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
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 si

Method used

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

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Experimental program
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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...

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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

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Application Information

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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
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