CN217535486U - White carbon black preparation system - Google Patents
White carbon black preparation system Download PDFInfo
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- CN217535486U CN217535486U CN202123183565.2U CN202123183565U CN217535486U CN 217535486 U CN217535486 U CN 217535486U CN 202123183565 U CN202123183565 U CN 202123183565U CN 217535486 U CN217535486 U CN 217535486U
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- white carbon
- tetraalkoxysilane
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Abstract
The utility model relates to a white carbon black preparation system, including tetraalkoxysilane vaporizer, water vaporizer, hydrolysis reactor is venturi type injection reactor, is equipped with two feed inlets, and a connection nozzle, another are the induction port, and the export of tetraalkoxysilane vaporizer and the export of water vaporizer are linked together with hydrolysis reactor's nozzle and induction port respectively, gas-solid separation ware, hydrolysis reactor's export with the entry of gas-solid separation ware is linked together, packagine machine, the solid phase outlet of gas-solid separation ware with packagine machine's entry is linked together to and the mellow wine recoverer, the gaseous phase outlet and the mellow wine recoverer entry of gas-solid separation ware are linked together. Adopt the utility model discloses white carbon black preparation system can avoid using the silicon chloride raw materials, and reaction condition is mild, requires lowly to the equipment material, and reducible equipment investment, reaction efficiency is high simultaneously, and product purity is big, therefore low in production cost, product quality is high.
Description
Technical Field
The utility model relates to a chemical production technical field, concretely relates to white carbon black preparation system.
Background
The white carbon black can be classified into precipitated hydrated white carbon black and gas-phase white carbon black according to different production technologies. The fumed silica is also called fumed silica, has a series of excellent performances such as high purity, low density, small particle size, large specific surface area, strong water absorption capacity and the like, is widely applied to traditional industries such as organic silicon rubber, coating ink, adhesive and the like, and has irreplaceable effects in emerging fields such as catalyst carriers, drug carriers and the like.
At present, the domestic industrialized production of fumed silica mainly adopts a high-temperature combustion method, and the fumed silica is generated by the hydrolysis reaction of silicon halide compounds or organosilicon halide compounds with water vapor generated by the combustion of hydrogen and oxygen at high temperature, the primary particle size is 10-50nm, and the BET surface area is 100-400m 2 Between/g. However, the adopted raw material of the existing production process is chlorosilane, so that a series of defects of low safety, high reaction energy consumption, pollution of byproducts such as hydrogen chloride and the like exist. Moreover, the product is still acidic even after strict dehydrochlorination treatment, and the pH value can only be controlled between 4 and 5, which is not beneficial to downstream application of the product.
Patent CN102001670A discloses a production method of fumed silica using silicon tetrachloride as inorganic silicon source, and patent CN203461824U discloses a method using trichlorosilane as main byproduct in the production process of organosilicon monomer trimethylchlorosilane as raw material, the reaction temperature is as high as 1000-1200 ℃, the energy consumption is high, and the problems of chlorine impurity pollution and corrosion are prominent. In order to reduce the reaction energy consumption, patent CN103224240A discloses a method for synthesizing fumed silica by hydrolyzing silicon tetrachloride at low temperature, wherein water vapor is used to replace water generated by combustion of hydrogen and oxygen to react with silicon tetrachloride, the reaction temperature is reduced to 300 ℃, but the pollution problem of chlorine impurities still exists. In addition, CN102351150A also discloses a method for preparing fumed silica by using silicon tetrafluoride to react with water vapor at the temperature of 200-800 ℃, and the corrosion of hydrogen fluoride by-products to equipment is a prominent problem. Therefore, the prior art has low conversion rate and high cost, and particularly, the problems of impurity pollution of halogen compounds, equipment corrosion and the like are not effectively overcome.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming the problems of low conversion rate, high cost, especially hydrogen chloride byproduct pollution and the like in the prior art, and providing a preparation system of chloridized-free white carbon black.
The purpose of the utility model is realized through the following technical scheme:
the white carbon black preparation system comprises:
a tetraalkoxysilane vaporizer for vaporizing the introduced tetraalkoxysilane raw material;
a water vaporizer for vaporizing the introduced water;
the hydrolysis reactor is a Venturi type spray reactor, and is provided with two feed inlets, one is connected with a nozzle, the other is an air suction port, and an outlet of the tetraalkoxysilane vaporizer and an outlet of the water vaporizer are respectively communicated with the nozzle and the air suction port of the hydrolysis reactor;
the gas-solid separator is used for separating gas-solid products, and an outlet of the hydrolysis reactor is communicated with an inlet of the gas-solid separator;
the packaging machine is used for collecting the white carbon black product, and a solid phase outlet of the gas-solid separator is communicated with an inlet of the packaging machine;
and the gas phase outlet of the gas-solid separator is communicated with the inlet of the alcohol recoverer.
