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Method for preparing nano-scale white carbon black product

A nano-scale, white carbon black technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of large particle size, high production cost, and coarse white carbon black products. Achieve the effect of low reaction temperature, fast heating speed and no amplification effect

Active Publication Date: 2013-02-27
贵州瓮福蓝天氟化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method uses organic alcohol silicate as raw material, which is expensive and its production cost is very high
Precipitation method is difficult to control the generation and growth rate of silica crystal nuclei, and the particle size distribution of the obtained silica product is wide, and the product quality is low
Chinese patent 200310117210 discloses a "preparation method of nano-silica", which uses an alkali metal silicate solution as a raw material, adds a water-soluble polymer or a water-soluble organic alcohol to the solution, raises the temperature, and then adds an organic carboxylic acid to prepare a nano-scale Silica, in the preparation process, surfactants are used to control the particle size of silica, and the process wastewater contains organic matter, which is difficult to treat
Chinese patent 200710066136.2 discloses "method for producing high-reinforcing white carbon black and high-concentration ammonium fluoride by ammoniation of fluorosilicate", adding ammonia water to fluorosilicate solution step by step, and then reacting, filtering, washing and drying. Silica products, the particle size of the product is large, can not meet the quality requirements of nano-scale silica
In the process of preparing raw material ammonium fluorosilicate, the existing technology mostly adopts continuous feeding to dissolve fluorine-containing silicon slag to prepare ammonium fluorosilicate. Since the dissolution reaction of fluorine-containing silicon slag is a slow reaction, continuous dissolution will make silicon It is difficult to completely dissolve the slag, and it takes a long time to dissolve
At the same time, in ordinary reactors, the reaction substances are not mixed uniformly, resulting in coarse and uneven particles of white carbon black products, which are prone to agglomeration, and are prone to amplification effects during industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method for a nanoscale white carbon black product, comprising the following steps:

[0021] (1) Batch dissolving reaction: Add fluorine-containing silicon slag and ammonium fluoride solution to the dissolution kettle with agitator and heating device. The ammonium fluoride solution is obtained from steps (4) and (5); at a temperature of 90 The dissolution reaction occurs under the condition of ~108°C and gauge pressure of -15KPa, until the silicon slag is completely dissolved, and a mixed solution of 8% ammonium fluorosilicate and a small amount of ammonium fluoride is obtained; the ammonia and water vapor produced by the dissolution reaction are passed through Cool to below 30°C to obtain dilute ammonia water and ammonia gas, which are sent to the phosphate fertilizer factory for fertilizer processing or other uses;

[0022] (2) Heat exchange: the mixed solution of ammonium fluorosilicate and ammonium fluoride is passed through a heat exchanger for indirec...

Embodiment 2

[0030] A preparation method for a nanoscale white carbon black product, comprising the following steps:

[0031] (1) Batch dissolving reaction: Add fluorine-containing silicon slag and ammonium fluoride solution to the dissolution kettle with agitator and heating device. The ammonium fluoride solution is obtained from steps (4) and (5); at a temperature of 90 The dissolution reaction occurs under the conditions of ~108°C and gauge pressure of -20 KPa, until the silicon slag is completely dissolved, and a mixed solution of 15% ammonium fluorosilicate and a small amount of ammonium fluoride is obtained; the ammonia and water vapor produced by the dissolution reaction After cooling to below 30°C, dilute ammonia water and ammonia gas are obtained, which are sent to the phosphate fertilizer factory for fertilizer processing or other uses;

[0032] (2) Heat exchange: pass the mixed solution of ammonium fluorosilicate and ammonium fluoride through a heat exchanger for indirect heat e...

Embodiment 3

[0040] A preparation method for a nanoscale white carbon black product, comprising the following steps:

[0041] (1) Pretreatment: adjust the pH to 6.5 with ammonium fluorosilicate at 15°C with a mass concentration of 3%;

[0042] (2) Micro-reaction: Then enter the micro-reactor, add the alkaline continuous phase substance ammonia water into the micro-reactor with an excess of 20%, the two substances contact and react quickly, after staying for 2s, a solid-liquid mixture is obtained, and aged for 1min ; Use the external heat exchanger to take away the heat of reaction in the micro-reactor, and maintain the temperature in the micro-reactor at 15°C;

[0043] (3) Filtration: Filtrate the solid-liquid mixture, and the solid part is nano-scale silica;

[0044] (4) Washing: In order to remove a small amount of ammonium fluoride and ammonia water trapped by nano-scale white carbon black, wash with water until the percentage of fluorine is less than 0.05% to obtain semi-finished nano...

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Abstract

The invention discloses a method for preparing a nano-scale white carbon black product, comprising the following steps of: regulating the PH value of 3-15% ammonium fluosilicate at 15-50 DEG C to a range of 6-7 by using an alkaline dispersion phase or continuous phase substance; and then feeding the ammonium fluosilicate into a micro-reactor, adding the alkaline dispersion phase or continuous phase substance into the micro-reactor with excess of 10-30%, staying for 1-3 seconds, and then keeping the temperature in the micro-reactor at 15-50 DEG C, thereby obtaining a solid-liquid mixture; filtering the solid-liquid mixture so as to obtain the solid part, namely the nano-scale white carbon black; washing the nano-scale white carbon black by using water until the mass percent content of fluoride is less than 0.05%, thereby obtaining semi-finished product nano-scale white carbon black; and feeding the semi-finished product nano-scale white carbon black into a microwave drier for drying until meeting the international standard, thereby obtaining the product nano-scale white carbon black. The method provided by the invention is short in reaction time, low in reaction temperature and low in energy consumption; and the particle sizes of the generated particles are evenly distributed.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of a nano-scale white carbon black product. [0002] Background technique [0003] The preparation methods of nano-scale silica mainly include precipitation method and sol-gel method. The sol-gel method uses organic alcohol silicate as raw material, which is expensive and its production cost is very high. Due to the difficulty in controlling the formation and growth rate of silica crystal nuclei in the precipitation method, the particle size distribution of the obtained silica product is wide and the product quality is low. Chinese patent 200310117210 discloses a "preparation method of nano-silicon dioxide", using an alkali metal silicate solution as a raw material, adding a water-soluble polymer or a water-soluble organic alcohol to the solution, raising the temperature, and then adding an organic carboxylic acid to prepare a nano-scale For sili...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y30/00
Inventor 李白玉冯胜波汤仁恒刘松林张瑞骆吉林张崇罗静
Owner 贵州瓮福蓝天氟化工股份有限公司
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