CN113493208A - Process for producing modified white carbon black by using silica fume as raw material - Google Patents
Process for producing modified white carbon black by using silica fume as raw material Download PDFInfo
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- CN113493208A CN113493208A CN202010265157.2A CN202010265157A CN113493208A CN 113493208 A CN113493208 A CN 113493208A CN 202010265157 A CN202010265157 A CN 202010265157A CN 113493208 A CN113493208 A CN 113493208A
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- silica fume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a process for producing modified white carbon black by taking silica fume as a raw material, which comprises the following steps: s1, separating silica fume by an airflow diffusion settling method: controlling the temperature of the airflow, the air flow rate and the volume ratio of silica fume to air so as to settle substances with different particles and different chemical components in the silica fume into different settling collection bins step by step; s2, acid washing: adding the components meeting the white carbon black manufacturing requirements into a hydrochloric acid solution, stirring and reacting for 2-6 hours, filtering, and collecting solid components; s3, alkali washing: adding the fixed component obtained in the step S2 into water, stirring, adding 0.2% sodium carbonate aqueous solution for neutralization, stirring for 30 minutes, filtering, collecting solid component, and washing with deionized water for 1-2 times; and S4, drying and grinding. The white carbon black produced by the process is non-toxic and tasteless, has excellent environmental protection performance, has physical and chemical properties close to those of the white carbon black produced by a gas phase method, has the production cost only 45-55% of that of the white carbon black produced by the gas phase method, and has obvious cost advantage.
Description
Technical Field
The invention relates to the technical field of sampling devices, in particular to a process for producing modified white carbon black by taking silica fume as a raw material.
Background
At present, most industrial silicon (single crystal and polycrystal) production enterprises and ferrosilicon production enterprises in China collect a large amount of silica fume (micro silicon powder) in a flue. Generally, one ton of high-quality silica fume (silica fume) can be recovered per 3 tons of industrial (monocrystalline, polycrystalline) silicon produced. One ton of silicon micropowder can be recovered per 4-5 tons of ferrosilicon produced. According to incomplete statistics, the total production of the silica fume (micro silicon powder) in 2019 years of the industrial silicon industry and the ferrosilicon industry in China reaches over 42 million tons, wherein most of the silica fume contains SiO2The silica fume is a crude product with the grade below 92 percent, and the current silica fume (micro silica fume) is mainly used in the fields of concrete and refractory materials. According to the detectionThe main component of the silica fume (silica fume) is SiO2(silica), SiO in silica fume2The (silicon dioxide) content is between 89 and 94 percent. Other components mainly comprise metal oxides, carbon, nitrogen, sulfur and the like (different chemical components of the silica fume from different manufacturers are different and have larger difference).
According to research tests, the main component SiO2 (silicon dioxide) in the silica fume (silica fume) is white amorphous flocculent semi-transparent solid colloidal nanoparticles (the particle diameter is less than 100nm) in a physical structure under a normal state, is non-toxic and has a huge specific surface area, more than 85 percent of the particles have the particle diameter of 22-62 nm, and the particles belong to nano silicon dioxide.
Disclosure of Invention
Aiming at the technical defects in the field of silica fume application, the invention aims to provide a process for producing modified white carbon black by using silica fume as a raw material, which extracts the main component SiO2 (silicon dioxide) in the silica fume (micro silicon powder) to ensure that the purity of SiO2 in a product reaches over 96 percent and the physicochemical property of the product is similar to that of the white carbon black by a gas phase method; the purified and refined product can be used in the rubber industry and the plastic industry, and the market price can be improved by more than 3 times. Has high economic value.
