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Synthetic method of sucrose polyoxypropylene

A polyoxypropylene ether and synthesis method technology, applied in the field of organic compounds, can solve problems such as uneven mixing of materials, residual propylene oxide, dark product color, etc., to reduce color deepening, increase yield, and save production time Effect

Inactive Publication Date: 2016-05-25
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, the melting point of sucrose is relatively high, reaching 186°C. The traditional synthesis method of sucrose polyoxypropylene ether is to react with propylene oxide at high temperature under pressure and KOH catalysis, which will cause the product to have a deep color, and because it cannot be used The external circulation device causes uneven mixing of materials, resulting in residual propylene oxide, which has caused environmental pollution and waste of resources, and uses KOH catalyst, which requires post-treatment dehydration, adsorption and desalination
Although the patent 201410159270.7 (application number) solved the problem that the external circulation device cannot be used in the synthesis of sucrose polyether, the use of organic amine catalysts did not solve the problem of deep color of the product

Method used

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  • Synthetic method of sucrose polyoxypropylene

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Experimental program
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Effect test

Embodiment 1

[0036] In the reaction kettle, add 513g of sucrose, 1.5g of boron trifluoride ether, and 500g of diethylene glycol diethyl ether. 2 The air in the reaction kettle was replaced, and after three replacements, the temperature was raised to 110 °C under nitrogen protection, and kept for 4 hours. After the material in the kettle was completely melted, vacuumed for 15 minutes, and then the reaction temperature was controlled to 115 °C, and the pressure of the reaction kettle was -0.05 -0.4Mpa, continue to add 914g of propylene oxide, after adding, keep warm and continue the reaction until the reaction pressure no longer drops. After the reaction is completed, the temperature is lowered to 70°C, and the unreacted propylene oxide is removed by vacuum degassing. The mother liquor is gradually heated to 115°C and subjected to vacuum distillation for 9 hours to obtain the product. After the solvent vapor is cooled, it can be used again.

[0037] The product was analyzed by liquid chromat...

Embodiment 2

[0039] In the reactor, add 513g of sucrose, 1.5g of boron trifluoride ethyl ether, and 492g of diethylene glycol diethyl ether obtained by recycling are evacuated with a vacuum pump, using N 2 The air in the reaction kettle was replaced, and after three replacements, the temperature was raised to 110 °C under nitrogen protection, and kept for 4 hours. After the material in the kettle was completely melted, vacuumed for 15 minutes, and then the reaction temperature was controlled to 115 °C, and the pressure of the reaction kettle was -0.05 -0.4Mpa, continue to add 914g of propylene oxide, after adding, keep warm and continue the reaction until the reaction pressure no longer drops. After the reaction is completed, the temperature is lowered to 70°C, and the unreacted propylene oxide is removed by vacuum degassing. The mother liquor is gradually heated to 115°C and subjected to vacuum distillation for 9 hours to obtain the product. After the solvent vapor is cooled, it can be use...

Embodiment 3

[0042] In the reaction kettle, add 513g of sucrose, 1.0g of boron trifluoride ether, 510g of ethylene glycol di-n-butyl ether and evacuated with a vacuum pump, using N 2 The air in the reactor was replaced, and after three replacements, the temperature was raised to 110 °C under nitrogen protection, and kept for 4 hours. After the material in the reactor was completely dissolved, vacuumize for 15 minutes, and then control the reaction temperature to 118 °C and the pressure of the reactor at -0.05 -0.4Mpa, continue to add 914g of propylene oxide, after adding, keep warm and continue the reaction until the reaction pressure no longer drops. After the reaction is completed, the temperature is lowered to 70°C, and the unreacted propylene oxide is removed by vacuum degassing. The mother liquor is gradually heated to 120°C and subjected to vacuum distillation for 9 hours to obtain the product. After the solvent vapor is cooled, it can be used again.

[0043] The product was analyzed...

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Abstract

The invention relates to sucrose polyoxypropylene and a synthetic method thereof, and belongs to the technical field of organic compounds. The synthetic method includes: taking sucrose and propylene oxide as raw materials, adding the sucrose, catalyst and ether solvent into a reaction kettle, performing vacuum pumping, and heating up in nitrogen protection till the sucrose is completely dissolved in the ether solvent; adding a chain extension agent, heating up to perform polyreaction of the sucrose polyoxypropylene prior to cooling, and subjecting crystallization mother liquor to normal pressure or decompression rectification to separate ether solvent which can be applied to a next reaction process. The method is applied to synthesis of the sucrose polyoxypropylene, realizes high yield and high hydroxyl value, and ensures that the color value is under 30, and the requirements on both degree of polymerization and color value can be met.

Description

technical field [0001] The invention relates to a method for synthesizing sucrose polyoxypropylene ether, and belongs to the technical field of organic compounds. Background technique [0002] Polyether polyol resin is the main raw material for the production of various polyurethane products. Although there are hundreds of polyether polyol resins of different brands produced at home and abroad, sucrose, mannitol, sorbitol and xylitol are used in rigid polyurethane foam. Among the polyether varieties such as , pentaerythritol, glucoside, ethylenediamine, urea, and glycerol, sucrose polyether occupies a dominant position. The reason is: [0003] (1) As a starting agent, sucrose has a larger molecular weight (342.3), and the production of polyether with the same molecular weight consumes less epoxide, which saves the amount of epoxide, which is beyond the reach of the other starting agents mentioned above. of. [0004] (2) Sucrose is relatively stable, and it is easier to re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2606C08G2650/26
Inventor 金洪财金一丰马定连颜吉校沈天维
Owner ZHEJIANG HUANGMA TECH
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