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Clean production process of alkyne diol serial products

A series of products, clean production technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of environmental pollution, large amounts of waste water, and high production costs

Inactive Publication Date: 2013-09-18
CHONGQING MINDONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Some of these synthetic methods require a high-pressure environment, and some require a special catalyst, which not only has high production costs, but also produces a large amount of waste water, which pollutes the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] After pumping 2535kg of n-heptane to the head tank for metering, add it to the reactor with a volume of 5000 liters; pump 450kg of methyl isobutyl ketone to the head tank. After feeding the n-heptane and let it stand for 30 minutes to separate the water, add 300kg of sodium hydroxide. After the feeding is completed, cover the feeding cover and tighten the bolts.

[0037] Replace with nitrogen for 15 minutes, close the vent valve and test the pressure with nitrogen leak test (pressure less than 0.04MP). After the pressure test, slowly inject 62kg of acetylene to start the reaction: the flow rate of acetylene is controlled at 2.5-15m 3 / h, the reaction stage controls the pressure in the kettle to be less than 0.08MPa by adjusting the flow rate of acetylene.

[0038] After the reaction was completed, the temperature was slightly lowered to 48° C., and 800 kg of water was slowly added, and stirred for 30 minutes after the addition of water was completed. The material is pr...

Embodiment 2

[0042] After pumping 2636kg of n-heptane to the head tank for metering, add it to the reactor with a volume of 5000 liters; pump 450kg of methyl isobutyl ketone to the head tank. After the n-heptane feeding is finished, let stand for 30 minutes to divide the water, add 350kg potassium hydroxide, cover the feeding cover after feeding, and tighten the bolts.

[0043] Replace with nitrogen for 20 minutes, close the vent valve and test the pressure with nitrogen leak test (pressure less than 0.04MP). After the pressure test, slowly inject 63kg of acetylene to start the reaction: the flow rate of acetylene is controlled at 2.5-15m 3 / h, the reaction stage controls the pressure in the kettle to be less than 0.08MPa by adjusting the flow rate of acetylene.

[0044] After the reaction was completed, the temperature was slightly lowered to 48° C., and 800 kg of water was slowly added, and stirred for 30 minutes after the addition of water was completed. The material is pressed into a ...

Embodiment 3

[0048] After pumping 2695kg of n-hexane to the head tank for metering, add it to the reactor with a volume of 5000 liters; pump 550kg of 2-methyl-2-pentanone to the head tank. After the n-heptane feeding is finished, let it stand for 30 minutes to separate the water, add 300kg of potassium hydroxide, cover the feeding cover after feeding, and tighten the bolts.

[0049] Replace with nitrogen for 20 minutes, close the vent valve and test the pressure with nitrogen leak test (pressure less than 0.04MP). After the pressure test, slowly inject 65kg of acetylene to start the reaction: the flow rate of acetylene is controlled at 2.5 ~ 15m 3 / h, in the reaction stage, the pressure in the kettle is controlled to be less than 0.08MPa by adjusting the acetylene flow rate.

[0050]After the reaction was completed, the temperature was slightly lowered to 45° C., and 1000 kg of water was slowly added, and stirred for 30 minutes after the addition of water was completed. Press the material...

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Abstract

The invention relates to a clean production process of alkyne diol serial products, and aims to provide a clean production process of the alkyne diol serial products mild in reaction condition and low in production cost. The clean production process of the alkyne diol serial products comprises the following steps: adding an organic solvent into a reaction kettle, standing, and then, adding alkali metal hydroxide; respectively adding acetylene and ketone by a pump into the reaction kettle for a reaction, and controlling the feeding speed, wherein in the feeding process, the pressure in the reaction kettle is not greater than 0.08MPa; after reaction, cooling to below 50 DEG C, and adding water to stir; and dropping an acid to adjust pH to 3-4, washing by water, standing and layering, and decompressing and distilling to recover n-heptane to obtain the product. According to the process provided by the invention, the use level of catalyst is fewer, so that the product belongs to bulk chemical product and the cost is low. The process temperature is not higher than 80 DEG C, the pressure is not greater than 0.08MPa, and the condition is mild. The yield of alkyne diol synthesized is greater than 85%. The solvent is decompressed, distilled, recovered and recycled, and no discharge waste exists.

Description

technical field [0001] The invention relates to a production process of acetylenic diol series products, in particular to a clean production process of acetylenic diol series products. Background technique [0002] Alkyne diols, as a class of nonionic surfactants with special structures, are widely used in many fields, such as pesticides, pharmaceutical and chemical intermediates, metal treatment, synthetic materials, and daily chemicals. [0003] The synthesis of acetylenic diols began in 1900 and has been developed for more than a century. At present, there are no more than ten manufacturers of acetylenic alcohols in the world, the largest of which is Gas Chemical in the United States, followed by BASF in Germany, and Kawaken in Japan. Except for one manufacturer in Eastern Europe, the rest are three to four in mainland China. manufacturers. [0004] In the prior art, the synthetic method of acetylenic alcohol roughly comprises the following several kinds: [0005] 1. A...

Claims

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Application Information

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IPC IPC(8): C07C33/044C07C29/42
Inventor 王立峰杨智孙健
Owner CHONGQING MINDONG CHEM
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