In order to solve the technical problems in the application field of the silica fume and improve the use value and value-added potential of the application field of the silica fume, the invention adopts the following technical scheme:
the invention provides a process for producing modified white carbon black by taking silica fume as a raw material, which comprises the following steps:
s1, separating silica fume by an airflow diffusion settling method: blowing the silica fume to a closed airflow settling chamber provided with 5-9 settling collection bins by using airflow, controlling certain airflow temperature, airflow rate and silica fume-air volume ratio to ensure that substances with different particles and different chemical components in the silica fume settle to different settling collection bins step by step, and selecting components meeting the requirements of producing the white carbon black for later use;
s2, acid washing: adding the components meeting the white carbon black manufacturing requirement into a hydrochloric acid solution with the concentration of 0.2-1.7%, stirring and reacting for 2-6 hours, wherein the solid content in the reaction mixture is 12-26%; when the acid content in the mixed solution is stable, the reaction end point is reached, and then the reaction mixture is filtered in a centrifugal separator, and solid components are collected for later use;
s3, alkali washing: adding the fixed component obtained in the step S2 into water, stirring, controlling the solid content to be between 15% and 30%, simultaneously adding 0.2% sodium carbonate aqueous solution for neutralization, controlling the pH value to be 7.5-8.0 during neutralization, stirring for 30 minutes, filtering in a centrifugal separator, collecting the solid component, washing the solid component for 1-2 times by deionized water, controlling the content of water-soluble impurities in the solid component to be not higher than 120PPM, and using the filtrate as pickling water;
s4, drying and grinding: and (5) testing and detecting the fixed components obtained in the step S3, determining that the purity of SiO2 reaches more than 96 percent to be qualified, drying the qualified solid components by using a converter, grinding the solid components into powder in a Raymond mill, and grinding the powder into white carbon black finished products with different fineness according to the requirements of users.
Preferably, the temperature of the airflow is 62-75 ℃, the air flow rate is 17-25 m/s, and the volume ratio of silica fume to air is 1.1-1.5: 100.
preferably, each settling and collecting bin is 25-30 meters in length, two stages of dust collectors are arranged at the tail ends of the airflow settling chambers, the first stage is a dry cloth bag dust collector, and the second stage is a wet water film dust collector.
Preferably, the stirring manner in steps S2 and S3 is a propeller type, and the speed is 65-85 rpm.
Preferably, the fineness of the finished white carbon black is 320-1200 meshes.
The invention has the beneficial effects that: the white carbon black produced by the process is non-toxic and odorless, has excellent environmental protection performance, the physical and chemical properties of the product are close to those of the white carbon black produced by the gas phase method, the production cost is only 45-55% of that of the white carbon black produced by the gas phase method, and the white carbon black has obvious cost advantage; can be used as plastic additive (plastic steel section additive, engineering plastic additive), and also can be used as additive for rubber products, textile products, papermaking products, pesticides, paint products and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural view (a transparent shell schematic view) of a gas flow settling chamber provided by an embodiment of the invention;
FIG. 2 is a process flow diagram of the present invention.
Description of reference numerals:
1-settling collection bin, 2-dry bag dust collector and 3-wet water film dust collector.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1 is a schematic structural diagram of the airflow settling chamber used in this embodiment, in which 5 to 9 settling collecting bins 1 are provided, each settling collecting bin 1 has a length of 25 to 30 meters, and the end of the airflow settling chamber is provided with two stages of dust collectors, a first stage is a dry bag dust collector 2, and a second stage is a wet water film dust collector 3.
Example 1
Referring to fig. 2, when silica fume is used as a raw material to produce modified white carbon black, the silica fume is blown to a closed airflow settling chamber provided with 5 settling and collecting bins by airflow, the airflow temperature is 6 ℃, the airflow speed is 17 m/s, and the volume ratio of the silica fume to the air is 1.1: 100, respectively;
so that substances with different particles and different chemical components in the silica fume are settled into different settling collection bins step by step, and components meeting the white carbon black manufacturing requirement are selected;
adding the components meeting the white carbon black manufacturing requirement into a hydrochloric acid solution with the concentration of 0.2%, stirring and reacting for 2 hours, wherein the stirring speed is 65 r/min, and the solid content in the reaction mixture is 12%; when the acid content in the mixed solution is stable, the reaction end point is reached, then the reaction mixture is filtered in a centrifugal separator, solid components are collected, the filtrate can be recycled, and the filtrate which cannot be used after being recycled for many times is neutralized and then is sent to a sewage treatment plant;
adding the obtained fixed component into water, stirring at a stirring speed of 65 revolutions per minute, controlling the solid content to be 15%, adding 0.2% sodium carbonate aqueous solution for neutralization, controlling the pH value to be 7.5 during neutralization, stirring for 30 minutes, filtering in a centrifugal separator, collecting the solid component, washing with deionized water for 1-2 times, controlling the content of water-soluble impurities in the solid component to be not higher than 120PPM, and using the filtrate as pickling water;
and testing and detecting the obtained fixed component, wherein the purity of the SiO2 reaches more than 96 percent, namely the fixed component is qualified, and the qualified solid component is dried by using a converter and then ground in a Raymond mill to obtain a white carbon black finished product with the fineness of 320-1200 meshes.
