CN110078080B - Chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction - Google Patents
Chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction Download PDFInfo
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- CN110078080B CN110078080B CN201910357954.0A CN201910357954A CN110078080B CN 110078080 B CN110078080 B CN 110078080B CN 201910357954 A CN201910357954 A CN 201910357954A CN 110078080 B CN110078080 B CN 110078080B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention relates to a chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction. After the materials recovered after the chlorosilane high-boiling residue slurry is pretreated by the slag slurry treatment device are separated, the chlorosilane low polymer enters a cracking reactor filled with a catalyst to react with hydrogen chloride to obtain a cracking product, and a monosilane product is obtained after subsequent separation. The chlorosilane high-boiling residue recovery process combining the slurry treatment and the cracking reaction has the following advantages: the slag slurry treatment device can effectively remove solid impurities such as metal chloride and the like contained in the material, and avoid the deactivation and coking phenomena of the cracking catalyst; the high-boiling-point substance separation tower is provided with a side line for extraction, so that liquid-phase high polymers can be separated, and accumulation is avoided; the cracking reaction rectifying tower can simultaneously carry out the cracking reaction and the separation process, and the cracking rate can be improved.
Description
Technical Field
The invention relates to the field of chlorosilane production, in particular to a chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction.
Background
At present, the domestic polycrystalline silicon production process mainly adopts an improved Siemens method, and the process mainly comprises the following steps: the method comprises a trichlorosilane preparation process, a trichlorosilane refining process, a trichlorosilane reduction process and a reduction recovery process. Due to the restriction of factors such as the purity of the silicon powder raw material, the catalyst, the process conditions and the like, a small amount of high-boiling-point substances consisting of compounds containing Si-C, Si-Si, Si-C-Si and Si-O-Si bonds, silicon powder, the catalyst, metal chloride and the like remained in the reaction can be generated in the trichlorosilane preparation process and the trichlorosilane reduction process. The high-boiling-point substance is a dark brown mixed liquid with pungent smell and strong corrosivity, is inflammable, explosive and difficult to store, has limited market capacity, can cause a large amount of overstocked warehouses due to untimely treatment, and brings great hidden danger to safety and environmental protection.
In the patent of 'method and device for cracking and recovering chlorosilane high-boiling-point substances in polycrystalline silicon production', an organic amine catalyst and hydrogen chloride are mixed to be used as a feed, and the chlorosilane high-boiling-point substances are used as another feed and simultaneously enter a cracking reaction tower for cracking reaction. The method does not pretreat chlorosilane high-boiling residues, does not recover silicon tetrachloride in the raw materials in advance, is one of cracking products, is limited by reaction balance, and cannot improve the cracking rate of the high-boiling residues. More importantly, the solid impurities in the high-boiling residues are not removed, so that the catalyst is deactivated, more catalyst is required to be used, and the production cost is increased.
Disclosure of Invention
In order to solve the problems, the invention provides a chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction. The invention integrates two different devices, improves the cracking rate of high-boiling residues and the service life of the catalyst, reduces the subsequent hazardous waste treatment capacity, and improves the economic benefit of enterprises.
The invention aims to provide a process for recovering chlorosilane high-boiling residues by combining a slag slurry treatment device and a cracking technology, wherein the high-boiling residues are pretreated by using the slag slurry treatment device, and the chlorosilane high-boiling residues after silicon tetrachloride and solid impurities are removed are subjected to separation and cracking reaction to obtain a monosilane product.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a process for recovering chlorosilane high-boiling-point substances by combining slag slurry treatment and cracking reaction comprises the steps of recovering silicon tetrachloride from chlorosilane high-boiling-point substance slurry through silicon tetrachloride recovery equipment of a slag slurry treatment unit, removing solid impurities through deslagging and drying equipment, enabling the obtained liquid phase to sequentially pass through a tetrachloro separating tower and a high-boiling-point substance separating tower to be used for recovering the silicon tetrachloride, removing high polymers and residual solid impurities, enabling the obtained chlorosilane low polymers and hydrogen chloride to enter a continuous cracking reactor filled with a catalyst for cracking reaction, enabling the reacted materials to enter a cracking reaction rectifying tower for reaction and rectification, finally, collecting a monosilane product from the top of the tower, recovering hydrogen chloride from tail gas, and returning materials in the bottom of the tower to the high-boiling-point substance separating tower to recover unreacted low polymers.