Further, the gas-solid separator is a bag filter.
Further, the alcohol recoverer is a rectifying tower.
Further, the rectifying tower can be a packed tower or a plate tower.
The white carbon black is prepared by the system, the tetraalkoxysilane is used as a raw material and reacts with the steam of water to generate the white carbon black, and the reaction temperature is not more than 300 ℃.
Preferably, the raw material tetraalkoxysilane is any one or a mixture of tetramethoxysilane, tetraethoxysilane and tetraisopropoxysilane.
Preferably, the water is deionized water, and the content of chloride ions in the water is less than 1.0ppm.
Preferably, the feed state of the tetraalkoxysilane raw material is gaseous and contains an inert carrier gas, and the volume fraction of the inert carrier gas is 0 to 95% and is not 0.
Preferably, the feed temperature of the tetraalkoxysilane raw material is in the range of 100 to 300 ℃ and the feed temperature of the steam of water is in the range of 120 to 300 ℃.
Preferably, the feed molar ratio of tetraalkoxysilane starting material to water vapor is from 1.
Compared with the prior art, the utility model discloses following beneficial effect has: the preparation system provided by the invention can ensure that no byproducts such as hydrogen chloride and the like are generated in the whole reaction process, the conversion rate is high, the reaction is green, environment-friendly and pollution-free, the reaction temperature is reduced, the reaction energy consumption is reduced, the gas-phase reaction operation is simple, the reaction condition is mild, and the obtained product has the advantages of good quality, small particle size, high purity and large specific surface area.
Drawings
FIG. 1 is a schematic structural view of a system for preparing white carbon black according to the present invention;
reference numerals: a 100-tetraalkoxysilane vaporizer; 200-a water vaporizer; 300-a hydrolysis reactor; 400-gas-solid separator; 500-packaging machine; 600-alcohol recoverer;
1-tetraalkoxysilane; 2-water; 3-alcohols; 4-white carbon black.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, the utility model also provides a white carbon black preparation system, which comprises a tetraalkoxysilane vaporizer 100, a water vaporizer 200, a hydrolysis reactor 300, a gas-solid separator 400, a packaging machine 500 and an alcohol recoverer 600; the hydrolysis reactor 300 is a venturi-type spray reactor comprising two feed inlets, one of which is connected to a nozzle and the other is an air entry; the outlet of the tetraalkoxysilane vaporizer 100 and the outlet of the water vaporizer 200 are respectively communicated with the nozzle and the air suction port of the hydrolysis reactor 300, the outlet of the hydrolysis reactor 300 is communicated with the inlet of the gas-solid separator 400, the solid phase outlet of the gas-solid separator 400 is communicated with the inlet of the packaging machine 500, and the gas phase outlet of the gas-solid separator 500 is communicated with the inlet of the alcohol recoverer 600.
In the present invention, the gas-solid separator 400 is a bag filter.
The utility model discloses in, alcohol recovery device 600 is the rectifying column, can be the packed column, also can be the plate column.
The preparation method of the white carbon black takes tetraalkoxysilane as a raw material, and the tetraalkoxysilane reacts with steam of water to generate the white carbon black, and the reaction temperature is not more than 300 ℃.
The tetraalkoxysilane of the present invention can be any one or a mixture of tetramethoxysilane, tetraethoxysilane, and tetraisopropoxysilane.
In the utility model, the raw material water is deionized water, and the content of chloride ions in the water is less than 1.0ppm.
The utility model discloses in, the feeding state of tetraalkoxysilane raw materials is the gaseous state, and contains the inert carrier gas, and the volume fraction of inert carrier gas is 0 ~ 95%, and is not 0.
In the utility model, the feeding temperature of the tetraalkoxysilane raw material is 100-300 ℃, and the feeding temperature of the steam of the water is 120-300 ℃.
The utility model discloses in, the feeding mole ratio of the steam of tetraalkoxysilane raw materials and water is 1 ~ 1.
The following is an example of the specific preparation of white carbon black by using the system of the present invention:
example 1
A certain chemical plant applies a white carbon black preparation method, tetraalkoxysilane is used as a raw material and reacts with steam of water to generate white carbon black, the reaction temperature does not exceed 300 ℃, and a white carbon black preparation system shown in figure 1 is applied. The tetraalkoxysilane feed was a mixture of tetramethoxysilane and inert gas nitrogen, and the water feed was deionized water having a chloride ion content of less than 1.0ppm. The volume fraction of nitrogen in the mixture was 95%. The tetramethoxysilane feed temperature in the hydrolysis reactor was 150 ℃. The water feed temperature in the hydrolysis reactor was 150 ℃. The feed molar ratio of tetramethoxysilane to water is 1:2. the reaction temperature in the hydrolysis reactor was 150 ℃.
