Preparation method of epoxy-terminated allyl alcohol polyether

A technology of allyl alcohol polyether and terminal allyl alcohol, which is applied in the field of preparation of epoxy-terminated allyl alcohol polyether, can solve the problems that catalysts cannot be recycled, ring-opening side reactions are many, and by-products are easily formed. Achieve the effect of good industrial application prospect, high ring-opening activity and good selectivity

Active Publication Date: 2022-01-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These two kinds of preparation methods all have the problem that ring-opening side reaction is many, easily form by-product, and by-product accounts for about 20% of total product, because by-product can't close ring and form epoxy terminal group, therefore cause product yield to be low; Secondly, Using Lewis acid or solid acid as catalyst, there are problems such as serious corrosion of equipment and catalyst cannot be recycled

Method used

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  • Preparation method of epoxy-terminated allyl alcohol polyether
  • Preparation method of epoxy-terminated allyl alcohol polyether
  • Preparation method of epoxy-terminated allyl alcohol polyether

Examples

Experimental program
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Effect test

Embodiment 4-10

[0047] In embodiment 4-10, allyl alcohol polyether synthesis method is as follows:

[0048]In a 10L autoclave, put 568g of allyl alcohol and 9.9g of potassium hydroxide catalyst into it. After full nitrogen replacement, the temperature is raised to 110°C, and 4378g of EO and PO mixture are fed. The EO in the mixture is 1095g, and PO is 3283g. After the material is finished, it is aged, singled out, and refined to prepare allyl alcohol polyether. The tested hydroxyl value is 111.08 mgKOH / g, and the converted average molecular weight is 505.

[0049] In a 5L high-pressure reactor, put 232g of allyl alcohol and 4.8g of potassium hydroxide catalyst. After fully replacing nitrogen, the temperature is raised to 110°C, and 1368g of EO and PO mixture is fed. The EO in the mixture is 904g, and PO is 464g. After the material is finished, it is aged, singled out, and refined to prepare allyl alcohol polyether. The tested hydroxyl value is 139.90 mgKOH / g, and the converted average molecul...

Embodiment 1

[0056] Weigh 3g of sodium dihydrogen phosphate, 9.2g of sodium metavanadate, 38.9g of manganese acetate, dissolve in deionized water, adjust the pH to 1.5 with sulfuric acid, stir, reflux at 70°C for 4.0h, extract with anhydrous ether, and distill the extract Dry water, crystallize to get phosphorus vanadium manganese heteropolyacid (H 3 PV 3 mn 9 o 40 ).

[0057] Weigh 20.0g of 20-40 mesh coconut shell activated carbon, H 3 PV 3 mn 9 o 40 1.0g, dissolved in deionized water, stirred and impregnated at 40°C for 5 hours, evaporated to dryness, dried in a vacuum drying oven for 12 hours to constant weight, then placed in a tube-type activation furnace, at N 2 Atmosphere, 400°C, activated for 4h to obtain solid catalyst A (H 3 PV 3 mn 9 o 40 / C) sealed and kept for later use.

Embodiment 2

[0059] Weigh 3g of potassium dihydrogen phosphate, 6.1g of potassium metavanadate, 39.5g of manganese nitrate, dissolve in deionized water, adjust the pH to 1.0 with a mixture of sulfuric acid and phosphoric acid, stir, reflux at 100°C for 5.0h, and extract with acetone. Evaporate to dryness, crystallize to get phosphorus vanadium manganese heteropolyacid (H 3 PV 2 mn 10 o 40 ).

[0060] Weigh 20.0g of 20-40 mesh coconut shell activated carbon, H 3 PV 2 mn 10 o 40 2.0g, dissolved in deionized water, stirred and impregnated at 60°C for 5 hours, evaporated to dryness, dried in a vacuum oven for 18 hours to constant weight, then placed in a tube-type activation furnace, at N 2 Atmosphere, 700°C, activated for 2h, to obtain solid catalyst B(H 3 PV 2 mn 10 o 40 / C) Sealed and stored for subsequent experimental applications.

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Abstract

The invention provides a preparation method of epoxy-terminated allyl alcohol polyether. The method is characterized by comprising the following steps of: a) adding a heteropolyacid catalyst into allyl alcohol polyether polyol, adding epoxy chloropropane, and carrying out a ring-opening reaction to prepare a chlorohydrin ether intermediate A; and b) in an oxygen-free environment, adding an alkaline aqueous solution into the chlorohydrin ether intermediate A, stirring, neutralizing and adsorbing after the reaction is finished, and filtering to obtain the epoxy-terminated allyl alcohol polyether. According to the invention, a solid catalyst is prepared by adopting activated carbon loaded phosphorus vanadium manganese heteropoly acid, so that the selectivity of the ring-opening reaction is high, the yield of the target product is high, the use amount of the heteropoly acid is reduced, and the solid catalyst is recycled and can be repeatedly used.

Description

technical field [0001] The invention belongs to the field of end-capped polyether synthesis, and in particular relates to a preparation method of epoxy-terminated allyl alcohol polyether. Background technique [0002] The terminal hydroxyl groups of allyl alcohol polyether are replaced by epoxy groups to form epoxy-terminated polyether. Due to the introduction of epoxy ring structure, the chemical stability of polyether is enhanced, and it is stable at different pH and higher temperature. It can be used for a long time and has a wide range of applications. It is suitable for fabric finishing agents, epoxy resin thinners, paint leveling agents, and modified silicone oils. At present, the price of epoxy-terminated polyether is about 30,000 yuan / ton, the annual demand in my country is 3,000 tons, the market output value is nearly 100 million, and the prospect is good. [0003] At present, the preparation methods of epoxy-terminated polyethers mainly include the Williamson one-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/32
CPCC08G65/2666C08G65/2609C08G65/32Y02P20/584
Inventor 周昕志刘瑞阳秦承群石正阳崔通通李仁志王久龙倪晨
Owner WANHUA CHEM GRP CO LTD
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