CN220165843U - Adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane - Google Patents

Adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane Download PDF

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CN220165843U
CN220165843U CN202321105729.6U CN202321105729U CN220165843U CN 220165843 U CN220165843 U CN 220165843U CN 202321105729 U CN202321105729 U CN 202321105729U CN 220165843 U CN220165843 U CN 220165843U
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adsorption
boron
trichlorosilane
pipeline
phosphorus element
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马国聪
宋帅兵
罗家斌
罗小良
王斌
陈静凯
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Ningxia Crystal New Energy Materials Co ltd
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Ningxia Crystal New Energy Materials Co ltd
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Abstract

The utility model discloses an adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane, which relates to the technical field of polysilicon production and comprises a feeding pipeline, an adsorption mechanism, a filtering mechanism, a buffer tank and a discharging pipeline which are sequentially arranged according to the material flow direction, wherein the adsorption mechanism is used for adsorbing boron and phosphorus elements in the trichlorosilane, the feeding pipeline and the discharging pipeline are connected to the feeding pipeline, and a control valve is arranged on the feeding pipeline between the feeding pipeline and the discharging pipeline. The utility model has reasonable design, and the adsorption mechanism for removing boron and phosphorus elements is added in the system, so that the content of boron and phosphorus in trichlorosilane can be reduced. The boron-containing and phosphorus-containing element impurities in the trichlorosilane are removed through adsorption, so that the level of stable production electron level of the polysilicon of the final product is ensured, and the difficult problem of polysilicon enterprises is well solved.

