Purifying agent for treating high-boiling pyrolysis failure catalyst of polysilicon and organosilicon

Abstract

The present application relates to a kind of polycrystalline silicon and organic silicon high boiling pyrolysis failure catalyst treatment purifying agent as mesoporous matrix material and metal oxide composite system, specifically including mesoporous matrix material and its supported metal oxide, it can efficiently adsorb and catalytically decompose organic amine class pollutants in organic silicon and polycrystalline silicon high boiling pyrolysis waste liquid hydrolysate, make the organic amine concentration in hydrolysate reduce to 10mg / L below, preferably is 5mg / L below, comply with the strict environmental protection emission limit value requirement.

Description

Technical Field

[0001] This invention relates to the field of environmental chemical engineering technology, specifically to a purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon, and its preparation method. Background Technology

[0002] Silicon is a fundamental raw material for the photovoltaic industry, and the high-boiling-point pyrolysis method is currently the mainstream method for silicon production. High-boiling-point pyrolysis refers to the breaking of chemical bonds in high-boiling-point silicon under high temperature, high pressure, and oxygen-free or low-oxygen environments, causing it to decompose into small molecule compounds such as oligomers, monomers, and hydrogen gas. The mechanism of this pyrolysis process is that under high temperature and high pressure conditions, the bonds in the molecular chain of high-boiling-point silicon are broken through a pyrolysis reaction, thereby achieving the decomposition of high-boiling-point silicon. The pyrolysis of high-boiling-point silicon typically requires the use of a catalyst.

[0003] In the high-boiling-point pyrolysis process of polysilicon and organosilicon, organic amines such as tri-n-butylamine and aniline, which are commonly used as catalysts, are often difficult to completely remove after hydrolysis of high-boiling-point pyrolysis waste liquid due to their extremely high toxicity and harmfulness to the ecological environment. This makes it difficult for existing treatment methods to completely remove the organic amines, resulting in wastewater discharge that fails to meet strict environmental protection standards.

[0004] Existing wastewater treatment methods primarily involve purification and recovery through graded recovery, extraction, distillation, and other means. However, these technologies suffer from complex processes and limitations in further reducing the concentration of organic amines in the waste hydrolysate.

[0005] Therefore, the present invention aims to solve the technical problems in the prior art where the treatment process for high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon is complex and the concentration of organic amines cannot be further reduced. Summary of the Invention

[0006] This invention provides a novel high-efficiency purifying agent and its preparation method, which solves the technical problems in the prior art where the treatment process of high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon is complex and the concentration of organic amines cannot be further reduced.

[0007] The technical solution adopted by this invention to solve its technical problem is:

[0008] A method for preparing a purifying agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon, characterized in that the method specifically includes:

[0009] Step 1: Preparation of mesoporous matrix materials;

[0010] Specifically, this includes: selecting carbon molecular sieve material as the initial raw material, placing the carbon molecular sieve powder in a continuous flow high-temperature reactor, maintaining a temperature range of 800-1000℃, while simultaneously controlling the reaction pressure between atmospheric pressure and -30 kPa, and using CO2 gas with a purity greater than 99.99% as the reaction gas; during this process, strictly controlling the molar percentage of CO2 within the range of 1%-5% of the entire gas mixture; and filling the remaining gas environment with Ar or He inert gas.

[0011] Step 2: Mixing and loading of active metal compounds;

[0012] Specifically, the process includes: preparing solutions of ethylenediaminetetraethyleneferric, ethylenediaminetetramanganese, and metatitanic acid; uniformly mixing the prepared metal compound mixture with 10 parts by mass of pre-prepared mesoporous CMS molecular sieve; adding 20 parts by mass of methylcellulose as a binder; and simultaneously adding 30 parts by mass of deionized water. All components are thoroughly mixed in a dedicated biaxial forced stirring kneader to ensure that the metal compound is uniformly loaded onto the mesoporous material; wherein, ethylenediaminetetraethyleneferric, ethylenediaminetetramanganese, and metatitanic acid are prepared in a molar ratio of 1:1:1.

