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

Hdrogenation synthesis method for preparing 2-methyl allyl alcohol by using recyclable catalyst

A technology of methacryl alcohol and methacrolein, which is applied in the field of organic intermediate synthesis, can solve the problems of large amount of by-product ether generation, difficult to control, low yield, etc., achieve simple recycling method and reduce separation cost , the effect of reducing production costs

Inactive Publication Date: 2011-08-31
武汉凯森化学有限公司
View PDF15 Cites 19 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the hydrolysis method has been widely used, there are many problems in this method: a large amount of alkali and organic solvent will be added in the hydrolysis process, the hydrolysis temperature and pressure are sometimes high, the conditions are harsh, and the solvent is difficult to recover; at the same time, the side effects The generation amount of product ether is also bigger, thereby causes the yield of target product to be on the low side
But its yield is low, only about 50%, in addition its nanometer Au25 (SR) 18 Catalyst preparation is quite complicated and difficult to manipulate
In α, β-unsaturated aldehyde molecules, since the C=O bond energy is greater than the C=C bond energy, it is difficult to selectively hydrogenate C=O without destroying the C=C bond, and hydrogenation often generates saturated Aldehydes or saturated alcohols, generally poor selectivity to unsaturated alcohols

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
  • Hdrogenation synthesis method for preparing 2-methyl allyl alcohol by using recyclable catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Add 70 grams of 2-methacrolein and 0.794 grams of Ru[(±)-BINAP]Cl to a 1-liter autoclave 2 , 0.1 gram cuprous chloride and 530 gram xylenes, airtight autoclave, pass into hydrogen twice in the autoclave to replace the original air in the autoclave; After replacement, lead the hydrogen of 3.5MPa in the autoclave, and 30 Reaction at ℃ for 6 hours;

[0032] 2. After the reaction is over, cool the reaction system to room temperature, discharge the remaining hydrogen, open the autoclave, and transfer the reaction solution to a 1-liter three-port still, and install a 15-plate fine distillation still on the still. Distillation column, heating the still, so that the temperature of the still rises gently from room temperature to 150 ° C, when there is reflux at the top of the tower, control the reflux ratio to 1.5, collect and obtain 5 grams of fractions at 30 to 80 ° C, 2-methacrolein The content is 85%, the fraction of 80-100°C is 3 grams, the content of 2-methacrolein is ...

Embodiment 2

[0037] 1. Add 70 grams of 2-methacrolein and 0.794 grams of Ru[(±)-BINAP]Cl to a 1-liter autoclave 2 , 0.05 grams of cuprous chloride and 600 grams of N, N-dimethylacetamide, sealed autoclave, into the autoclave twice hydrogen to replace the original air in the autoclave; 2.5MPa hydrogen, and react at 20°C for 8 hours;

[0038] 2. After the reaction is over, cool the reaction system to room temperature, discharge the remaining hydrogen, open the autoclave, and transfer the reaction solution to a 1-liter three-port distillation kettle, and install a 18-plate fine distillation kettle on the distillation kettle. Distillation column, heating the still, so that the temperature of the still rises gently from room temperature to 150 ° C, when there is reflux at the top of the tower, control the reflux ratio to 2.0, collect and obtain 4 grams of fractions at 30 to 80 ° C, 2-methacrolein The content is 88%, the fraction of 80-100°C is 4 grams, the content of 2-methacrolein is 90%, the...

Embodiment 3

[0041] 1. Add 140 grams of 2-methacrolein and 0.16 grams of Ru[(±)-BINAP]Cl to a 2-liter autoclave 2 , 0.1 gram of cuprous chloride and 1200 gram of dimethylbenzenes, airtight autoclave, pass into hydrogen twice in the autoclave to replace the original air in the autoclave; After replacement, lead the hydrogen of 4.5MPa in the autoclave, and 30 Reaction at ℃ for 10 hours;

[0042] 2. After the reaction is over, cool the reaction system to room temperature, discharge the remaining hydrogen, open the autoclave, and transfer the reaction solution to a 2-liter three-port distillation kettle, and install a 20-plate fine distillation kettle on the distillation kettle. Distillation column, heating the still, so that the temperature of the still rises gently from room temperature to 150 ° C, when there is reflux at the top of the tower, control the reflux ratio to 1.0, collect 12 grams of 30-80 ° C fractions, 2-methacrolein The content is 84%, the 80-100°C fraction is 5 grams, the co...

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 discloses a method for synthesizing 2-methylacrolein into 2-methyl allyl alcohol by using a catalytic hydrogenation method, belonging to the technical field of synthesis of organic intermediates. A catalyst used in the method is recyclable. The synthesis method comprises the following steps of: (1) adding 2-methylacrolein, a catalyst, a polymerization inhibitor and a high-boiling-point solvent into a high-pressure kettle and introducing hydrogen for reacting; (2) after reacting, exhausting excessive hydrogen and rectifying reaction liquid to obtain 2-methylacrolein; and (3) adding the 2-methylacrolein and the solvent into residual liquid in a rectifying kettle, transferring into the high-pressure kettle and undergoing a reaction for preparing 2-methylacrolein through hydrogenation to realize the recycling of the catalyst. The method has the advantages of atom economy, environmental friendliness, high yield, simple post-treatment and the like.

Description

technical field [0001] The invention belongs to the technical field of organic intermediate synthesis, in particular to a method for preparing 2-methacryl alcohol by hydrogenating 2-methacrolein, wherein the catalyst used can be recycled. Background technique [0002] 2-methacryl alcohol (also known as 2-methacryl alcohol, methacrolein or methallyl alcohol) is a very important organic intermediate, which itself can undergo self-polymerization and copolymerization reactions. Using 2-methacrylic alcohol as the starting material, methacrylic acid and its esters can be prepared. In addition, 2-methacryl alcohol can also form allyl-containing esters with other organic acids. Therefore, 2-methacryl alcohol is widely used in the fields of polymer monomers and surfactants. [0003] The earliest synthesis method of 2-methacryl alcohol is to prepare propylene chloride by hydrolysis under alkaline conditions. Subsequently, US2072015, US2323781, US2313767 and JP2009107949 etc. have i...

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): C07C33/03C07C29/141
CPCY02P20/584
Inventor 刘裴陈建程艳东冯薇伟宋晓波张敏袁攀柏宏章卢宏宇张晓郭志荣王庆利
Owner 武汉凯森化学有限公司
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