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Production of micron-solid epoxy-resin microsphere containing surface active group

A technology of porous epoxy resin and active groups, which is applied in the field of preparation of micron-scale non-porous epoxy resin microspheres, can solve the problems of wide particle size distribution, limited application range, and porosity of phenolic resin-based microspheres, and achieve good Toughness, low cost, and high productivity

Inactive Publication Date: 2007-11-21
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese invention patent "An Epoxy Resin Cured Microsphere Water Base and Its Preparation Method" (CN 1139614C) discloses a method for preparing micron-sized epoxy resin microspheres with active groups on the surface by using phase inversion technology. Stir the epoxy resin and emulsifier evenly according to the weight ratio of 10-99.9:0.1-90, add the curing agent at 10-50°C, add water under stirring, and carry out the curing reaction at 50-99°C for 1-10 hours to obtain the product , but the microspheres with active groups on the surface are porous microspheres
Chinese invention patent "a preparation method of phenolic resin-based microspheres" (CN 1255457C) discloses a method of mixing novolak resin with hexamethylenetetramine and dissolving it in methanol and / or ethanol to form phenolic resin alcohol solution; make surfactant and water into an aqueous solution containing surfactant; add the phenolic resin alcohol solution to the aqueous solution containing surfactant, and heat to 110-130°C under constant stirring conditions for 30-180 minutes to obtain phenolic Resin-based microspheres, although the preparation method is simple and easy, but the obtained phenolic resin-based microspheres have a wide particle size distribution and no active groups on the surface, so its application range is limited

Method used

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  • Production of micron-solid epoxy-resin microsphere containing surface active group
  • Production of micron-solid epoxy-resin microsphere containing surface active group
  • Production of micron-solid epoxy-resin microsphere containing surface active group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of epoxy resin microspheres containing -OH groups on the surface: Add 0.8g gum arabic, 0.4g sodium dodecylbenzene sulfonate and 80ml deionized water into a 250ml three-necked reaction flask, and stir to make it fully Dissolve. Under stirring conditions, 10 g of bisphenol A epoxy resin E51, 10 g of propylene oxide butyl ether and 1.6 g of modified liquid imidazole JH-0512 are mixed uniformly to obtain an oil phase system. Then the oil phase system was added to a three-necked flask, stirred and emulsified for 20 minutes, slowly heated to a temperature between 80-85°C, and reacted at a constant temperature for 4 hours. After the reaction, the heating was stopped and allowed to cool to room temperature naturally. The product is filtered and dried to obtain the initial product. The initial product was post-cured at 150° C. for 1 hour to obtain epoxy resin microspheres with a synthesis yield of 95%.

[0025] Referring to Figure 1, the epoxy resin microsphere ...

Embodiment 2

[0028] A preparation method of epoxy resin microspheres containing -OH groups on the surface: adding 1 g of gum arabic and 100 ml of deionized water into a 250 ml three-necked reaction flask, and stirring to make them fully dissolved. Under stirring conditions, mix 5g of bisphenol A epoxy resin E51, 5g of alicyclic epoxy resin TDE-85, 10g of propylene oxide butyl ether and 1.6g of 2-ethyl-4-methylimidazole. An oil phase system is obtained. Then the oil phase system was added to a three-necked flask, stirred and emulsified for 30 minutes, slowly heated to a temperature between 80-85°C, and reacted at a constant temperature for 5 hours. After the reaction, the heating was stopped and allowed to cool to room temperature naturally. The product is filtered and dried to obtain the initial product, which is post-cured at 100° C. for 3 hours to obtain epoxy resin microspheres. Its IR spectrum is at 3300cm -1 There are absorption peaks on the left and right, indicating that the prepared ep...

Embodiment 3

[0030] A preparation method of epoxy resin microspheres containing -OH groups on the surface: 0.375g gum arabic, 0.8g sodium dodecylbenzene sulfonate, 0.2g polyethylene glycol and 70ml deionized water were added to a 250ml three-necked reaction flask , Stir to fully dissolve. Under stirring conditions, 10 g of bisphenol A type epoxy resin E51, 8 g of bifunctional epoxy resin active diluent 6690 and 2 g of 2-ethyl-4-methylimidazole are mixed uniformly to obtain an oil phase system. Then the oil phase system was added to a three-necked flask, stirred and emulsified for 10 minutes, slowly heated to a temperature between 80-85°C, and reacted at a constant temperature for 3.5 hours. After the reaction, the heating was stopped and allowed to cool to room temperature naturally. The product is filtered and dried to obtain the initial product, which is post-cured at 120° C. for 2 hours to obtain epoxy resin microspheres. Its IR spectrum is at 3300cm -1 There are absorption peaks on the lef...

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Abstract

Production of micron-solid epoxy-resin micro-pill containing activated group on surface is carried out by mixing Arabic gum with emulsifier accessory and deionized water proportionally, preparing into aqueous-phase system, mixing epoxy resin with activated diluting agent and liquefied imidazole curing agent, preparing into oil-phase system, agitating, pouring oil-phase system into aqueous-phase system, mixing, emulsifying, reacting at 80-85 degree, cooling, filtering and drying to obtain final product containing -OH group. It's simple, cheap, efficient and controllable. It has homogeneous grain size distribution and can be used for chromatographic separation, eigen toughening and biological medicine.

Description

Technical field [0001] The invention relates to a preparation method of micron-level non-porous epoxy resin microspheres containing active groups on the surface, and belongs to the field of synthetic chemical materials. Background technique [0002] Micron-sized polymer microspheres are a new type of functional material with excellent performance. Its surface effect, volume effect, magnetic effect and biocompatibility make it useful in solid-phase organic synthesis, medicine and biochemistry, biomedicine, Analytical chemistry, colloidal science, and chromatographic separation have shown great application prospects. The synthesis and surface modification of micron-sized polymer microspheres are currently one of the new hotspots in the field of functional polymers. [0003] Micron-sized non-porous epoxy resin microspheres are a kind of polymer microspheres that have attracted people's attention in recent years. They have outstanding chemical stability, good ...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08G59/00B01J13/02
Inventor 梁国正顾嫒娟谢建强袁莉张增平
Owner SUZHOU UNIV
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