[0013] Step 3: Shaping and Drying;

[0014] After mixing, the material is quantitatively extruded using an extruder to produce strip-shaped granules; then placed in a constant temperature and humidity environment to dry naturally, ensuring that the moisture is completely evaporated and does not affect the internal structural stability of the purifying agent.

[0015] Step 4: Heat treatment and activation;

[0016] The dried purifying agent strips were heat-treated in a controlled atmosphere furnace with oxygen accounting for 0.5% of the total gas, with the temperature precisely controlled within the range of 600-700℃ and the heat treatment time being 3 hours. During the heat treatment process, SO2 gas accounting for 1.8-2.8% of the total gas was introduced as an activator.

[0017] Specifically, the constant temperature and humidity environment conditions are 25 degrees Celsius and 40% humidity.

[0018] Specifically, the diameter of the strip-shaped particles is 2-5 mm and the length is 3-6 mm;

[0019] Specifically, the average pore size of carbon molecular sieves is 0.3-1 nm.

[0020] Specifically, between steps three and four, there is also a surface loosening treatment step, which specifically includes: preparing a 1.5% by mass aqueous solution of methylcellulose, placing the shaped and dried strip-shaped particles on a tray, immersing them in the above methylcellulose aqueous solution and letting them stand for 10-15 seconds, then lifting the tray and placing the strip-shaped particles on the tray back into a constant temperature and humidity environment to dry naturally.

[0021] The purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon prepared according to the preparation method described above is a mesoporous matrix material and a metal oxide composite.

[0022] Specifically, the mesoporous matrix material is a carbon molecular sieve (CMS) matrix material.

[0023] Specifically, the metal oxides are Fe, Mn, and Ti metal oxides, which are obtained by high-temperature oxidation activation of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid in a heat treatment process.

[0024] The purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon prepared according to the preparation method described above has an outer material porosity that is 1.2-1.5 times that of the inner material porosity.

[0025] Specifically, the ratio of the outer material thickness to the inner material thickness is between 3:7 and 4:6.

[0026] This invention provides a purifying agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon, and its preparation method, which has the following technical effects:

[0027] 1. The carbon molecular sieve-based purifier simplifies the treatment of high-boiling-point degraded catalysts of polycrystalline silicon and organosilicon, and effectively improves the purification rate of organic amines.

[0028] 2. During the sintering of mesoporous materials, the molar percentage of CO2 is strictly controlled within the range of 1%-5% of the total gas. By controlling the molar percentage of CO2, the pore size and relative volume of the molecular sieve are adjusted, thereby modulating the pore size and porosity of the molecular sieve to achieve efficient adsorption of organic amines.

[0029] 3. The preparation ratio of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid solutions is 1:1:1 molar ratio. This ratio ensures that the three metal oxides are uniformly distributed when loaded onto the mesoporous matrix material, forming a composite metal oxide structure. This balanced ratio helps improve the overall catalytic activity and stability of the composite material, as each metal oxide may make a unique contribution to the adsorption and catalytic degradation of organic amines. Furthermore, by precisely controlling the molar ratio, the optimal synergistic effect between the metal ions is achieved, resulting in a composite catalyst exhibiting higher catalytic activity and selectivity when treating organic amines.

[0030] 4. The secondary absorption process of methylcellulose aqueous solution concentration results in the purifier particles having a higher porosity on the outer material than on the inner material. This allows more liquid to flow into the particles during purification and react with the metal oxides carried inside the particles. This avoids the blockage of surface pores caused by the concentrated reaction of liquid with the metal oxides carried on the surface material, thus improving the purification performance and lifespan of the purifier. Attached Figure Description

[0031] To clearly illustrate the technical solution of the present invention, the accompanying drawings of the specific embodiments will be briefly described below.

[0032] Appendix Figure 1 This is a flowchart of the preparation method provided in Example 1 of this application.

[0033] Appendix Figure 2 This is a flowchart of the preparation method provided in Example 2 of this application. Detailed Implementation

[0034] The present invention will now be described in more detail with reference to the accompanying drawings, which illustrate preferred embodiments of the invention. It should be understood that those skilled in the art can modify the invention described herein while still achieving the beneficial effects of the invention. Therefore, the following description should be understood as being of broad knowledge to those skilled in the art and is not intended to limit the invention.

