Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Polymer metal complex catalyst for synthesizing methyl isobutyl ketone

A technology of methyl isobutyl ketone and metal complexation, applied in the field of catalysis, can solve the problems of easy corrosion of equipment, many by-products, and low selectivity

Active Publication Date: 2016-10-26
NANJING UNIV +2
View PDF8 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Published patents CN1488617, CN101765577, CN102744061, etc. all use metal composite catalysts to prepare MIBK, and the selectivity of MIBK is between 40% and 70%. The low product selectivity causes complex production process, high operating cost, and raw materials are converted into more by-products, which are not Beneficial to the economic benefits of the enterprise
[0008] There are several main problems in the method for producing MIBK at present: (1) when adopting non-precious metal catalyst, selectivity is lower, and by-product is many, affects product purity; (2) reaction needs high pressure equipment; (3) reaction uses liquid strong base Or solid strong alkali as a catalyst, which has high requirements on the material of the equipment, and the equipment is easy to corrode, which affects the service life

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Polymer metal complex catalyst for synthesizing methyl isobutyl ketone
  • Polymer metal complex catalyst for synthesizing methyl isobutyl ketone
  • Polymer metal complex catalyst for synthesizing methyl isobutyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Preparation of metal complex monomer

[0047] 0.17g ruthenium chloride trihydrate (containing ruthenium 37.0wt%), 0.09g ferric chloride (containing iron 34.5wt%), 5g deionized water and 14.17g organic ligand I (n is 2, R 1 , R 2 Both are methyl) mixed, under the protection of nitrogen, slowly add the mixed liquid dropwise to 200mL n-hexane in a reflux state at a temperature of 69°C. The paraffin oil layer was cooled to 0-5°C and left to stand for 12 hours. The precipitated solid was filtered and dried in vacuum (-0.095MPa) at 30°C for 24 hours to obtain 11.63g of a mixture of ligand I and monomer I with a yield of 80.8%.

[0048] (2) Preparation of polymer catalyst

[0049] Add 6.32g of the mixture of ligand I and monomer I prepared in the previous step, 0.80g of monomer II, 0.12g of monomer III, and 0.09g of the initiator benzoyl peroxide (BPO) into the 100mL reaction eggplant bottle with branch pipe in sequence and 15mL N,N-dimethylformamide (DMF), stirred to d...

Embodiment 2

[0051] (1) Preparation of metal complex monomer

[0052] With 0.83g hexahydrate chloroplatinic acid (containing platinum 37.5wt%), 0.45g ferric chloride (containing iron 34.5wt%), 0.06g hexahydrate nickel chloride (containing nickel 24.5wt%), 0.03g cupric chloride ( Copper 47.2wt%), 5g deionized water and 14.17g organic ligand I (n is 2, R 1 , R 2 Both are methyl) mixed, under the protection of nitrogen, slowly add the mixed solution to 111 ° C, 200mL of toluene in the reflux state, after the dropwise addition, keep the reaction for 24 hours, separate layers while hot, the obtained toluene oil layer, Cool down to 0-5°C, let stand for 12 hours, filter the precipitated solid, and dry under vacuum (-0.095MPa) at 30°C for 24 hours to obtain 13.04g of a mixture of ligand I and monomer I, with a yield of 85.0%.

[0053] (2) Preparation of polymer catalyst

[0054] Add 2.06g of the mixture of ligand I and monomer I prepared in the previous step, 0.80g of monomer II, 0.23g of monom...

Embodiment 3

[0056] (1) Preparation of metal complex monomer

[0057] With 1.63g chloroplatinic acid hexahydrate (containing platinum 37.5wt%), 1.62 chromium chloride hexahydrate (containing chromium 19.1wt%), 0.06g copper chloride (containing copper 47.2wt%), 5g deionized water and 14.17g Organic ligand I (n is 2, R 1 , R 2 Both are methyl) mixed, under the protection of nitrogen, slowly add the mixture dropwise to 200mL methylene chloride under reflux at 40°C. The methyl chloride oil layer was cooled to 0-5°C and left to stand for 12 hours, and the precipitated solid was filtered and dried under vacuum (-0.095MPa) at 30°C for 24 hours to obtain 14.91g of a mixture of ligand I and monomer I, with a yield of 84.6%.

[0058] (2) Preparation of polymer catalyst

[0059] Add 3.51g of the mixture of ligand I and monomer I prepared in the previous step, 0.80g monomer II, 0.35g monomer III, 0.12g initiator azobisisobutyronitrile (AIBN ) and 15mL of methanol, stirred and dissolved, deoxygenat...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of catalysis and relates to a preparation method for synthesizing a methyl isobutyl ketone catalyst and application thereof, particularly to a preparation method for synthesizing methyl isobutyl ketone at a single state by using acetone and isopropanol as materials, and application of the method. The acetone and isopropanol are catalyzed with the self-made polymer metal complex catalyst to directly synthesize MIBK at one step, the temperature is 80-120 DEG C, reaction time is 10-24 hours, 35.9-38% of acetone conversion rate, MIBK is 94.3-95.9% in selectivity, and the catalyst may be used stably. During reaction, the isopropanol is used as a hydrogen source to release hydrogen of a molecule, the byproduct is acetone and may be used as a material for synthetic MIBK for reuse, and at the consideration of a while, the method has no need for hydrogen, reacting is at normal pressure or micro normal powder, no waste is produced, and the need for green and clean production is met.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and relates to a method for preparing a catalyst for synthesizing methyl isobutyl ketone and its application; specifically, it relates to the preparation of a catalyst for synthesizing methyl isobutyl ketone in one step using acetone and isopropanol as raw materials method and its application. Background technique [0002] Methyl isobutyl ketone (4-methyl-2-pentanone, Methyl isobutyl ketone, referred to as MIBK) is a widely used organic chemical product, mainly used as a solvent for high-grade coatings, and as a rubber antioxidant for synthetic tires 4020, lubricating oil dewaxing agent, organic synthesis extractant and diluent and surfactant, etc. [0003] The traditional production method is a three-step method: Acetone is catalyzed by acid or base to condense liquid-phase aldol to generate diacetone alcohol (DAA), and then DAA is dehydrated by acid to generate mesityl oxide (MO). Finally, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): B01J31/22C07C49/04C07C45/45
CPCC07C45/45B01J31/1805B01J2531/847B01J2531/842B01J2531/62B01J2531/828B01J2531/824B01J2531/821B01J2531/822B01J2531/16B01J2231/42B01J2531/0213C07C49/04
Inventor 徐林王芳黄杰军范以宁俞磊丁克鸿徐清顾克军
Owner NANJING UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com