CN115636416B - Synthesis method of silicon tetrachloride - Google Patents
Synthesis method of silicon tetrachloride Download PDFInfo
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- CN115636416B CN115636416B CN202211413615.8A CN202211413615A CN115636416B CN 115636416 B CN115636416 B CN 115636416B CN 202211413615 A CN202211413615 A CN 202211413615A CN 115636416 B CN115636416 B CN 115636416B
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- 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 44
- 239000005049 silicon tetrachloride Substances 0.000 title claims abstract description 44
- 238000001308 synthesis method Methods 0.000 title claims abstract description 4
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 78
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000000227 grinding Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000011541 reaction mixture Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 46
- 239000007789 gas Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims 6
- 238000006243 chemical reaction Methods 0.000 abstract description 40
- 230000002776 aggregation Effects 0.000 abstract description 8
- 238000004220 aggregation Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 description 34
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 15
- 229910052801 chlorine Inorganic materials 0.000 description 15
- 238000010189 synthetic method Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010606 normalization Methods 0.000 description 2
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of chemical substance synthesis, and particularly discloses a method for synthesizing silicon tetrachloride. The synthesis method of the invention comprises the following steps: (1) Crushing and grinding Si powder raw materials to 160-200 meshes; (2) Carrying out Si powder obtained by grinding in the step (1)Drying; (3) SiO is added into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture; (4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The mixed gas of the above is reacted in a fluidized bed reactor at 1000-1100 ℃. The invention greatly improves the problem of Si powder aggregation through simple process control and process treatment, improves the reaction depth and the reaction efficiency, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of synthesis of organosilicon monomers, and particularly relates to a method for synthesizing silicon tetrachloride.
Background
Silicon tetrachloride (chemical SiCl) 4 ) Is colorless liquid, is a raw material for producing high-purity silicon (different specifications of industrial grade, electronic grade and the like) and organosilicon compounds (such as trichlorosilane, tetraethoxysilane, organic silicone oil and the like), has wide application field, is a necessary industrial chemical raw material, and especially has the largest production amount of optical fibers, ethyl silicate and the like.
In the prior art, various synthetic methods of silicon tetrachloride, such as an industrial silicon chlorination method, a ferrosilicon chlorination method, a diatomite method and the like, and some technical methods for preparing silicon tetrachloride by utilizing industrial byproducts, such as silicon tetrachloride by-produced by polysilicon, silicon tetrachloride prepared by rice hulls, silicon tetrachloride by-produced by zircon sand and the like, exist. Wherein, the industrial silicon chlorination method is that industrial silicon directly reacts with chlorine to prepare SiCl 4 Is a process which is developed earlier and more mature, and is a silicon tetrachloride synthesis process which is actually produced and applied more. Patent document CN103420382a provides a method for synthesizing silicon tetrachloride and a production system thereof, which cover all links from the synthesis to rectification of silicon tetrachloride. However, in the actual production process of the industrial silicon chlorination method, the Si powder has obvious agglomeration phenomenon, and the stability of production operation and the conversion rate and yield of silicon tetrachloride are directly affected. Therefore, how to improve or avoid the agglomeration of Si powder in the reaction process is a technical problem which is very urgent to solve in the silicon tetrachloride production process.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for synthesizing silicon tetrachloride, which comprises the steps of adding SiO into Si powder 2 The method has the advantages that the problems of Si powder aggregation are greatly improved, and the reaction depth and the reaction efficiency are improved due to SiC and the process flow related to adjustment.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to 160-200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1);
(3) SiO is added into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The mixed gas of the above is reacted in a fluidized bed reactor at 1000-1100 ℃.
As a preferable technical scheme of the invention, in the step (1), the purity of Si powder is not less than 99%.
As a preferable technical scheme of the invention, in the step (2), oxygen is isolated during drying, the drying temperature is 100-120 ℃, and the water content after drying is not more than 0.8%.
As a preferred embodiment of the present invention, siO in step (3) 2 Not less than 98% and not less than 97% SiC.
As a preferred embodiment of the present invention, siO in step (3) 2 And SiC has a particle size of 80 to 100 meshes and 80 to 100 meshes, respectively.
