Method for superfine particle surface modification

A technology of ultra-fine particles and surface modification, which is applied in the treatment of dyed polymer organic compounds, etc., and can solve problems such as complex processes, harsh reaction conditions, and numerous steps

Inactive Publication Date: 2006-06-21
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many steps, harsh reaction conditions, complicated process and other problems

Method used

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  • Method for superfine particle surface modification
  • Method for superfine particle surface modification
  • Method for superfine particle surface modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] AB 2 (A: ester group, B: hydroxyl) monomer: the synthesis of N, N-dihydroxyethyl-3-propionic acid methyl ester monomer:

[0020] Weigh diethanolamine and methyl acrylate at a molar ratio of 1:1, use methanol as solvent, and place in a four-neck flask under N 2 Protected, 40°C, constant temperature under magnetic stirring for 4h, the solvent methanol was distilled off under reduced pressure to obtain a light yellow transparent liquid, which was N,N-dihydroxyethyl-3-propionic acid methyl ester monomer.

[0021] nano-SiO 2 Modification reaction of grafted hyperbranched poly(amine-ester) (AB 2 monomer, melt polymerization):

[0022] Weigh 1g nano-SiO 2 , 0.023~0.0702molN, N-dihydroxyethyl-3-propionic acid methyl ester monomer and 0.03~0.07g p-toluenesulfonic acid were placed in a four-necked bottle, and vigorously stirred at 120°C for 10h under nitrogen protection. A light yellow viscous substance was obtained, which was washed with ethanol and centrifuged to precipita...

Embodiment 2

[0032] A 2 Synthesis of B monomer (A: ester group, B: hydroxyl group): N-hydroxyethyl-3-amino-N, N-methyl dipropionate):

[0033] Weigh ethanolamine and methyl acrylate at a molar ratio of 1:2, use methanol as solvent, and place in a four-neck flask under N 2 Protected, 40 ℃, constant temperature under magnetic stirring for 4h, solvent methanol was distilled off under reduced pressure to obtain a colorless and transparent liquid, namely N-hydroxyethyl-3-amino-N,N-methyl dipropionate) .

[0034] nano-SiO 2 Modification reaction of grafted hyperbranched poly(amine-ester) (A 2 B, solution polymerization):

[0035] Weigh 1g nano-SiO 2 , 0.01~0.0468mol 2-hydroxyethyl-N, N-di(methyl propionate) monomer and 0.01~0.04g p-toluenesulfonic acid and 15ml decahydronaphthalene in a four-necked bottle, under nitrogen protection at 140 ℃, vigorously stirred for 12h. A yellow sticky substance was obtained, which was washed with chloroform and centrifuged to precipitate (1.5×10 4 rpm), th...

Embodiment 3

[0045] Modification reaction of nano carbon black surface grafted hyperbranched poly(amine-ester)(AB 2 monomer, melt polymerization):

[0046] Weigh 1g of nano-carbon black, 14g of N,N-dihydroxyethyl-3-propionic acid methyl ester monomer and 0.07g of p-toluenesulfonic acid into a four-necked bottle, and vigorously stir at 130°C for 10h under nitrogen protection. A black sticky substance was obtained, which was washed with ethanol and centrifuged to precipitate (1.5×10 4 rpm), the precipitate was washed with ethanol and centrifuged again, and the above steps were repeated until no unreacted substance was detected in the washing solution. The precipitate was vacuum-dried at 30° C. for 6 hours to obtain hydroxyl-terminated hyperbranched poly(amine-ester) graft-modified nano-carbon black.

[0047] Compared with ungrafted nano-carbon black, 1700cm on the FT-IR spectrogram of the product after reaction -1 The characteristic absorption peak of C=O carbonyl group is obviously stren...

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Abstract

The invention relates to a new method for surface modification of ultrafine inorganic solid particles. It includes under the conditions of certain temperature, mechanical stirring, nitrogen protection and the presence of catalyst, with ultrafine particles as the reaction center core, and AB x or A x One-step polycondensation reaction of monomer B occurs, and a hyperbranched polymer is grafted on the surface of ultrafine particles. The surface properties of the superfine particles modified by the hyperbranched polymer grafting obtained are greatly changed, and can be well dispersed in various resin matrices and solvents. The method is simple and easy to complete in one step, and the modified inorganic solid particles can be widely used in polymer composite materials, electronic packaging materials, plastics, coatings, rubber, antibacterial materials and other fields, and the industrial application prospect is broad.

Description

technical field [0001] The invention relates to a new method for surface modification of ultrafine particles. Background technique [0002] As we all know, the application fields of ultrafine particles are very extensive. Taking nano-silica as an example, it can be widely used in electronic packaging materials, resin-based composite materials, plastics, coatings, rubber and antibacterial materials and other fields. However, due to the large surface energy of ultrafine particles, they are easy to agglomerate, making it difficult to disperse evenly into the polymer matrix. Directly add untreated ultrafine particles, the addition amount is generally at a very low level (generally below 1%), then the effect of ultrafine particles cannot be fully reflected. Therefore, solving the problem of ultrafine particle agglomeration and improving its dispersion in the matrix has become an important research direction. The method to solve the agglomeration and poor dispersion of ultrafin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C3/10
Inventor 罗运军赵辉
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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