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Method for preparing phenolic resin microspheres by adopting imidazole binuclear alkaline functionalized ionic liquid as catalyst

A technology of ionic liquid and phenolic resin, which is applied in the field of preparing phenolic resin microspheres, can solve the problems of low yield, long time consumption, and low catalyst activity, and achieve high yield, improved alkali strength distribution, and high catalytic activity.

Inactive Publication Date: 2019-04-05
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the disadvantages of low catalyst activity, long time-consuming preparation process of phenolic resin microspheres, and low yield of target microspheres with a diameter of 0.01-0.15mm in the prior art, and to provide a catalyst using dual-nuclear alkaline ionic liquids. Method for preparing phenolic resin microspheres

Method used

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  • Method for preparing phenolic resin microspheres by adopting imidazole binuclear alkaline functionalized ionic liquid as catalyst
  • Method for preparing phenolic resin microspheres by adopting imidazole binuclear alkaline functionalized ionic liquid as catalyst
  • Method for preparing phenolic resin microspheres by adopting imidazole binuclear alkaline functionalized ionic liquid as catalyst

Examples

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Embodiment 1

[0024] Phenol and formaldehyde are used as raw material monomers. First, prepare a 6.5wt% polyvinyl alcohol solution, pour it into a 1L reactor, heat it to 70°C, then add phenol and formaldehyde with a molar ratio of 1:1.6, and add 0.9wt% imidazole dinuclear alkaline Functionalized ionic liquid catalyst (1) and 500ml deionized water, at the same temperature, reacted for 4h at a stirring speed of 150r / min, then changed the stirring speed to 300r / min, added 6.0wt% hexamethylenetetramine, And slowly raise the temperature to 90°C, and finally react at this stirring speed and temperature for 4h to terminate. After the reaction temperature drops to normal temperature, unload the material, wash repeatedly with 70°C deionized water until the upper layer solution is clear, then filter and dry at 110°C for a period of time to obtain phenolic resin microspheres. After the filtrate is cooled to room temperature, the imidazole-based binuclear basic functionalized ionic liquid and water ar...

Embodiment 2

[0026] Phenol and formaldehyde are used as raw material monomers. First, prepare a 6.5wt% polyvinyl alcohol solution, pour it into a 1L reactor, heat it to 80°C, then add resorcinol and formaldehyde with a molar ratio of 1:1.8, and add 0.5wt% imidazole dinuclear Alkaline functionalized ionic liquid catalyst (2) and 500ml deionized water, at the same temperature, react at 150r / min stirring speed for 4h, then change the stirring speed to 300r / min, add 6.0wt% hexamethylene tetra Amine, and slowly warming up to 95 ° C, and finally reacted at this stirring speed and temperature for 4h to terminate. After the reaction temperature drops to normal temperature, unload the material, wash repeatedly with 70°C deionized water until the upper layer solution is clear, then filter and dry at 110°C for a period of time to obtain phenolic resin microspheres. After the filtrate is cooled to room temperature, the imidazole-based binuclear basic functionalized ionic liquid and water are automati...

Embodiment 3

[0028] Phenol and formaldehyde are used as raw material monomers. First, prepare a 6.5wt% polyvinyl alcohol solution, pour it into a 1L reactor, heat it to 85°C, then add p-cresol and formaldehyde with a molar ratio of 1:1.7, and add 0.3wt% imidazole at the same time The dual-nuclear alkaline functionalized ionic liquid catalyst (3) and 500ml of deionized water were reacted at the same temperature for 4 hours at a stirring speed of 150r / min, and then the stirring speed was changed to 300r / min, and 6.0wt% hexamethylene was added Tetramine, and slowly warming up to 100°C, and finally reacting at this stirring speed and temperature for 4h to terminate. After the reaction temperature drops to normal temperature, unload the material, wash repeatedly with 70°C deionized water until the upper layer solution is clear, then filter and dry at 110°C for a period of time to obtain phenolic resin microspheres. After the filtrate is cooled to room temperature, the imidazole-based binuclear...

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Abstract

The invention belongs to the field of ionic liquid catalysis, in particular to a method for preparing phenolic resin microspheres by adopting an imidazole binuclear alkaline functionalized ionic liquid as a catalyst. The method includes adopting phenol and formaldehyde as raw materials and the imidazole binuclear basic functionalized ionic liquid as a catalyst to catalyze and prepare the phenolicresin microspheres; and after the reaction is finished, filtering and separating the phenolic resin microspheres when the resin is hot, cooling the filtrate water phase to room temperature, automatically separating the ionic liquid and the water, and separating the imidazole binuclear alkaline functionalized ionic liquid to reuse. The ionic liquid adopted by the method has simple preparation process and high catalytic activity, the ionic liquid can be reused, the prepared phenolic resin microspheres have smooth surfaces, uniform sphere diameters and high product yield with a target microspherediameter of 0.01-0.15 mm.

Description

technical field [0001] The invention belongs to the field of ionic liquid catalysis, and in particular relates to a method for preparing phenolic resin microspheres by using imidazole dinuclear basic functionalized ionic liquid as a catalyst. Background technique [0002] As one of the three major thermosetting resins, phenolic resin has gained industrial recognition due to its easy-to-obtain raw materials, low price, simple and mature production process, low investment in manufacturing and processing equipment, easy molding, and performance after curing to meet various requirements. Wide range of applications. At present, the process of synthesizing phenolic resin balls adopts traditional techniques (Qin Zhengyong. Preparation and application of phenolic resin-based spherical activated carbon [D]. East China University of Science and Technology, 2012.), using inorganic acids and bases as catalysts, the synthesis process is complicated and time-consuming Longer, the condens...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10
CPCC08G8/10Y02P20/584
Inventor 李为民李娜张杨任庆功
Owner CHANGZHOU UNIV
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