Production process for performing oxyalkylation on alkynol

A production process and oxygenation technology, which is applied in the production process field of alkoxylation of alkynols, can solve the problems of increased production cost, high requirements on reaction vessels, dangerous operators, etc., and achieves improved production efficiency and full controllability. , the effect of low reaction temperature

Inactive Publication Date: 2013-08-14
YUEYANG INTECH SYNTHETIC MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The high pressure method requires high pressure, which is dangerous to the operator, and has high requirements for the reaction vessel, that is, the production cost also increases accordingly; and because the volume of the pressure vessel is limited, the high pressure method cannot add more rings at one time. Oxyalkylene, when more alkylene oxide needs to be added, it needs to be added step by step in multiple steps
The solvent method, however, has low production efficiency, requires a large amount of heat when the solvent is evaporated, and needs to add evaporation equipment in the process flow, which consumes energy and time; in addition, the product will have residual organic solvents, making the prepared alkyne The purity of alcohol alkoxylation products is not high, so it cannot be applied in some fields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 20% ethylene oxide to 2,4,7,9-tetramethyl-5-decyne-4,7-diol, the production process includes:

[0033] a. Use a pump to transport 4000kg of 2,4,7,9-tetramethyl-5-decyne-4,7-diol melted in advance at 55~65°C to the head tank for metering, and put it into a volume of 6m 3 In the sealed low-pressure reactor, the reactor is a standard reactor with heat transfer oil or steam heating on the outer coil, water cooling on the inner coil, and frame or paddle type stirring. Add the mixture of 24.6kg trimethylamine and 0.4kg potassium hydroxide through the feeding device on the reactor.

[0034] b. Add 1050kg of ethylene oxide into the reactor at a rate of 4-5kg / min through the ethylene oxide metering pump. During the addition process, control the temperature in the reactor at 50-55°C and the pressure not to exceed 0.35MPa. When the pressure exceeds 0.35MPa, suspend feeding, and continue feeding when the pressure is lower than 0.3MPa. After the feeding is completed, keep the ...

Embodiment 2

[0040] 2,5,8,11-Tetramethyl-6-dodeyn-5,8-diol is added with 30% ethylene oxide, the production process includes:

[0041] a. Use a pump to transport 3500kg of 2,5,8,11-tetramethyl-6-dodecanyne-5,8-diol melted at 65~70℃ in advance to the head tank for metering, then put it into a closed low-pressure reactor middle. Add the mixture of 29.85kg triethylamine, 0.06kg potassium hydroxide and 0.09kg aluminum trichloride through the feeding device on the reactor.

[0042] b. Add 1600kg of ethylene oxide into the reactor at a rate of 3-4kg / min through the ethylene oxide metering pump. During the addition, control the temperature in the reactor at 65-70°C and the pressure not to exceed 0.4MPa. When the pressure exceeds 0.4MPa, stop feeding, and when the pressure is lower than 0.35MPa, continue feeding. After the feeding is completed, keep the temperature for about 3 hours, and wait until the pressure in the kettle drops to no longer changes.

[0043] c. Cool down after the reaction, ...

Embodiment 3

[0048] 2,4,7,9-tetramethyl-5-decyne-4,7-diol is added with 20% ethylene oxide and 10% propylene oxide. The production process includes:

[0049] a. Use a pump to transport 3500kg of 2,4,7,9-tetramethyl-5-decyne-4,7-diol melted in advance at 55~60°C to the head tank for metering, then put it into a closed low-pressure reactor . Add the mixture of 16.5kg trimethylamine, 12.9kg triethylamine, 0.3kg potassium hydroxide, 0.3kg zinc chloride through the feeding device on the reaction kettle.

[0050] b. Add 1050kg of ethylene oxide and 550kg of propylene oxide into the reactor at a speed of 1.5-2kg / min through the ethylene oxide metering pump. More than 0.4MPa. When the pressure exceeds 0.4MPa, stop feeding, and when the pressure is lower than 0.35MPa, continue feeding. Keep the temperature for about 4 hours after the feeding is completed, and wait until the pressure in the kettle drops to no longer changes.

[0051] c. Cool down after the reaction, replace the remaining ethylen...

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PUM

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Abstract

The invention relates to a production process for performing oxyalkylation on alkynol. The invention aims to provide an alkynol oxyalkylation production process, in which the reaction condition is mild and the reaction process can be controlled. According to the technical scheme, the production process comprises the following steps of: adding preheated alkynol into a reaction kettle, adding a catalyst, and stirring uniformly at constant temperature; adding one or more alkylene oxides into the reaction kettle, controlling the temperature and the pressure of the reaction kettle to be within a certain range in the alkylene oxide adding process, keeping constant temperature for a period of time after adding the alkylene oxides, and neutralizing; and distilling under reduced pressure to remove water and light components from materials thus obtaining the product. According to the production process, the reaction condition is mild, high-pressure equipment is not needed, and complete controllability in a production process is achieved; the reaction temperature is low, so the strongly alkaline component contained in the catalyst component can improve the catalytic efficiency and does not cause side reaction such as alkynol cracking; the reaction temperature is low, so the alkylene oxide with low boiling point is not gasified during reaction to increase the pressure, and the safety is improved; and the production efficiency is improved, the product has high purity and energy is saved.

Description

technical field [0001] The invention relates to a production process for the alkoxylation of acetylenic alcohols. Background technique [0002] Alkynyl alcohols are a class of fine chemical products widely used in many fields. From the perspective of molecular structure, alkynyl alcohol contains alkynyl group, polar group hydroxyl group and non-polar group aliphatic carbon chain. This structure determines that alkynyl alcohol compounds have many excellent properties, such as surface active properties. [0003] However, due to the small volume of the hydrophilic group (hydroxyl group) of acetylenic alcohols, the hydrophilicity of acetylenic alcohols is poor, which limits its application in the water-based field. Under the trend of environmental protection, modifying acetylenic alcohols to make them have good hydrophilicity can make acetylenic alcohols more widely used and more environmentally friendly. [0004] There are many methods for the modification of acetylenic alcoh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/178
Inventor 张一甫程霜莉宋自旗
Owner YUEYANG INTECH SYNTHETIC MATERIALS
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