CN108217663B - Low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride - Google Patents
Low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride Download PDFInfo
- Publication number
- CN108217663B CN108217663B CN201810087038.5A CN201810087038A CN108217663B CN 108217663 B CN108217663 B CN 108217663B CN 201810087038 A CN201810087038 A CN 201810087038A CN 108217663 B CN108217663 B CN 108217663B
- Authority
- CN
- China
- Prior art keywords
- tower
- gas
- deacidification
- carbon black
- white carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 51
- 239000006229 carbon black Substances 0.000 title claims abstract description 50
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 49
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000005049 silicon tetrachloride Substances 0.000 title claims abstract description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000007789 gas Substances 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012159 carrier gas Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 230000002572 peristaltic effect Effects 0.000 claims description 23
- 239000007921 spray Substances 0.000 claims description 15
- 239000002699 waste material Substances 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 238000009692 water atomization Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 239000000523 sample Substances 0.000 claims description 4
- 230000009123 feedback regulation Effects 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims 16
- 238000009413 insulation Methods 0.000 claims 1
- 239000012808 vapor phase Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 12
- 229910021485 fumed silica Inorganic materials 0.000 description 11
- 238000002485 combustion reaction Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Images
Classifications
-
- 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
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
-
- 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
- C01P2006/12—Surface area
-
- 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
- C01P2006/14—Pore volume
-
- 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
- C01P2006/16—Pore diameter
-
- 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
-
- 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
- C01P2006/90—Other properties not specified above
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The low-temperature gas-phase hydrolysis equipment for preparing the white carbon black from the silicon tetrachloride comprises a feeding system, a carrier gas system, a gas-phase hydrolysis system, a cyclone separation system, a primary deacidification system, a secondary deacidification system and a tertiary deacidification system. Continuously feeding silicon tetrachloride and pure water according to a molar ratio of 1 (4-8), forming uniform liquid drops through an atomizing nozzle, gasifying the liquid drops in a high-temperature carrier gas, and reacting in a gas-phase hydrolysis tower at 120-180 ℃ to generate white carbon black and hydrogen chloride gas; the mixed product realizes gas-solid separation through a cyclone separation system, and then is dried for 4 hours at 160 ℃ to obtain a white carbon black product; recovering a concentrated hydrochloric acid byproduct from the hydrogen chloride mixed gas through a primary deacidification system and a secondary deacidification system; the tail gas is treated by a three-stage deacidification system to realize pollution-free emission. The method can effectively reduce reaction energy consumption, slow down equipment corrosion and reduce production cost, can realize the white carbon black production capacity of 100-200kg/d and the byproduct concentrated hydrochloric acid, and the prepared white carbon black product has excellent performance and wide production and application prospects.
Description
Technical Field
The invention belongs to the technical field of resource and material chemical industry, and particularly relates to low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride.
Background
Silicon tetrachloride (SiCl)4) Is a byproduct generated in the production process of polycrystalline silicon in the photovoltaic industry, has extremely strong corrosivity and toxicity, and is listed in dangerous chemical directory (2012). Silicon tetrachloride has strong stimulation to human skin and respiratory tract, is extremely easy to decompose in the air to form hydrochloric acid mist, and if the hydrochloric acid mist is directly discharged without being treated, the hydrochloric acid mist seriously harms human health and ecological environment. Silicon tetrachloride belongs to dangerous chemicals in national hazardous waste directory (2008) and needs to be disposed according to hazardous waste management regulations, so that research on resource utilization and safe disposal technology of silicon tetrachloride is of great significance for sustainable development of photovoltaic industry.
The silicon tetrachloride recycling technology comprises the preparation of fumed silica, optical fibers, organic silicon products and the like. Wherein, the gas phase white carbon black ratio tableLarge area (200-380 m)2Per g), good chemical stability and good dispersibility, has incomparable performance advantages of precipitated silica, and is an important additive in the fields of rubber, plastics, paint, medicine, papermaking and the like. At present, the fumed silica is generally prepared at home and abroad by adopting an oxyhydrogen combustion technology (silicon tetrachloride, hydrogen and oxygen are mixed and combusted at 1800 ℃). However, the core process of the hydrogen-oxygen combustion technology is monopolized by foreign companies for a long time, and the international level difference of the indexes such as the surface hydroxyl content, the particle size distribution, the specific surface area and the like of the domestic fumed silica is large, so that the import dependence of the fumed silica market in China is extremely high.
