CN1760125A - Technique for producing carbon white through using waste residue of aluminium sulphate - Google Patents

Technique for producing carbon white through using waste residue of aluminium sulphate Download PDF

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Publication number
CN1760125A
CN1760125A CN 200510045102 CN200510045102A CN1760125A CN 1760125 A CN1760125 A CN 1760125A CN 200510045102 CN200510045102 CN 200510045102 CN 200510045102 A CN200510045102 A CN 200510045102A CN 1760125 A CN1760125 A CN 1760125A
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waste residue
aluminum sulfate
white carbon
carbon black
sulfate waste
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CN 200510045102
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宋军
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Individual
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Abstract

A process for preparing white carbon black from rejected aluminium sulfate dregs includes such steps as water washing until the dregs become neutral, adding alkali solution, stirring while reacting at 50-100 deg.C for 1-3 hr to obtain the solution of sodium silicate, filtering, adding clean water, stirring while adding diluted sulfuric acid at 50-100 deg.C, reaction to obtain coarse white carbon block, filter, water washing, baking and pulverizing.

Description

Process for producing white carbon black by using aluminum sulfate waste residues
Technical Field
The invention relates to a production process of white carbon black, in particular to a process for producing white carbon black by using aluminum sulfate waste residues.
Background
At present, more than 190 enterprises producing aluminum sulfate nationwide have the production capacity of 115 ten thousand tons, the yield of the enterprises is more than 95 ten thousand tons, and only after the United states and Japan, about 0.5 ton of waste residue is produced when one ton of aluminum sulfate is produced, if 50% of aluminum sulfate is produced by taking bauxite as a raw material, at least 25 ten thousand tons of waste residue are discharged every year, the treatment cost of each ton of aluminum sulfate waste residue (silicon residue) is 20 yuan/ton, the treatment cost of each year of waste residue reaches more than 500 yuan, and the aluminum sulfate waste residue pollutes the environment. White carbon black is widely used in the industries of filling reinforcing agents of rubber and plastics, printing ink thickening agents, paint coating additives, synthetic lubricating grease and silicone grease thickening agents, tanning flattening agents, papermaking fillers, additives of synthetic resins, insulating and heat insulating fillers of electronic and electrical industries, daily chemical raw materials and the like. And can be used as an opening agent for polypropylene and nontoxic polyvinyl chloride plastic films, and an anti-caking agent and a carrier for food, pesticide and medicine. The existing white carbon black preparation methods comprise a dry production method, a hydrochloric acid precipitation method and a nitric acid precipitation method, wherein raw materials used in the dry production method and the nitric acid precipitation method are expensive, high in requirements on equipment and complex in technology, so that the hydrochloric acid precipitation method is most applied, the main raw materials of the method are quartz sand, soda ash, hydrochloric acid and carbon dioxide, and the process route is as follows: firstly, using fuel oil or high-quality coal, making quartz sand and soda ash react at high temperature to prepare water glass, then under a certain condition, preparing white carbon black from water solution of water glass, said method has the following defects: firstly, the energy consumption is high, secondly, the requirements on raw materials are strict, and the product cost is high, so that the application is limited and import is often required.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and provide a process for producing white carbon black by using aluminum sulfate waste residues, which is beneficial to waste utilization, simple in production process and low in production cost.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the process for producing white carbon black by using aluminum sulfate waste residues comprises the following steps: (1) washing the aluminum sulfate waste residue after the aluminum sulfate preparation process to be neutral by using clear water; (2) alkali liquor with the mass percentage concentration of 10-60% and the washed aluminum sulfate waste residue are fully stirred and react for 1-3 hours at the temperature of 50-100 ℃ to prepare sodium silicate solution; (3) filtering the prepared sodium silicate solution, and adding clear water to ensure that the mass percentage concentration of the clear water is 10-30%; (4) fully stirring the sodium silicate solution uniformly, adding dilute sulfuric acid with the mass percent concentration of 5-30% at the temperature of 50-100 ℃ to react for 1-3 hours, and precipitating a crude white carbon black product; (5) filtering the crude white carbon black, washing with water until the pH value is 6-7, drying and crushing to obtain a finished product;
the process for producing the white carbon black by using the aluminum sulfate waste residue comprises the steps of preparing aluminum sulfate from raw materials containing aluminum and silicon, wherein the aluminum sulfate waste residue is bauxite waste residue, kaolin waste residue or alunite waste residue;
in the process for producing the white carbon black by using the aluminum sulfate waste residue, the content of silicon dioxide in the aluminum sulfate waste residue is 20-90 percent;
in the process for producing the white carbon black by using the aluminum sulfate waste residue, the alkali liquor is sodium hydroxide with the mass percentage concentration of 10-60%.
Compared with the prior art, the invention has the beneficial effects that:
project index National standard White carbon black produced by the invention
The content (%) of silicon dioxide is not less than 90 91.5~93.5
Heating loss (%) 4.0~8.0 5.5~7.0
The ignition loss (percent) is less than or equal to 7.0 5.7~6.0