[0035] For clarity, not all features of the actual embodiments are described. In the following description, well-known functions and structures are not detailed in detail, as they would confuse the invention with unnecessary detail. It should be understood that in the development of any actual embodiment, numerous implementation details must be made to achieve the developer's specific objectives.

[0036] To make the objectives and features of the present invention more apparent and understandable, the specific embodiments of the present invention will be further described below with reference to the accompanying drawings. It should be noted that the drawings are all in a very simplified form and use non-precise ratios, intended only to facilitate and clearly illustrate the objectives of the embodiments of the present invention.

[0037] The following will provide a more detailed description of the purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon, and its preparation method.

[0038] This application provides a purification agent for treating high-boiling-point decomposition failure catalysts of polysilicon and organosilicon, which is a composite system of mesoporous matrix material and metal oxide. Specifically, it includes a mesoporous matrix material and the metal oxide it supports. It can efficiently adsorb and catalytically decompose organic amine pollutants in the hydrolysis products of high-boiling-point decomposition waste liquid of organosilicon and polysilicon, reducing the concentration of organic amines in the hydrolysate to below 10 mg / L, preferably below 5 mg / L, which meets the stringent environmental emission limits.

[0039] Specifically, the mesoporous matrix material is a carbon molecular sieve (CMS) matrix material, which is formed by mixing treated carbon molecular sieve powder with a binder, extruding, drying, and heat treatment activation.

[0040] Specifically, the metal oxides are Fe, Mn, and Ti metal oxides, obtained through high-temperature oxidation activation using ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid in a heat treatment process. Specifically, the Fe, Mn, and Ti metal oxides may include, but are not limited to, FeOOH, MnOOH, TiO2, and other metal oxides with strong redox capabilities and catalytic activity. These oxides can chemically react with organic amines, promoting the oxidative decomposition of organic amines into harmless or low-toxicity substances, thereby achieving effective removal.

[0041] The preparation method of the purification agent for treating the above-mentioned polycrystalline silicon and organosilicon high-boiling decomposition failure catalysts is described below.

[0042] Example 1

[0043] The preparation method of the above-mentioned purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon specifically includes:

[0044] Step 1: Preparation of mesoporous matrix materials.

[0045] Specifically, this involves selecting carbon molecular sieve material as the initial raw material, with an average pore size of 0.3-1 nm. A certain amount of carbon molecular sieve powder is placed in a continuous flow high-temperature reactor, and the reaction is carried out within a precise temperature range of 800-1000℃, while the reaction pressure is controlled between atmospheric pressure and -30 kPa. The reaction gas is CO2 gas with a purity greater than 99.99%. During this process, the molar percentage of CO2 is strictly controlled within the range of 1%-5% of the total gas. By controlling the molar percentage of CO2, the pore size and relative volume of the molecular sieve can be adjusted, thereby modulating the pore size and porosity of the molecular sieve. This is crucial for subsequent loading of metal oxides and achieving efficient adsorption of organic amines.

[0046] The remaining gaseous environment is filled with Ar or He inert gas to ensure the stable progress of the reaction, prevent unnecessary side reactions of CMS molecular sieve under high temperature conditions, and ensure its structural stability and functional integrity.

[0047] Step 2: Mixing and loading of active metal compounds.

[0048] Specifically, this includes: preparing solutions of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid; uniformly mixing the prepared metal compound mixture with 10 parts by weight of pre-prepared mesoporous CMS molecular sieve; adding 20 parts by weight of methylcellulose as a binder; and simultaneously adding 30 parts by weight of deionized water. All components are thoroughly mixed in a dedicated biaxial forced stirring kneader to ensure that the metal compound is uniformly loaded onto the mesoporous material.

