Adsorbent for removing phosphorus impurities in trichlorosilane as well as preparation method and application of adsorbent

By depositing and heating metal salts on the inorganic porous material support, an oxidized metal is formed to adsorb phosphorus impurities in trichlorosilicon, the problem of high cost and low efficiency of removing phosphorus impurities in the prior art is solved, and an efficient and low-cost phosphorus impurities removal effect is achieved.

CN119500053APending Publication Date: 2025-02-25GCL NEW (SHANGHAI) PHOTOVOLTAIC TECH CO LTD
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Patent Information

Application Number
CN202411841304.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-13
Publication Date
2025-02-25

AI Technical Summary

Technical Problem

The prior art is difficult to remove phosphorus impurities in trichlorosilicon at low cost and efficiently, resulting in large energy consumption and production quality in the production process of polycrystalline silicon.

Method used

The metal salt solution is deposited on the support using an inorganic porous material, and the metal salt is oxidized into an oxidized metal by heating, which is used to adsorb phosphorus impurities in trichlorosilicon.

Benefits of technology

The ability and rate of phosphorus removal impurities are improved, the cost is reduced, and due to the stability of the inorganic porous materials, the adsorbent has good cycling renewability, avoiding combustion risks.

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Abstract

The invention provides an adsorbent for removing phosphorus impurities in trichlorosilane as well as a preparation method and application of the adsorbent. The preparation method comprises the following steps: performing ultrasonic cleaning and drying treatment on an inorganic porous material; preparing metal salt into a metal salt solution, mixing the inorganic porous material with the metal salt solution, depositing under vacuum, drying, and carrying out heat treatment on the dried inorganic porous material deposited with the metal salt to obtain the phosphorus impurity removal adsorbent. According to the preparation method provided by the invention, the inorganic porous material is adopted as the carrier, the metal salt is deposited on the carrier and is heated to be converted into the oxidation-state metal, and the carrier with high specific surface area and the oxidation-state metal are utilized, so that phosphorus impurities can be rapidly enriched, and the adsorption effect on the phosphorus impurities is improved; and the oxidation-state metal and the phosphorus impurities are subjected to an oxidation-reduction reaction, so that the phosphorus impurities are removed. The used adsorbent can be regenerated through heating treatment, so that the adsorbent can be reused, and the dephosphorization cost is reduced.
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Description

Technical Field

[0001] The present application relates to the technical field of polysilicon production, and in particular to an adsorbent for removing phosphorus impurities in trichlorosilane, and a preparation method and application thereof. Background Art

[0002] As a raw material for producing semiconductors and photovoltaic materials, polysilicon requires strict control over its impurity content. The purity of polysilicon products mainly depends on the purity of trichlorosilane. Domestic and foreign countries mainly use multi-stage distillation separation methods to remove impurities in trichlorosilane. Compounds such as iron, copper, and manganese can be removed relatively easily through distillation. However, the volatility of phosphorus compound impurities in trichlorosilane is close to that of trichlorosilane. The distillation method requires increasing the reflux ratio and reducing the extraction volume during multi-stage distillation to ensure product quality indicators. This process not only consumes a lot of energy, but also affects production and quality. At present, how to remove phosphorus compound impurities in trichlorosilane at low cost and high efficiency has become a major problem in the domestic polysilicon industry for many years. Summary of the invention

[0003] The purpose of the present application is to provide an adsorbent for removing phosphorus impurities in trichlorosilane, and a preparation method and application thereof. In the preparation method, an inorganic porous material is used as a carrier, the carrier is mixed with a metal salt solution, the metal salt solution is deposited on the carrier, and after heating, it is used to adsorb phosphorus impurities in trichlorosilane, thereby solving the problem of high cost of removing phosphorus impurities in trichlorosilane in the prior art.

[0004] In order to achieve one of the above-mentioned purposes of the invention, an embodiment of the present application provides a method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane, comprising the following steps:

[0005] Pretreatment: ultrasonically clean the inorganic porous material, and dry the cleaned inorganic porous material;

[0006] Deposition: dissolving the metal salt in water to prepare a metal salt solution, and mixing the inorganic porous material and the metal salt solution, and depositing them under vacuum;

[0007] Drying: placing the inorganic porous material deposited in the metal salt solution into a drying oven for drying;

[0008] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent.

[0009] As a further improvement of one embodiment of the present application, the metal salt is selected from one or more of CuCl2, CuCl, ZnCl2, FeCl2, and CoCl2.

