Method for preparing white carbon black hybridized material prepared by modification with end chlorosilane polymer

A hybrid material and polymer technology, applied in the treatment of dyed polymer organic compounds, fibrous fillers, etc., can solve the problems of unsatisfactory compatibility, blending of silica and polymers, etc., to reduce the phenomenon of agglomeration, Good economic and social benefits, the effect of improving affinity

Active Publication Date: 2011-11-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to solve the problem of unsatisfactory compatibility between white carbon black and polymer blending in the prior art, and to provide a preparation of polymer-based chlorosilane-white carbon black organic-inorganic hybrid material with simple process method

Method used

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  • Method for preparing white carbon black hybridized material prepared by modification with end chlorosilane polymer
  • Method for preparing white carbon black hybridized material prepared by modification with end chlorosilane polymer
  • Method for preparing white carbon black hybridized material prepared by modification with end chlorosilane polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1) Take a three-neck bottle, put C 4 h 9 SiCl 3 Formulated to 5×10 -5 mol / ml cyclohexane solution, filled with nitrogen, and set aside. Formulate tetramethylethylenediamine into 5×10 -4 mol / ml cyclohexane solution, filled with nitrogen, and set aside. Take another three-necked bottle, weigh 100g of fumed silica and put it into it, then place the three-necked bottle in a vacuum oven at 120°C with a relative vacuum pressure of about 0.1MPa and bake for 2 hours, then fill it with nitrogen, and set it aside.

[0036] 2) Add 20 g of anionic active butadiene-styrene random polymer into a 250 ml three-necked bottle, and sample 1. Use a pipette to take 23.5ml of C 4 h 9 SiCl 3 The cyclohexane solution was added into the polymerization bottle, and reacted at 30°C for 10 minutes to obtain a terminal chlorosilylated polymer, sample 2.

[0037] 3) Take a cyclohexane solution containing 10 g of a terminal chlorosilylated polymer and add it to 100 g of white carbon black, mi...

Embodiment 2

[0042] 1) Take a three-neck bottle, put CH 3 SiCl 3 Formulated to 5×10 -5 mol / ml cyclohexane solution, filled with nitrogen, and set aside. Make triethylamine into 5×10 -4 mol / ml cyclohexane solution, filled with nitrogen, and set aside. Take another three-necked bottle, weigh 80g of precipitated silica and put it into it, then place the three-necked bottle in a vacuum oven at 120°C with a relative vacuum pressure of about 0.1MPa and bake for 2 hours, then fill it with nitrogen, and set it aside.

[0043] 2) Add 20 g of anionic active butadiene-styrene random polymer into a 250 ml three-necked flask, and sample 1. Take 18.6ml CH with a pipette 3 SiCl 3 The cyclohexane solution was added into the polymerization bottle, and reacted at 40°C for 10 minutes to obtain a terminal chlorosilylated polymer, sample 2.

[0044] 3) Take 10 g of the obtained terminal chlorosilylated polymer / cyclohexane and add it to 80 g of white carbon black, mix well, and add 1.9 ml of triethylamin...

Embodiment 3

[0049] 1) Take a three-neck bottle, put CH 3 SiCl 3 Formulated to 5×10 -5 mol / ml cyclohexane solution, filled with nitrogen, and set aside. Take another three-necked bottle, weigh 20g of fumed silica and put it into it, then place the three-necked bottle in a vacuum oven at 120°C with a relative vacuum pressure of about 0.1MPa and bake for 2 hours, then fill it with nitrogen, and set it aside.

[0050] 2) Add 20 g of anionic active butadiene-styrene random polymer into a 250 ml three-necked flask, and sample 1. Take 13ml CH with a pipette 3 SiCl 3 The cyclohexane solution was added into the polymerization bottle, and reacted at 50°C for 10 minutes to obtain a terminal chlorosilylated polymer, sample 2.

[0051] 3) Take 10 g of the prepared cyclohexane of the terminal chlorosilylated polymer, add 20 g of white carbon black into it, mix well, and react for 5 hours. Reaction conditions: heating in a water bath at 50° C., and the whole reaction process is carried out under ni...

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Abstract

The invention discloses a method for preparing a white carbon black hybridized material prepared by modification with an end chlorosilane polymer, belonging to the field of synthesis of hybridized materials. The method comprises the following steps of: (1) adding chlorosilane in an anionic reactive polymer, reacting at 30-60 DEG C for 10-40 minutes to obtain the end chlorosilane polymer, wherein the reactive polymer includes styrene polymers, polymers of derivatives of styrene, alkadiene polymers and mixtures of two or more than two of the styrene polymers, the polymers of derivatives of styrene and the alkadiene polymers; (2) mixing white carbon black and the end chlorosilane polymer uniformly, reacting at 25-100 DEG C for 1-48 hours, removing a solvent to obtain an organic/inorganic hybridized material of the end chlorosilane polymer bonded with white carbon black, wherein the mass ratio of the end chlorosilane polymer to the white carbon black is 20:1-1:10. According to the invention, the aggregation of the white carbon black is reduced, affinity between the white carbon black and the polymer is improved, phase separation is reduced obviously, and the prepared material has excellent comprehensive performance. The method is easy to operate, the grafting efficiency is between 50% and 90%, and the prepared white carbon black as an organic hybridized material has the grafting grade being about 0.025:1-9:1.

Description

technical field [0001] The invention belongs to the synthesis field of organic-inorganic hybrid materials formed by grafting polymer compounds with inorganic substances, and in particular relates to a method for preparing organic-inorganic hybrid materials of polymer-based chlorosilane and inorganic material white carbon black. Background technique [0002] Silica is a nanomaterial with small particle size, large specific surface area, high surface activity and easy to form high-structure aggregates. There are a large number of hydroxyl groups on the surface of silica, and these hydroxyl groups are divided into two types, one is a single hydroxyl group, called an isolated hydroxyl group; the other is a continuous adjacent hydroxyl group, and these hydroxyl groups will form hydrogen bonds with each other . Silica is mainly used as a rubber reinforcing filler, in addition, it is also widely used in the plastic industry, coatings and other industries. When silica is blended w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/10C08K9/06C08K3/36C08F8/42
Inventor 韩丙勇路蓬鲁建民张立群
Owner BEIJING UNIV OF CHEM TECH
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