As a preferred embodiment of the present invention, in step (3), siO 2 And SiC in a mass ratio of 2-3:1.
As a preferred embodiment of the present invention, in step (3), siO 2 And the total addition amount of SiC is 1 to 1.5 percent of the mass of Si powder.
As a preferable technical scheme of the invention, the pressure of the reactor in the step (4) is 0.1-0.15 MPa.
As a preferable technical scheme of the invention, in the step (4), the air bed flow rate of the gas is 0.04-0.09 m/s.
As a preferable technical scheme of the invention, in the step (4), N in the mixed gas 2 And Cl 2 The volume ratio of (2) is 1:8-12.
Compared with the prior art, the invention has the following beneficial effects:
(1)in the crushing and grinding stage of Si powder, si powder may be agglomerated together due to static electricity, van der Waals force and other acting forces; meanwhile, in the high-temperature reaction process, si powder is more easily agglomerated together due to high-temperature melting of the Si powder, so that the reaction contact area of the Si powder and chlorine is reduced, and the reaction efficiency of the Si powder and the chlorine is further influenced. In view of the problems, the invention is characterized in that the Si powder is doped with SiO material 2 And SiC and adjusting process parameters, can well solve the above-mentioned existing problems, specifically: the invention adds a certain amount of SiO into Si powder 2 And SiC, where SiO 2 The melting point of SiC is about 1600-1700 ℃ and exceeds 2000 ℃, so that the reaction temperature is strictly controlled within the range of 1000-1100 ℃ in the invention, and SiO is at the temperature 2 SiC can not be melted and fully reacted with chlorine, but is mainly dispersed in a reaction system in the form of fine particles and is entrained in Si powder in the fluidization reaction process in a reactor, so that the aggregation, growth and agglomeration of the Si powder are avoided; with the consumption and continuous supplementation of Si powder reaction, siO 2 And SiC micropowder particles are also continuously exposed to further impact Si powder which is possibly agglomerated, so that the tendency of Si powder aggregation is reduced;
(2) The reaction pressure in the invention is micro positive pressure, cl 2 A small amount of N is mixed in 2 ，N 2 The existence of the atmosphere flow can continuously impact the Si powder, further reduce the agglomeration tendency of the Si powder, improve the dispersibility of the Si powder and improve the Si powder and the Cl 2 Further promoting the reaction to proceed fully; however, N 2 The excessive dosage of the N-type compound fertilizer can influence the production efficiency, and the too small dosage can influence the use effect, and the invention leads N to be 2 And Cl 2 The volume ratio of (2) is optimally controlled to be 1:8-12.
(3) SiO in the present invention 2 And SiC has a particle size slightly larger than that of Si powder, so that SiO 2 And SiC is not encapsulated by Si powder; in addition, siO is formed 2 And the best effect is obtained by controlling the dosage ratio of SiC to 2-3:1.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
In the invention, si powder and SiO 2 And SiC are commercially available.
It is particularly emphasized that the fluidized bed reactors and the like used in the present invention are all prior art.
The purity of the silicon tetrachloride is detected by adopting a gas chromatography (thermal conductivity detector) (area normalization method); silicon tetrachloride is analyzed and detected by a gas chromatograph (thermal conductivity detector) (area normalization method); the chlorine conversion is obtained by dividing the obtained silicon tetrachloride mass conversion into the chlorine mass divided by the total amount of introduced chlorine.
Example 1
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to a particle size of 200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 110 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1% of the total mass of the Si powder into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The reaction was carried out in a fluidized bed reactor at 1020℃and 0.11 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 Not less than 98% and not less than 97% SiC.
Wherein in the step (3), siO 2 And the particle size of SiC was 100 mesh and 100 mesh, respectively.
Wherein in the step (3), siO 2 And SiC (SiC)The dosage ratio is 2.5:1.
Wherein in the step (4), the air bed flow rate of the gas is 0.06m/s.
Wherein in the step (4), N in the mixed gas 2 And Cl 2 Is 1:9 by volume.
The chlorine conversion in the above reaction was determined to be 95.8% and the purity of silicon tetrachloride was determined to be 96.7%.
