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Synthetic method for 2-butyne-1-ol

A synthesis method and technology for butene are applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., and can solve the problems of shortage of 2-butyn-1-ol, low product purity, and expensive raw materials, etc. Achieve the effect of reducing labor and resources, simple synthesis method, and cheap raw materials

Inactive Publication Date: 2014-09-17
姜树林
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Problems solved by technology

[0002] 2-Butyn-1-ol is a colorless and transparent liquid with a melting point of -2.2°C and a boiling point of 142-143°C. Its molecular formula is C 4 h 6 O, flammable, may cause an allergic reaction in contact with skin, harmful to aquatic organisms, may cause long-term adverse effects in the aquatic environment
[0003] At present, there are not many technical processes for producing 2-butyn-1-ol, so the demand for 2-butyn-1-ol is in short supply, and the production process of 2-butyn-1-ol is often complicated in the prior art. The raw materials are expensive, there are likely to be potential safety hazards, and the product yield is not high, and the product purity is low

Method used

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  • Synthetic method for 2-butyne-1-ol

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Embodiment 1

[0023] A kind of synthetic method of 2-butyn-1-alcohol:

[0024] 1. Hydrolysis step

[0025] ⑴. Put 40g of raw materials (recycled rubber production waste liquid, the content of 1,3-dichloro-2-butene is 28.2%), 80ml of water, and 14g of sodium carbonate water into the three-necked flask, heat up and control the temperature After reflux reaction at 89-98°C for 8 hours, sample was taken for analysis.

[0026] (2) When the content of 1,3-dichloro-2-butene is less than 0.5%, stop the reaction, cool down, and extract 3 times with (200ml) ethyl acetate after the reflux reaction, and use (60g) solid calcium carbonate after the extraction Carry out drying, after drying, carry out vacuum distillation to remove ethyl acetate, set the time of vacuum distillation to be 0.5~2h, the temperature of vacuum drying is -0.085MPa.

[0027] (3) Rectification, under 72mmHg, collect the fraction at 78-85°C, cool, and weigh to obtain 9.4g of 3-chloro-2-buten-1-ol, with a yield of 94.2%.

[0028] T...

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Abstract

The invention discloses a synthetic method for 2-butyne-1-ol. Innovation points of the invention are as follows: a waste liquid containing 1,3-dichloro-2-butylene and produced in rubber production is used as a starting raw material and undergoes hydrolysis so as to obtain 3-chloro-2-butenyl-1-ol, then elimination is carried out so as to obtain 2-butyne-1-ol, and finally high-purity 2-butyne-1-ol is prepared. According to the synthetic method for 2-butyne-1-ol, the raw material is the waste liquid produced in rubber production and is cheap and widely available, so utilization of the waste, greenness and environmental protection are realized. The synthetic method is simple and is safe and easy to operate; and consumed labor force and resources by the method are substantially reduced. Product yield reaches more than 88%, and product purity reaches 96 to 98%.

Description

technical field [0001] The invention relates to a synthesis method of 2-butyn-1-ol, which belongs to the field of chemical synthesis. Background technique [0002] 2-Butyn-1-ol is a colorless and transparent liquid with a melting point of -2.2°C and a boiling point of 142-143°C. Its molecular formula is C 4 h 6 O, flammable, may cause allergic reaction in contact with skin, harmful to aquatic organisms, may cause long-term adverse effects in the aquatic environment. Mainly used in the production of electrophile 1-bromo-2-butyne, 1-bromo-2-butyne is an important intermediate in the synthesis of axial chiral ternary compounds. [0003] At present, there are not many technical processes for producing 2-butyn-1-ol, so the demand for 2-butyn-1-ol is in short supply, and the production process of 2-butyn-1-ol is often complicated in the prior art. The raw materials are expensive, there are potential safety hazards, and the product yield is not high, and the product purity is lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/58C07C33/042
CPCC07C29/124C07C29/58C07C33/042C07C33/423
Inventor 王德峰俞健钧石飞
Owner 姜树林
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