Description

Adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane
Technical Field
The utility model relates to the technical field of polysilicon production, in particular to the technical field of an adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane.
Background
In the production of polysilicon, trichlorosilane and hydrogen are subjected to reduction reaction in a reduction furnace to generate polysilicon, the trichlorosilane which does not participate in the reaction cannot completely participate in the reaction process, the unreacted trichlorosilane and hydrogen enter a tail gas recovery system together with the generated byproduct silicon tetrachloride and dichlorosilane, chlorosilane liquid and gaseous hydrogen are separated, the separated chlorosilane liquid enters a rectification purification system for separation and purification, and qualified raw material trichlorosilane is obtained, in the process, boron, phosphorus components and the like contained in the chlorosilane cannot be separated and removed, enrichment exists through repeated system circulation, and the indexes of boron and phosphorus in the trichlorosilane product are abnormal, so that the quality of the polysilicon product is directly influenced.
The siemens process is the dominant process for producing polysilicon today: and generating trichlorosilane by metallurgical grade silicon powder and hydrogen chloride in a reactor, purifying and refining the trichlorosilane, and finally obtaining high-purity polysilicon by reduction reaction of the trichlorosilane and hydrogen in a reduction furnace. Trichlorosilane is the most important circulating material in the process, and even if the trichlorosilane contains ppb-level impurities, the purity of the polysilicon product is influenced finally. The main source of impurities is the introduction of metallurgical grade silicon powder in the process, including metal chlorides, chlorides and hydrides containing boron and phosphorus, carbon-containing organic matters and the like, so that the chlorosilane inevitably contains trace impurities such as boron, phosphorus and the like, and the impurities can have great influence on the quality of the polysilicon of the final product
The current purification and refining technology of trichlorosilane mainly adopts a rectification method. The trichlorosilane is generally subjected to repeated light impurity removal and heavy impurity removal in China, and the number of the rectifying tower stages is large (6 towers or even more towers are connected in series generally). Because the boiling points of part of impurities and chlorosilane are close, the problems of high energy consumption, high equipment investment, unstable product quality and the like can be brought by the traditional rectification method.
Disclosure of Invention
The utility model aims at: the utility model provides an adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane, which aims to solve the technical problems of high impurity removal difficulty and high energy consumption of boron and phosphorus elements in the existing recycled trichlorosilane.
The utility model adopts the following technical scheme for realizing the purposes:
the utility model provides an adsorption edulcoration system of boron and phosphorus element impurity in trichlorosilane, includes feeding pipeline, adsorption equipment, filtering mechanism, buffer tank and the ejection of compact pipeline that set gradually according to the material flow direction, and adsorption equipment is arranged in adsorbing boron, the phosphorus element in the trichlorosilane, and feeding pipeline and ejection of compact pipeline all are connected on the feeding pipeline, are provided with the control valve on the feeding pipeline that is located between feeding pipeline and the ejection of compact pipeline.
Specifically, before a side line of a dry tail gas recovery tower is used for reduction, an adsorption impurity removal system for removing boron and phosphorus element impurities in trichlorosilane is adopted, an adsorption mechanism for removing boron and phosphorus elements is added in the system, the content of boron and phosphorus in the trichlorosilane can be reduced, and no adsorption mechanism impurities predict and enrich 0.35ppb and 3.5ppb of boron; the boron content after the adsorption column is 0.1ppb and the phosphorus content after the adsorption column is 1ppb. The boron-containing and phosphorus-containing element impurities in the trichlorosilane are removed through adsorption, so that the level of stable production electron level of the polysilicon of the final product is ensured, and the difficult problem of polysilicon enterprises is well solved.
Further, the adsorption mechanism comprises at least two adsorption components which are arranged in parallel.
Further, the adsorption mechanism comprises two adsorption components which are arranged in parallel, the outlet end of each adsorption component is provided with a regulating valve group for controlling the flow direction and the flow rate of fluid, and the two adsorption components are a first adsorption component and a second adsorption component respectively.
Specifically, taking two adsorption components as examples, two filters are named as a first adsorption component and a second adsorption component respectively, the liquid inlet ends of the two adsorption components are connected together, and the liquid outlet ends of the two adsorption components are also connected together. When adsorption components are a plurality of, the connection mode is the same as that of two adsorption components, and in addition, the number of the adsorption components can be selected according to the needs, and the adsorption components are not necessarily two, but also can be other numbers meeting the design requirements, and in the scheme, the two adsorption components are the optimal number.
Further, each adsorption component is an adsorption column, the adsorption column comprises a shell and a tube array structure arranged in the shell, the tube array structure is filled with adsorption resin, and the adsorption resin is macroporous weak alkaline anion adsorption resin.
Specifically, the shell is filled with adsorption resin, a material inlet and a material outlet which are communicated with two ends of the inner shell structure are arranged on the shell, and the shell side is filled with heat conduction oil to regulate and control the adsorption temperature, wherein the adsorption temperature is in the range of 40-110 ℃ by taking the lower inlet and the upper outlet of materials as examples. The macroporous weak-alkaline anion-absorbent resin is modified by polyhydroxy acid amine and takes polystyrene as a framework.
In addition, the adsorption resin is used as an adsorbent, and boron and phosphorus element impurities in the trichlorosilane are removed through adsorption, so that the level of stable production electron level of the final product polysilicon is ensured, and the difficult problem of a polysilicon enterprise is well solved.
Further, the total volume exchange capacity of the adsorption column is more than 1.5eq/l, the particle size distribution of the adsorption resin is 500-1400 mu m, and the bulk density of the adsorption resin is 550-850 kg/m3.
Further, the filtering mechanism is at least two filters arranged in parallel.
Specifically, taking two filters as examples, the two filters are named as a first precise filter and a second precise filter respectively, the liquid inlet ends of the two filters are connected together, and the liquid outlet ends of the two filters are also connected together. When the number of filters is plural, the connection mode is the same as that of two filters, and the number of filters can be selected as required.
Further, a control valve is arranged on the discharging pipeline, and a regulating valve group for controlling the flow direction and the flow rate of the fluid is also arranged on the discharging pipeline.
Further, the buffer tank comprises a buffer tank body, a feed inlet, a discharge outlet and a return inlet, wherein the feed inlet, the discharge outlet and the return inlet are communicated with the inside of the buffer tank body, the feed inlet is communicated with the filtering mechanism through a pipeline, a return pipe communicated with the discharge pipeline is connected to the return inlet, and a liquid outlet connecting pipe communicated with the discharge pipeline is connected to the discharge outlet.
Further, at least two liquid return control valves are arranged on the material return pipe.
Further, a pressure gauge, a shielding pump and at least two liquid outlet control valves are arranged on the liquid outlet connecting pipe, and the shielding pump is positioned between the two liquid outlet control valves.
The beneficial effects of the utility model are as follows:
1. the utility model has reasonable design, and the adsorption mechanism for removing boron and phosphorus elements is added in the system, so that the content of boron and phosphorus in trichlorosilane can be reduced, and the impurity prediction enrichment of no adsorption mechanism is carried out, wherein the content of boron is 0.35ppb and the content of phosphorus is 3.5ppb; the boron content after the adsorption column is 0.1ppb and the phosphorus content after the adsorption column is 1ppb. The method for removing boron and phosphorus element impurities in the trichlorosilane through adsorption ensures that the final product polysilicon stably produces the level of electron level, well solves the difficult problem of polysilicon enterprises, realizes the process method for removing the boron and phosphorus element impurities in the trichlorosilane through the adsorption process by recycling the trichlorosilane through a dry method, greatly reduces the content of the boron and phosphorus element impurities in the trichlorosilane, improves the quality of the trichlorosilane, breaks through technological monopoly, and lays a foundation for realizing stable production of electron level polysilicon in the future. The process flow is simple, the operation is simple and convenient, the energy consumption is low, and the impurity removal effect is obvious.