The white carbon black is prepared by adopting a low-temperature (120-180 ℃) gas-phase hydrolysis technology, compared with an oxyhydrogen combustion technology, the reaction energy consumption can be effectively reduced, the equipment corrosion is slowed down, and the production cost is reduced, and meanwhile, the performance indexes of the product, such as the surface hydroxyl content, the particle size distribution, the specific surface area and the like, can reach the international advanced level, so that the product can partially replace the gas-phase white carbon black and reduce the import dependence on foreign countries. At the present stage, on the basis of laboratory scale research, the continuous production equipment for preparing the white carbon black by the technology is researched, and the method has important significance for enlarging the production scale and realizing industrial application. At present, low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride is not reported at home and abroad.
Disclosure of Invention
In order to overcome the problems of high reaction energy consumption, high equipment requirement, high production cost and the like in the preparation of fumed silica by the oxyhydrogen combustion technology and the current situation of high dependence degree of China on foreign technologies, the invention aims to provide the low-temperature fumed hydrolysis equipment for preparing the fumed silica by the silicon tetrachloride, and aims to realize large-scale production of the fumed silica by the low-temperature fumed hydrolysis technology, partially replace the fumed silica and reduce the dependence degree of foreign import.
In order to achieve the purpose, the invention adopts the technical scheme that:
the low-temperature gas phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride comprises:
the feeding system comprises a silicon tetrachloride storage tank 2 and a pure water storage tank I3;
the carrier gas system comprises a fan 7, the fan 7 is connected with a gas heat exchanger 8, and the gas heat exchanger 8 is connected with a gas phase hydrolysis tower 9 through a pipeline;
the gas phase hydrolysis system comprises a gas phase hydrolysis tower 9, wherein the right lower part of the gas phase hydrolysis tower 9 is connected with a residual liquid collecting tank 11, and the lateral lower part of the gas phase hydrolysis tower is connected with a cyclone separation tower 12 through a pipeline;
the cyclone separation system comprises a cyclone separation tower 12, wherein the lateral upper part of the cyclone separation tower 12 is connected with the gas-phase hydrolysis tower 9 through a pipeline, the right lower part of the cyclone separation tower is connected with a white carbon black collecting tank 13, and the right upper part of the cyclone separation tower is connected with the deacidification tower through a pipeline;
the deacidification system comprises the deacidification tower.
Silicon tetrachloride storage tank 2 connects three-layer through peristaltic pump 4 and presss from both sides cover atomizer 6, and pure water storage tank 3 connects three-layer through peristaltic pump two 5 and presss from both sides cover atomizer 6, and silence oil-free air compressor 1 connects three-layer and presss from both sides cover atomizer 6, and three-layer presss from both sides cover atomizer 6 and is located the top of gas phase hydrolysis tower 9.
The three-layer jacket atomizing spray head 6 is divided into three layers from the center to the outside, namely a compressed air layer, a silicon tetrachloride layer and a pure water layer, the caliber of a nozzle is 2-4 mm, the feeding molar ratio of silicon tetrachloride to pure water is 1 (4-8), the compressed air layer is connected with the first silent oilless air compressor 1, the silicon tetrachloride layer is connected with the first peristaltic pump 4, and the pure water layer is connected with the second peristaltic pump 5.
The fan 7 is provided with an air filter, and the flow can be adjusted so that the retention time of the materials in the gas phase hydrolysis tower 9 is 2-10 s; the controllable range of the outlet gas temperature of the gas heat exchanger 8 is 25-200 ℃.
The side part of the gas phase hydrolysis tower 9 is provided with a visual window 10, the outer wall of the gas phase hydrolysis tower 9 comprises an electric heating layer and a heat preservation layer, temperature probes are respectively arranged at the top, the middle and the bottom of the tower, and the temperature in the feedback regulation tower is 120-180 ℃.
