Method for synthesizing 3-methyl-3-butene-1-ol

A synthesis method and technology of butene, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem of low content of 3-methyl-3-butene-1-ol finished products and long holding time and other problems, to achieve the effects of less harsh reaction conditions, less waste, and high reaction selectivity

Active Publication Date: 2015-03-04
SHANDONG NHU PHARMA
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Problems solved by technology

[0013] Because the product is held for too long under acidic and alkaline conditions, side reactions are likely to o

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  • Method for synthesizing 3-methyl-3-butene-1-ol

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preparation example Construction

[0038] A kind of synthetic method of 3-methyl-3-butene-1-alcohol, comprises the following steps:

[0039] a, preparation of paraformaldehyde isopropanol solution

[0040] Throw paraformaldehyde and isopropanol into a single-necked flask with magnetic stirring, and stir at 50-90°C until all formaldehyde is dissolved to obtain a formaldehyde-isopropanol solution.

[0041] b. Add catalyst

[0042] Then add a certain amount of catalyst into the flask, continue to stir to dissolve it completely, and then cool down to room temperature to obtain the formaldehyde isopropanol solution in a one-necked bottle sealed for storage, and detect the formaldehyde content and catalyst content in the solution.

[0043] c. Reaction with isobutene

[0044] Take the formaldehyde isopropanol solution and isobutylene prepared in step b, fill it into an autoclave with mechanical stirring, the reaction pressure is 5-10 MPa, keep stirring at a speed of 200r / min and heat up;

[0045] When the temperatu...

Embodiment 1

[0051] A kind of synthetic method of 3-methyl-3-buten-1-ol, throws 58g paraformaldehyde, 200g isopropanol in the single-necked flask with magnetic stirring, stirs at 50~70 ℃ until formaldehyde is all dissolved, A solution of formaldehyde in isopropanol was prepared.

[0052] Then add 0.20g of aluminum hydroxide to the flask as a catalyst and continue stirring to dissolve it completely, then cool down to room temperature to obtain a formaldehyde isopropanol solution and store it in a one-necked bottle. The formaldehyde content of the solution is 20.2%, and the aluminum hydroxide content is 0.08%. .

[0053] Take 15g of formaldehyde isopropanol solution and 56g of isobutene, fill them into an autoclave with mechanical stirring, the reaction pressure is 8MPa, keep stirring at a speed of 200r / min and start to heat up, when the temperature reaches 200°C, start timing and heat preservation reaction for 1 hour. After cooling down to room temperature, the autoclave was opened to slow...

Embodiment 2

[0057] A kind of synthetic method of 3-methyl-3-buten-1-ol, throws 58g paraformaldehyde, 200g isopropanol in the single-necked flask with magnetic stirring, stirs at 50~70 ℃ until formaldehyde is all dissolved, A solution of formaldehyde in isopropanol was prepared.

[0058] Then add 0.34g basic aluminum chloride to the flask and continue to stir to make it all dissolve, then cool down to room temperature to obtain formaldehyde isopropanol solution and store it in a one-necked bottle. The formaldehyde content of the solution is 20.2%, and the basic aluminum chloride content is 20.2%. 0.13%.

[0059] Take 15g of formaldehyde isopropanol solution and 56g of isobutylene, fill them into an autoclave with mechanical stirring, the reaction pressure is 8 MPa, keep stirring at a speed of 200r / min and start to heat up, when the temperature reaches 200°C, start timing and heat preservation reaction for 1 hour . After cooling down to room temperature, the autoclave was opened to slowly...

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Abstract

The invention discloses a method for synthesizing 3-methyl-3-butene-1-ol. The method comprises the following steps of preparing a paraformaldehyde isopropanol solution, adding a catalyst, carrying out the reaction of the paraformaldehyde isopropanol solution with isobutene, and purifying a crude 3-methyl-3-butene-1-ol. The added catalyst can be aluminium isopropoxide, aluminium propoxide, aluminium ethylate, aluminium methoxide, basic aluminium chloride and aluminium hydroxide, and the addition amount of the catalyst is 0.1-1% of the mass of formaldehyde. The reaction condition of the method is not critical, and the catalysts containing acids, alkalis and halogens are not used. According to the method, the requirement on production equipment is not high, and the low-temperature low-pressure reaction condition has low requirement on the safety of industrial production, and the investment on equipment is low. The method has the advantages that the selectivity and the conversion rate are high, the reaction selectivity of formaldehyde is more than or equal to 95.6%, the conversion rate of formaldehyde is more than or equal to 96.7%, the purity of purified 3-methyl-3-buten-1-ol is more than 99.5%, and the content of water in 3-methyl-3-buten-1-ol is less than 0.1%.

Description

technical field [0001] The invention relates to a synthesis method of 3-methyl-3-buten-1-ol, which belongs to the technical field of fine chemicals. Background technique [0002] 3-Methyl-3-butene-1-ol is a colorless and transparent liquid, which can be used as a raw material for the production of a new generation of polycarboxylic acid series high-efficiency water reducers; in addition, 3-methyl-3-butene- 1-alcohols can be isomerized to produce prenol, which can be used in the synthesis of pyrethroids and in the production of citral. [0003] In 1955, Blomguist et al. first published that the target product was obtained by reacting isobutylene, polyoxymethylene, glacial acetic acid and acetic anhydride at 190°C and 3.6Mpa for 8 hours, but the yield was low. After that, most of the related research on the synthesis of 3-methyl-3-buten-1-ol focused on the catalytic system, reaction solvent, reactor design, etc., domestic and foreign related technical personnel have conducted...

Claims

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Application Information

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IPC IPC(8): C07C33/03C07C29/38
CPCC07C29/38C07C33/025
Inventor 郝文涛马啸邱金倬孟建波黄珊珊
Owner SHANDONG NHU PHARMA
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