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New method for superfine particle surface modification

A technology of ultra-fine particles and surface modification, which can be used in the treatment of dyed polymer organic compounds, etc., and can solve the problems of harsh reaction conditions, numerous steps, and complicated processes.

Inactive Publication Date: 2005-02-16
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

Method used

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  • New method for superfine particle surface modification
  • New method for superfine particle surface modification
  • New method for superfine particle surface modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] AB 2 (A: ester group, B: hydroxyl) monomer: the synthesis of N, N-dihydroxyethyl-3-propionic acid methyl ester monomer:

[0021] 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.

[0022] nano-SiO 2 Modification reaction of grafted hyperbranched poly(amine-ester) (AB 2 monomer, melt polymerization):

[0023] 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

[0033] A 2 Synthesis of B monomer (A: ester group, B: hydroxyl group): N-hydroxyethyl-3-amino-N, N-methyl dipropionate):

[0034] 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) .

[0035] nano-SiO 2 Modification reaction of grafted hyperbranched poly(amine-ester) (A 2 B, solution polymerization):

[0036]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), t...

Embodiment 3

[0046] Modification reaction of nano carbon black surface grafted hyperbranched poly(amine-ester)(AB 2 monomer, melt polymerization):

[0047] 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.

[0048] 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 refers to a kind of new method of superfine inorganic solid particle's surface modification method. It includes the following steps: in the condition of certain temperature, mechanical milling, the protection of nitrogen gas and the existence of catalyzer, choose the superfine particle as the reaction core, pass through the polycondensation with the monomer of ABx or AxB and graft the super-ramus polymer onto the surface of superfine particle. The surface character of superfine particle modified by the super-ramus polymer grafting is changed greatly and can disperse well in all kind of matrixes of rosin and solvent. The method can finish the task in one step. The modified inorganic solid particle can be applied to macromolecule composites, electric bloching material, plastics, dope, latex, antibiotic material and other fields and has a promising industrial application.

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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IPC IPC(8): C09C3/10
Inventor 罗运军赵辉
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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