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Method of preparing precipitation method white carbon black by improved dropwise adding process

A precipitation method of silica and process technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of affecting purity, unsuitable for rubber reinforcing fillers, and increasing investment in environmental management and governance. The effect of emissions

Active Publication Date: 2019-02-22
ZHUZHOU XINGLONG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101659415A adds a silane coupling agent to the water glass solution before the reaction, and then uses hydrochloric acid as a precipitating agent to prepare precipitation white carbon black. Although it can solve the problem that white carbon black particles are prone to agglomeration, it affects its purity and is not suitable for use. Reinforcing filler for rubber
CN14347000A proposes two-step method to prepare the method for precipitated white carbon black, by adding acidulant in water glass to react to medium pH7.0~9.2, under the situation of keeping pH constant, import remaining acidulant and water glass simultaneously, Preparation of silica powder, but this method is prone to gelation, uncontrollable particle size, low stability, and limitations
Moreover, in the above-mentioned synthesis process of precipitation method silica, due to the need for continuous dripping during the synthesis process of acid and alkali, a certain amount of water vapor and acid gas will be discharged, which increases the investment in environmental management and treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The method for preparing the precipitated white carbon black by improving the dripping process specifically comprises the following steps:

[0055] (1) Add 37 cubic meters of process hot water (soft water with 600kg of sodium chloride electrolyte) into the white carbon black reaction kettle, start the synthesis reaction kettle to stir, and control the stirring speed at 400rpm; raise the temperature of the reaction bottom liquid to the required 90 After ±0.1°C, gradually pre-drop the water glass solution whose concentration was adjusted to 2.2mol / L and filtered to remove impurities, so that the content of water glass in the bottom liquid of the reaction kettle was controlled at about 0.07mol / L, and the volume of the bottom liquid was synthesized 37% of the reactor volume;

[0056] (2) After the reaction starts, the water glass solution is sprayed at a rate of 13.73 cubic meters per hour from the injection line on the tank top of the reactor, and sulfuric acid is added fr...

Embodiment 2

[0062] The method for preparing precipitated white carbon black by improving the drop-adding process specifically comprises the following steps:

[0063] ⑴. Add 45 cubic meters of process hot water (tap water) into the white carbon black reaction kettle, start the synthesis reaction kettle to stir, and control the stirring speed at 150rpm; raise the temperature of the reaction bottom liquid to 80±0.1℃ required for the reaction, and gradually prepare Add dropwise the water glass solution whose concentration is adjusted to 2.46mol / L and filter to remove impurities, so that the content of water glass in the bottom liquid of the reactor is controlled at about 0.07mol / L, and the volume of the bottom liquid is 45% of the volume of the synthesis reactor;

[0064] (2) After the reaction starts, the water glass solution is sprayed at a rate of 12.45 cubic meters per hour from the injection line on the tank top of the reactor, and sulfuric acid is added from the tank bottom injection lin...

Embodiment 3

[0070] The method for preparing the precipitated white carbon black by improving the dripping process specifically comprises the following steps:

[0071] ⑴. Add 43 cubic meters of process hot water (pure water) into the silica reaction kettle, start the synthesis reaction kettle to stir, and control the stirring speed at 300rpm; after the temperature of the reaction bottom liquid is raised to 85±0.1℃ required for the reaction, gradually Pre-drop the water glass solution that has been adjusted to a concentration of 2.2mol / L and filtered to remove impurities, so that the content of water glass in the bottom liquid of the reactor is controlled at about 0.07mol / L, and the volume of the bottom liquid is 43% of the volume of the synthesis reactor ;

[0072] (2) After the reaction starts, spray the water glass solution from the top of the reactor tank and the bottom of the reactor tank at a rate of 6.225 cubic meters per hour, and add sulfuric acid from the tank bottom spray pipelin...

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Abstract

The invention provides a method of preparing precipitation method white carbon black by an improved dropwise adding process. The method comprises the following steps: preparing a base solution in a reaction kettle and controlling the content of water glass; controlling the stirring speed and the reaction temperature according to different generated products, spraying sulfuric acid from the bottomof the reaction kettle and spraying a water glass solution from the bottom or top of the reaction kettle till the water glass solution is sprayed over; raising the temperature, spraying sulfuric acidfrom the bottom of the reaction kettle, controlling the pH of the reaction system, and carrying out acidification and curing till the reaction is completed; and carrying out filter pressing, washing,pulpifying and drying on the obtained synthesized liquid to obtain the precipitation method white carbon black. Compared with an existing precipitation method, as white carbon black of different specifications is prepared by spraying sulfuric acid from the bottom and adding the water glass solution from the bottom or top, the specific surface areas and oil factors of different white carbon block products can be improved. In the production process, acidic emission is converted into neutral emission in tail gas emission, so that the product quality can be improved effectively, novel products aredeveloped, and the method is fully environment-friendly.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing precipitation white carbon black by improving a dropping process. Background technique [0002] White carbon black is also known as hydrated silica, and the current conventional production methods mainly include gas phase method and precipitation method. Among them, silica is mainly used as a reinforcing agent for silicone rubber, a thickener for coatings and unsaturated resins, a reinforcing agent for natural rubber and synthetic rubber, and a friction agent for toothpaste. [0003] The precipitation method refers to the production of silicon dioxide with sulfuric acid, hydrochloric acid, carbon dioxide and water glass as the basic raw materials. The precipitation method production process mainly uses sulfuric acid and water glass as raw materials for production, and the white carbon black synthesis liquid obtained after the reaction is a mixed ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/193C08K3/36C08L21/00
CPCC01B33/193C01P2006/12C01P2006/19C01P2006/80C01P2006/82C08K3/36C08L21/00
Inventor 周敏傅舟平彭令军唐任志唐志凡刘翠杰姜大明
Owner ZHUZHOU XINGLONG CHEM IND
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