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Acetylene diol polyether and preparation method thereof

A technology of acetylene glycol polyether and acetylene glycol, which is applied in the field of acetylene glycol polyether and its preparation, can solve problems such as high cost and complex process, and achieve the effects of low production cost, high catalytic activity, and low conductivity

Active Publication Date: 2021-06-04
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this synthesis method requires solvents such as anhydrous ether, tetrahydrofuran and methyl ethyl ether as extraction agents, and after layers, rectification and other processes, the process is complicated and the cost is high.

Method used

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  • Acetylene diol polyether and preparation method thereof

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preparation example Construction

[0030] Such as figure 1 Shown, the preparation method of acetylenic glycol polyether of the present invention comprises the following steps:

[0031] Step 100. First add the solid metal oxide support to the impregnation solution for impregnation, and then calcinate the impregnated solid metal oxide support to obtain a supported solid catalyst; the impregnation time is preferably 8 hours, and the calcination temperature is preferably 500°C ~550°C, the calcination time is preferably 5 hours; the specific operation can be: first add the solid metal oxide carrier to the impregnation solution for 8 hours, and then put the impregnated solid metal oxide carrier into the muffle furnace, at 500- Calcined at 550°C for 5 hours to obtain a supported solid catalyst.

[0032] Step 200. Add the supported solid catalyst and acetylenic diol into the reaction kettle, and replace the nitrogen in the reaction kettle, add epoxy oxide dropwise at a certain reaction temperature and pressure, and co...

Embodiment 1

[0040] First put 226g of molten 2,4,7,9-tetramethyl-5-decyne-4,7-diol into the polymerization reactor, then drop into 2.6g of loaded solid catalyst, the loaded solid catalyst consists of 10%wt Al impregnation with phosphoric acid solution 2 o 3 The carrier was prepared by calcination; then after the feeding was completed, the air in the kettle was replaced with nitrogen twice, and at the same time, the stirring was started to fully mix the materials; then the temperature of the reaction kettle was raised to 60°C, and 176g ring Ethylene oxide and 116g propylene oxide, and control the reaction temperature in the kettle to 60±2°C and the pressure in the kettle to 0.3-0.5MPa, and continue to ripen the reaction until the pressure does not change after the dropwise addition, and the ripening temperature is 60±2 °C; finally, after the aging reaction is completed, vacuum remove traces of unreacted ethylene oxide and propylene oxide, lower the temperature to 50 °C, and filter to obtai...

Embodiment 2

[0053] First put 226g of molten 2,4,7,9-tetramethyl-5-decyne-4,7-diol into the polymerization reactor, and then put into 6.34g of supported solid catalyst, which is 10%wt nitric acid Potassium solution impregnated Al 2 o 3 The carrier was prepared by calcination; then, after the feeding was completed, the air in the kettle was replaced with nitrogen for 2 times, and at the same time, the stirring was started to fully mix the materials; then the temperature of the reaction kettle was raised to 90°C, and 176g ring Ethylene oxide and 232g propylene oxide, and control the reaction temperature in the kettle to 90±2°C and the pressure in the kettle to 0.3-0.5MPa, and continue to ripen the reaction until the pressure does not change after the dropwise addition is completed, and the ripening temperature is 90±2 °C; Finally, after the aging reaction is completed, vacuum remove traces of unreacted ethylene oxide and propylene oxide, lower the temperature to 50 °C, and filter to obtain ...

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Abstract

The invention relates to alkyne diol polyether and a preparation method thereof. The structural general formula of the alkyne diol polyether is shown in the specification, wherein R1 and R4 are methyl or ethyl, R2 and R3 are C3-C8 saturated alkyl groups, and n+m+x+y are integers from 1 to 20; and the alkyne diol polyether is prepared from a solid metal oxide carrier, alkyne diol, a dipping solution and epoxide. The preparation method comprises the steps: adding the solid metal oxide carrier into the dipping solution, dipping, and calcining to obtain a supported solid catalyst; and then adding the supported solid catalyst and alkyne diol into a reaction kettle, filling the reaction kettle with nitrogen, dropwise adding epoxide at a certain reaction temperature and pressure, continuously keeping the temperature until the pressure does not change after dropwise adding is completed, cooling to remove a small amount of unreacted epoxide, and filtering the catalyst to obtain alkyne diol polyether. The alkyne diol polyether is good in wettability, light in color and luster, low in conductivity, simple in preparation operation, low in cost, green and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of acetylene glycol polyether, and in particular relates to an acetylene glycol polyether and a preparation method. Background technique [0002] Alkyne glycol polyether is a new type of multi-functional surfactant. Its carbon-hydrogen main chain has a triple bond structure in the center, and hydroxyethoxy groups or propoxy groups are symmetrically distributed on both sides. This special structure makes it have a good reduction Dynamic Surface Tension Capability. Its good wetting performance makes it perform well in the field of inkjet ink additives, which can significantly improve the fluency of inkjet printing and the definition of printing lines. In the continuous inkjet process, it is necessary to ensure that the inkjet nozzle is not blocked and the jetting performance is good. Therefore, high-quality inkjet ink must have good dispersibility, and the salt content or conductivity should be as low as poss...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2654C08G65/266C08G65/2696Y02P20/584
Inventor 郏超伟金一丰殷其文高洪军
Owner ZHEJIANG HUANGMA TECH
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