CN213912399U - Reaction rectification system for treating high-boiling-point substances in polycrystalline silicon by-products - Google Patents
Reaction rectification system for treating high-boiling-point substances in polycrystalline silicon by-products Download PDFInfo
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Abstract
The utility model discloses a reaction rectification system for treating high-boiling residues of polysilicon byproducts, which comprises a clapboard reaction rectification tower (1), a condenser (8), a storage tank (9), a circulating pump (6) and a reboiler (15); a vertical partition plate (13) is arranged in the partition plate reaction rectifying tower (1) to divide the reaction rectifying tower into four parts, namely a public rectifying section, a public stripping section, a feeding side and a product side; the feed side is divided into I \ J sections; the product side is divided into F \ G sections; monosilane products with the boiling point range of 5-40 ℃ under 1 standard atmospheric pressure are obtained at the top of the partition reaction rectifying tower, and monosilane products with the boiling point range of 50-90 ℃ under 1 standard atmospheric pressure are obtained at the product side of the partition reaction rectifying tower; and tower kettle materials of the clapboard reaction rectifying tower return to the feeding side through a circulating pump (6). The utility model provides a technical problem be applied to many silicon compound catalytic cracking reaction with baffle reaction rectifying column technique to investment saving and operating cost are high, and the energy can be saved realizes reducing cost and improving effect.
Description
Technical Field
The utility model relates to a polycrystalline silicon preparation technical field, especially relate to polycrystalline silicon byproduct processing field.
Background
The polycrystalline silicon is a main raw material for manufacturing products such as photovoltaic solar cells, and in the method for manufacturing high-purity polycrystalline silicon, the improved Siemens method is the mainstream polycrystalline silicon production method at present; in the improved Siemens method, an electrode is arranged on a chassis of a reduction furnace, a graphite assembly is arranged on the electrode, silicon cores are fixed on the graphite assembly, and the silicon cores on the two graphite assemblies are overlapped by a short silicon core to form an n-shaped current loop; the silicon core is broken down by high voltage to be a conductor, and the silicon core is heated to 900-1200 ℃ by current; introducing trichlorosilane and hydrogen gas into a reduction furnace for reaction, reducing silicon in the trichlorosilane to deposit on the surface of a silicon core, stopping introducing raw materials after forming a polycrystalline silicon rod with the diameter of 120 plus 200mm, gradually reducing the current until the current is stopped, gradually cooling the polycrystalline silicon rod in the reduction furnace, replacing the polycrystalline silicon rod with nitrogen after cooling to a certain temperature, taking the polycrystalline silicon rod out of the reduction furnace, crushing the polycrystalline silicon rod taken out of the reduction furnace into block-shaped materials, packaging and transporting the block-shaped materials to the downstream of a photovoltaic industry chain for use.
9 pairs, 12 pairs and 24 pairs of polysilicon rods are produced in each batch by an early polysilicon reduction furnace, the reduction furnace for polysilicon deposition is generally large-sized at present, and large reduction furnaces such as 36 pairs, 40 pairs, 48 pairs, 60 pairs, 66 pairs and 72 pairs of rods are put into production and use; since the internal temperature in the large-scale reduction furnace is higher, the silicon polymer is more easily produced than the reduction furnace with a lower number of polysilicon rods, the silicon polymer contains chlorosilane containing more than two silicon atoms, the boiling point of the silicon polymer is higher, and the silicon polymer is generally called as high-boiling-point substances after the polysilicon reduction tail gas is recovered and separated. With the expansion of the production scale of polycrystalline silicon, the yield of high-boiling-point substances is increased, the direct hydrolysis treatment of the high-boiling-point substances causes the loss of silicon element and chlorine element, and most enterprises recover trichlorosilane and silicon tetrachloride by a cracking method at present, or recover and separate the trichlorosilane and the silicon tetrachloride to be used as high-value-added products or used as raw materials to produce silicone oil.
In addition, the organosilicon industry also produces higher-boiling compounds than organosilicon during the synthesis of organosilicon monomers, the main component of which is a disilane-based polysilicone compound, also commonly referred to as high-boiling compounds.
In the process of producing polycrystalline silicon or in the process of synthesizing organic silicon monomer, the generated polysilicone compound can be cracked with hydrogen chloride or chlorine gas in the presence of catalyst to generate reusable monosilicone compound.
