Method for inactivating silicone slurry and inactivating agent

Abstract

The present application relates to a method for inactivating organic silicon slurry and an inactivating agent, the inactivating agent has a chemical formula of X-NH-Y, wherein X and Y are selected from the same or different combinations of groups of H, C n H 2n+1 (n = 1-10), or a phenyl group.

Description

Technical Field

[0001] This invention belongs to the field of environmental protection technology, specifically relating to a method for deactivating organosilicon slag slurry and a deactivating agent. Background Technology

[0002] Organosilicon slurry residue is mainly a byproduct of organosilicon production. Its main components include high-boiling-point substances, silicon powder, and metal powder. The high-boiling-point substances, with boiling points above 70℃, are primarily composed of disilanes, disiloxanes, and silanes, containing silicon-silicon bonds, silicon-carbon-silicon bonds, and silicon-oxygen-silicon structures. Silicon powder consists of fine silicon particles suspended in the slurry residue, representing unreacted or side-reaction solid residues. The metal powder consists of residues of metal catalysts such as copper and tin, which are used as catalysts in organosilicon synthesis. Organosilicon slurry residue is a fluid liquid-solid mixture, with the total discharge accounting for approximately 2% of the mixed monomer mass fraction, and a liquid-to-solid mass ratio of 5:1.

[0003] The organosilicon slurry contains high-boiling-point organosilicon compounds, such as high-boiling-point siloxanes and silanes. These substances typically have low flash points and high vapor pressures, easily volatilizing into the air to form flammable vapors that can ignite upon contact with an ignition source. In the organosilicon production process, copper catalysts are used as important catalytic materials. However, in the slurry, unreacted copper catalysts, upon contact with air, especially in humid environments, can oxidize and generate heat, leading to spontaneous combustion. Under certain conditions, the organic loading on the copper catalyst can accelerate the oxidation reaction, releasing sufficient heat to ignite surrounding flammable materials. Furthermore, although silicon powder itself is not easily flammable, it can act as a combustion aid, increasing the combustion rate and intensity of the fire. Therefore, organosilicon slurry is prone to spontaneous combustion during transportation and requires deactivation treatment.

[0004] Current inactivation methods primarily involve hydrolysis, which leaves behind copper and high-boiling-point residues. These residues still pose a risk of spontaneous combustion. Furthermore, the products obtained from hydrolysis and their state require additional separate processing steps in subsequent high-boiling-point and Cu recovery processes, increasing the complexity of subsequent procedures.

[0005] Therefore, there is a need to provide a method, system, and inactivating agent that can fully deactivate organosilicon slurry, thereby solving the problems of the prior art and achieving chemical deactivation effect. Summary of the Invention

[0006] The technical problem this invention aims to solve is the presence of residual copper and high-boiling-point substances, which still pose a certain risk of spontaneous combustion. Furthermore, the products obtained from the hydrolysis method and their state require additional separate processing steps in the subsequent high-boiling-point substance and Cu recovery process, increasing the complexity of subsequent processes. Therefore, there is a need to provide a method, system, and inactivation agent capable of fully deactivating organosilicon slurry to address these problems.

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

[0008] An inactivating agent for organosilicon slurry, the inactivating agent having the chemical formula X-NH-Y, wherein X and Y are substances selected from the same or different combinations of groups H, CnH2n+1 (n=1-10), or phenyl.

[0009] Specifically, the chemical formulas of the inactivating agents are NH3, CH3-NH-CH3, NH2-CH3, and NH2-C6H5.

[0010] A method for deactivating organosilicon slag slurry, which uses an inactivating agent with the chemical formula X-NH-Y, wherein X and Y are substances selected from the same or different combinations of groups H, CnH2n+1 (n=1-10), or phenyl.

[0011] Specifically, the chemical formulas of the inactivating agents are NH3, CH3-NH-CH3, NH2-CH3, and NH2-C6H5.

[0012] Specifically, the method also includes: passing a gaseous inactivating agent into organosilicon slurry powder.

[0013] Specifically, the organosilicon slurry powder is obtained by vacuum drying.

