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A kind of synthetic method of epoxy-terminated polyether

A technology of end-capping polyether and synthesis method, which is applied in the field of synthesis of epoxy-terminated polyether, and can solve problems such as inconvenient use, poor selectivity, and insufficient epoxy end-capping rate

Active Publication Date: 2021-07-06
扬州晨化新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] But the above methods are generally all carried out on common reactors, and the catalysts in the reported patents are generally Lewis acid catalysts such as boron trichloride ether, titanium tetrachloride or protonic acids such as concentrated sulfuric acid and perchloric acid. The acidic catalyst will corrode the reaction equipment, and it is inconvenient to use; the ring-opening reaction is the key in the synthetic method of the two-step method, which has the disadvantage of poor selectivity, and the intermediate product α-chlorohydrin will continue to react with excess epichlorohydrin to form Polyepoxy polyether with higher degree of polymerization; more importantly, when the second step uses alkali for ring-closing reaction, due to a large amount of excess alkali, the alkali has both ring-closing and ring-opening effects. If the amount is not well controlled, it will The ring-closing of the intermediate α-chlorohydrin with good ring opening to generate terminal epoxy polyether is further opened to α-chlorohydrin and other by-products, so that the epoxy end-capping rate of the product is insufficient or the chlorine content in the product exceeds the standard

Method used

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  • A kind of synthetic method of epoxy-terminated polyether
  • A kind of synthetic method of epoxy-terminated polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 166g of ZnCl 2 Dissolve in 1000ml of distilled water, add 6mol / l NaOH solution drop by drop to form a white precipitate, wash the precipitate until there is no chloride ion, then add 1mol / l HClO dropwise 4 Solution, until the white precipitate is basically dissolved, filter, remove a small amount of insoluble matter, obtain a colorless liquid, transfer it to an evaporating dish, heat until white crystals appear, and dry at 70 ° C in an oven to obtain 261g of Zn(ClO 4 ) 2 catalyst.

Embodiment 2

[0034] Weigh 133g of AlCl 3 Dissolve in 1000ml of distilled water, add 6mol / l NaOH solution drop by drop to form a white precipitate, wash the precipitate until there is no chloride ion, then add 1mol / l HClO dropwise 4 Solution, until the white precipitate is basically dissolved, filter, remove a small amount of insoluble matter, obtain a colorless liquid, transfer to an evaporating dish, heat until white crystals appear, and dry in an oven at 70°C to obtain 305g of Al(ClO 4 ) 3 catalyst.

Embodiment 3

[0036] Add 1000 g of methoxypolyether (molecular weight 200, n≈4) and 3 g of the catalyst of Example 1 into a 5 L reaction bottle, turn on the stirrer, stir for 1 h, and then move it into metering tank 1, and the 472 g ring that was drawn into metering tank 2 in advance Oxychloropropane was continuously fed into the microchannel reactor (at a constant temperature of 40° C.) by a plunger pump to react in proportion. The reaction time in the microchannel reactor was 5 seconds, and the reaction solution was continuously collected to obtain semi-finished α-chlorohydrins.

[0037] Transfer the collected α-chlorohydrin semi-finished product into a closed-loop reactor, start stirring, cool down to room temperature, add 200g of solid NaOH, react at 35-40°C for 3 hours, cool down to room temperature, and obtain a crude product.

[0038] After the crude product is filtered to desalt, the filtrate is collected and transferred to a refining reactor, then phosphoric acid is added to neutral...

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Abstract

The invention discloses a synthesis method of epoxy-terminated polyether, which adopts self-made solid acid Zn(ClO 4 ) 2 or Al(ClO 4 ) 3 As a catalyst, the ring-opening reaction of polyether and epichlorohydrin is carried out in a microchannel reactor, and then the ring-closing reaction is carried out in the presence of a solid base to obtain a crude product, and the crude product is refined to obtain an epoxy-terminated polyether. The invention has the characteristics of high selectivity, short reaction time, less side reactions, less consumption of epichlorohydrin and the like.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to a synthesis method of epoxy-terminated polyether. Background technique [0002] Epoxy-terminated polyether can directly react with amino crude oil to produce amino silicone oil. The finished product aqueous solution is extremely stable and has excellent compatibility. Finishing agents and additives for coatings improve the recoatability of the same or different coatings, improve the boiling water resistance, superheated steam resistance, scratch resistance, etc. of the coatings. It can be used in epoxy resin diluent, catalyst, crosslinking agent and chain transfer agent, chloride stabilizer, fabric finishing agent and modified silicone oil, etc. It is an important intermediate in the synthesis of various surfactants. [0003] At present, there are two main methods of epoxy-terminated polyether: [0004] (1) One-step method, that is, phase transfer method: usi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2654C08G65/266
Inventor 房连顺董晓红陆国玲管丹
Owner 扬州晨化新材料股份有限公司
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