The white carbon black collecting tank 13 is provided with a white carbon black discharge port 14 at the bottom, the outer wall of the cyclone separation tower 12 comprises an electric heating layer and a heat preservation layer, temperature probes are respectively arranged at the top, the middle and the bottom of the tower, and the temperature in the feedback adjusting tower is 120-180 ℃.
The deacidification system comprises a primary deacidification system, a secondary deacidification system and a tertiary deacidification system.
The primary deacidification system comprises a primary deacidification tower 15, the lower part of the side of the primary deacidification tower 15 is connected with a cyclone separation tower 12 through a pipeline, the right upper part of the primary deacidification tower is connected with a hydrochloric acid atomizing spray head 18, the right lower part of the primary deacidification tower is connected with a concentrated hydrochloric acid collecting tank 19, and the upper part of the side of the primary deacidification tower is connected with a secondary deacidification tower 22 through a pipeline; a dilute hydrochloric acid feeding port 20 is formed in the upper portion of the side of the concentrated hydrochloric acid collecting tank 19, a concentrated hydrochloric acid discharging port 21 is formed in the bottom of the concentrated hydrochloric acid collecting tank, the right lower portion of the concentrated hydrochloric acid collecting tank is connected with a peristaltic pump III 16, and the peristaltic pump III 16 is connected with a hydrochloric acid atomizing nozzle 18; and the second silent oilless air compressor 17 is connected with a hydrochloric acid atomizing spray head 18.
The secondary deacidification system comprises a secondary deacidification tower 22, the lower part of the side of the secondary deacidification tower 22 is connected with a primary deacidification tower 15 through a pipeline, the right upper part is connected with a pure water atomization spray head 25, the right lower part is connected with a dilute hydrochloric acid collecting tank 26, and the upper part of the side is connected with a tertiary deacidification tower 28 through a pipeline; the second pure water storage tank 23 is connected with a fourth peristaltic pump 24, and the fourth peristaltic pump 24 is connected with a pure water atomizing nozzle 25; the mute oil-free air compressor II 17 is connected with the pure water atomizing nozzle 25; the bottom of the dilute hydrochloric acid collecting tank 26 is provided with a dilute hydrochloric acid discharge port 27.
The three-stage deacidification system comprises a three-stage deacidification tower 28, the lower part of the side of the three-stage deacidification tower 28 is connected with a second-stage deacidification tower 22 through a pipeline, the right upper part of the side is connected with an alkali liquor atomization spray head 30, the upper part of the side is provided with a purified air outlet 31, and the right lower part of the side is connected with a waste liquid collecting tank 32; an alkali liquor feeding hole 33 is formed in the upper portion of the side of the waste liquor collecting tank 32, a waste liquor discharging hole 34 is formed in the bottom of the waste liquor collecting tank, the right lower portion of the waste liquor collecting tank is connected with a peristaltic pump five 29, and the peristaltic pump five 29 is connected with an alkali liquor atomizing nozzle 30; the mute oil-free air compressor II 17 is connected with the alkali liquor atomizing nozzle 30.
Compared with the prior art, the invention has the beneficial effects that:
1. the white carbon black is prepared by adopting a low-temperature gas-phase hydrolysis technology, and compared with an oxyhydrogen combustion technology, the method can effectively reduce reaction energy consumption, slow down equipment corrosion and reduce production cost.
2. The prepared white carbon black product has high purity (>99.8 wt.%), high hydroxyl content ((s)>5mmol/g) and a large specific surface area (>200m2The structure performance is excellent, and the white carbon black can partially replace the fumed silica.
3. The equipment has the white carbon black production capacity of 100-200kg/d, can produce concentrated hydrochloric acid as a byproduct, has small investment scale and obvious product benefit, and is suitable for large-scale production and application.
Drawings
Fig. 1 is a schematic diagram of the structure and working flow of the apparatus of the present invention.
Detailed Description
The apparatus of the present invention will now be described in more detail with reference to the accompanying FIG. 1 and the specific embodiments, but is not limited to these embodiments.