[0014] Specifically, a separation and filtration step was performed before vacuum drying.

[0015] Specifically, the method includes heating while introducing a gaseous inactivating agent.

[0016] Specifically, the method includes applying plasma while introducing a gaseous inactivating agent.

[0017] The present invention has the following beneficial effects:

[0018] 1) The inactivator X-NH-Y interacts with residual high-boiling substances and elemental copper catalysts. For elemental copper catalysts, X-NH-Y is an amine compound in which the nitrogen atom forms a stable complex with copper ions through coordination. Coordination refers to the formation of coordinate bonds. This process can encapsulate copper ions, inhibiting their activity, thereby "passivating" or "inactivating" the copper catalyst and reducing the risk of spontaneous combustion. For high-boiling substances, which contain reactive functional groups (such as carbonyl and carboxyl groups), amines can react with them through addition and condensation reactions to form more stable, less volatile, or less reactive derivatives. Furthermore, amines may also prevent the spontaneous combustion tendency of high-boiling substances by providing a relatively inert environment, capturing free radicals, or inhibiting oxidation reactions. In summary, the aforementioned X-NH-Y inactivator alters the chemical properties of hazardous substances through chemical reactions, rendering them ineligible for spontaneous combustion and thus increasing the safety of material transportation.

[0019] 2) For fine particles with a very large specific surface area, fine and coarse particles are treated separately. Heat-enhanced methods are used to ensure the fine particles react fully with a high concentration of inactivating agent, while plasma-enhanced methods are used to ensure the coarse particles react fully with the inactivating agent. This reduces the amount of inactivating agent used and improves the inactivation effect.

[0020] 3) This invention uses amine inactivators, avoiding conventional hydrolysis methods. The hydrolysis products are strongly acidic, requiring a necessary neutralization step before subsequent processing, thus saving process steps in slurry treatment.

[0021] 4) Before the inactivation step, the high-boiling materials in the slurry are fully vaporized and recovered under the combined action of low pressure and high temperature. In the initial stage, most of the high-boiling components are removed, reducing the possibility of spontaneous combustion of the slurry and reducing the consumption of inactivating agent by high-boiling materials in subsequent treatment processes. Attached Figure Description

[0022] To clearly illustrate the technical solution of the present invention, the accompanying drawings of the specific embodiments will be briefly described below.

[0023] Figure 1 The process flow of the organosilicon slag slurry deactivation method provided by the present invention

[0024] Figure 2 The inactivation treatment system used in the organosilicon slurry inactivation method provided by the present invention

[0025] Figure 3 The vacuum drying device in the inactivation treatment system provided by the present invention

[0026] Figure 4 The coarse particle inactivation device in the inactivation treatment system provided by the present invention

[0027] Figure 5 The inactivation powder integrated recovery system provided by the present invention is an inactivation treatment system. Detailed Implementation

[0028] 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.

[0029] 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.

[0030] 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.

[0031] Example 1

[0032] This invention first provides an inactivating agent for organosilicon slurry, the chemical formula of which is X-NH-Y, wherein X and Y are substances selected from the same or different combinations of groups H, CnH2n+1 (n=1-10), or phenyl groups. Preferably, the chemical formula of the inactivating agent is NH3, CH3-NH-CH3, NH2-CH3, NH2-C6H5, etc.

[0033] The deactivator X-NH-Y interacts with residual high-boiling substances and elemental copper catalysts. For elemental copper catalysts, X-NH-Y is an amine compound in which the nitrogen atom forms a stable complex with copper ions through coordination. Coordination refers to the formation of coordinate bonds. This process encapsulates copper ions, inhibiting their activity, thereby "passivating" or "deactivating" the copper catalyst and reducing the risk of spontaneous combustion. For high-boiling substances, which contain reactive functional groups (such as carbonyl and carboxyl groups), amines can react with them through addition and condensation reactions to form more stable, less volatile, or less reactive derivatives. Furthermore, amines may also prevent the spontaneous combustion tendency of high-boiling substances by providing a relatively inert environment, capturing free radicals, or inhibiting oxidation reactions. In summary, the aforementioned X-NH-Y deactivator alters the chemical properties of hazardous substances through chemical reactions, rendering them ineligible for spontaneous combustion and thus increasing the safety of material transportation.