Example 2
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to a particle size of 200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 120 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1.2 percent of the total mass of the Si powder into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The reaction was carried out in a fluidized bed reactor at 1050℃and 0.11 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 Not less than 98% and not less than 97% SiC.
Wherein in the step (3), siO 2 And the particle size of SiC was 100 mesh and 100 mesh, respectively.
Wherein in the step (3), siO 2 And the dosage ratio of SiC was 2.7:1.
Wherein in the step (4), the air bed flow rate of the gas is 0.09m/s.
Wherein in the step (4), N in the mixed gas 2 And Cl 2 Is 1:10 by volume.
The chlorine conversion in the above reaction was determined to be 96.1% and the purity of silicon tetrachloride was determined to be 96.9%.
Example 3
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to 180 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 120 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1.3 percent of the total mass of the Si powder into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The reaction was carried out in a fluidized bed reactor at 1050℃and 0.12 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 Not less than 98% and not less than 97% SiC.
Wherein in the step (3), siO 2 And the particle diameters of SiC were 80 mesh and 80 mesh, respectively.
Wherein in the step (3), siO 2 And the dosage ratio of SiC was 2.8:1.
Wherein in the step (4), the air bed flow rate of the gas is 0.08m/s.
Wherein in the step (4), N in the mixed gas 2 And Cl 2 Is 1:11 by volume.
The chlorine conversion in the above reaction was determined to be 95.5% and the purity of silicon tetrachloride was determined to be 96.8%.
Example 4
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to 170 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 110 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1.2 percent of the total mass of the Si powder into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 Is fluidized by the mixed gas of (2)The reaction was carried out in a bed reactor at 1040℃and 0.12 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 Not less than 98% and not less than 97% SiC.
Wherein in the step (3), siO 2 And the particle diameters of SiC were 90 mesh and 90 mesh, respectively.
Wherein in the step (3), siO 2 And the dosage ratio of SiC was 2.6:1.
Wherein in the step (4), the air bed flow rate of the gas is 0.07m/s.
Wherein in the step (4), N in the mixed gas 2 And Cl 2 Is 1:10 by volume.
The chlorine conversion in the above reaction was determined to be 95.3% and the purity of silicon tetrachloride was determined to be 96.8%.
Example 5
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to 2000 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 120 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1.4 percent of the total mass of the Si powder into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The mixed gas of (2) was reacted in a fluidized bed reactor at 1060℃and 0.14 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 Not less than 98% and not less than 97% SiC.
Wherein in the step (3), siO 2 And the particle diameters of SiC were 90 mesh and 90 mesh, respectively.
Wherein in the step (3), siO 2 And the dosage ratio of SiC was 2.9:1.
Wherein in the step (4), the air bed flow rate of the gas is 0.08m/s.
Wherein in the step (4), N in the mixed gas 2 And Cl 2 Is 1:9 by volume.
The chlorine conversion in the above reaction was 97%, and the purity of silicon tetrachloride was 96.3%.
Comparative example 1
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to a particle size of 200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 120 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) The Si powder dried in the step (2) and N-containing Si powder 2 And Cl 2 The reaction was carried out in a fluidized bed reactor at 1050℃and 0.11 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), the air bed flow rate of the gas is 0.09m/s.
Wherein in the step (3), N in the mixed gas 2 And Cl 2 Is 1:10 by volume.
The chlorine conversion in the above reaction was 92.8% and the purity of silicon tetrachloride was 94.7%.
Comparative example 2
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to a particle size of 200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 120 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1.2 percent of the total mass of the Si powder into the Si powder dried in the step (2) 2 Obtaining a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 Is fed into a fluidized bed reactor at 1050 ℃ and 0.11MPaAnd (3) carrying out reaction.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 The purity of (2) is not lower than 98%.
Wherein in the step (3), siO 2 The particle diameters of (2) were 100 mesh, respectively.
Wherein in the step (4), the air bed flow rate of the gas is 0.09m/s.
Wherein in the step (4), N in the mixed gas 2 And Cl 2 Is 1:10 by volume.
The chlorine conversion rate in the above reaction was measured to be 93.9%, and the purity of silicon tetrachloride was measured to be 95.1%.