2. The utility model has reasonable design, and the dry recovery unit is provided with no boron and phosphorus adsorption device, and the dry recovery material is directly used for reduction after being separated by the reduction system, and the recovery material separating tower has no purification function because of only separation function, so as to avoid the fluctuation of material quality and influence on the quality of polysilicon products, therefore, the quality of the extracted trichlorosilane is ensured to be within the required range of technological indexes by adding the boron and phosphorus adsorption device in the dry recovery unit.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
reference numerals: 1-first adsorption component, 2-second adsorption component, 3-first precision filter of precision filter, 4-second precision filter, 5-buffer tank, 6-canned motor pump.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present utility model more apparent, the technical solutions of the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model, and it is apparent that the described embodiments are some embodiments of the present utility model, but not all embodiments of the present utility model. The components of the embodiments of the present utility model generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the utility model, as presented in the figures, is not intended to limit the scope of the utility model, as claimed, but is merely representative of selected embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures. Furthermore, the terms "first," "second," and the like, are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
In describing embodiments of the present utility model, it should be noted that the directions or positional relationships indicated by the terms "inner", "outer", "upper", etc. are directions or positional relationships based on those shown in the drawings, or those that are conventionally put in place when the inventive product is used, are merely for convenience of description and simplification of description, and are not indicative or implying that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the present utility model.
Example 1
As shown in fig. 1, this embodiment provides an adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane, which comprises a feeding pipeline, an adsorption mechanism, a filtering mechanism, a buffer tank 5 and a discharging pipeline which are sequentially arranged according to the material flow direction, wherein the adsorption mechanism is used for adsorbing boron and phosphorus elements in trichlorosilane, the feeding pipeline and the discharging pipeline are both connected on the feeding pipeline, and a control valve is arranged on the feeding pipeline between the feeding pipeline and the discharging pipeline.
Specifically, before a side line of a dry tail gas recovery tower is used for reduction, an adsorption impurity removal system for removing boron and phosphorus element impurities in trichlorosilane is adopted, an adsorption mechanism for removing boron and phosphorus elements is added in the system, the content of boron and phosphorus in the trichlorosilane can be reduced, and no adsorption mechanism impurities predict and enrich 0.35ppb and 3.5ppb of boron; the boron content after the adsorption column is 0.1ppb and the phosphorus content after the adsorption column is 1ppb. The boron-containing and phosphorus-containing element impurities in the trichlorosilane are removed through adsorption, so that the level of stable production electron level of the polysilicon of the final product is ensured, and the difficult problem of polysilicon enterprises is well solved.
The adsorption mechanism comprises at least two adsorption components which are arranged in parallel.
Example 2
The embodiment is further optimized based on the embodiment 1, specifically:
the adsorption mechanism comprises two adsorption components which are arranged in parallel, the outlet end of each adsorption component is provided with a regulating valve group for controlling the flow direction and the flow rate of fluid, and the two adsorption components are a first adsorption component 1 and a second adsorption component 2 respectively.
Specifically, taking two adsorption assemblies as examples, two filters are named as a first adsorption assembly 1 and a second adsorption assembly 2 respectively, the liquid inlet ends of the two adsorption assemblies are connected together, and the liquid outlet ends of the two adsorption assemblies are also connected together. When adsorption components are a plurality of, the connection mode is the same as that of two adsorption components, and in addition, the number of the adsorption components can be selected according to the needs, and the adsorption components are not necessarily two, but also can be other numbers meeting the design requirements, and in the scheme, the two adsorption components are the optimal number.
Example 3
This example was further optimized based on example 1 or 2, specifically:
each adsorption component is an adsorption column, the adsorption column comprises a shell and a tube array structure arranged in the shell, the tube array structure is filled with adsorption resin, and the adsorption resin is macroporous weak alkaline anion adsorption resin.
The total volume exchange capacity of the adsorption column is more than 1.5eq/l, the granularity distribution of the adsorption resin is 500-1400 mu m, and the bulk density of the adsorption resin is 550-850 kg/m3.
Specifically, the shell is filled with adsorption resin, a material inlet and a material outlet which are communicated with two ends of the inner shell structure are arranged on the shell, and the shell side is filled with heat conduction oil to regulate and control the adsorption temperature, wherein the adsorption temperature is in the range of 40-110 ℃ by taking the lower inlet and the upper outlet of materials as examples. The macroporous weak-alkaline anion-absorbent resin is modified by polyhydroxy acid amine and takes polystyrene as a framework.
In addition, the adsorption resin is used as an adsorbent, and boron and phosphorus element impurities in the trichlorosilane are removed through adsorption, so that the level of stable production electron level of the final product polysilicon is ensured, and the difficult problem of a polysilicon enterprise is well solved.
In the technical process, liquid-phase trichlorosilane purified by rectification firstly enters a first adsorption column, the adsorption column is a vertical fixed adsorption column, materials enter downwards and go upwards, a heating medium of a shell side of the adsorption column is 900kPa saturated steam, and the temperature is 179.03 ℃. The liquid phase trichlorosilane (used in the activation process) enters the first adsorption column and the second adsorption column. And (3) adsorbing boron and phosphorus element impurities, filling adsorption resin in an adsorption column, feeding materials downwards, feeding materials upwards, and recycling the dry tail gas after adsorption treatment to reduce the boron and phosphorus element impurities in the trichlorosilane from 10ppba to below 0.05ppba, so that the requirement of stable production of electronic grade polysilicon of a polysilicon enterprise is met.
B, P impurities in trichlorosilane are reduced to meet the requirements of producing solar grade or electronic grade polysilicon, and specific reference technical indexes are as follows:
example 4
This example is further optimized on the basis of any one of examples 1 to 3, in particular:
the filtering mechanism is at least two filters which are arranged in parallel.
Specifically, taking two filters as examples, the two filters are named as a first precise filter and a second precise filter 4 respectively, the liquid inlet ends of the two filters are connected together, and the liquid outlet ends of the two filters are also connected together. When the number of filters is plural, the connection mode is the same as that of two filters, and the number of filters can be selected as required.
The discharge pipeline is provided with a control valve, and the discharge pipeline is also provided with a regulating valve group for controlling the flow direction and the flow rate of the fluid.
Example 5
This example is further optimized on the basis of any one of examples 1 to 4, in particular:
the buffer tank 5 comprises a buffer tank body, a feed inlet, a discharge outlet and a feed back opening, wherein the feed inlet, the discharge outlet and the feed back opening are all communicated with the inside of the buffer tank body, the feed inlet is communicated with the filtering mechanism through a pipeline, a feed back pipe communicated with a discharge pipeline is connected to the feed back opening, and a liquid outlet connecting pipe communicated with the discharge pipeline is connected to the discharge outlet.
At least two liquid return control valves are arranged on the liquid return pipe.
The liquid outlet connecting pipe is provided with a pressure gauge, a shielding pump 6 and at least two liquid outlet control valves, and the shielding pump 6 is positioned between the two liquid outlet control valves.