The main cracking products of the polysilicone compound produced in the production process of the polycrystalline silicon are silicon tetrachloride, trichlorosilane and dichlorosilane; the main cracking products of the polysilicone compound generated in the synthetic process of the organic silicon monomer are methyl trichlorosilane, dimethyl dichlorosilane, methyl monohydroxy dichlorosilane and the like.
At present, the types of catalysts for cracking of polysilicone compounds in the polysilicon and organosilicon industries are mainly organic amine catalysts (the organic amine catalysts can be liquid or solid according to the difference of carbon chain structures), aluminum trichloride catalysts, palladium-phosphorus coordination compound catalysts, phosphate catalysts, molecular sieve catalysts and activated carbon catalysts.
The product of cracking the high-boiling-point substance by the catalyst usually needs to be separated from the raw material polysilicone compound and the product monosilicone compound by a rectifying tower; at present, when the cracking treatment is carried out on the polysilicone compound, most of the reaction unit and the separation unit are carried out in two types of independent equipment, the equipment investment and the operation cost are high, the cracking reaction with high boiling is mainly an exothermic reaction, and part of heat can not be effectively utilized, so that the energy waste is caused.
Patent CN101659672B discloses a cracking treatment method of waste residue slurry formed in the process of synthesizing organosilicon monomers; adding high-boiling residues with the same mass into a liquid-solid mixture with the solid content of the organic silicon waste residue slurry of 20% to prepare a cracking raw material liquid; the catalyst is tributylamine, the cracking reaction temperature is 80-160 ℃, HCl gas is introduced, the feeding speed of hydrogen chloride and the mixed liquid ratio of the raw materials are 1: 1.05-1: 1.12; the high-boiling-point substance is a mixture of slag slurry with the solid content of 20 percent and the high-boiling-point substance, the product monosilane is directly separated in the cracking process, the conversion rate is more than 70 percent, the selectivity of the dimethyldichlorosilane is more than 35 percent, and the selectivity of the monomethylhydrosilane is more than 40 percent.
Patent CN104130279A discloses a method for catalytically cracking high boiling point organic silicon by solid alkali, which comprises the steps of carrying out load reaction on tri-n-butylamine, dioctadecylsecondary amine, perfluorinated triethylamine and macroporous cross-linked polyhydroxyethyl methacrylate resin, obtaining a composite catalyst after the reaction is finished, adding the organic silicon high boiling point substance and the composite catalyst after impurity removal into a cracking kettle with a fractionating tower, then introducing hydrogen chloride gas, reacting to generate a mixed product mainly containing four monomers of dimethyldichlorosilane, trimethylchlorosilane, monomethyldichlorosilane and monomethyltrichlorosilane, and condensing and collecting the mixed product through a condenser at the top of the fractionating tower.
Patent CN109384233A relates to a method for treating silicon polymer, which uses ionic liquid as catalyst, uses silicon polymer and anhydrous hydrogen chloride as raw materials, and the silicon polymer and the anhydrous hydrogen chloride react in a reactor at 30-180 ℃ and 0.02-1.2 MPa to obtain chlorosilane product containing 1 silicon atom, and the chlorosilane mixture comes out from the top of the reactor.
In patent CN103663460A, chlorosilane high-boiling residues and hydrogen chloride are cracked in a cracking reaction tower under the action of an organic amine catalyst, the cracking reaction is carried out at 100-140 ℃ under normal pressure, and a product mixture is directly extracted from the top of the tower after the chlorosilane mixture is generated by the reaction.
In the method or the device for catalytically cracking the high-boiling-point substances, chlorosilane mixed gas is produced in the reaction in the process of cracking the polysilicone compound, and in a system without reaction rectification coupling, products produced in the reaction contain high-boiling-point substances with higher content; in a reaction system of reactive distillation coupling, only simple reactive coupling is performed, high-boiling-point substances return to the reaction system through distillation, monosilane in a reaction product is not subjected to rough separation, a subsequent process is required to separately perform separation operation by using a rectifying tower, and the problems of high investment and operation cost and energy waste are caused.
Disclosure of Invention
The utility model aims to solve the technical problem of providing a reaction rectification system for treating high-boiling residues of polysilicon by-products, which aims to solve the problem that the existing non-reaction rectification coupling and simple reaction rectification coupling are not enough.