[0010] As a further improvement of an embodiment of the present application, the concentration of the metal salt solution is 0.1 to 2 mol / L.

[0011] As a further improvement of one embodiment of the present application, the inorganic porous material is selected from one or more of ZrO2, SiO2, α-Al2O3, β-Al2O3, γ-Al2O3, CeO2, TiO2, and 13X molecular sieve.

[0012] As a further improvement of one embodiment of the present application, the inorganic porous material has a bulk density of 0.3 to 1.2 g / ml, a diameter distribution of 2 to 6 mm, and a specific surface area of ​​200 to 300 m 2 / g.

[0013] As a further improvement of an embodiment of the present application, in the heat treatment step, the heating temperature of the heat treatment is 300-750°C, the heating time is 2-6h, and the heating rate is 2-10°C / min.

[0014] As a further improvement of an embodiment of the present application, in the deposition step, the inorganic porous material and the metal salt solution are deposited for 30 to 120 minutes under vacuum to -0.2 to 0 MPa.

[0015] One embodiment of the present application also provides an adsorbent for removing phosphorus impurities in trichlorosilane, using an inorganic porous material as a carrier, and the carrier is loaded with an oxidized metal, wherein the inorganic porous material is selected from one or more of ZrO2, SiO2, α-Al2O3, β-Al2O3, γ-Al2O3, CeO2, TiO2, and 13X molecular sieve.

[0016] As a further improvement of one embodiment of the present application, the oxidized metal is formed by heating and oxidizing one or more metal salts of CuCl2, CuCl, ZnCl2, FeCl2, and CoCl2.

[0017] One embodiment of the present application also provides a use of the above-mentioned adsorbent for removing phosphorus impurities in trichlorosilane, wherein the adsorbent for removing phosphorus impurities is used to adsorb phosphorus impurities in trichlorosilane.

[0018] One or more technical solutions provided by this application have at least the following technical effects or advantages:

[0019] In the preparation method of the adsorbent for removing phosphorus impurities in trichlorosilane provided in the present application, an inorganic porous material is used as a carrier, the carrier is added to a metal salt solution, the metal salt solution is deposited on the carrier, and the metal salt is converted into an oxidized metal by heating. The large specific surface area of ​​the inorganic porous material can adsorb impurities, and the oxidized metal can complex with the phosphorus impurities in trichlorosilane, so that the phosphorus impurities are enriched on the carrier, thereby improving the ability to remove phosphorus impurities. DETAILED DESCRIPTION

[0020] The present invention will be described in detail below in conjunction with specific embodiments, but these embodiments do not limit the present invention, and changes in reaction conditions, reactants or raw material amounts made by ordinary technicians in the field according to these embodiments are all included in the protection scope of the present invention.

[0021] The present application provides a method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane, comprising the following steps:

[0022] Pretreatment: ultrasonically clean the inorganic porous material, and dry the cleaned inorganic porous material;

[0023] Deposition: dissolving the metal salt in water to prepare a metal salt solution, and mixing the inorganic porous material and the metal salt solution, and depositing them under vacuum;

[0024] Drying: placing the inorganic porous material deposited in the metal salt solution into a drying oven for drying;

[0025] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent.

[0026] In the present application, an inorganic porous material is used as a carrier, and the inorganic porous material as a carrier is mixed with a metal salt solution, and after being deposited under vacuum, it is dried to remove moisture, so that the metal salt in the metal salt solution is attached to the inorganic porous material. The inorganic porous material has a strong adsorption due to its own large specific surface area. After the metal salt deposited on the inorganic porous material is heated for heat treatment, the metal salt is oxidized into an oxidized metal, trichlorosilane has a very weak polarity, and the phosphorus impurities in trichlorosilane have a very strong polarity, tending to form an addition chemical bond, and the oxidized metal loaded on the inorganic porous material is very easy to react with the phosphorus impurities in trichlorosilane through redox reaction to form a complex, so that the phosphorus impurities are removed from trichlorosilane. Therefore, the metal salt is attached to the surface of the inorganic porous material with a large specific surface area, and then the metal salt is oxidized into an oxidized metal for complexing with the phosphorus impurities, which greatly improves the adsorption efficiency and rate of the phosphorus impurities in trichlorosilane.

