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Preparation method of 2-methyl-3-butyne-2-ol

A technology of butyne and methyl, applied in the field of preparation of 2-methyl-3-butyne-2-ol, can solve the problems of difficulty in automation, complicated production procedures, large temperature difference and concentration difference, etc. The effect of less quantity, simple process and low cost

Inactive Publication Date: 2014-09-17
SICHUAN LUZHOU JUHONG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional industrial method for synthesizing 2-methyl-3-butyn-2-ol is mainly based on acetylene, sodium acetonate or potassium acetonate as raw material, solid (mostly powder) potassium hydroxide as catalyst, or liquid sodium hydroxide As a catalyst, calcium chloride or organic solvents are used for azeotropic dehydration, and useful salts cannot be recovered, and the condensed water is directly discharged without being used
The alkyne ketone condensation reaction adopts a tower reactor. In the tower reactor, the mixture of alkyne and ketone flows from top to bottom, and the catalyst flows from top to bottom. It is mixed with it in the axial direction by density difference, and the radial direction is mainly by diffusion mixing. The temperature difference and concentration difference of the system are large, resulting in low reaction yield and serious side reactions, due to excessive local concentration
In post-processing and refining, the rectification adopts batch method, the production cycle is long, and it is difficult to realize automation
There is a lot of industrial waste, and the organic residual liquid is not conducive to treatment because it contains inorganic salts
The production process is complicated, the production energy consumption is high, the product yield is low, the production cost is high, and the three wastes are difficult to treat

Method used

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  • Preparation method of 2-methyl-3-butyne-2-ol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the present embodiment, its reaction steps are:

[0026] a. Turn on the liquid ammonia switch, and the ammonia in the liquid ammonia cylinder will be throttled and charged into the 2000L gas storage tank. Turn on the acetylene switch, and the acetylene will pass into the gas storage tank after being sealed with water. Acetylene gas and ammonia are mixed in the gas storage tank to adjust the amount of acetylene and ammonia entering, 520g of acetylene and 780g of liquid ammonia (the ratio of acetylene to ammonia: 1:1.5).

[0027] b. The acetylene-ammonia mixed gas passes through a 2.0L gas-liquid separator to separate the entrained liquid, and then goes to the acetylene compressor to a pressure of 1.5Mpa.

[0028] c. The acetylene ammonia mixture gas is condensed through the condenser and cooled to 30°C. According to the amount of acetone of 234 g, that is, the ratio of acetylene: acetone = 1:0.45, the acetylene ammonia mixture gas enters the 2.5L acetylenization reac...

Embodiment 2

[0038] In the present embodiment, its reaction steps are:

[0039] a. Turn on the liquid ammonia switch, and the ammonia in the liquid ammonia cylinder will be throttled and charged into the 2000L gas storage tank. Turn on the acetylene switch, and the acetylene will pass into the gas storage tank after being sealed with water. Acetylene gas and ammonia are mixed in the gas holder to adjust the amount of acetylene and ammonia entering, 260g of acetylene and 1040g of liquid ammonia (ratio of acetylene to ammonia: 1:4.0).

[0040] b. The mixed gas of acetylene and ammonia passes through a 2.0L gas-liquid separator to separate the entrained liquid, and then goes to the acetylene compressor to a pressure of 2.1Mpa.

[0041] c. The acetylene ammonia mixture gas is condensed through the condenser, cooled to 40°C, and the amount of acetone is 286 g, that is, the ratio of acetylene: acetone = 1:1.10, the acetylene ammonia mixture gas and acetone enter the 2.5L acetylenization reactor...

Embodiment 3

[0051] In the present embodiment, its reaction steps are:

[0052] a. Turn on the liquid ammonia switch, and the ammonia in the liquid ammonia cylinder will be throttled and charged into the 2000L gas storage tank. Turn on the acetylene switch, and the acetylene will pass into the gas storage tank after being sealed with water. Acetylene gas and ammonia are mixed in the gas storage tank to adjust the amount of acetylene and ammonia entering, acetylene 390g, liquid ammonia 1170g (alkyne-ammonia ratio: 1:3.0).

[0053] b. The mixed gas of acetylene and ammonia passes through a 2.0L gas-liquid separator to separate the entrained liquid, and then goes to the acetylene compressor to a pressure of 2.7Mpa.

[0054] c. The acetylene ammonia mixture gas is condensed through the condenser and cooled to 50°C. According to the amount of acetone of 292.5 g, that is, the ratio of acetylene: acetone = 1:0.75, the acetylene ammonia mixture gas enters the 2.5L acetylenization reactor together...

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Abstract

The invention provides a preparation method of 2-methyl-3-butyne-2-ol, and the preparation method is as follows: acetylene and acetone are used as raw materials, liquid potassium hydroxide is used as a catalyst, by use of the characteristics of the acetylene, the acetylene is dissolved in liquid ammonia for homogeneous reaction with the acetone to obtain crude 2-methyl-3-butyne-2-ol product, ammonia is flashed out, and the finished product is obtained by salting-out dehydration and then continuous rectification. The preparation method has the advantages of simple equipment, less investment, simple process, easy control, easy operation, less catalyst consumption, uniform reaction system, less adverse reactions, easy recovery and recycling of solvents, high product yield, short production period, high finished product yield, saving energy and low production cost.

Description

technical field [0001] The invention relates to a preparation method of 2-methyl-3-butyn-2-ol. Background technique [0002] 2-Methyl-3-butyn-2-ol, CAS No. 115-19-5, molecular formula: C 5 h 8 O. Molecular weight: 84.11. The traditional industrial method of synthesizing 2-methyl-3-butyn-2-ol is mainly based on acetylene, sodium acetonate or potassium acetonate as raw material, solid (mostly powder) potassium hydroxide as catalyst, or liquid sodium hydroxide As a catalyst, calcium chloride or organic solvents are used for azeotropic dehydration, and useful salts cannot be recovered, and the condensed water is directly discharged without being used. The alkyne ketone condensation reaction adopts a tower reactor. In the tower reactor, the mixture of alkyne and ketone flows from top to bottom, and the catalyst flows from top to bottom. It is mixed with it in the axial direction by density difference, and the radial direction is mainly by diffusion mixing. The temperature di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/042C07C29/42C07C29/74
CPCC07C29/42C07C29/76C07C29/80C07C29/82C07C33/042
Inventor 高远明
Owner SICHUAN LUZHOU JUHONG CHEM CO LTD
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