin. , in oil refining, as a petroleum dewaxing agent for the production of refined paraffin, which has a wide range of uses. [0003] Among the industrial production methods of MIBK, there are acetone three-step method, acetone one-step method and isopropanol one-step method. The three-step process of acetone was the main production process before the 1970s. The technology is mature and can produce DAA (diace...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/73C07C31/12C07C29/10
CPCC07C29/103C07C45/73C07C49/04C07C31/12
Inventor 何岩吕艳红黎源林建平刘军董如伟孙安乐袁帅王中华黄少峰张文韬吴华杰王文
Owner WANHUA CHEM GRP CO LTD
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