Hollow glass micro-spheres surface modification method

A hollow glass microsphere, surface modification technology, applied in chemical instruments and methods, inorganic pigment treatment, dyed polymer organic compound treatment, etc., can solve the problem of insignificant modification effect, poor compatibility, easy cracking, etc. problems, to achieve the effect of improving mechanical properties, simple operation process, and increasing toughness

Inactive Publication Date: 2014-11-05
SHANGHAI MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The use of hollow glass microspheres is mostly compounded with matrix resin, especially epoxy resin. However, the preparation of such composite materials is to directly add hollow glass microspheres to the resin matrix. Untreated glass microspheres are combined with The compatibility of matrix resin is not good, there is obvious interfacial effect, and the obtained product is relatively brittle and easy to crack; although the surface treatment of hollow glass microspheres can also be seen in some documents, such as Chinese patent CN201110294464.4, directly use ethanol of KH550 Solution treatment of glass microspheres, but its modification effect is not obvious

Method used

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  • Hollow glass micro-spheres surface modification method

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Experimental program
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Effect test

Embodiment 1

[0015] Add 5g of K37 purchased from 3M to a 250ml glass beaker, then add 50ml of acetone, stir at room temperature for 3h, filter out the hollow glass microspheres, dry them in an oven at 55°C for 10h, and then transfer them into 250ml In the glass beaker, add 50ml of sodium hydroxide solution with a mass concentration of 25%, stir at room temperature for 5 hours, filter and take out the glass microbeads, then wash with acetic acid solution with a mass concentration of 1%, and finally wash with a large amount of deionized water. Finally, it was dried in a vacuum oven at 80 °C for 10 h. Put the obtained glass beads into 80ml of ethanol-deionized water mixed solution with a volume ratio of 1:1, add 1g of silane coupling agent kh550, stir at room temperature for 5h, then filter and separate the glass beads, and place them at room temperature until After the solution evaporated completely, it was dried in a vacuum oven at 60° C. for 10 h. Move the obtained hollow glass microspher...

Embodiment 2

[0017] Add 5g of K37 purchased from 3M to a 250ml glass beaker, then add 50ml of acetone, stir at room temperature for 3h, filter out the hollow glass microspheres, dry them in an oven at 55°C for 10h, and then transfer them into 250ml In the glass beaker, add 50ml of sodium hydroxide solution with a mass concentration of 25%, stir at room temperature for 5 hours, filter and take out the glass microbeads, then wash with acetic acid solution with a mass concentration of 1%, and finally wash with a large amount of deionized water. Finally, it was dried in a vacuum oven at 80 °C for 10 h. Put the obtained glass beads into 80ml of ethanol-deionized water mixed solution with a volume ratio of 1:1, add 1g of silane coupling agent kh550, stir at room temperature for 5h, then filter and separate the glass beads, and place them at room temperature until After the solution evaporated completely, it was dried in a vacuum oven at 60° C. for 10 h. Move the obtained hollow glass microspher...

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Abstract

The invention discloses a hollow glass micro-spheres surface modification method. The specific steps of the method are: (1) acetone or ethanol are used for washing the surfaces of hollow glass micro-spheres, such that dirt is removed; and a sodium hydroxide solution is used for treating, such that the surfaces of the hollow glass micro-spheres are hydroxylated; (2) the surface-hydroxylated hollow glass micro-spheres obtained in the step (1) are treated by using an ethanol-water mixed solution containing kh550; with hydrolysis of a silane coupling agent and condensation of silanol, the material is grafted on the surface of the hollow glass micro-spheres; (3) the hollow glass micro-spheres obtained in the step (2) are subjected to phosgene treatment in dichlorobenzene, such that the surface amino groups of the hollow glass micro-spheres are subjected to isocyanate modification; and with the reaction of isocyanate and hydroxyl, polyethylene glycol is grafted on the surfaces of the hollow glass micro-spheres. The hollow glass micro-spheres provided by the invention can be better dispersed in epoxy resin. Bonding strength and acting force between epoxy resin and glass micro-spheres can be improved, and strength and toughness of an epoxy resin composite material can be further enhanced.

Description

technical field [0001] The invention relates to a method for surface modification of hollow glass microspheres. The hollow glass microspheres are widely used in the fields of thermal insulation materials, military stealth materials, solid buoyancy materials and the like. Background technique [0002] Hollow glass microspheres are a new type of material developed in recent years with wide application and excellent performance. The main component of this product is borosilicate, and the particle size is generally tens of microns. In recent years, more than a dozen domestic companies have been able to produce this kind of hollow glass microspheres. The better one is Sinosteel Ma'anshan Mining Research Institute Co., Ltd., whose compressive strength can reach 14Mpa; the better foreign companies include the United States. Companies such as 3M and AGSCO, especially 3M, have developed and produced a variety of products, including K series, S series and HS, etc., especially recently...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/10C09C3/06
Inventor 吴新锋杨小瑞王瑛刘丽娜刘海燕张希琴
Owner SHANGHAI MARITIME UNIVERSITY
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