The invention relates to a device for recovering chlorosilane high-boiling residues by combining a slag slurry treatment device and a cracking technology, which comprises the following steps:
the device is formed by connecting silicon tetrachloride recovery equipment (A), slag removal drying equipment (B), a silicon tetrachloride separation tower (C), a high-boiling-point substance separation tower (D), a continuous cracking reactor (E) and a cracking reaction rectifying tower (F).
The main equipment of the continuous cracking reactor (E) is one of a jacket reaction kettle or a fixed bed reactor structure, and a catalyst containing ammonium salt functional groups is filled in the reactor.
The cracking reaction rectifying tower (F) is provided with two feed inlets which are respectively used for feeding reaction products of gas-phase hydrogen chloride and the continuous cracking reactor (E), and can perform two processes of separation of the reaction products while performing cracking reaction of chlorosilane oligomers and hydrogen chloride in the tower.
The hydrogen chloride feed inlet of the cracking reaction rectifying tower (F) adopts a gas phase tubular distributor.
The invention relates to a method for recovering chlorosilane high-boiling residues by combining a slag slurry treatment device and a cracking technology, which comprises the following steps:
1. the chlorosilane high-boiling residue slurry enters a silicon tetrachloride recovery device (A) of a slag slurry treatment unit to recover silicon tetrachloride in the material, and in order to ensure the fluidity of the residual slurry, the slurry is allowed to contain part of silicon tetrachloride;
2. the high-boiling-point substance slurry after the silicon tetrachloride is recovered enters a deslagging drying device (B) for removing solid impurities in the material, and the obtained liquid-phase material enters a silicon tetrachloride separation tower of a high-boiling cracking unit;
3. purifying by a silicon tetrachloride separation tower (C), and recovering silicon tetrachloride from the tower top; feeding the tower bottom material into a high-boiling-point substance separation tower;
4. feeding the material extracted from the tower kettle of the silicon tetrachloride separating tower (C) into a high-boiling-point substance separating tower (D), feeding chlorosilane oligomers obtained from the tower top into a continuous cracking reactor, extracting chlorosilane high polymers from the middle lower part side of the tower, and intermittently discharging solid-containing materials from the tower kettle to return to a slag slurry system for recycling;
5. the silicon chloride oligomer and gas-phase hydrogen chloride are used as reactants and enter a continuous cracking reactor (E) filled with the catalyst for cracking reaction, and a reaction product enters a cracking reaction rectifying tower;
6. the material reacted by the continuous cracking reactor (E) enters from the middle upper part of a cracking reaction rectifying tower (F), gas-phase hydrogen chloride enters from the middle lower part of the tower (F), oligomer cracking reaction and reaction product separation processes simultaneously occur in the tower, monosilane products are extracted from the top of the tower, hydrogen chloride is recovered from tail gas, and the material obtained from the bottom of the tower returns to a high-boiling-point substance separation tower (D) to recover oligomers.
The invention has the following advantages:
1. the high-boiling-point substance cracking unit is connected with the slag slurry processing unit in series, the slag slurry processing unit is utilized to carry out pretreatment on the chlorosilane high-boiling-point substance, part of silicon tetrachloride is recycled to improve the cracking rate of oligomers, solid impurities in materials are removed, particularly metal chloride which is extremely easy to cause the poisoning of a cracking catalyst is used, and the service life of the catalyst is prolonged.