[0049] Ethylenediaminetetraethyleneferric, ethylenediaminetetramanganese, and metatitanic acid contain Fe, Mn, and Ti elements, respectively. During high-temperature heat treatment, they can be converted into corresponding metal oxides, such as FeOOH, MnOOH, TiO2, or other forms of oxides. These metal oxides typically possess strong redox capabilities and catalytic activity. These oxides can chemically react with organic amines, promoting their oxidative decomposition into harmless or low-toxicity substances, thereby achieving effective removal.

[0050] Ethylenediaminetetraacetic acid (EDTA), acting as a ligand, can form stable complexes with metal ions through its four carboxyl functional groups. This facilitates the loading and dispersion of metal ions during heat treatment, improving the uniformity of metal oxide distribution and the active surface area on mesoporous matrix materials. The combined use of EDTA-1,EDTA-1,0-manganese and metatitanic acid aims to construct a highly active purification system using the metal oxides obtained from their conversion. This system efficiently adsorbs and decomposes toxic and harmful organic amines in high-boiling-point pyrolysis residues of polycrystalline silicon and organosilicon, ensuring that wastewater treatment meets environmental discharge standards.

[0051] Preferably, the ratio of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid solutions is 1:1:1 molar ratio. This ratio ensures that the three metal oxides are uniformly distributed when loaded onto the mesoporous matrix material, forming a composite metal oxide structure. This balanced ratio helps improve the overall catalytic activity and stability of the composite material, as each metal oxide may make a unique contribution to the adsorption and catalytic degradation of organic amines. Furthermore, by precisely controlling the molar ratio, optimal synergistic effects between the metal ions can be achieved, resulting in a composite catalyst exhibiting higher catalytic activity and selectivity when treating organic amines.

[0052] Step 3: Shaping and drying.

[0053] The mixed materials are quantitatively extruded using an extruder to produce strip-shaped granules. Preferably, the diameter of the strip-shaped granules is 2-5 mm and the length is 3-6 mm.

[0054] It is then placed in a constant temperature and humidity environment (25 degrees Celsius, 40% humidity) to air dry naturally, ensuring that the moisture evaporates completely and does not affect the internal structural stability of the purifier.

[0055] Step 4: Heat treatment and activation.

[0056] The dried purifying agent strips were heat-treated in a controlled atmosphere furnace with an oxygen content of 0.5% of the total gas volume. The temperature was precisely controlled within the range of 600-700℃, and the heat treatment time was 3 hours. During the heat treatment process, SO2 gas with a molar ratio of 1.8-2.8% of the total gas volume was introduced as an activator. Through a sulfidation reaction at high temperature, Fe, Mn, and Ti metal oxides were encouraged to generate more active sites on their surfaces, significantly improving the adsorption and catalytic conversion efficiency of the purifying agent for organic amines.

[0057] SO2 gas, as an activator, can promote the reduction or sulfidation of metal oxides, generating metal sulfides or low-valence metal oxides with higher catalytic activity. It can also form new active sites on the material surface, which have a stronger adsorption and catalytic effect on organic amines, thereby improving the overall performance of the purifier.

[0058] Experiments have shown that if the molar content of SO2 is too low (e.g., below 1.8%), it is insufficient to effectively react with metal oxides to form highly catalytically active metal sulfides or low-oxidation-state metal oxides. This prevents SO2 from fully functioning as an activator, reducing the adsorption and conversion efficiency of the purifier for organic amines. Furthermore, a low SO2 concentration may not effectively regulate the pore structure and active sites of the purifier, making it difficult for organic amine molecules to fully contact the active centers, further affecting the purification effect. If the molar content of SO2 is too high (e.g., above 2.8%), excessive SO2 may react excessively with metal oxides, leading to the formation of excessive sulfides or other products. These products may cover the original active sites, reducing the catalyst's activity and weakening the purifier's adsorption and conversion capacity for organic amines. Excessive SO2 may also alter the physical structure of the purifier, such as causing pore shrinkage or blockage, affecting the diffusion and adsorption processes of organic amine molecules, thereby reducing purification efficiency.

[0059] Testing experiment:

[0060] Organic amine adsorption performance test: The prepared purifying agent was applied to simulated wastewater containing organic amines generated from the high-boiling-point cracking of polycrystalline silicon and organosilicon. Experimental results showed that, with an initial organic amine concentration of 500 mg / L, the concentration was reduced to 7.52 mg / L after treatment with the purifying agent, achieving a removal rate exceeding 98%, demonstrating the strong adsorption and conversion capabilities of the purifying agent.

[0061] Stability and reusability testing: The same batch of purifier was continuously used to treat organic amine solutions of the same concentration, with regeneration performed after each cycle to evaluate the purifier's lifespan and stability. Experiments showed that after fifteen consecutive cycles of use and regeneration, the organic amine removal rate of the purifier remained above 87%, demonstrating good stability and reusability.

[0062] Example 2

[0063] The preparation method of the above-mentioned purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon specifically includes:

[0064] Step 1: Preparation of mesoporous matrix materials.

[0065] Specifically, this involves selecting carbon molecular sieve material as the initial raw material, with an average pore size of 0.3-1 nm. A certain amount of carbon molecular sieve powder is placed in a continuous flow high-temperature reactor, and the reaction is carried out within a precise temperature range of 800-1000℃, while the reaction pressure is controlled between atmospheric pressure and -30 kPa. The reaction gas is CO2 gas with a purity greater than 99.99%. During this process, the molar percentage of CO2 is strictly controlled within the range of 1%-5% of the total gas. By controlling the molar percentage of CO2, the pore size and relative volume of the molecular sieve can be adjusted, thereby modulating the pore size and porosity of the molecular sieve. This is crucial for subsequent loading of metal oxides and achieving efficient adsorption of organic amines.

[0066] The remaining gaseous environment is filled with Ar or He inert gas to ensure the stable progress of the reaction, prevent unnecessary side reactions of CMS molecular sieve under high temperature conditions, and ensure its structural stability and functional integrity.

[0067] Step 2: Mixing and loading of active metal compounds.

[0068] Specifically, this includes: preparing solutions of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid; uniformly mixing the prepared metal compound mixture with 10 parts by weight of pre-prepared mesoporous CMS molecular sieve; adding 20 parts by weight of methylcellulose as a binder; and simultaneously adding 30 parts by weight of deionized water. All components are thoroughly mixed in a dedicated biaxial forced stirring kneader to ensure that the metal compound is uniformly loaded onto the mesoporous material.

[0069] Preferably, the ratio of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid solutions is 1:1:1 molar ratio. This ratio ensures that the three metal oxides are uniformly distributed when loaded onto the mesoporous matrix material, forming a composite metal oxide structure. This balanced ratio helps improve the overall catalytic activity and stability of the composite material, as each metal oxide may make a unique contribution to the adsorption and catalytic degradation of organic amines. Furthermore, by precisely controlling the molar ratio, optimal synergistic effects between the metal ions can be achieved, resulting in a composite catalyst exhibiting higher catalytic activity and selectivity when treating organic amines.

[0070] Step 3: Shaping and drying.

[0071] The mixed materials are quantitatively extruded using an extruder to produce strip-shaped granules. Preferably, the diameter of the strip-shaped granules is 2-5 mm and the length is 3-6 mm.

[0072] It is then placed in a constant temperature and humidity environment (25 degrees Celsius, 40% humidity) to air dry naturally, ensuring that the moisture evaporates completely and does not affect the internal structural stability of the purifier.

[0073] Step 4: Surface loosening treatment

[0074] Prepare a 1.5% (w / w) aqueous solution of methylcellulose. Place the dried strip-shaped particles on a tray and immerse them in the methylcellulose aqueous solution for 10-15 seconds. Then, lift the tray and place the strip-shaped particles on the tray in a constant temperature and humidity environment (25 degrees Celsius, 40% humidity) to dry naturally.

[0075] After soaking and re-drying, the strip-shaped particles, because their surface was soaked in the methylcellulose aqueous solution, had some of the surface material reabsorb the methylcellulose aqueous solution, making the texture more porous than the material in the center of the particles that did not reabsorb the methylcellulose aqueous solution.

[0076] In this step, the concentration of the methylcellulose aqueous solution and the soaking time are crucial parameters. If the concentration of the methylcellulose aqueous solution is too high, the solution viscosity will be too large, which is not conducive to liquid penetration. If the concentration of the methylcellulose aqueous solution is too low, the liquid may penetrate too deeply into the particles, making it impossible to ensure that the center of the particles does not undergo secondary liquid absorption. In addition, if the soaking time is too long, it will damage the particles or fail to ensure that the center of the particles does not undergo secondary liquid absorption. If the soaking time is too short, it will not allow particles of appropriate thickness to complete secondary liquid absorption.

[0077] Step 5: Heat treatment and activation.

[0078] The purified strips, after being dried again, were heat-treated in a controlled atmosphere furnace with an oxygen content of 0.5% of the total gas. The temperature was precisely controlled within the range of 600-700℃, and the heat treatment time was 3 hours.

[0079] After drying, the particles absorbed by the secondary liquid exhibit a state where the outer material is relatively loose and has a slightly higher methylcellulose content, while the inner material has not undergone loosening and has a lower methylcellulose content. During heat treatment, the temperature exceeds the decomposition temperature of methylcellulose, leaving behind a certain number of voids after decomposition. Furthermore, the outer material of the particles is already relatively loose after secondary liquid absorption. Therefore, after heat treatment, the purifying agent particles exhibit a state where the porosity of the outer material is greater than that of the inner material. Preferably, the porosity of the outer material is 1.2-1.5 times that of the inner material, and the ratio of the outer material thickness to the inner material thickness is between 3:7 and 4:6.

[0080] The purifier particles exhibit a higher porosity on the outer material than on the inner material, allowing more liquid to flow into the particles during purification and react with the metal oxides carried inside. This avoids clogging of surface pores caused by the concentrated reaction of liquid with the metal oxides carried on the surface material, thus improving the purification performance and lifespan of the purifier.

[0081] Testing experiment:

[0082] Organic amine adsorption performance test: The prepared purifying agent was applied to simulated wastewater containing organic amines generated from the high-boiling-point cracking of polycrystalline silicon and organosilicon. The experimental results showed that, with an initial organic amine concentration of 500 mg / L, the concentration of organic amines could be reduced to 4.84 mg / L after treatment with the purifying agent, demonstrating the strong adsorption and conversion capabilities of the purifying agent.

[0083] Stability and reusability testing: The same batch of purifier was continuously used to treat organic amine solutions of the same concentration, with regeneration performed after each cycle to evaluate the purifier's lifespan and stability. Experiments showed that after fifteen consecutive cycles of use and regeneration, the organic amine removal rate of the purifier remained above 94%, demonstrating good stability and reusability.

[0084] The present invention provides a method for preparing a purifying agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon, and the purifying agent prepared by this method has the following technical effects:

[0085] 1. The carbon molecular sieve-based purifier simplifies the treatment of high-boiling-point degraded catalysts of polycrystalline silicon and organosilicon, and effectively improves the purification rate of organic amines.

[0086] 2. During the sintering of mesoporous materials, the molar percentage of CO2 is strictly controlled within the range of 1%-5% of the total gas. By controlling the molar percentage of CO2, the pore size and relative volume of the molecular sieve are adjusted, thereby modulating the pore size and porosity of the molecular sieve to achieve efficient adsorption of organic amines.

[0087] 3. The preparation ratio of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid solutions is 1:1:1 molar ratio. This ratio ensures that the three metal oxides are uniformly distributed when loaded onto the mesoporous matrix material, forming a composite metal oxide structure. This balanced ratio helps improve the overall catalytic activity and stability of the composite material, as each metal oxide may make a unique contribution to the adsorption and catalytic degradation of organic amines. Furthermore, by precisely controlling the molar ratio, the optimal synergistic effect between the metal ions is achieved, resulting in a composite catalyst exhibiting higher catalytic activity and selectivity when treating organic amines.

[0088] 4. The secondary absorption process of methylcellulose aqueous solution concentration results in the purifier particles having a higher porosity on the outer material than on the inner material. This allows more liquid to flow into the particles during purification and react with the metal oxides carried inside the particles. This avoids the blockage of surface pores caused by the concentrated reaction of liquid with the metal oxides carried on the surface material, thus improving the purification performance and lifespan of the purifier.

[0089] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a purifying agent for treating high-boiling-point degraded catalysts of polycrystalline silicon and organosilicon, characterized in that: The method specifically includes: Step 1: Preparation of mesoporous matrix materials; Specifically, this includes: selecting carbon molecular sieve material as the initial raw material, placing the carbon molecular sieve powder in a continuous flow high-temperature reactor, maintaining a temperature range of 800-1000℃, while simultaneously controlling the reaction pressure between atmospheric pressure and -30 kPa, and using CO2 gas with a purity greater than 99.99% as the reaction gas; during this process, strictly controlling the molar percentage of CO2 within the range of 1%-5% of the entire gas mixture; and filling the remaining gas environment with Ar or He inert gas. Step 2: Mixing and loading of active metal compounds; Specifically, the process includes: preparing solutions of ethylenediaminetetraethyleneferric, ethylenediaminetetramanganese, and metatitanic acid; uniformly mixing the prepared metal compound mixture with 10 parts by mass of pre-prepared mesoporous CMS molecular sieve; adding 20 parts by mass of methylcellulose as a binder; and simultaneously adding 30 parts by mass of deionized water. All components are thoroughly mixed in a dedicated biaxial forced stirring kneader to ensure that the metal compound is uniformly loaded onto the mesoporous material; wherein, ethylenediaminetetraethyleneferric, ethylenediaminetetramanganese, and metatitanic acid are prepared in a molar ratio of 1:1:

1. Step 3: Shaping and Drying; After mixing, the material is quantitatively extruded using an extruder to produce strip-shaped granules; then placed in a constant temperature and humidity environment to dry naturally, ensuring that the moisture is completely evaporated and does not affect the internal structural stability of the purifying agent. Step 4: Heat treatment and activation; The dried purifying agent strips were heat-treated in a controlled atmosphere furnace with oxygen accounting for 0.5% of the total gas, with the temperature precisely controlled within the range of 600-700℃ and the heat treatment time being 3 hours. During the heat treatment process, SO2 gas accounting for 1.8-2.8% of the total gas was introduced as an activator.

2. The preparation method according to claim 1, characterized in that: The constant temperature and humidity environment conditions are 25 degrees Celsius and 40% humidity.

3. The preparation method according to claim 1, characterized in that: The diameter of the strip-shaped particles is 2-5 mm and the length is 3-6 mm.

4. The preparation method according to claim 1, characterized in that: The average pore size of carbon molecular sieves is 0.3-1 nm.

5. The preparation method according to claim 1, characterized in that: Between steps three and four, there is also a surface loosening treatment step, which specifically includes: preparing a 1.5% by mass aqueous solution of methylcellulose, placing the shaped and dried strip-shaped particles on a tray, immersing them in the above methylcellulose aqueous solution and letting them stand for 10-15 seconds, then lifting the tray and placing the strip-shaped particles on the tray back into a constant temperature and humidity environment to dry naturally.

6. The purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon prepared by the preparation method according to any one of claims 1-4, characterized in that: The purifying agent is a composite of mesoporous matrix material and metal oxide.

7. The purifying agent according to claim 6, characterized in that: The mesoporous matrix material is a carbon molecular sieve (CMS) matrix material.

8. The purifying agent according to claim 6, characterized in that: The metal oxides are Fe, Mn, and Ti metal oxides, which are obtained by high-temperature oxidation activation of ethylenediaminetetraethyleneferric, ethylenediaminetetraethylenemanganese, and metatitanic acid in a heat treatment process.

9. The purification agent for treating high-boiling-point decomposition failure catalysts of polycrystalline silicon and organosilicon prepared by the method according to claim 5, characterized in that: The porosity of the outer material is 1.2 to 1.5 times that of the inner material.

10. The purifying agent according to claim 9, characterized in that: The ratio of the outer material thickness to the inner material thickness is between 3:7 and 4:6.

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