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Preparation method of tert-alkynol polyether

A technology for tertiary alkynol and polyether, which is applied in the field of preparation of tertiary alkynol polyether, can solve the problem of ineffectiveness by specifically providing methods for reducing raw material residues or reducing product distribution, reducing product added value and price competitiveness, and increasing product production. Cost and other issues, to achieve the effect of improving market competitiveness, ingenious process design, and reducing production input costs

Active Publication Date: 2019-07-05
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As we all know, since propylene oxide is less reactive than ethylene oxide, it is more difficult to react, and propylene oxide is easy to chain transfer to generate allyl groups, and the production of small molecules leads to a broad product distribution, so it meets the requirements for the preparation of tertiary alkyne alcohols. The method of polyoxyethylene ether is not necessarily suitable for the preparation of tertiary alkyne alcohol polyoxypropylene ether
[0019] 2. The existing method only provides a preparation method for preparing tert-alkynyl alcohol polyether, and it is useless to specifically provide a method for reducing raw material residues or reducing product distribution
[0020] 3. In order to reduce the color of the product and increase the degree of unsaturation in the existing method, the process is relatively complicated, or the catalyst needs to be removed by filtration, or organic solvents need to be used, which increases the production cost of the product and reduces the added value of the product and price competition. force

Method used

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  • Preparation method of tert-alkynol polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Add 452g of melted 2,4,7,9-tetramethyl-5-decyne-4,7-diol into the polymerization reactor, place nitrogen three times, then quickly add 0.67g (polyether mass 0.05%) sodium amide, and nitrogen three times, and keep the temperature of the reactor at 50-55°C and the pressure ≤-0.098MPa to remove ammonia for 1h. Then turn off the vacuum pump, slowly and uniformly add 176g of ethylene oxide, control the feeding time to 2h, the reaction temperature is 50-55°C, and the pressure is -0.01MPa~0.01MPa. After the addition, continue to react at 50-55°C until the pressure does not change, continue to add the remaining 704g of ethylene oxide, and gradually raise the temperature to 100-105°C, continue to react at 100-105°C until the pressure does not change , lower the temperature to 40-45°C to remove a small amount of unreacted ethylene oxide, add glacial acetic acid to neutralize, and discharge to obtain 2,4,7,9-tetramethyl-5-decyne-4,7-di Alcohol polyoxyethylene (10) ether.

[0058...

Embodiment 2

[0064] Add 252g of 2-methyl-3-butyn-2-ol into the polymerization reactor, set nitrogen three times, then quickly add 4.9g (0.3% of polyether mass) sodium amide in a nitrogen atmosphere, then set nitrogen three times, keep Ammonia gas is removed for 1 hour under the conditions of reaction kettle temperature of 40-45°C and pressure of -0.045~-0.05MPa. Then turn off the vacuum pump, slowly and uniformly add 209g of propylene oxide, control the feeding time to 5h, the reaction temperature is 50-55°C, and the pressure is 0.05MPa-0.10MPa. Continue to react at 50-55°C until the pressure does not change after the addition is complete, continue to add the remaining 1183g of propylene oxide, and gradually raise the temperature to 100-105°C, and continue to react at 100-105°C after the addition is completed until the pressure does not change. Lower the temperature to 40-45°C to remove a small amount of unreacted propylene oxide, add phosphoric acid for neutralization, and discharge to ob...

Embodiment 3

[0077] Add 126g of 4-methyl-1-heptyn-3-ol and 282g of 7,10-dimethyl-8-hexadecane-7,10-diol into the polymerization reactor, place nitrogen three times, and then Quickly add 0.5g (0.13% of the polyether mass) of potassium amide, then place nitrogen three times, and keep the temperature of the reactor at 45-50°C and the pressure of -0.045-0.05MPa to remove ammonia for 1h. Then turn off the vacuum pump, slowly and uniformly add 132g of ethylene oxide, control the feeding time to 2h, the reaction temperature is 50-55°C, and the pressure is -0.04MPa~-0.03MPa. Continue to react at 50-55°C until the pressure does not change after the addition is complete, continue to add the remaining 132g of ethylene oxide, and gradually raise the temperature to 100-105°C, continue to react at 100-105°C after the addition is completed until the pressure does not change , lower the temperature to 40-45° C. to remove a small amount of unreacted propylene oxide, add phosphoric acid for neutralization, ...

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Abstract

The invention relates to a preparation method of tert-alkynol polyether, and belongs to the field of fine chemical engineering. The preparation method comprises following steps: (1) adding a catalystand tert-alkynol into a reactor, carrying out degassing for 1 hour at a certain temperature under a certain pressure, controlling the reaction temperature and reaction pressure, slowly and evenly adding part of olefin oxide into the reactor within a certain period, and after addition, maintaining the temperature until the pressure becomes stable; and (2) keeping on adding olefin oxide at a certaintemperature until the reactions are finished, maintaining the temperature until the pressure becomes stable, cooling to remove a little of unreacted olefin oxide, adding an acid to carry out neutralization, and discharging obtained tert-alkynol polyether. The invention provides a preparation method of tert-alkynol polyether, which has the advantages of light color, high unsaturation degree, narrow distribution, low residual raw materials, and low PEG / PPG content.

Description

technical field [0001] The invention relates to a preparation method of tertiary alkyne alcohol polyether, which belongs to the field of fine chemical industry. Background technique [0002] In order to avoid the insufficient dynamic surface tension of traditional nonionic surfactants, although many anionic surfactants have small dynamic surface tensions, they have the disadvantages of easy foaming, hard water resistance, and poor acid and alkali resistance. Alkynyl alcohols and their alkoxylates have a good balance in terms of dynamic surface tension and foaming properties, resistance to hard water, acid and alkali resistance, etc. At the same time, this type of surfactant has excellent wettability, so that it can It is widely used in water-based coatings, printing inks, adhesives, pesticides and building materials. [0003] The preparation method of traditional fatty alcohol polyether is to adopt strong base (such as sodium hydroxide, potassium hydroxide, sodium methylate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C07C41/09C07C43/178
CPCC07C41/09C08G65/2606C08G65/2648C07C43/1785
Inventor 金一丰王俊糜泽峰高洪军
Owner ZHEJIANG HUANGMA TECH
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