2. The high-boiling-point substance separation tower (D) adopts a structure with side line extraction, chlorosilane low polymers are extracted from the top of the tower, chlorosilane high polymers are extracted from the middle lower part of the side line, and solid-containing materials are intermittently discharged from the bottom of the tower. Through the arrangement of side extraction, the accumulation of chlorosilane high polymers is avoided, and solid-containing materials intermittently discharged from the tower kettle can be returned to the slurry treatment unit for recovery.
3. Two processes of the cracking reaction of the chlorosilane oligomers and the separation of reaction products can be simultaneously carried out in the tower of the cracking reaction rectifying tower (F), which is favorable for improving the cracking rate of the chlorosilane oligomers.
Drawings
FIG. 1: the invention relates to a process flow chart.
FIG. 2: example 1 "apparatus for treating chlorosilane high boiler slurry of 1000 kg/h" and material balance diagram of the invention.
FIG. 3: example 2 "treatment apparatus for chlorosilane high boiler slurry of 2000 kg/h" of the invention is a process flow and material balance diagram.
Description of reference numerals:
a-silicon tetrachloride recovery equipment; b-slag removal and drying equipment; c-silicon tetrachloride separation tower, D-high boiling residue separation tower, E-continuous cracking reactor and F-cracking reaction rectifying tower.
1-chlorosilane high-boiling-point material slurry; 2-removing the silicon tetrachloride to obtain high-boiling-point substance slurry; 3-silicon tetrachloride I; 4-removing the high-boiling-point substance after solid impurities are removed; 5-solid slag charge; 6-silicon tetrachloride II; 7-mixing high boiling residues; an 8-chlorosilane oligomer; 9-chlorosilane polymers; 10-solid containing material; 11-gaseous hydrogen chloride; 12-a cleavage product; 13-monosilane product and hydrogen chloride; 14-chlorosilane oligomers and byproducts.
Detailed Description
The technical solutions in the embodiments of the present invention are further described below by way of examples in conjunction with the accompanying drawings, which are drawn for illustrating the present invention and do not limit the specific application forms of the present invention.
The chlorosilane high-boiling residue after removing the solid impurities mainly comprises compounds containing Si-C, Si-Si, Si-C-Si and Si-O-Si bonds. Experiments show that Si-C and Si-Si bonds can be broken under the action of halogen, alcohol, hydrogen, halide, hydrogen chloride and the like to generate monosilane containing various functional groups. The invention respectively uses CH 3 SiCl 3 、Si 2 Cl 6 And (CH) 3 ) 2 Si 2 Cl 4 For example, the reaction equation involved is as follows:
the cleavage mechanism of this reaction is:
the electronegativity of Cl atom is large, so that the electron cloud of Si-Cl bond shifts to Cl, and Si δ+ Has electropositivity, and adopts an electron-rich nucleophilic reagent as a catalyst to attack Si δ+ Polarization and breakage of Si-C bond or Si-Si bond are carried out, and protonation is carried out under the action of hydrogen chloride.
The invention relates to a device for a chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction, which comprises the following steps:
the device is formed by connecting silicon tetrachloride recovery equipment (A), slag removal drying equipment (B), a silicon tetrachloride separation tower (C), a high-boiling-point substance separation tower (D), a continuous cracking reactor (E) and a cracking reaction rectifying tower (F).
The main equipment of the continuous cracking reactor (E) is one of a jacket reaction kettle or a fixed bed reactor structure, and the reactor is filled with a catalyst containing an ammonium salt functional group.
The cracking reaction rectifying tower (F) is provided with two feed inlets which are respectively used for feeding reaction products of gas-phase hydrogen chloride and the continuous cracking reactor (E), and can perform two processes of separation of the reaction products while performing cracking reaction of chlorosilane oligomers and hydrogen chloride in the tower.
The hydrogen chloride feed inlet of the cracking reaction rectifying tower (F) adopts a gas phase tubular distributor.