The equipment of the invention has the working flow as follows:
(A) feeding: silicon tetrachloride, pure water and compressed air are respectively sprayed into a gas phase hydrolysis tower 9 through a three-layer jacket atomizing nozzle 6, and the compressed air instantaneously atomizes the silicon tetrachloride and the pure water into uniform liquid drops. The feeding amount of the silicon tetrachloride is 8-16L/h, and the feeding molar ratio of the silicon tetrachloride to the pure water is 1 (4-8).
(B) Gas-phase hydrolysis reaction: the atomized silicon tetrachloride droplets and pure water droplets are gasified when meeting high-temperature carrier gas, and a gas-phase hydrolysis reaction occurs in the gas-phase hydrolysis tower 9 to generate white carbon black and hydrogen chloride gas (formula (1)). By adjusting the flow rate of the high-temperature carrier gas, the residence time of the reaction materials in the gas phase hydrolysis tower 9 is controlled to be 2-10 s, and the temperature in the gas phase hydrolysis tower 9 is controlled to be 120-180 ℃.
(C) And (3) recycling white carbon black: the mixture of the white carbon black and the hydrogen chloride gas generated by the reaction enters a cyclone separation tower 12, and the temperature in the cyclone separation tower 12 is controlled to be 120-180 ℃. The hydrogen chloride gas enters the first-stage deacidification tower 15 along with the high-temperature carrier gas, the solid white carbon black enters the white carbon black collecting tank 13, and then the solid white carbon black is intermittently discharged through the white carbon black discharge port 14 and dried for 4 hours at 160 ℃ to obtain a white carbon black product.
(D) And (3) recovering concentrated hydrochloric acid: the dilute hydrochloric acid intermittently discharged from the dilute hydrochloric acid discharge port 27 is intermittently added into a concentrated hydrochloric acid collecting tank 19 through a dilute hydrochloric acid feed port 20, is uniformly sprayed into the primary deacidification tower 15 through a peristaltic pump III 16, a silent oilless air compressor II 17 and a hydrochloric acid atomizing spray head 18, circularly absorbs hydrogen chloride gas for many times to form concentrated hydrochloric acid, and is intermittently discharged from a concentrated hydrochloric acid discharge port 21 to recover a concentrated hydrochloric acid byproduct.
(E) Recovering dilute hydrochloric acid: pure water is uniformly sprayed into the secondary deacidification tower 22 through a peristaltic pump IV 24, a silent oilless air compressor II 17 and a pure water atomization nozzle 25, dilute hydrochloric acid is formed after residual hydrogen chloride gas in tail gas of the primary deacidification tower 15 is absorbed once, and the dilute hydrochloric acid is discharged intermittently through a dilute hydrochloric acid discharge port 27 and is reused in the primary deacidification tower 15.
(F) Tail gas treatment: alkali liquor is added into a waste liquor collecting tank 32 through an alkali liquor feeding hole 33, then is uniformly sprayed into the third-stage deacidification tower 28 through a peristaltic pump 29, a silent oilless air compressor II 17 and an alkali liquor atomizing spray head 30, waste liquor is formed after residual hydrogen chloride gas in tail gas of the second-stage deacidification tower 22 is circularly absorbed for multiple times, and finally the waste liquor is intermittently discharged through a waste liquor discharging hole 34. The carrier gas from which the hydrogen chloride gas is completely removed is evacuated through the purified air outlet 31.
Example 1
The steps are the same as the working process of the equipment, and the difference is that: in the step (A), the feeding amount of the silicon tetrachloride is 16L/h, and the feeding molar ratio of the silicon tetrachloride to the pure water is 1: 4; the residence time of the reaction materials in the gas phase hydrolysis tower 9 in the step (B) is 2s, and the temperature in the gas phase hydrolysis tower 9 is 120 ℃; the temperature in the hydrochloric acid separation column 12 in the step (C) is 120 ℃.
Example 2
The steps are the same as the working process of the equipment, and the difference is that: in the step (A), the feeding amount of the silicon tetrachloride is 16L/h, and the feeding molar ratio of the silicon tetrachloride to the pure water is 1: 6; the residence time of the reaction materials in the gas phase hydrolysis tower 9 in the step (B) is 5s, and the temperature in the gas phase hydrolysis tower 9 is 150 ℃; the temperature in the hydrochloric acid separation column 12 in the step (C) is 150 ℃.