[0034] Example 2

[0035] Based on the above-mentioned inactivating agent, this application also provides a method for inactivating organosilicon slurry using the above-mentioned inactivating agent, such as... Figure 1 As shown, the method specifically includes:

[0036] Step 1: Solid-liquid separation pretreatment of organosilicon slurry

[0037] The raw organosilicon slurry is passed through filter separator 1 to initially separate the solid and liquid components of the slurry.

[0038] Specifically, the original organosilicon slurry can be poured into the filter separation cylinder 1, where the solid-liquid mixture is separated into solid and liquid components. The solid component of the original slurry can then be used as the raw material for subsequent inactivation, and the waste liquid from the solid-liquid separation can be recycled.

[0039] Step 2: The solid organosilicon slurry after solid-liquid separation is subjected to vacuum drying and grinding treatment, so that the high-boiling materials in the organosilicon slurry are vaporized and recovered.

[0040] The specific process includes: feeding the organosilicon slurry into the vacuum drying drum unit 2 via a transmission system. After the organosilicon slurry is conveyed into the vacuum drying drum unit 2, the following steps are performed sequentially:

[0041] The first step is the grinding process, specifically: after the organic slurry enters the vacuum drying drum equipment 2, the drying drum 2-2 is sealed, nitrogen gas is introduced into the drum at a flow rate of 5000 sccm, and the grinding mode is turned on. The internal stirring rod 2-4, which is coaxially set in the center of the drying drum 2-2, rotates. The internal stirring rod 2-4 is equipped with grinding protrusions 2-6 extending radially along it. The internal stirring rod 2-4 causes the slurry to tumble and undergo grinding within the drying drum 2-2. The grinding time is 40-80 minutes.

[0042] Second, turn on the vacuum pump connected to the vacuum drying mixing drum device 2 to evacuate the gas inside the drum that has been cleaned with nitrogen and maintain the vacuum state. The preferred gas pressure is 0.5-1 mbar.

[0043] Third, once the vacuum level reaches the target decompression state, the heating device (not shown) embedded in the wall of the drying drum 2-2 is activated to perform decompression drying on the drying drum 2-2 and the slurry inside it, while maintaining the rotation of the internal stirring rod 2-4 during drying. As an alternative embodiment, the heating device can also be a medium-frequency heating, radiation heating, or indirect heating device. The specific process for decompression drying is as follows: the heating temperature is maintained at 180-200 degrees Celsius, the rotation speed of the internal stirring rod 2-4 is 150-250 revolutions per minute, and the drying time is 1-2 hours.

[0044] To facilitate understanding of the invention, the structure of the vacuum drying mixing drum device 2 is described herein. The vacuum drying mixing drum device 2 includes a drying drum 2-2, an openable sealing cover 2-1, an openable sealing bottom 2-3, and an inner stirring rod 2-4. The inner stirring rod 2-4 is provided with grinding protrusions 2-6 extending radially therefrom. Preferably, 3-5 grinding protrusions are arranged side-by-side at the same height on the inner stirring rod 2-4, and these grinding protrusions are hemispherical or irregular in shape. The drying drum 2-2 is a cylindrical component with open top and bottom surfaces. Heating components are embedded inside the sidewalls of the drying drum 2-2 to heat the material inside. A gas inlet port (not shown) is provided at the lower part of the sidewall of the drying drum 2-2, and an exhaust port (not shown) is provided at the upper part of the sidewall of the drying drum 2-2, which is connected to a vacuum pump. Furthermore, a vacuum gauge can be installed on the upper part of the sidewall of the drying drum 2-2 to measure the vacuum level inside the drum.