Colour(s) Is superior to or equal to the standard sample Is superior to or equal to the standard sample
pH value 5.0~8.0 6.0~7.0
DBP absorption cm3/g 2.0~3.5 3.2
Specific surface area m2/g Divided into six gears A-F 175~200
Other indicators Reach the standard Reach the standard
Specific surface area: a is greater than 190; b161-190; c136-160; d106 to 135; e71-105; f is less than 70(GB 10517-89); the determination method comprises the following steps: ST-03A surface and an aperture analyzer.
The particle size of the white carbon black measured by the ohm-mei instrument is shown in fig. 1.
Although the waste residue and the sulfuric acid washing mother liquor are generated in the process, the waste residue can be used as a silicon fertilizer for crops, and the sulfuric acid washing mother liquor can be recycled, so that the process is pollution-free.
The invention has wide raw material source, changes waste into valuable, reduces the environmental pollution and solves the problem that the waste residue of aluminum sulfate manufacturers is difficult to treat; in addition, the invention has simple process, low cost and high profit, and is easy to realize industrial production.
Drawings
The invention is explained in more detail below with reference to the figures and examples:
FIG. 1 is a particle size distribution diagram of white carbon black of the present invention.
Example one
Washing 100 g of aluminum sulfate waste residue (the content of silicon dioxide is 90%) with water to be neutral, then weighing 10 g of sodium hydroxide to be dissolved in 100 ml of water, fully stirring the sodium hydroxide solution and the aluminum sulfate waste residue, reacting for 3 hours at 100 ℃ to prepare sodium silicate, then filtering out reaction residues, adding water to ensure that the concentration of the sodium silicate solution is 10% and fully stirring, adding dilute sulfuric acid with the mass percentage concentration of 5% at 100 ℃ to react for 3 hours, fully finishing, precipitating white carbon black, then filtering, washing with water to the pH value of 7, and finally drying and crushing to obtain the white carbon black.
The reaction process is divided into two reactions, and is specifically represented as follows:
1. reacting aluminum sulfate waste residue with a sodium hydroxide solution:
2. reacting sodium silicate with dilute sulfuric acid:
example two
100 g of aluminum sulfate waste residue (the content of silicon dioxide is 70%) is washed by water to be neutral, 10 g of sodium hydroxide is weighed and dissolved in 50 ml of water, the sodium hydroxide solution and the aluminum sulfate waste residue are fully stirred and react for 2 hours at 80 ℃ to prepare sodium silicate, then reaction residues are filtered out, water is added to ensure that the concentration of the sodium silicate solution is 15% and fully stirred, dilute sulfuric acid with the mass percentage concentration of 15% is added at 50 ℃ to react for 2 hours, white carbon black is precipitated, then the white carbon black is filtered, washed by water until the PH value is 6, and finally the white carbon black is obtained by drying and crushing.
EXAMPLE III
100 g of aluminum sulfate waste residue (the content of silicon dioxide is 30%) is washed by water to be neutral, 10 g of sodium hydroxide is weighed and dissolved in 16.7 ml of water, the sodium hydroxide solution and the aluminum sulfate waste residue are fully stirred and react for 1 hour at 50 ℃ to prepare sodium silicate, then reaction residue is filtered, water is added to ensure that the concentration of the sodium silicate solution is 30% and fully stirred, dilute sulfuric acid with the mass percentage concentration of 30% is added at 80 ℃ to fully react for 1 hour, white carbon black is precipitated, then the white carbon black is filtered, washed by water until the PH value is 6.5, and finally dried and crushed to obtain the white carbon black.
Example four
100 g of aluminum sulfate waste residue (the content of silicon dioxide is 50%) is washed by water to be neutral, 10 g of sodium hydroxide is weighed and dissolved in 30 ml of water, the sodium hydroxide solution and the aluminum sulfate waste residue are fully stirred and react for 1.5 hours at 75 ℃ to prepare sodium silicate, then the reaction residue is filtered, water is added to ensure that the concentration of the sodium silicate solution is 20% and fully stirred, dilute sulfuric acid with the mass percentage concentration of 20% is added at 60 ℃ to fully react for 1.5 hours, white carbon black is precipitated, then the solution is filtered, washed by water until the PH value is 6, and finally the white carbon black is obtained by drying and crushing.
EXAMPLE five
100 g of aluminum sulfate waste residue (the content of silicon dioxide is 20%) is washed by water to be neutral, 10 g of sodium hydroxide is weighed and dissolved in 20 ml of water, the sodium hydroxide solution and the aluminum sulfate waste residue are fully stirred and react for2 hours at 60 ℃ to prepare sodium silicate, then reaction residues are filtered, water is added to ensure that the concentration of the sodium silicate solution is 25% and fully stirred, dilute sulfuric acid with the mass percentage concentration of 15% is added at 80 ℃ to react for 2 hours, white carbon black is precipitated, then the solution is filtered, washed by water until the PH value is 6.5, and finally the white carbon black is obtained by drying and crushing.
The indexes of the white carbon black in the above examples measured by the measuring method of the ST-03A surface and pore size measuring instrument are as follows:
project index National standard Examples
The content (%) of silicon dioxide is not less than 90 91.5~93.5
Heating loss (%) 4.0~8.0 5.5~7.0
The ignition loss (percent) is less than or equal to 7.0 5.7~6.0
Colour(s) Is superior to or equal to the standard sample Is superior to or equal to the standard sample
pH value 5.0~8.0 6.0~7.0
DBP absorption cm3/g 2.0~3.5 3.2
Specific surface area m2/g Divided into six gears A-F 175~200
Other indicators Reach the standard Reach the standard
The particle size of the white carbon black measured by the ohm-mei instrument is shown in fig. 1.