Claims (10)

1. The utility model provides an adsorption edulcoration system of boron and phosphorus element impurity in trichlorosilane, its characterized in that includes feeding pipeline, adsorption equipment, filtering mechanism, buffer tank (5) and the ejection of compact pipeline that set gradually according to the material flow direction, and adsorption equipment is used for adsorbing boron, the phosphorus element in trichlorosilane, feeding pipeline with ejection of compact pipeline all connects on the feed pipeline, is located feeding pipeline with be provided with the control valve on the feed pipeline between the ejection of compact pipeline.
2. The adsorption and impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 1, wherein the adsorption mechanism comprises at least two adsorption assemblies arranged in parallel.
3. The adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 2, wherein the adsorption mechanism comprises two adsorption assemblies which are arranged in parallel, an outlet end of each adsorption assembly is provided with a regulating valve group for controlling the flow direction and the flow rate of fluid, and the two adsorption assemblies are a first adsorption assembly (1) and a second adsorption assembly (2) respectively.
4. The adsorption and impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 2 or 3, wherein each adsorption component is an adsorption column, the adsorption column comprises a shell and a tubular structure arranged in the shell, the tubular structure is filled with adsorption resin, and the adsorption resin is modified macroporous weak-alkaline anion adsorption resin.
5. The adsorption and impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 4, wherein the total volume exchange capacity of the adsorption column is more than 1.5eq/l, the particle size distribution of the adsorption resin is 500-1400 μm, and the bulk density of the adsorption resin is 550-850 kg/m3.
6. The adsorption and impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 1, wherein the filtering mechanism is at least two filters arranged in parallel.
7. The adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 1, wherein the discharge pipeline is provided with a control valve, and the discharge pipeline is further provided with a regulating valve group for controlling the flow direction and the flow rate of fluid.
8. The adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 1, wherein the buffer tank (5) comprises a buffer tank body, a feed inlet, a discharge outlet and a return inlet, the feed inlet, the discharge outlet and the return inlet are all communicated with the interior of the buffer tank body, the feed inlet is communicated with the filtering mechanism through a pipeline, the return inlet is connected with a feed back pipe communicated with the discharge pipeline, and the discharge outlet is connected with a liquid outlet connecting pipe communicated with the discharge pipeline.
9. The adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 8, wherein at least two liquid return control valves are arranged on the feed back pipe.
10. The adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane according to claim 8, wherein a pressure gauge, a shielding pump (6) and at least two liquid outlet control valves are arranged on the liquid outlet connecting pipe, and the shielding pump (6) is positioned between the two liquid outlet control valves.
CN202321105729.6U 2023-05-09 2023-05-09 Adsorption impurity removal system for boron and phosphorus element impurities in trichlorosilane Active CN220165843U (en)

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