The invention relates to a method for a chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction, which comprises the following steps:
1. the chlorosilane high-boiling residue slurry enters a silicon tetrachloride recovery device (A) of a slag slurry treatment device to recover silicon tetrachloride in the material, and in order to ensure the fluidity of the residual slurry, the slurry is allowed to contain part of silicon tetrachloride;
2. the high-boiling-point substance slurry after the silicon tetrachloride is recovered enters a deslagging drying device (B) for removing solid impurities in the material, and the obtained liquid-phase material enters a silicon tetrachloride separation tower of a high-boiling cracking device;
3. purifying by a silicon tetrachloride separation tower (C), and recovering silicon tetrachloride from the tower top; the material in the tower kettle enters a high-boiling-point substance separation tower;
4. feeding the material extracted from the tower kettle of the silicon tetrachloride separating tower (C) into a high-boiling-point substance separating tower (D), feeding chlorosilane oligomers obtained from the tower top into a continuous cracking reactor, extracting chlorosilane high polymers from the middle lower part side of the tower, and intermittently discharging solid-containing materials from the tower kettle to return to a slag slurry system for recycling;
5. the silicon chloride oligomer and gas-phase hydrogen chloride are used as reactants and enter a continuous cracking reactor (E) filled with the catalyst for cracking reaction, and a reaction product enters a cracking reaction rectifying tower;
6. the material reacted by the continuous cracking reactor (E) enters from the middle upper part of a cracking reaction rectifying tower (F), gas-phase hydrogen chloride enters from the middle lower part of the tower (F), oligomer cracking reaction and reaction product separation processes simultaneously occur in the tower, monosilane products are extracted from the top of the tower, hydrogen chloride is recovered from tail gas, and the material obtained from the bottom of the tower returns to a high-boiling-point substance separation tower (D) to recover oligomers.
The specific application case is as follows:
example 1
The processing amount of the chlorosilane high-boiling residue slurry is 1000kg/h, wherein the content of silicon tetrachloride is 70 percent, and Si is used 2 Cl 6 The accounting is performed for the material with the typical content of chlorosilane oligomer being 12%, the content of chlorosilane polymer being 10% and the content of solid impurities being 8%. The specific process flow and material balance are shown in figure 2.
1000kg/h of chlorosilane high-boiling residue slurry enters a silicon tetrachloride recovery device (A), the recovered silicon tetrachloride amount is 350kg/h, and the residual 650kg/h of material enters a deslagging drying device (B). 80kg of solid impurities are removed by the device (B) per hour to obtain 570kg of liquid phase high-boiling residues which are sent to a silicon tetrachloride recovery tower (C) of a high-boiling cracking device. The operating pressure of the tower (C) is 0.1MPa (G), the silicon tetrachloride content recovered from the top of the tower is 340kg/h through the separation of the tower (C), and 230kg/h of high-boiling-point substance containing a small amount of silicon tetrachloride is discharged from the bottom of the tower and enters a high-boiling-point substance separation tower (D). The feeding of the tower (D) also comprises tower bottom materials of a cracking reaction rectifying tower (F), the operating pressure of the tower (D) is 0.1MPa (G), 170kg/h of materials (wherein the silicon tetrachloride is 15kg/h, the oligomer is 150kg/h, and the high polymer is 5kg/h) are extracted from the top of the tower, the side extraction amount of the middle lower part of the tower is 100kg/h of high polymer, and part of solid-containing materials are intermittently discharged from the bottom of the tower and returned to a slag slurry treatment device. The material extracted from the top of the tower (D) is sent to a continuous cracking reactor (E), and gas-phase hydrogen chloride serving as a reactant is also continuously fed into the reactor according to the flow of 24 kg/h; the structure of the continuous cracking reactor is a jacket reaction kettle type with stirring, and macroporous weak-base anion exchange resin is added into the kettle as a catalyst; the operation pressure of the reaction kettle is controlled to be 0.25MPa (G), the temperature is controlled to be 90 ℃, and the materials after the cracking reaction enter a cracking reaction rectifying tower (F). Gas-phase hydrogen chloride is continuously introduced into the middle lower part of the tower (F) according to the flow of 10kg/h, the cracking reaction of oligomers and the separation process of reaction products are simultaneously carried out in the tower (F), 146kg/h of monochlorosilane product is extracted from the liquid phase at the top of the tower and returned to a crude distillation unit, unreacted gas-phase hydrogen chloride is recovered from tail gas at the top of the tower for 24kg/h recycling, and the tower kettle is discharged according to the flow of 40kg/h (wherein, the silicon tetrachloride is 5kg/h, the oligomers are 30kg/h, and the high polymer is 5kg/h) and returned to the high-boiling-point substance separation tower (D) for material recovery.
