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Method for preparing modified white carbon black

A white carbon black and modified technology, applied in the direction of fibrous filler, dyed low molecular organic compound treatment, dyed high molecular organic compound treatment, etc. Carbon black and coupling agent bond energy, complex process operability and other problems, to achieve the effect of low price, good dispersion and simple process

Active Publication Date: 2016-08-17
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN200910142771.3 mentioned a preparation method of modified white carbon black, adopting activated white carbon black to mix with silane coupling agent under the action of ethanol, carry out primary modification, then mix with toluene isocyanate, carry out secondary modification , this method belongs to wet modification, the coupling agent and silica are still combined by hydrogen bonds and van der Waals forces with low bond energy, and its process operation is complicated
CN201010504667.7 mentions a method for modifying nano-silica used in highly dispersed rubber compounding agents, using nano-silica to disperse in deionized water, and then adding a silane coupling agent absolute ethanol solution dropwise to the mixed solution method, this method belongs to wet modification, and does not solve the problem of low bond energy between silica and coupling agent
201110356195.X mentioned a gas-phase silica modification method, adding pre-activated silica to a slightly acidic liquid-phase modification system composed of water, ethanol, and silane coupling agent for modification, and then through 150 ° C vacuum Remove low molecular weight to obtain modified products. This method belongs to wet modification. The purpose of the vacuum process is to dry and devolatilize, and it does not promote the silanization reaction.
Therefore, the existing modification technology cannot effectively solve the technical problems that white carbon black is difficult to disperse and easy to agglomerate, and the modification effect is limited.

Method used

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  • Method for preparing modified white carbon black
  • Method for preparing modified white carbon black
  • Method for preparing modified white carbon black

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preparation example Construction

[0026] A preparation method of modified white carbon black, comprising the steps of:

[0027] Step 1: Add white carbon black to the reaction kettle, vacuumize, heat to 130-150°C, and stir for 2-3 hours;

[0028] Step 2: Using an inert gas to raise the pressure to 4-6MPa, keep the temperature constant, and shear for 1-1.5 hours; and

[0029] Step 3: Spray the modifying agent, raise the temperature to 150-165°C, vacuumize and stir at the same time, react for 1-2 hours, dry and discharge.

[0030] (1) Source of material

[0031] Silica Rhodia

[0032] Modifier bis(triethoxysilylpropyl)tetrasulfide Degussa

[0033] Modifier γ-(2,3-Glycidoxy)propyltrimethoxysilane Shanghai Jingrong Biotechnology Co., Ltd.

[0034] Modifier Pentaerythritol Jinan Century Tongda Chemical Co., Ltd.

[0035] Rubber solution polystyrene butadiene rubber SSBR2557S Dushanzi Petrochemical Branch

[0036] Other additives are commonly used additives in the rubber industry.

[0037] (2) Analysis method ...

Embodiment 1

[0043] (1) Add 1000 grams of white carbon black into the grafting reactor, vacuumize, stir (speed 50r / min), heat to 135°C, and activate the white carbon black structure for 2 hours.

[0044] (2) Use inert gas to raise the pressure to 4MPa, keep the temperature at 140°C, and forcefully shear (shear rate 950r / min), and dissociate the structure for 1 hour.

[0045] (3) 80 grams of bis(triethoxysilylpropyl) tetrasulfide was sprayed slowly and uniformly in the form of a spray, stirred (speed 90r / min), heated to 155°C, and vacuumed at the same time, and the grafting reaction was carried out for 1.5 hours .

[0046] (4) After drying and cooling, graft-modified white carbon black is obtained.

Embodiment 2

[0059] (1) Add 1000 grams of white carbon black into the grafting reactor, vacuumize, stir (speed 60r / min), heat to 135°C, and activate the white carbon black structure for 2 hours.

[0060] (2) Use inert gas to increase the pressure to 4MPa, keep the temperature at 140°C, and forcefully shear (shear rate 1100r / min), dissociate the structure for 1.5 hours.

[0061] (3) 120 grams of γ-(2,3-glycidyloxy)propyltrimethoxysilane was sprayed slowly and uniformly in the form of a spray, stirred (speed 90r / min), heated to 155°C, and vacuumed at the same time, The grafting reaction was carried out for 1.5 hours.

[0062] (4) Drying and cooling to obtain graft modified white carbon black.

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Abstract

The invention provides a method for preparing primary structure-grafted and modified white carbon black. Under conditions of high temperature, high pressure and high shear, a white carbon black aggregation is dissociated, and a primary structure is formed, through a grafting reaction of the primary structure white carbon black and a modifier, finally, a primary-structure white carbon black modifier grafting substance is formed. According to the invention, problem of self agglomeration of the white carbon black can be effectively solved, and uniform modification of the white carbon black is realized.

Description

technical field [0001] The invention relates to the field of inorganic non-metallic materials, in particular to a preparation method of modified white carbon black. Background technique [0002] White carbon black, also known as silica, has the characteristics of multi-structure, large specific surface area, good chemical stability, and high temperature resistance. It has been widely used in rubber reinforcing agents. As an excellent active reinforcing agent, it can significantly improve The tear resistance of the compound is already the second largest reinforcing agent after carbon black. However, due to the presence of a large number of active silanol groups and hydroxyl groups on its surface, it has strong hydrophilicity and self-polymerization, so its application performance is greatly affected. [0003] In recent years, people have done a lot of research on silica modification technology. CN200910050337.2 mentioned a method of coupling agent modified silica to enhance ...

Claims

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Application Information

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IPC IPC(8): C09C1/28C09C3/12C09C3/08C09C3/10C08K9/06C08K9/04C08K3/36C08L9/06
Inventor 赵洪国吴宇崔英张华强杨玉琼李波何连成燕鹏华胡海华王锋宋中勤朱晶郑红兵董静宋同江丛日新
Owner PETROCHINA CO LTD
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