In this example, using the method and system of the present invention, the white carbon black product obtained from the outlet of the packaging machine had an average particle size of 148.2nm and a BET specific surface area of 565m 2 (ii)/g, the water content of the methanol obtained from the alcohol recovery unit is not more than 1%.
Example 2
A certain chemical plant applies a white carbon black preparation method, tetraalkoxysilane is used as a raw material and reacts with steam of water in a hydrolysis reactor, the reaction temperature does not exceed 300 ℃, and a white carbon black preparation system shown in figure 1 is applied. The tetraalkoxysilane feed was a mixture of tetraethoxysilane and inert gas nitrogen, and the water feed was deionized water having a chloride ion content of less than 1.0ppm. The volume fraction of nitrogen in the mixture was 95%. The tetraethoxysilane feed temperature in the hydrolysis reactor was 200 ℃. The water feed temperature in the hydrolysis reactor was 200 ℃. The molar ratio of tetraethoxysilane to water fed is 1:2. the reaction temperature in the hydrolysis reactor was 200 ℃.
In this embodiment, the white carbon black obtained from the outlet of the packaging machine by using the method and system of the present invention has an average particle size of 205.3nm and a BET specific surface area of 427m 2 (ii)/g, the water content of the methanol obtained from the alcohol recovery unit is not more than 1%.
Example 3
White carbon black was prepared by using the method and system of example 1, except that the temperature of the hydrolysis reactor was 200 ℃.
In this embodiment, the method and system of the present invention are applied to a slave packageThe average grain diameter of the white carbon black product obtained from the outlet of the charging machine is 192.4nm, the BET specific surface area is 511m 2 The water content of the methanol obtained from the alcohol recoverer is not more than 1 percent.
Example 4
White carbon black was prepared using the method and system of example 1, except that the volume fraction of nitrogen in the mixture of tetramethoxysilane and inert gas nitrogen was 20%.
In this example, the white carbon black product obtained from the outlet of the packaging machine by using the method and system of the present invention has an average particle size of 429.5nm and a BET specific surface area of 405m 2 The water content of the methanol obtained from the alcohol recoverer is not more than 1 percent.
Example 5
White carbon black preparation was performed using the method and system of example 1, except that the molar ratio of tetramethoxysilane to water fed was 1:20.
in this example, the white carbon black product obtained from the outlet of the packaging machine by using the method and system of the present invention has an average particle size of 152.6nm and a BET specific surface area of 472m 2 The water content of the methanol obtained from the alcohol recoverer is not more than 1 percent.
Example 6
White carbon black was prepared by using the method and system of example 1, except that the tetramethoxysilane feed temperature in the hydrolysis reactor was 120 ℃ and the water feed temperature in the hydrolysis reactor was 100 ℃.
In this embodiment, the white carbon black product obtained from the outlet of the packaging machine by using the method and system of the present invention has an average particle size of 182.1nm and a BET specific surface area of 489m 2 The water content of the methanol obtained from the alcohol recoverer is not more than 1 percent.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention according to the disclosure of the present invention.
Claims (4)
1. The white carbon black preparation system is characterized by comprising the following components:
a tetraalkoxysilane vaporizer (100) for vaporizing the introduced tetraalkoxysilane raw material;
a water vaporizer (200) for vaporizing the introduced water;
the hydrolysis reactor (300) is used for reacting gaseous tetraalkoxysilane with water vapor, the hydrolysis reactor (300) is a Venturi type spray reactor and is provided with two feed inlets, one feed inlet is connected with a nozzle, the other feed inlet is an air suction inlet, and an outlet of the tetraalkoxysilane vaporizer (100) and an outlet of the water vaporizer (200) are respectively communicated with the nozzle and the air suction inlet of the hydrolysis reactor (300);
the gas-solid separator (400) is used for separating gas-solid products, and the outlet of the hydrolysis reactor (300) is communicated with the inlet of the gas-solid separator (400);
the packaging machine (500) is used for collecting the white carbon black, and the solid phase outlet of the gas-solid separator (400) is communicated with the inlet of the packaging machine (500);
and the gas phase outlet of the gas-solid separator (400) is communicated with the inlet of the alcohol recoverer (600).
2. The white carbon black preparation system according to claim 1, wherein the gas-solid separator (400) is a bag filter.
3. The white carbon black preparation system according to claim 1, wherein the alcohol recovery unit (600) is a rectifying tower.
4. The white carbon black preparation system according to claim 3, wherein the rectifying tower is a packed tower or a plate tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123183565.2U CN217535486U (en) | 2021-12-17 | 2021-12-17 | White carbon black preparation system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123183565.2U CN217535486U (en) | 2021-12-17 | 2021-12-17 | White carbon black preparation system |
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| CN217535486U true CN217535486U (en) | 2022-10-04 |
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2021
- 2021-12-17 CN CN202123183565.2U patent/CN217535486U/en active Active
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