Example 3
The steps are the same as the working process of the equipment, and the difference is that: in the step (A), the feeding amount of the silicon tetrachloride is 8L/h, and the feeding molar ratio of the silicon tetrachloride to the pure water is 1: 8; in the step (B), the retention time of the reaction materials in the gas phase hydrolysis tower 9 is 10s, and the temperature in the gas phase hydrolysis tower 9 is 180 ℃; the temperature in the hydrochloric acid separation column 12 in the step (C) is 180 ℃.
Analysis and comparison of the products of the examples:
the purity of the white carbon black product is measured by adopting an X-ray fluorescence spectrometer (ARL PERFORM X type); determining the hydroxyl content of the white carbon black product by adopting a thermogravimetric analyzer (TGA/DSC type 2, Mettler Switzerland), wherein the heating rate is 10 ℃/min; the specific surface area, average pore diameter and pore volume of the white carbon black product were measured by a specific surface and porosity analyzer (model ASAP 2020, mck, usa).
The test analysis data of the performance of the white carbon black products in examples 1 to 3 are shown in Table 1. The purity of the white carbon black product reaches more than 99.8 wt.%, and is superior to national standard fumed silica (GB/T20020-2005). The hydroxyl content of the white carbon black product is more than 5mmol/g, and the white carbon black product has better hydrophilicity. The specific surface area of the white carbon black product is more than 200m2A pore volume of 0.7 to 0.9cm, an average pore diameter of 8 to 10nm3The structural performance of the carbon black is similar to that of fumed silica. Therefore, the white carbon black prepared by the equipment has excellent performance, can realize large-scale production and has wide application prospect.
TABLE 1 analysis of the properties of the white carbon black products of examples 1 to 3
Claims (7)
1. The utility model provides a low temperature vapor phase hydrolysis equipment of silicon tetrachloride preparation white carbon black which characterized in that includes:
the feeding system comprises a silicon tetrachloride storage tank (2) and a pure water storage tank I (3);
the carrier gas system comprises a fan (7), the fan (7) is connected with a gas heat exchanger (8), and the gas heat exchanger (8) is connected with a gas phase hydrolysis tower (9) through a pipeline;
the gas phase hydrolysis system comprises a gas phase hydrolysis tower (9), wherein the right lower part of the gas phase hydrolysis tower (9) is connected with a residual liquid collecting tank (11), and the lateral lower part of the gas phase hydrolysis tower is connected with a cyclone separation tower (12) through a pipeline;
the cyclone separation system comprises a cyclone separation tower (12), wherein the lateral upper part of the cyclone separation tower (12) is connected with the gas-phase hydrolysis tower (9) through a pipeline, the right lower part of the cyclone separation tower is connected with a white carbon black collecting tank (13), and the right upper part of the cyclone separation tower is connected with the deacidification tower through a pipeline;
a deacidification system comprising the deacidification tower;
the silicon tetrachloride storage tank (2) is connected with a three-layer jacket atomizing spray head (6) through a peristaltic pump I (4), a pure water storage tank I (3) is connected with the three-layer jacket atomizing spray head (6) through a peristaltic pump II (5), a mute oil-free air compressor I (1) is connected with the three-layer jacket atomizing spray head (6), and the three-layer jacket atomizing spray head (6) is positioned at the top of a gas phase hydrolysis tower (9);
the three-layer jacket atomizing spray head (6) is divided into three layers from the center to the outside, namely a compressed air layer, a silicon tetrachloride layer and a pure water layer, the caliber of a spray nozzle is 2-4 mm, the feeding molar ratio of silicon tetrachloride to pure water is 1 (4-8), the compressed air layer is connected with the silent oilless air compressor I (1), the silicon tetrachloride layer is connected with the peristaltic pump I (4), and the pure water layer is connected with the peristaltic pump II (5);
the fan (7) is provided with an air filter, and the flow can be adjusted so that the retention time of the materials in the gas phase hydrolysis tower (9) is 2-10 s; the controllable range of the outlet gas temperature of the gas heat exchanger (8) is 25-200 ℃.
