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Synthetic method of 2-methallyl alcohol

A technology of methallyl alcohol and a synthesis method, which is applied in the field of synthesis of 2-methallyl alcohol, can solve the problems of equipment corrosion, large amount of waste water and high hydrogenation pressure, achieves improved product yield, reduced condition requirements, The effect of prolonging the service life

Inactive Publication Date: 2015-11-11
ZHEJIANG LYUKEAN CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] Chinese patents CN103588622A and CN101759528A all adopt the direct hydrolysis method of methallyl chloride and alkali, and the main disadvantages are that there are many etherification by-products, and the concentration of alkali solution is low to produce a large amount of waste water.
[0004] Chinese patents CN102167657B and CN103755523A use methallyl aldehyde or first oxidize isobutylene to methallyl aldehyde and then hydrogenate and reduce methallyl alcohol to prepare methallyl alcohol, but there are high hydrogenation pressure, high oxidation temperature and poor hydrogenation selectivity of the catalyst And the shortcomings of easy polymerization of methallyl aldehyde
But this method adds water in the esterification reaction step, because reaction needs to be carried out in airtight container, under higher temperature condition, the aqueous chloride solution of generation easily corrodes general equipment, especially more can accelerate the equipment to equipment under higher temperature. Corrosion, so it has higher requirements on the equipment conditions of industrial production
At the same time, the organic phase after the esterification reaction is directly hydrolyzed, because it still contains a certain amount of methallyl chloride, which will generate a slightly higher amount of methallyl ether in the hydrolysis process, thereby affecting product quality

Method used

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  • Synthetic method of 2-methallyl alcohol
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  • Synthetic method of 2-methallyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Esterification reaction: In the autoclave, put 588g 2-methallyl chloride, 532.8g anhydrous sodium acetate (the molar ratio of 2-methallyl chloride and anhydrous sodium acetate is 1.0:1.0) and 10.6 g tetrabutylammonium chloride, seal the reaction kettle, start stirring and raise the temperature to 100°C, with the increase of temperature, the pressure is up to 0.3MPa, and keep warm for 20h. After the reaction was completed, the material was transferred to a still, and 739.6 g of the organic phase was distilled out. According to gas chromatography analysis, the content of methacryl acetate was 96.2%, and the content of 2-methallyl chloride was 3.8%. The solid in the still is mainly sodium chloride 391.8g, wherein the sodium chloride content is 97.2%, and the moisture is 0.4%. The organic phase was rectified under the conditions of -0.040MPa at the top of the tower and 70°C at the top of the tower to obtain 669.7g of refined methallyl acetate with a methallyl chloride conte...

Embodiment 2

[0040] Esterification reaction: In the autoclave, put 588g 2-methallyl chloride, 410g anhydrous sodium acetate (the molar ratio of 2-methallyl chloride and anhydrous sodium acetate is 1.3:1) and 6.1g Tetrabutylammonium chloride, seal the reaction kettle, start stirring and raise the temperature to 120°C. With the increase of temperature, the pressure is up to 0.4MPa, and the temperature is kept for 15h. After the reaction was complete, the material was transferred to a distillation pot, and 706.0 g of the organic phase was distilled out. According to gas chromatography analysis, the content of methacryl acetate was 80.2%, and the content of 2-methallyl chloride was 19.8%. The solid in the still is mainly sodium chloride 298.1g, wherein the sodium chloride content is 98.2%, and the moisture is 0.3%. The organic phase was rectified under the conditions of -0.040MPa at the top of the tower and 70°C at the top of the tower to obtain 541.8g of refined methallyl acetate with a metha...

Embodiment 3

[0043] Esterification reaction: In the autoclave, put 588g 2-methallyl chloride, 355.2g anhydrous sodium acetate (the molar ratio of 2-methallyl chloride and anhydrous sodium acetate is 1.5:1) and 3.6 g tetrabutylammonium chloride, seal the reaction kettle, start stirring and raise the temperature to 140°C. With the increase of temperature, the pressure is up to 0.5MPa, and the temperature is kept for 10h. After the reaction was completed, the material was transferred to a still, and 689.5 g of the organic phase was distilled out. According to gas chromatography analysis, the content of methacryl acetate was 71.6%, and the content of 2-methallyl chloride was 28.4%. The solid in the still is mainly 257.3g of sodium chloride, wherein the content of sodium chloride is 98.5%, and the moisture is 0.3%. The organic phase was rectified at -0.040MPa at the top of the tower and the temperature at the top of the tower was 70°C to obtain 469.2g of refined methallyl acetate with a methall...

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Abstract

The invention relates to a synthetic method of 2-methallyl alcohol. The synthetic method comprises the step of carrying out esterification reaction, refinement and separation and hydrolysis reaction on 2-methallyl chloride and sodium carboxylate to prepare 2-methallyl alcohol, wherein the formulas of the esterification reaction and the hydrolysis reaction are respectively formula (1) and formula (2) both referring to the description; the R is CH3 or CH3CH2, namely, methyl or ethyl. According to the invention, the synthetic method is reasonable in technology and easy to operate; the product is high selectivity and relatively high in quality; carboxylic sodium in the esterification reaction stage and water in the hydrolysis reaction stage are recycled and need no external supplement, so that cyclic utilization is achieved, and the product yield is improved.

Description

technical field [0001] The invention relates to a method for synthesizing 2-methallyl alcohol, which belongs to the technical field of organic chemical industry. Background technique [0002] 2-Methallyl alcohol, also known as 2-methyl-2-propen-1-ol, 3-hydroxy-2-methylpropene, isobutenol, molecular formula CH 2 C(CH 3 )CH 2 OH, molecular weight 72.11, boiling point 113-115°C. Methallyl alcohol is an important fine chemical raw material, which can be used in many fields such as medicine, pesticide, fragrance, resin, polycarboxylate superplasticizer, etc. It is soluble in water and organic solvents, and its performance is similar to that of allyl alcohol. Similar, but much less toxic than allyl alcohol, it can be used as a substitute for allyl alcohol in many fields. [0003] Chinese patents CN103588622A and CN101759528A both adopt the direct hydrolysis method of methallyl chloride and alkali, and the main disadvantages are many etherification by-products, low concentratio...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C27/02
CPCC07C29/095C07C67/10C07C33/03C07C69/145C07C69/24
Inventor 王胜利陈志荣王新荣马振祥赵兴军
Owner ZHEJIANG LYUKEAN CHEM
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