Example 2
The processing amount of the chlorosilane high-boiling residue slurry is 2000kg/h, wherein the content of silicon tetrachloride is 65 percent, and Si is used 2 Cl 6 The accounting is performed for the material with the typical content of chlorosilane oligomer being 15%, the content of chlorosilane polymer being 10% and the content of solid impurities being 10%. The specific process flow and material balance are shown in figure 3.
The amount of silicon tetrachloride recycled after 2000kg/h of chlorosilane high-boiling residue slurry enters a silicon tetrachloride recycling device (A) is 650kg/h, and the rest 1350kg/h of chlorosilane high-boiling residue slurry enters a deslagging drying device (B). 200kg of solid impurities are removed by the device (B) per hour to obtain 1150kg of liquid phase high-boiling residues which are sent to a silicon tetrachloride recovery tower (C) of a high-boiling cracking device. The operating pressure of the tower (C) is 0.1MPa (G), the silicon tetrachloride content recovered from the top of the tower is 635kg/h through the separation of the tower (C), 515kg/h of high-boiling-point substance containing a small amount of silicon tetrachloride is discharged from the bottom of the tower, and the high-boiling-point substance enters a high-boiling-point substance separation tower (D). The feeding of the tower (D) also comprises tower bottom materials of a cracking reaction rectifying tower (F), the operating pressure of the tower (D) is 0.1MPa (G), 410kg/h of materials (25 kg/h of silicon tetrachloride, 375kg/h of oligomers and 10kg/h of high polymers) are extracted from the top of the tower, the side extraction amount of the high polymers at the middle lower part of the tower is 200kg/h, and part of solid-containing materials are intermittently discharged from the tower bottom and returned to a slag slurry treatment device. The material extracted from the top of the tower (D) is sent to a continuous cracking reactor (E), and gas-phase hydrogen chloride as a reactant is also continuously introduced into the reactor according to the flow of 60 kg/h; the structure of the continuous cracking reactor is a fixed bed reactor, macroporous weak-base anion exchange resin is filled in the reactor as a catalyst, and special catalyst interception components are adopted at two ends of the fixed bed to ensure that the catalyst does not leak; the operation pressure of the reaction kettle is controlled to be 0.25MPa (G), the temperature is controlled to be 90 ℃, and the materials after the cracking reaction enter a cracking reaction rectifying tower (F). Gas-phase hydrogen chloride is continuously introduced into the middle lower part of the tower (F) according to the flow of 20kg/h, the cracking reaction of oligomers and the separation process of reaction products are simultaneously carried out in the tower (F), 355kg/h of monochlorosilane products are extracted from the liquid phase at the top of the tower and returned to a crude distillation unit, 40kg/h of unreacted gas-phase hydrogen chloride is recovered from tail gas at the top of the tower for recycling, and the tower kettle is discharged according to the flow of 95kg/h (wherein the silicon tetrachloride is 10kg/h, the oligomers are 75kg/h, and the high polymer is 10kg/h) and returned to the high-boiling-point substance separation tower (D) for material recovery.