[0027] In addition, the inorganic porous material in the present application is an inorganic substance and will not burn when heated. The dephosphorus impurity adsorbent provided in the present application has no combustion risk. Based on the structural stability of the inorganic porous material, the dephosphorus impurity adsorbent prepared by the preparation method provided in the present application can be desorbed by heating to decompose the complex produced by the oxidized metal and phosphorus impurities, and the porous structure of the inorganic porous material will not collapse, which makes the dephosphorus impurity adsorbent extremely recyclable and greatly reduces the cost of dephosphorus impurities with trichlorosilane.

[0028] In the preparation method provided in the present application, in order to avoid the introduction of new impurities during impurity removal, the inorganic porous material is firstly ultrasonically cleaned before adding a metal salt solution to the inorganic porous material for deposition to remove dust and oil stains on the surface of the inorganic porous material.

[0029] Among them, an ultrasonic cleaner is used for ultrasonic cleaning, the cleaning time is 20 to 80 minutes, and the frequency of the ultrasonic cleaner is 10kHz to 90kHz to ensure that the inorganic porous material is cleaned. The cleaning agent is any one of ultrapure water, deionized water, and anhydrous ethanol. The aforementioned solvents are easy to volatilize and not easy to remain, which can avoid the introduction of new impurities caused by incomplete drying. Of course, in addition to ultrapure water, deionized water and anhydrous ethanol, other easy-to-dry solvents can also be used.

[0030] After cleaning, the inorganic porous material is placed in a drying oven and dried at a temperature of 80 to 120° C. for 12 to 24 hours. Since there are many pores in the inorganic porous material, it is necessary to ensure that the cleaning agent in the inorganic porous material is completely dried to obtain a clean inorganic porous material after drying.

[0031] In some embodiments, the metal salt is selected from one or more of CuCl2, CuCl, ZnCl2, FeCl2, and CoCl2.

[0032] In some embodiments, the concentration of the metal salt solution is 0.1-2 mol / L. For CuCl which is poorly soluble in water, ultrasonic dispersion or other methods can be used to dissolve it in water to increase its concentration.

[0033] In some embodiments, the inorganic porous material is selected from one or more of ZrO2, SiO2, α-Al2O3, β-Al2O3, γ-Al2O3, CeO2, TiO2, and 13X molecular sieve. The various inorganic compounds listed above are not flammable and have high melting points, and there is no risk of combustion when exposed to fire. When the dephosphorus impurity adsorbent fails to adsorb, heating it can decompose the complex formed by the oxidized metal and phosphorus impurities on the aforementioned inorganic porous material, so that the dephosphorus impurity adsorbent can be reused. Since the porous material formed by the inorganic substance has a stable structure, its porous structure will not collapse even if it is heated.

[0034] In some embodiments, the inorganic porous material has a bulk density of 0.3 to 1.2 g / ml, a diameter distribution of 2 to 6 mm, and a specific surface area of ​​200 to 300 m 2 / g. The aforementioned diameter distribution of the inorganic porous material enables the smaller-sized inorganic porous material to be filled in the pores of the larger inorganic porous material, so that the inorganic porous materials are filled more fully. The larger the specific surface area of ​​the inorganic porous material, the more adsorption sites it has, that is, the stronger the adsorption capacity.

[0035] In some embodiments, in the heat treatment step, the heating temperature of the heat treatment is 300-750° C., the heating time is 2-6 hours, and the heating rate is 2-10° C. / min. Heating to 300-750° C. is sufficient to oxidize the metal salt to an oxidized state, thereby avoiding increasing the manufacturing cost of the adsorbent. Controlling the heating rate to 2-10° C. / min can prevent the oxidized metal supported on the inorganic porous material from sintering into agglomerates.

[0036] In some embodiments, in the deposition step, the inorganic porous material and the metal salt solution are placed in a vacuum container, evacuated to -0.2 to 0 MPa, and the deposition time is 30 to 120 minutes. Since there are many pores in the inorganic porous material, even if the inorganic porous material is completely immersed in the metal salt solution, it cannot guarantee that the metal salt can well enter the numerous pores of the inorganic porous material and adhere to the surface. Vacuuming can promote the adhesion rate and adhesion speed of the metal salt on the inorganic porous material.

[0037] After the deposition is completed, the inorganic porous material is placed in a drying oven for drying to remove the water in the metal salt solution so that only the metal salt is attached to the surface of the inorganic porous material, wherein the drying temperature is 80 to 120° C. and the drying time is 24 to 48 hours. The drying time is relatively longer than that in the pretreatment step, which can avoid the possibility of residual cleaning agents in the pores of the inorganic porous material due to incomplete drying in the pretreatment step, such as ultrapure water, deionized water, anhydrous ethanol, etc., and the drying time is increased to ensure that the water or cleaning agent in the pores of the inorganic porous material is completely dried.