Comparative example 3
A synthetic method of silicon tetrachloride comprises the following steps:
(1) Crushing and grinding Si powder raw materials to a particle size of 200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1) at 120 ℃ under the condition of isolating oxygen, so as to ensure that the water content after drying is not higher than 0.8%;
(3) Adding SiO accounting for 1.2 percent of the total mass of the Si powder into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) Mixing the reaction mixture obtained in the step (3) with Cl 2 The reaction was carried out in a fluidized bed reactor at 1050℃and 0.11 MPa.
Wherein, in the step (1), the purity of Si powder is not less than 99%.
Wherein in the step (3), siO 2 Not less than 98% and not less than 97% SiC.
Wherein in the step (3), siO 2 And the particle size of SiC was 100 mesh and 100 mesh, respectively.
Wherein in the step (3), siO 2 And the dosage ratio of SiC was 2.7:1.
Wherein in the step (4), the air bed flow rate of the gas is 0.09m/s.
The chlorine conversion in the above reaction was 94.2% and the purity of silicon tetrachloride was 95.5% as determined.
The technical idea of the present invention is described by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must be implemented depending on the above embodiments. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of individual raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (6)
1. The synthesis method of the silicon tetrachloride is characterized by comprising the following steps of:
(1) Crushing and grinding the Si powder raw material to 160-200 meshes;
(2) Drying the Si powder obtained by grinding in the step (1);
(3) SiO is added into the Si powder dried in the step (2) 2 And SiC to obtain a reaction mixture;
(4) The reaction mixture obtained in the step (3) and N-containing 2 And Cl 2 The mixed gas of the silicon tetrachloride is reacted in a fluidized bed reactor at the temperature of 1000-1100 ℃ to obtain the silicon tetrachloride;
wherein SiO in step (3) 2 And the particle size of SiC is 80-100 meshes and 80-100 meshes respectively;
wherein in the step (3), siO 2 The mass ratio of the SiC to the silicon carbide is 2-3:1;
wherein in the step (3), siO 2 The total addition amount of the SiC is 1-1.5% of the mass of the Si powder;
wherein in the step (4), N in the mixed gas 2 And Cl 2 The volume ratio of (2) is 1:8-12.
2. The method for synthesizing silicon tetrachloride according to claim 1, wherein in the step (1), the purity of Si powder is not less than 99%.
3. The method for synthesizing silicon tetrachloride according to claim 1, wherein in the step (2), oxygen is isolated during drying, the drying temperature is 100-120 ℃, and the water content after drying is not more than 0.8%.
4. The method for synthesizing silicon tetrachloride according to claim 1, wherein SiO in the step (3) is 2 Not less than 98% and not less than 97% SiC.
5. The method for synthesizing silicon tetrachloride according to claim 1, wherein the reactor pressure in the step (4) is 0.1 to 0.15mpa.
6. The method for synthesizing silicon tetrachloride according to claim 1, wherein in the step (4), the flow rate of the air bed is 0.04-0.09 m/s.
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| JPS5934128B2 (en) * | 1980-06-17 | 1984-08-20 | 宇部興産株式会社 | Method for producing silicon tetrachloride |
| CN103011174B (en) * | 2012-12-26 | 2014-10-22 | 重庆大学 | Device and method for preparing SiCl4 through silicon ore carbochlorination |
| CN107601512B (en) * | 2017-11-02 | 2020-08-21 | 成都蜀菱科技发展有限公司 | Mixture and production method of silicon tetrachloride |
| CN109467091A (en) * | 2018-12-25 | 2019-03-15 | 天津中科拓新科技有限公司 | A kind of energy saver and method of silicon tetrachloride synthesis |
| CN217568765U (en) * | 2022-07-14 | 2022-10-14 | 内蒙古自治区浩森新材料开发有限公司 | Reactor for producing silicon tetrachloride by comprehensively utilizing superfine silicon powder |
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Denomination of invention: A synthesis method of silicon tetrachloride Granted publication date: 20230502 Pledgee: Bank of China Limited Qianjiang Branch Pledgor: WUHAN XINGUI TECHNOLOGY QIANJIANG Co.,Ltd. Registration number: Y2024980013384 |