The chlorosilane high boiler recovery process combining slurry treatment and cracking reaction proposed by the present invention has been described by way of example, and it will be apparent to those skilled in the art that the techniques of the present invention can be implemented by modifying or appropriately modifying or combining the systems and methods described herein without departing from the spirit, scope and spirit of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (2)
1. A process for recovering chlorosilane high-boiling residues by combining slurry treatment and cracking reaction comprises a silicon tetrachloride recovery device (A), a slag removal drying device (B), a silicon tetrachloride separation tower (C), a high-boiling residue separation tower (D), a continuous cracking reactor (E) and a cracking reaction rectifying tower (F), and is characterized in that a high-boiling cracking unit is connected behind a chlorosilane slurry treatment unit in series, chlorosilane oligomers obtained by separating materials pretreated by the slurry treatment unit through the high-boiling cracking unit enter a cracking device filled with a catalyst for continuous cracking reaction, and a monosilane product is obtained by subsequent separation; feeding the chlorosilane high-boiling residue slurry into silicon tetrachloride recovery equipment (A) to recover silicon tetrachloride, and feeding the residual material into slag-removing drying equipment (B); the device (B) is used for removing solid impurities in the material, and the obtained liquid-phase material enters a silicon tetrachloride separation tower (C); recovering silicon tetrachloride from the top of the silicon tetrachloride separation tower (C), and feeding the tower kettle material into a high-boiling-point substance separation tower (D); chlorosilane oligomers obtained from the top of the high-boiling-point substance separation tower (D) enter a continuous cracking reactor (E), a lateral line is arranged at the middle lower part of the tower to discharge chlorosilane high polymers, solid-containing materials are intermittently discharged from the tower bottom and return to a deslagging and drying device (B); performing cracking reaction on the chlorosilane oligomer and hydrogen chloride in a continuous cracking reactor (E); the cracking reaction product and gas phase hydrogen chloride enter a cracking reaction rectifying tower (F), oligomer cracking reaction and reaction product separation are carried out in the tower at the same time, monosilane products are extracted from the top of the tower, hydrogen chloride is recovered from tail gas, and the tower kettle material returns to a high-boiling-point substance separation tower (D) for material recovery.
2. The process for recovering chlorosilane high-boiling residues through combination of slurry treatment and cracking reaction as claimed in claim 1, wherein the catalyst filled in the continuous cracking reactor (E) is a catalyst containing ammonium salt functional groups, and the catalyst containing ammonium salt functional groups is macroporous strongly basic anion exchange resin or macroporous weakly basic anion exchange resin.
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| CN201910357954.0A CN110078080B (en) | 2019-04-26 | 2019-04-26 | Chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction |
| PCT/CN2019/119207 WO2020215706A1 (en) | 2019-04-26 | 2019-11-18 | Chlorosilane high-boiling residue recovery process combining slurry treatment and cracking reaction |
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| CN110078080B (en) * | 2019-04-26 | 2022-09-02 | 天津科技大学 | Chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction |
| CN110950342A (en) * | 2019-11-29 | 2020-04-03 | 天华化工机械及自动化研究设计院有限公司 | Polysilicon slag slurry non-hydration treatment process |
| CN111643916B (en) * | 2020-05-22 | 2022-07-15 | 湖北晶星科技股份有限公司 | Process for preparing high-purity hexachlorodisilane |
| CN111875800B (en) * | 2020-06-30 | 2022-04-26 | 鲁西化工集团股份有限公司硅化工分公司 | Organosilicon pyrolysis residue recovery system and process and organosilicon production system |
| CN113772677B (en) * | 2021-09-30 | 2023-03-28 | 四川永祥新能源有限公司 | Cracking reaction column and cracking process for byproduct chlorosilane high-boiling-point substances in polycrystalline silicon production |
| CN114437125A (en) * | 2022-01-25 | 2022-05-06 | 杭州四马化工科技有限公司 | Continuous cracking process for silane in wire loop body |
| CN115106045B (en) * | 2022-07-26 | 2024-03-29 | 乐山协鑫新能源科技有限公司 | High-boiling treatment system for slurry |
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| CN110078080B (en) * | 2019-04-26 | 2022-09-02 | 天津科技大学 | Chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction |
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- 2019-11-18 WO PCT/CN2019/119207 patent/WO2020215706A1/en active Application Filing
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| "多晶硅副产物综合处理研究进展";王海霞 等;《化工管理》;20180321;第2018卷(第09期);第17-18页 * |
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