The utility model adopts a reaction rectification system for processing high-boiling residues of polysilicon by-products, which adds a vertical baffle plate in a rectification tower to separate a feed side from a withdrawal side, thereby reducing the back mixing of materials in the tower; separating the polysilicone compound in the product in the clapboard rectifying tower, returning the polysilicone compound to the polysilicone compound cracking device for continuous treatment, and performing primary separation on the cracked product and extracting the cracked product from the middle part and the top part of the clapboard rectifying tower respectively; and meanwhile, complete thermal coupling is formed in the tower, so that the investment is further reduced, and the energy consumption is reduced.
The technical scheme of the utility model as follows:
the partition reaction rectification system comprises a partition reaction rectification tower 1, a condenser 8, a storage tank 9, a circulating pump 6 and a reboiler 15; a vertical partition 13 is arranged in the partition reaction rectifying tower 1 to divide the reaction rectifying tower into four parts, namely a common rectifying section A, a common stripping section E, a feeding side and a product side; monosilane products having a boiling point range of 5 to 40 ℃ at 1 atm are taken out from the top of the baffle reactive rectifying column 1, monosilane products having a boiling point range of 50 to 90 ℃ at 1 atm are taken out from the product side, and a mixture of the polysilicone compound and the monosilicone compound is returned to the feed side by a circulating pump 6 for the bottom material of the column bottom.
The feed side can be divided into 2 to 4 stages, preferably 2 to 3 stages; when the cracking reaction of the polysilicate compound of the baffle reaction feeding system is carried out in the tower kettle of the baffle reaction rectifying system, the catalyst is not filled at the feeding side, and the catalyst is added into the tower kettle of the baffle reaction rectifying tower through a feeding pipeline.
When the cracking reaction of the polysilicone compound is carried out in the bottom of the rectifying tower, 1 feeding hole on the feeding side is connected with a feeding pipeline, a mixture of the polysilicone compound and monosilane returned by a circulating pump 6 is fed in, and the position of the feeding hole connected with a feeding pipe is selected between any two parts; the rectifying tower has 2 material inlets connected to the material inlet pipe, 1 material inlet connected to the material inlet pipe and filled with anhydrous hydrogen chloride or chlorine as reaction material, and the other 1 material inlet connected to the material inlet pipe and filled with polysilicone compound or mixture of polysilicone compound and monosilane.
The product side can be divided into 2-4 sections, preferably 2 sections, the product can be extracted from the middle of any two sections, and when the product side is divided into 3-4 sections, 1-2 extraction ports can be arranged, but 1 extraction port is preferably arranged.
The operating pressure range of the rectifying tower 1 is 0.2-1.0 MPa. The catalyst filled on the feeding side is nitrogen-containing ion exchange resin, an immobilized quaternary ammonium salt catalyst or a similar catalytic catalyst; the catalyst participating in the reaction in the tower bottom of the rectifying tower can be nitrogen-containing ion exchange resin, immobilized quaternary ammonium salt catalyst or similar catalyst, and can also be quaternary ammonium salt as cation and CF as anion3SO3 -、CF3COO-、PF6-、N(CF3SO2)2 -、C(CF3SO2)3 -、N(CN)2 -、Cl-Ionic liquid, or amino group-containing compounds such as phenethylamine and triethylamine.
Use above-mentioned baffle reaction rectification system of handling polysilicone compound, can effectually carry out the schizolysis with polysilicone compound in this reactor, produce silicon tetrachloride, dichlorosilane, trichlorosilane etc. compare with prior art, the utility model has the advantages of further reduce the investment, reduce the energy consumption.
Drawings
FIG. 1 shows a reactive distillation system with 1 feed inlet at the feed side for treating high-boiling residues as by-products of polysilicon.
In the figure, 1-partition reaction rectifying tower, 2-pipeline I, 3-pipeline II, 4-pipeline III, 5-pipeline IV, 6-circulating pump, 7-pipeline V, 8-condenser, 9-storage tank, 10-pipeline VI, 11-pipeline VII, 12-pipeline VIII, 13-partition, 14-partition rectifying tower kettle, 15-reboiler and 16-pipeline VII.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described with reference to the accompanying drawings of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, those skilled in the art can implement all other embodiments without creative changes, and all other embodiments belong to the protection scope of the present invention.