2. The low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride according to claim 1, wherein a visual window (10) is arranged on the side of the gas-phase hydrolysis tower (9), the outer wall of the gas-phase hydrolysis tower (9) comprises an electric heating layer and an insulating layer, temperature probes are respectively arranged at the top, the middle and the bottom of the tower, and the temperature in the feedback regulation tower is 120-180 ℃.
3. The low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride according to claim 2, wherein a white carbon black discharge port (14) is formed in the bottom of the white carbon black collecting tank (13), the outer wall of the cyclone separation tower (12) comprises an electric heating layer and a heat insulation layer, temperature probes are respectively arranged at the top, the middle and the bottom of the tower, and the temperature in the feedback regulation tower is 120-180 ℃.
4. The low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride according to claim 1, wherein the deacidification system comprises a primary deacidification system, a secondary deacidification system and a tertiary deacidification system.
5. The low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride according to claim 4, wherein the primary deacidification system comprises a primary deacidification tower (15), the lower side part of the primary deacidification tower (15) is connected with a cyclone separation tower (12) through a pipeline, the upper part of the primary deacidification tower is connected with a hydrochloric acid atomizing spray head (18), the lower part of the primary deacidification tower is connected with a concentrated hydrochloric acid collecting tank (19), and the upper side part of the primary deacidification tower is connected with a secondary deacidification tower (22) through a; a dilute hydrochloric acid feeding port (20) is formed in the upper portion of the side of the concentrated hydrochloric acid collecting tank (19), a concentrated hydrochloric acid discharging port (21) is formed in the bottom of the concentrated hydrochloric acid collecting tank, the positive lower portion of the concentrated hydrochloric acid collecting tank is connected with a peristaltic pump III (16), and the peristaltic pump III (16) is connected with a hydrochloric acid atomizing nozzle (18); and the mute oil-free air compressor II (17) is connected with the hydrochloric acid atomization nozzle (18).
6. The low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride according to claim 4, wherein the secondary deacidification system comprises a secondary deacidification tower (22), the lower side part of the secondary deacidification tower (22) is connected with a primary deacidification tower (15) through a pipeline, the upper part of the secondary deacidification tower is connected with a pure water atomization spray head (25), the lower part of the secondary deacidification tower is connected with a dilute hydrochloric acid collecting tank (26), and the upper side part of the secondary deacidification tower is connected with a third deacidification tower (28) through a; the second pure water storage tank (23) is connected with a fourth peristaltic pump (24), and the fourth peristaltic pump (24) is connected with a pure water atomizing nozzle (25); the second silent oilless air compressor (17) is connected with the pure water atomizing nozzle (25); the bottom of the dilute hydrochloric acid collecting tank (26) is provided with a dilute hydrochloric acid discharge port (27).
7. The low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride according to claim 4, wherein the three-stage deacidification system comprises a three-stage deacidification tower (28), the lower part of the side of the three-stage deacidification tower (28) is connected with a second-stage deacidification tower (22) through a pipeline, the upper part of the side is connected with an alkali liquor atomization nozzle (30), the upper part of the side is provided with a purified air outlet (31), and the lower part of the side is connected with a waste liquor collecting tank (32); an alkali liquor feeding hole (33) is formed in the upper portion of the side of the waste liquor collecting tank (32), a waste liquor discharging hole (34) is formed in the bottom of the waste liquor collecting tank, the right lower portion of the waste liquor collecting tank is connected with a peristaltic pump five (29), and the peristaltic pump five (29) is connected with an alkali liquor atomizing nozzle (30); the mute oil-free air compressor II (17) is connected with the alkali liquor atomization nozzle (30).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810087038.5A CN108217663B (en) | 2018-01-30 | 2018-01-30 | Low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810087038.5A CN108217663B (en) | 2018-01-30 | 2018-01-30 | Low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108217663A CN108217663A (en) | 2018-06-29 |