Claims (4)

1. The process for producing the white carbon black by using the aluminum sulfate waste residue is characterized by comprising the following steps of: (1) washing the aluminum sulfate waste residue after the aluminum sulfate preparation process to be neutral by using clear water; (2) alkali liquor with the mass percentage concentration of 10-60% and the washed aluminum sulfate waste residue are fully stirred and react for 1-3 hours at the temperature of 50-100 ℃ to prepare sodium silicate solution; (3) filtering the prepared sodium silicate solution, and adding clear water to ensure that the mass percentage concentration of the clear water is 10-30%; (4) fully stirring the sodium silicate solution uniformly, adding dilute sulfuric acid with the mass percent concentration of 5-30% at the temperature of 50-100 ℃ to react for 1-3 hours, and precipitating a crude white carbon black product; (5) filtering the crude white carbon black, washing with water until the pH value is 6-7, drying and crushing to obtain the finished product.
2. The process for producing white carbon black by using aluminum sulfate waste residue as claimed in claim 1, which is characterized in that: the aluminum sulfate waste residue is the waste residue after aluminum sulfate is prepared from raw materials containing aluminum and silicon, and is bauxite waste residue, kaolin waste residue or alunite waste residue.
3. The process for producing white carbon black by using aluminum sulfate waste residue according to claim 1 or 2, which is characterized in that: the content of silicon dioxide in the aluminum sulfate waste residue is 20-90%.
4. The process for producing white carbon black by using aluminum sulfate waste residue as claimed in claim 1, which is characterized in that: the alkali liquor is sodium hydroxide with the mass percent concentration of 10-60%.
CN 200510045102 2005-11-11 2005-11-11 Technique for producing carbon white through using waste residue of aluminium sulphate Pending CN1760125A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100431966C (en) * 2006-05-31 2008-11-12 张道洪 Method for preparing iron-free aluminium sulfate and superfine active carbon white utilizing aluminium first-class ore
CN107934974A (en) * 2017-12-13 2018-04-20 武汉理工大学 A kind of method by the high silicon waste residue production white carbon of kaolinite soil matrix

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100431966C (en) * 2006-05-31 2008-11-12 张道洪 Method for preparing iron-free aluminium sulfate and superfine active carbon white utilizing aluminium first-class ore
CN107934974A (en) * 2017-12-13 2018-04-20 武汉理工大学 A kind of method by the high silicon waste residue production white carbon of kaolinite soil matrix

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