[0038] An embodiment of the present application also provides an adsorbent for removing phosphorus impurities in trichlorosilane, with an inorganic porous material as a carrier, and an oxidized metal loaded on the carrier, wherein the inorganic porous material is selected from one or more of ZrO2, SiO2, α-Al2O3, β-Al2O3, γ-Al2O3, CeO2, TiO2, and 13X molecular sieve.

[0039] The above-mentioned inorganic porous material has a large specific surface area, high structural stability, high melting point and non-flammability. The oxidized metal can undergo a complex reaction with the phosphorus impurities in trichlorosilane, so that the adsorbent has further improved adsorption properties in addition to the strong adsorption properties brought by the large specific surface area of ​​the inorganic porous material, and has excellent adsorption effect and efficiency. The decomposition of the complex can be achieved by heating, and heating will not cause the porous structure of the carrier to collapse, so that the adsorbent has good cyclic regenerative properties, and there is no risk of combustion.

[0040] In some embodiments, the oxidized metal is formed by heating and oxidizing one or more metal salts of CuCl2, CuCl, ZnCl2, FeCl2, and CoCl2.

[0041] The present application also provides an application of an adsorbent for removing phosphorus impurities in trichlorosilane as described above, and the adsorbent for removing phosphorus impurities is used to adsorb phosphorus impurities in trichlorosilane. Based on the characteristics of the adsorbent for removing phosphorus impurities in the above-mentioned adsorbent, the adsorbent for removing phosphorus impurities in trichlorosilane provided in the embodiment of the present application has a high adsorption rate and adsorption speed when adsorbing phosphorus impurities in trichlorosilane, and is regenerable and non-combustible.

[0042] The technical solution of the present application is further described below in conjunction with some specific embodiments.

[0043] Example 1

[0044] Pretreatment: Add the inorganic porous material γ-Al2O3 into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning. The working frequency of the ultrasonic cleaner is 30kHz. After cleaning for 30 minutes, put the γ-Al2O3 into a blast drying oven and dry it at 100°C for 12 hours. Among them, the bulk density of the inorganic porous material γ-Al2O3 is 0.7g / ml, the diameter is distributed in the range of 2 to 5mm, and the specific surface area is 260m 2 / g.

[0045] Deposition: Weigh 13.4 g of CuCl2 to prepare a 1 mol / L CuCl2 solution, mix the cleaned γ-Al2O3 with the CuCl2 solution and put them into a vacuum container, evacuate the container to -0.1 MPa, and deposit for 60 minutes.

[0046] Drying: After deposition, the γ-Al2O3 deposited with CuCl2 was placed in a drying oven and dried at 100°C for 24 h.

[0047] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent, wherein the heating temperature of the heat treatment is 450°C, the heating time is 4h, and the heating rate is 5°C / min.

[0048] The above synthesized adsorbent was used to adsorb and remove phosphorus impurities in trichlorosilane. The experimental method is as follows:

[0049] Before adsorption, the adsorbent was dried at 150 °C for 4 h.

[0050] Weigh 5g of the prepared adsorbent and add it to 100ml of trichlorosilane solution. Seal the solution containing the adsorbent in a 100mL square-mouthed bottle with a lid, and then oscillate at a constant temperature for 2 hours. After adsorption equilibrium, take the mixed solution for ICP test. The results show that the adsorbent has a removal rate of 98% for phosphorus impurities and a removal rate of 35% for boron impurities.

[0051] Example 2

[0052] Pretreatment: Add the inorganic porous material γ-Al2O3 into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning. The working frequency of the ultrasonic cleaner is 30kHz. After cleaning for 30 minutes, put the γ-Al2O3 into a blast drying oven and dry it at 100°C for 12 hours. Among them, the bulk density of the inorganic porous material γ-Al2O3 is 0.7g / ml, the diameter is distributed in the range of 2 to 5mm, and the specific surface area is 260m 2 / g.

[0053] Deposition: Weigh 13.6 g of ZnCl2 to prepare a 1 mol / L ZnCl2 solution. Mix the cleaned γ-Al2O3 and the ZnCl2 solution and put them into a vacuum container. Evacuate the container to -0.1 MPa and deposit for 60 minutes.

[0054] Drying: After the deposition is completed, the γ-Al2O3 deposited with ZnCl2 is placed in a drying oven and dried at 100°C for 24 hours.