| CN108217663B true CN108217663B (en) | 2020-06-02 |
Family
ID=62669345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810087038.5A Active CN108217663B (en) | 2018-01-30 | 2018-01-30 | Low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108217663B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686791A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Technique of energy saving vapor phase process in high efficiency for synthesizing carbon white |
| JP2006199525A (en) * | 2005-01-19 | 2006-08-03 | Shin Etsu Chem Co Ltd | Method and apparatus for producing high purity silica powder and high purity silica powder |
| WO2006110961A2 (en) * | 2005-04-22 | 2006-10-26 | A J Scientific Pty Ltd | Novel corrosion inhibiting materials |
| CN101723384A (en) * | 2009-12-25 | 2010-06-09 | 上海竟茨环保科技有限公司 | Synthesis method and device for gas phase white carbon black |
| CN103224240A (en) * | 2013-04-15 | 2013-07-31 | 清华大学 | Method for synthesis of nanoscale silica by vapor-phase hydrolysis of silicon tetrachloride |
-
2018
- 2018-01-30 CN CN201810087038.5A patent/CN108217663B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006199525A (en) * | 2005-01-19 | 2006-08-03 | Shin Etsu Chem Co Ltd | Method and apparatus for producing high purity silica powder and high purity silica powder |
| CN1686791A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Technique of energy saving vapor phase process in high efficiency for synthesizing carbon white |
| WO2006110961A2 (en) * | 2005-04-22 | 2006-10-26 | A J Scientific Pty Ltd | Novel corrosion inhibiting materials |
| CN101723384A (en) * | 2009-12-25 | 2010-06-09 | 上海竟茨环保科技有限公司 | Synthesis method and device for gas phase white carbon black |
| CN103224240A (en) * | 2013-04-15 | 2013-07-31 | 清华大学 | Method for synthesis of nanoscale silica by vapor-phase hydrolysis of silicon tetrachloride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108217663A (en) | 2018-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103224240B (en) | Method for synthesis of nanoscale silica by vapor-phase hydrolysis of silicon tetrachloride | |
| CN108840358B (en) | Device and method for preparing anhydrous aluminum fluoride | |
| CN107115892B (en) | The preparation of 4- methyl -5- vinylthiazole base polymeric ionic liquid and application | |
| CN106115720A (en) | A kind of method utilizing rice hull ash to prepare nano silicon | |
| CN108217663B (en) | Low-temperature gas-phase hydrolysis equipment for preparing white carbon black from silicon tetrachloride | |
| CN110003002B (en) | Production process of high-yield ethyl trifluoroacetate | |
| CN1699146A (en) | Analytical pure sulfuric acid production process | |
| CN109319736A (en) | Ammonia tank periodic off-gases recyclable device and its technique | |
| CN105237402B (en) | A kind of continuous method and device for preparing nitrous acid ester | |
| CN101708852B (en) | Method for purifying liquid phase silica recovered from solar polysilicon tail gas | |
| CN111453740A (en) | Method for preparing large-pore-volume silicon dioxide by airflow atomization carbonization method | |
| CN204643838U (en) | Based on the residual air heat exchange combustion-supporting system of methanol-water hydrogen production system employing reforming technology | |
| CN215137005U (en) | System for utilize dividing wall tower to prepare high-purity DMAC | |
| CN216703358U (en) | Methanol vaporizer of silver method formaldehyde production technology | |
| CN109574065A (en) | The foliated Zn of one type0.2Cd0.8The preparation method of S material | |
| CN104262395B (en) | The high-pressure oxidation synthesis technique of a kind of trihydroxy methyl phosphine oxide and equipment | |
| CN210796289U (en) | High-efficient low energy consumption sodium methoxide purification equipment | |
| CN110090543A (en) | It is a kind of to realize continuous separation CH using fluidized bed4/CO2Method | |
| CN111439763A (en) | Preparation method of lithium carbonate | |
| CN102826518B (en) | Concentrated waste acid recovery technology | |
| CN217535486U (en) | White carbon black preparation system | |
| CN211771103U (en) | Biomass gas purification and dehydration system | |
| CN215626916U (en) | Device with adjustable temperature and humidity for producing strong oxidizing gas | |
| CN213172199U (en) | Biomass pyrolysis gas purification device | |
| CN216785728U (en) | System for recycling hydrogen sulfide and coupling green hydrogen production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |