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A kind of method that carries out ethoxylation reaction and generates polyether under photocatalytic condition

A technology of ethoxylation and photocatalysis, which is applied in the field of polyether preparation, can solve the problems of high pressure and temperature, long time and long production cycle of reaction conditions, and achieve system pressure reduction, service life extension and safety improvement Effect

Active Publication Date: 2016-09-14
SHANXI KAIDI BUILDING MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect that this method exists is that reaction condition pressure and temperature are high, time is long, product molecular weight is wider, product hydroxyl value is unstable, energy consumption is high, production cycle is long, and production cost is big

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of nano-TiO by sol-gel method 2 catalyst of light. Slowly add 8.5 kg of tetrabutyl titanate into 30 kg of absolute ethanol and stir for 0.5 h. Then add 1.2 kg of glacial acetic acid, continue to stir for 0.5 h, then add 0.6 kg of nitric acid dropwise, so that the pH of the solution is about 3. After 2 hours, slowly add a mixture of 5 kg ethanol and 0.5 kg deionized water dropwise, and continue to stir. After about 2 hours, the solution turns into a transparent sol. Stand still at room temperature for 5-6 days to obtain its gel. White TiO was obtained by drying in a drying oven at 100 °C for 8 h and calcining in a muffle furnace for 4 h. 2 powder.

Embodiment 2

[0020] Weigh 10kg of methacryl alcohol and add it to a pressure-resistant container with a sight glass, then add 180g of nanometer TiO 2 After photocatalyst and 15g anhydrous formaldehyde, pass into N 2 Replace the air and vent to normal pressure, add 325kg of ethylene oxide, mix the materials evenly by stirring and external circulation, irradiate ultraviolet light into the reaction system through the peep mirror, and raise the temperature of the reaction system to 70°C to make the reaction system The pressure reaches 2.5kg / cm 2 . Keep the temperature of the reaction system at 70-75°C by a heat exchanger, stop the reaction after 2.5 hours, and release the material.

Embodiment 3

[0022] Weigh 10kg of methacryl alcohol and add it to a pressure-resistant container with a sight glass, then add 200g of nanometer TiO 2 After the photocatalyst and 15 g of anhydrous formaldehyde, N 2 Replace the air and vent to normal pressure, add 325kg of ethylene oxide, mix the materials evenly by stirring and external circulation, irradiate ultraviolet light into the reaction system through the peep mirror, and raise the temperature of the reaction system to 75 ° C, so that the reaction system The pressure reaches 2.5kg / cm 2 . The temperature of the reaction system is kept at 75-80°C by a heat exchanger, and the reaction is stopped after 2 hours, and the materials are released.

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PUM

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Abstract

The invention relates to a method for generating polyether by virtue of ethoxylation reaction under photocatalysis conditions. The method comprises the following steps: adding an alkenyl alcohol compound into a reaction reactor; adding a nanometer TiO2 photocatalyst and a reducing agent, introducing ethylene oxide or epoxypropane after N2 replacement, fully contacting the materials by virtue of a stirring and outer circulation mode, uniformly mixing, and maintaining the pressure of the reaction system to be 2-3kg / cm<2>; introducing a light source into the reaction system for irradiating, heating to the temperature of 70-80 DEG C, and reacting in the temperature range for 2-3 hours. The environment-friendly photocatalytic polymerization process is adopted, the reaction conditions are mild, the production process is easy to control, the hydroxyl value of the product is stable, the reaction activity is high, the molecular weight distribution is uniform, and the production cost is low.

Description

technical field [0001] The invention relates to a preparation method of polyether, in particular to a method for producing polyether by reaction under photocatalytic conditions. Background technique [0002] The method of producing methacryl alcohol polyoxyethyl ether with methacryl alcohol and ethylene oxide as raw materials has been applied in industrial production. The specific steps are: first add methacryl alcohol into a pressure-resistant container, then add catalyst and stir evenly , and heat up to 100~110°C, then feed ethylene oxide, gradually polymerize the material through external circulation, and the pressure in the reaction system during the production process reaches 4~5kg / cm 2 . Since this process is an exothermic reaction, the temperature of the system is lowered through a heat exchanger to control the reaction temperature at about 110°C. Continue the reaction under these conditions until the addition of ethylene oxide is complete. After passing the product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28
Inventor 张智敏张平秦勇杨仁旺
Owner SHANXI KAIDI BUILDING MATERIALS
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