[0055] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent, wherein the heating temperature of the heat treatment is 450°C, the heating time is 4h, and the heating rate is 5°C / min.

[0056] The above synthesized adsorbent was used to adsorb and remove phosphorus impurities in trichlorosilane. The experimental method is as follows:

[0057] Before adsorption, the adsorbent was dried at 150 °C for 4 h.

[0058] Weigh 5g of the prepared adsorbent and add it to 100ml of trichlorosilane solution. Seal the solution containing the adsorbent in a 100mL square-mouthed bottle with a lid, and then oscillate at a constant temperature for 2 hours. After adsorption equilibrium, take the mixed solution for ICP test. The results show that the adsorbent has a removal rate of 55% for phosphorus impurities and a removal rate of 32% for boron impurities.

[0059] Example 3

[0060] Pretreatment: Add the inorganic porous material γ-Al2O3 into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning. The working frequency of the ultrasonic cleaner is 30kHz. After cleaning for 30 minutes, put the γ-Al2O3 into a blast drying oven and dry it at 100°C for 12 hours. Among them, the bulk density of the inorganic porous material γ-Al2O3 is 0.7g / ml, the diameter is distributed in the range of 2 to 5mm, and the specific surface area is 260m 2 / g.

[0061] Deposition: Weigh 13.0 g of CoCl2 to prepare a 1 mol / L CoCl2 solution, mix the cleaned γ-Al2O3 with the CoCl2 solution and put them into a vacuum container, evacuate the container to -0.1 MPa, and deposit for 60 minutes.

[0062] Drying: After deposition, the γ-Al2O3 deposited with CoCl2 was placed in a drying oven and dried at 100°C for 24 h.

[0063] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent, wherein the heating temperature of the heat treatment is 450°C, the heating time is 4h, and the heating rate is 5°C / min.

[0064] The above synthesized adsorbent was used to adsorb and remove phosphorus impurities in trichlorosilane. The experimental method is as follows:

[0065] Before adsorption, the adsorbent was dried at 150 °C for 4 h.

[0066] Weigh 5g of the prepared adsorbent and add it to 100ml of trichlorosilane solution. Seal the solution containing the adsorbent in a 100mL square-mouthed bottle with a lid, and then oscillate at a constant temperature for 2 hours. After adsorption equilibrium, take the mixed solution for ICP test. The results show that the adsorbent has a removal rate of 68% for phosphorus impurities and a removal rate of 37% for boron impurities.

[0067] Example 4

[0068] Pretreatment: Add the inorganic porous material γ-Al2O3 into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning. The working frequency of the ultrasonic cleaner is 30kHz. After cleaning for 30 minutes, put the γ-Al2O3 into a blast drying oven and dry it at 100°C for 12 hours. Among them, the bulk density of the inorganic porous material γ-Al2O3 is 0.7g / ml, the diameter is distributed in the range of 2 to 5mm, and the specific surface area is 260m 2 / g.

[0069] Deposition: Weigh 6.7 g of CuCl2 to prepare a 0.5 mol / L CuCl2 solution. Mix the cleaned γ-Al2O3 and the CuCl2 solution and put them into a vacuum container. Evacuate the container to -0.1 MPa and deposit for 60 minutes.

[0070] Drying: After deposition, the γ-Al2O3 deposited with CuCl2 was placed in a drying oven and dried at 100°C for 24 h.

[0071] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent, wherein the heating temperature of the heat treatment is 450°C, the heating time is 4h, and the heating rate is 5°C / min.

[0072] The above synthesized adsorbent was used to adsorb and remove phosphorus impurities in trichlorosilane. The experimental method is as follows:

[0073] Before adsorption, the adsorbent was dried at 150 °C for 4 h.

[0074] Weigh 5g of the prepared adsorbent and add it to 100ml of trichlorosilane solution. Seal the solution containing the adsorbent in a 100mL square-mouthed bottle with a lid, and then oscillate at a constant temperature for 2 hours. After adsorption equilibrium, take the mixed solution for ICP test. The results show that the adsorbent has a removal rate of 81% for phosphorus impurities and a removal rate of 36% for boron impurities.

[0075] Example 5

[0076] Pretreatment: Add the inorganic porous material γ-Al2O3 into an ultrasonic cleaner filled with deionized water for ultrasonic cleaning. The working frequency of the ultrasonic cleaner is 30kHz. After cleaning for 30 minutes, put the γ-Al2O3 into a blast drying oven and dry it at 100°C for 12 hours. Among them, the bulk density of the inorganic porous material γ-Al2O3 is 0.7g / ml, the diameter is distributed in the range of 2 to 5mm, and the specific surface area is 260m 2 / g.

[0077] Deposition: Weigh 26.8 g of CuCl2 to prepare a 2 mol / L CuCl2 solution, mix the cleaned γ-Al2O3 with the CuCl2 solution and put them into a vacuum container, evacuate the container to -0.1 MPa, and deposit for 60 minutes.

[0078] Drying: After deposition, the γ-Al2O3 deposited with CuCl2 was placed in a drying oven and dried at 100°C for 24 h.

[0079] Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heated for heat treatment to obtain a phosphorus removal impurity adsorbent, wherein the heating temperature of the heat treatment is 450°C, the heating time is 4h, and the heating rate is 5°C / min.

[0080] The above synthesized adsorbent was used to adsorb and remove phosphorus impurities in trichlorosilane. The experimental method is as follows:

[0081] Before adsorption, the adsorbent was dried at 150 °C for 4 h.

[0082] Weigh 5g of the prepared adsorbent and add it to 100ml of trichlorosilane solution. Seal the solution containing the adsorbent in a 100mL square-mouthed bottle with a lid, and then oscillate at a constant temperature for 2 hours. After adsorption equilibrium, take the mixed solution for ICP test. The results show that the adsorbent has a removal rate of 91% for phosphorus impurities and a removal rate of 36% for boron impurities.

[0083] It should be understood that although this specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each implementation mode may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

[0084] The series of detailed descriptions listed above are only specific descriptions of feasible implementation methods of the present application. They are not intended to limit the scope of protection of the present application. Any equivalent implementation methods or changes that do not deviate from the technical spirit of the present application should be included in the scope of protection of the present application.

Claims

1. A method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane, characterized in that: The steps include: Pretreatment: ultrasonically clean the inorganic porous material, and dry the cleaned inorganic porous material; Deposition: dissolving the metal salt in water to prepare a metal salt solution, and mixing the inorganic porous material and the metal salt solution, and depositing them under vacuum; Drying: placing the inorganic porous material deposited in the metal salt solution into a drying oven for drying; Heat treatment: The inorganic porous material on which the metal salt is deposited after drying is heat treated to obtain a phosphorus removal impurity adsorbent.

2. The method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane according to claim 1, characterized in that: The metal salt is selected from one or more of CuCl2, CuCl, ZnCl2, FeCl2, and CoCl2.

3. The method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane according to claim 2, characterized in that: The concentration of the metal salt solution is 0.1-2 mol / L.

4. The method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane according to claim 1, characterized in that: The inorganic porous material is selected from one or more of ZrO2, SiO2, α-Al2O3, β-Al2O3, γ-Al2O3, CeO2, TiO2, and 13X molecular sieve.

5. The method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane according to claim 4, characterized in that: The bulk density of inorganic porous materials is 0.3-1.2 g / ml, the diameter is distributed in the range of 2-6 mm, and the specific surface area is 200-300 m 2 / g.

6. The method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane according to claim 1, characterized in that: In the heat treatment step, the heating temperature of the heat treatment is 300-750°C, the heating time is 2-6h, and the heating rate is 2-10°C / min.

7. The method for preparing an adsorbent for removing phosphorus impurities in trichlorosilane according to claim 1, characterized in that: In the deposition step, the inorganic porous material and the metal salt solution are deposited for 30 to 120 minutes under vacuum to -0.2 to 0 MPa.

8. An adsorbent for removing phosphorus impurities in trichlorosilane, characterized in that: An inorganic porous material is used as a carrier, and an oxidized metal is loaded on the carrier, wherein the inorganic porous material is selected from one or more of ZrO2, SiO2, α-Al2O3, β-Al2O3, γ-Al2O3, CeO2, TiO2, and 13X molecular sieve.

9. The adsorbent for removing phosphorus impurities in trichlorosilane according to claim 8, characterized in that: The oxidized metal is formed by heating and oxidizing one or more metal salts of CuCl2, CuCl, ZnCl2, FeCl2, and CoCl2.

10. Use of the adsorbent for removing phosphorus impurities in trichlorosilane as claimed in claim 8 or 9, characterized in that: The phosphorus impurity removal adsorbent is used for adsorbing phosphorus impurities in trichlorosilane.