Example 2
When the silica fume is used as a raw material to produce the modified white carbon black, blowing the silica fume to a closed airflow settling chamber provided with 5 settling collecting bins by using airflow, wherein the airflow temperature is 70 ℃, the airflow speed is 20 m/s, and the volume ratio of the silica fume to the air is respectively 1.3: 100, respectively;
so that substances with different particles and different chemical components in the silica fume are settled into different settling collection bins step by step, and components meeting the white carbon black manufacturing requirement are selected;
adding the components meeting the white carbon black manufacturing requirement into a hydrochloric acid solution with the concentration of 1%, stirring and reacting for 4 hours, wherein the stirring speed is 75 r/min, and the solid content in the reaction mixture is 20%; when the acid content in the mixed solution is stable, the reaction end point is reached, then the reaction mixture is filtered in a centrifugal separator, solid components are collected, the filtrate can be recycled, and the filtrate which cannot be used after being recycled for many times is neutralized and then is sent to a sewage treatment plant;
adding the obtained fixed component into water, stirring at a stirring speed of 75 revolutions per minute, controlling the solid content to be 20 percent, adding 0.2 percent sodium carbonate aqueous solution for neutralization, controlling the pH value to be 7.8 during neutralization, stirring for 30 minutes, filtering in a centrifugal separator, collecting the solid component, washing with deionized water for 1-2 times, controlling the content of water-soluble impurities in the solid component to be not higher than 120PPM, and using the filtrate as pickling water;
and testing and detecting the obtained fixed component, wherein the purity of the SiO2 reaches more than 96 percent, namely the fixed component is qualified, and the qualified solid component is dried by using a converter and then ground in a Raymond mill to obtain a white carbon black finished product with the fineness of 320-1200 meshes.
Example 3
When the silica fume is used as a raw material to produce the modified white carbon black, blowing the silica fume to a closed airflow settling chamber provided with 5 settling collecting bins by using airflow, wherein the airflow temperature is 75 ℃, the airflow speed is 25 m/s, and the volume ratio of the silica fume to the air is respectively 1.5: 100, respectively;
so that substances with different particles and different chemical components in the silica fume are settled into different settling collection bins step by step, and components meeting the white carbon black manufacturing requirement are selected;
adding the components meeting the white carbon black manufacturing requirement into a hydrochloric acid solution with the concentration of 1.7%, stirring and reacting for 6 hours, wherein the stirring speed is 85 revolutions per minute, and the solid content in the reaction mixture is 26%; when the acid content in the mixed solution is stable, the reaction end point is reached, then the reaction mixture is filtered in a centrifugal separator, solid components are collected, the filtrate can be recycled, and the filtrate which cannot be used after being recycled for many times is neutralized and then is sent to a sewage treatment plant;
adding the obtained fixed component into water, stirring at a stirring speed of 85 revolutions per minute, controlling the solid content to be 30 percent, simultaneously adding 0.2 percent sodium carbonate aqueous solution for neutralization, controlling the pH value to be 8.0 during neutralization, filtering in a centrifugal separator after stirring for 30 minutes, collecting the solid component, washing the solid component for 1-2 times by deionized water, controlling the content of water-soluble impurities in the solid component to be not higher than 120PPM, and using the filtrate as pickling water;
and testing and detecting the obtained fixed component, wherein the purity of the SiO2 reaches more than 96 percent, namely the fixed component is qualified, and the qualified solid component is dried by using a converter and then ground in a Raymond mill to obtain a white carbon black finished product with the fineness of 320-1200 meshes.
Physical and chemical data:
the physical and chemical properties of the white carbon black produced in the above examples are as follows
First, main chemical index
The content of SiO2 (dry product) is more than or equal to 90 percent
Screen remnants (4.5 mu m) less than or equal to 0.5%
Heating and reducing weight: 4.0 to 8.0 percent
Ignition decrement: (dry product) is less than or equal to 7.0 percent
pH value: 5.0-8.0
Total copper content: less than or equal to 30mg/kg
Total manganese content: less than or equal to 50mg/kg
Total iron content: less than or equal to 1000mg/kg
DBP absorption value: 2.00-3.50cm/g
Specific surface area: different applications can be in different ranges, typically 145-165m/g (HT2)165-185m/g (HT1)
200-300m/g(HT3)
Second, main physical properties (matching rubber)
Tensile strength of 17.0MPa or more and 500% elongation at break of 6.3MPa or more
The elongation at break is more than or equal to 675 percent.
And (3) cost comparison analysis: the cost of the process is compared with that of the white carbon black produced by a gas phase method
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (5)
1. A process for producing modified white carbon black by using silica fume as a raw material is characterized by comprising the following steps
S1, separating silica fume by an airflow diffusion settling method: blowing the silica fume to a closed airflow settling chamber provided with 5-9 settling collection bins by using airflow, controlling certain airflow temperature, airflow rate and silica fume-air volume ratio to ensure that substances with different particles and different chemical components in the silica fume settle to different settling collection bins step by step, and selecting components meeting the requirements of producing the white carbon black for later use;
s2, acid washing: adding the components meeting the white carbon black manufacturing requirement into a hydrochloric acid solution with the concentration of 0.2-1.7%, stirring and reacting for 2-6 hours, wherein the solid content in the reaction mixture is 12-26%; when the acid content in the mixed solution is stable, the reaction end point is reached, and then the reaction mixture is filtered in a centrifugal separator, and solid components are collected for later use;
s3, alkali washing: adding the fixed component obtained in the step S2 into water, stirring, controlling the solid content to be between 15% and 30%, simultaneously adding 0.2% sodium carbonate aqueous solution for neutralization, controlling the pH value to be 7.5-8.0 during neutralization, stirring for 30 minutes, filtering in a centrifugal separator, collecting the solid component, washing the solid component for 1-2 times by deionized water, controlling the content of water-soluble impurities in the solid component to be not higher than 120PPM, and using the filtrate as pickling water;
s4, drying and grinding: and (5) testing and detecting the fixed components obtained in the step S3, determining that the purity of SiO2 reaches more than 96 percent to be qualified, drying the qualified solid components by using a converter, grinding the solid components into powder in a Raymond mill, and grinding the powder into white carbon black finished products with different fineness according to the requirements of users.
2. The process for producing modified silica white by using silica fume as raw material according to claim 1, wherein the airflow temperature is 62-75 ℃, the airflow rate is 17-25 m/s, and the silica fume-air volume ratio is 1.1-1.5: 100.
3. the process for producing modified silica white from silica fume as claimed in claim 1, wherein each settling and collecting bin is 25-30 m in length, and a two-stage dust collector is disposed at the end of the airflow settling chamber, wherein the first stage is a dry bag dust collector and the second stage is a wet water film dust collector.
4. The process for producing modified silica white using silica fume as raw material according to claim 1, wherein the stirring manner in steps S2 and S3 is propeller stirring at a speed of 65-85 rpm.
5. The process for producing modified silica white using silica fume as raw material as claimed in claim 1, wherein the fineness of the finished silica white is 320-1200 mesh.
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- 2020-04-07 CN CN202010265157.2A patent/CN113493208B/en active Active
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CN101148332A (en) * | 2007-09-12 | 2008-03-26 | 长安大学 | Method for increasing content of silicon dioxide in silicon ash and producing white carbon black |
CN102424392A (en) * | 2011-09-11 | 2012-04-25 | 中国科学院过程工程研究所 | Method for preparing white carbon black cogeneration nanometer calcium carbonate by integrally utilizing micro silicon powder |
CN103991875A (en) * | 2014-06-17 | 2014-08-20 | 武汉科技大学 | Method for recovering white carbon black from waste generated in optical fiber preform preparation process |
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