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Refining process of polyoxypropylene ether

A technology of polyoxypropylene ether and process, which is applied in the field of polyoxypropylene ether refining technology, can solve the problems of inability to prepare high-purity polyoxypropylene ether, and achieve the effect of promoting development and improving purity

Active Publication Date: 2017-12-26
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conventional process is neutralization-washing-dehydration, but this conventional process can only wash away 80%-90% of the acid catalyst, and cannot prepare high-purity polyoxypropylene ether

Method used

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  • Refining process of polyoxypropylene ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In Example 1, crude polyoxypropylene ether was obtained by using hydroxypropyl methacrylate and propylene oxide with boron trifluoride as a catalyst.

[0040] Add 1000 parts of crude polyoxypropylene ether (including 5 parts of boron trifluoride) and 250 parts of water into a four-necked flask according to the mass ratio, stir evenly, raise the temperature to 75°C, add 10 parts of sodium hydroxide to neutralize and stir for 5-10 Minutes, adjust the pH to between 6-8, then add 3 parts of adsorbent as a pH buffer to absorb slightly excess acid or alkali, and stir for 5-10 minutes.

[0041] The salt obtained after neutralization is sodium fluoride and sodium borate, because sodium borate is more soluble in water at 60-80°C, while the solubility of sodium fluoride at 60-80°C is only about 4.5. Therefore, we add seeds when sodium fluoride is in a supersaturated state. It is calculated that the solution contains 9.3 parts of sodium fluoride, and it needs 207 parts of water t...

Embodiment 2

[0044] In Example 2, crude polyoxypropylene ether was obtained by using hydroxypropyl methacrylate and propylene oxide with boron trifluoride as a catalyst.

[0045] Add 1000 parts of crude polyoxypropylene ether (including 5 parts of boron trifluoride) and 250 parts of water into a four-necked flask according to the mass ratio, stir evenly, raise the temperature to 75°C, add 10 parts of sodium hydroxide to neutralize and stir for 5-10 Minutes, adjust the pH to between 6-8, then add 3 parts of adsorbent as a pH buffer to absorb slightly excess acid or alkali, and stir for 5-10 minutes.

[0046] After decompression and vacuum dehydration, adjust the vacuum to 300-250mbar, add 0.2 parts of NaH when the effluent is measured to 30 parts 2 P0 4 ·6H 2 0 as the seed crystal. Continue dehydration and keep the vacuum at 300-250mbar for 2 hours, 250-200mbar for 1 hour, 200-0mbar for 1 hour, raise the temperature to 85°C and keep 0mbar for 1 hour. Then stop dehydration and add 3 part...

Embodiment 3

[0048] In Example 3, crude polyoxypropylene ether was obtained by using hydroxypropyl methacrylate and propylene oxide with boron trifluoride as a catalyst.

[0049] Add 1000 parts of crude polyoxypropylene ether (including 5 parts of boron trifluoride) and 250 parts of water into a four-necked flask according to the mass ratio, stir evenly, raise the temperature to 75°C, add 10 parts of sodium hydroxide to neutralize and stir for 5-10 Minutes, adjust the pH to between 6-8, then add 3 parts of adsorbent as a pH buffer to absorb slightly excess acid or alkali, and stir for 5-10 minutes.

[0050] After decompression and vacuum dehydration, adjust the vacuum to 300-250mbar, add 0.2 parts of NaH when the effluent is measured to 40 parts 2 P0 4 ·6H 2 0 as the seed crystal. Continue dehydration and keep the vacuum at 300-250mbar for 2 hours, 250-200mbar for 1 hour, 200-0mbar for 1 hour, raise the temperature to 85°C and keep 0mbar for 1 hour. Then stop dehydration and add 3 part...

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Abstract

The invention relates to a refining process of polyoxypropylene ether. The refining process comprises the following steps: (1) polymerizing polyoxypropylene ether: polymerizing and reacting hydroxypropyl methacrylate and propylene epoxide under the condition of acidic catalysts; (2) neutralizing a catalyst: adding water and alkali into the polyoxypropylene ether obtained in step (1), and uniformly stirring; (3) adding a seed crystal: adding inorganic salt hydrate as a seed crystal; (4) after the seed crystal in step (3) is added, forming a new crystal nucleus; and (5) filtering: adding a filter aid, and filtering in a pressurizing or vacuumizing manner. The refining process solves the problem in the traditional refining process of the polyoxypropylene ether that the removal rate of the acidic catalyst is not high, improves the purity of the polyoxypropylene ether, and promotes the industrial development.

Description

technical field [0001] The invention relates to a refining process of polyoxypropylene ether, which belongs to the post-treatment process of polyoxypropylene ether. Background technique [0002] In the preparation process of polyoxypropylene ether, it is often necessary to use a catalyst, which can be a basic catalyst or an acidic catalyst. When the polyoxypropylene ether is finally prepared, the catalyst needs to be removed or neutralized. If there is an un-neutralized catalyst, it may cause the desired reaction to be over-catalyzed, resulting in the polymerization of polyoxypropylene ether itself or affecting the downstream application effect of the product. [0003] The polyoxypropylene ether involved in the present invention is prepared under acidic catalyst conditions, and the acidic catalyst is one or more compositions of Lewis acids, such as tin chloride, boron trifluoride, aluminum chloride, ferric chloride, etc. Catalysts are all weak acids, and when the salt part...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/30C08G65/28
CPCC08G65/2609C08G65/30
Inventor 杜明强金一丰钱建芳董楠万庆梅严立峰
Owner ZHEJIANG HUANGMA TECH
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