FIG. 1 shows a specific embodiment of the present invention, in this embodiment, the partition reactive distillation column 1 is divided into 4 parts by the partition 13, which are respectively a public distillation section A, a public stripping section E, a feed side and a product side, the feed side is divided into two sections I \ J, the product side is divided into two sections F \ G, and the I section and the J section are not filled with the polysilicone compound cracking catalyst. Introducing a polysilicone compound or a mixture of the polysilicone compound and monosilane into a tower kettle 14 of the clapboard rectifying tower through a second pipeline 3, introducing anhydrous HCl or chlorine into the tower kettle 14 of the clapboard rectifying tower through a fourth pipeline 5, and adding a catalyst into the tower kettle 14 of the clapboard reactive rectifying tower through the second pipeline 3 or the fourth pipeline 5; the polysilicone compounds are cracked to monosilane in the bottom 14 of the baffle reactive distillation column. 1 monosilane product with the boiling point range of 5-40 ℃ under the standard atmospheric pressure enters a condenser 8 through a tower top pipeline five 7 to be condensed and then enters a storage tank 9, one part of monosilane product flows back through a pipeline seven 11, and the other part of monosilane product is extracted through a pipeline six 10; 1 monosilane product with a boiling point range of 50-90 ℃ at normal atmospheric pressure is extracted from the pipeline eight 12; the polysilicone compound returns to the tower bottom 14 through the public stripping section E, and returns to the feeding side of the clapboard rectifying tower through a pipeline III 4 and a pipeline I2 by using a circulating pump 6; the heat required for the reaction is supplemented by reboiler 15 and removed through line nine 16 when necessary for maintenance or removal of material from column 14.
Although the embodiments of the present invention have been described and illustrated in detail with reference to the accompanying drawings, it is to be understood that various equivalent changes and modifications can be made therein by those skilled in the art according to the concept of the present invention, and that the functional effects thereof are within the scope of the present invention without departing from the spirit of the present invention.
Claims (3)
1. A reaction rectification system for treating high-boiling residues of polysilicon byproducts comprises a clapboard reaction rectification tower (1), a condenser (8), a storage tank (9), a circulating pump (6) and a reboiler (15); a vertical partition plate (13) is arranged in the partition plate reaction rectifying tower (1) to divide the reaction rectifying tower into four parts, namely a public rectifying section, a public stripping section, a feeding side and a product side; it is characterized in that the feeding side is divided into I \ J sections; the product side is divided into F \ G sections.
2. The reactive distillation system for treating high boiling residues of polysilicon byproducts as recited in claim 1, wherein when the feed side is divided into sections I \ J, no cracking catalyst is filled in the sections I \ J, and the catalyst is added into the column bottom of the baffle reactive distillation column (1).
3. The reactive distillation system for treating high boiling residues by-product of polysilicon as claimed in claim 1, wherein when the feed side is divided into sections I \ J, feed inlets are disposed in the middle of the sections I \ J and at the lower part of the sections J to connect with the feed pipeline, and a feed inlet is disposed at the bottom of the baffle reactive distillation column (1) to connect with the feed pipeline.
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| CN202021762382.9U CN213912399U (en) | 2020-08-21 | 2020-08-21 | Reaction rectification system for treating high-boiling-point substances in polycrystalline silicon by-products |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478613A (en) * | 2022-02-15 | 2022-05-13 | 聊城市鲁西化工工程设计有限责任公司 | Method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organic silicon crude monomer |
| CN116173536A (en) * | 2023-03-30 | 2023-05-30 | 清电光伏科技有限公司 | Polysilicon rectifying system and rectifying method |
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2020
- 2020-08-21 CN CN202021762382.9U patent/CN213912399U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478613A (en) * | 2022-02-15 | 2022-05-13 | 聊城市鲁西化工工程设计有限责任公司 | Method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organic silicon crude monomer |
| CN116173536A (en) * | 2023-03-30 | 2023-05-30 | 清电光伏科技有限公司 | Polysilicon rectifying system and rectifying method |
| CN116173536B (en) * | 2023-03-30 | 2023-10-24 | 清电光伏科技有限公司 | Polysilicon rectifying system and rectifying method |
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