[0045] A sealing cover 2-1 with an openable and closable state is connected to the top surface of the drying drum 2-2. When the sealing cover is open, it can be used to add organosilicon slurry; when the sealing cover 2-1 is closed, it provides an airtight seal. A sealing bottom 2-3 is provided on the bottom surface of the drying drum 2-2. When the sealing bottom 2-3 is open, the material stored inside the drying drum 2-2 can be unloaded; when the sealing bottom 2-3 is closed, it provides an airtight seal. A drive motor 2-5 is also provided inside the sealing bottom 2-3 or on the outside of the bottom surface. The drive motor 2-5 transmits rotational motion to the inner stirring rod 2-4 through a transmission shaft 2-7. Specifically, the top end of the transmission shaft 2-7 includes a shaft connecting key 2-8. When the sealing bottom 2-3 covers the drying drum 2-2, the shaft connecting key 2-8 can be embedded into a groove of a corresponding shape in the inner stirring rod 2-4, thereby fixing the transmission shaft and the inner stirring rod relative to each other and transmitting the rotation of the drive motor 2-5 to the inner stirring rod 2-4.

[0046] In this vacuum drying process, the organosilicon slurry is heated to 180-200 degrees Celsius. Under the combined action of low pressure and high temperature, the high-boiling materials in the slurry are more fully vaporized and recovered. In the initial stage, most of the high-boiling components are removed, reducing the possibility of spontaneous combustion of the slurry and reducing the consumption of inactivating agents by high-boiling materials in subsequent processing.

[0047] In the aforementioned vacuum drying process, most of the high-boiling-point components are first separated physically through a low-pressure and high-temperature environment. Furthermore, during vacuum drying, the slurry is subjected to gravity and centrifugal force, resulting in thorough contact between the slurry and the grinding portions of the internal stirring rods 2-4 inside the vacuum drying cylinder. This grinding of the solid slurry significantly reduces its particle size, which is beneficial for subsequent reactions.

[0048] To verify the effectiveness of the above steps in removing high-boiling-point substances, after five repeated experiments in the above embodiment, two 50g samples (a total of 10 samples) of the slurry obtained after vacuum drying in each experiment were selected and measured by gas chromatography. The mass percentage of high-boiling-point substances relative to the total slurry mass in the 10 samples was 2.01%. This indicates that the vacuum drying treatment effectively reduced the content of high-boiling-point substances in the slurry.

[0049] Step 3: Separate the solid organosilicon slurry powder into fine and coarse particles.

[0050] The slurry powder after vacuum drying is conveyed and fed into the inlet of cyclone separator 3, where it is separated into fine slurry powder and coarse slurry powder.

[0051] Specifically, the process involves: discharging the vacuum-dried slurry powder from the outlet of the vacuum drying drum device 2; conveying the discharged solid slurry powder to the inlet at the top of the cyclone separator 3; inside the cyclone separator, coarse slurry powder particles are thrown against the inner wall of the separator due to centrifugal force and fall vertically into the coarse particle collector below the separator; fine slurry powder particles flow with the airflow, spiraling upwards to the bottom of the separator, and finally flowing out from the outlet at the top of the cyclone separator. This achieves the separation of particles of different sizes in the powder slurry. Preferably, fine particles refer to particles with a diameter less than 10 micrometers, and coarse particles refer to particles with a diameter greater than 10 micrometers.

[0052] The reason for treating fine and coarse particles separately is that, due to the extremely large specific surface area of ​​fine particles, if copper or residual high-boiling-point substances are coated on the slurry, the oxidation and heat accumulation effects are very intense. Therefore, the treatment of fine particles is more important for the deactivation effect. Thus, this invention improves the overall deactivation effect of the slurry by more optimized treatment through the separation of fine particles from coarse particles.

[0053] Since cyclone separators are common equipment in the chemical industry, their structure will not be described in detail here.

[0054] Step 4: Perform inactivation treatment on coarse-particle slurry powder and fine-particle slurry powder respectively.

[0055] The airflow containing fine particulate slurry powder from the upper outlet of the cyclone separator 3 is introduced into the fine particle inactivation device 5 through a conveying pipe. Preferably, a pressure replenishment device is installed near the outlet of the cyclone separator in the conveying pipe. This pressure replenishment device can replenish the pipeline with an appropriate amount of nitrogen gas flow through a fixed pressure regulating device, thereby ensuring that the airflow containing fine particles from the outlet of the cyclone separator flows fully into the fine particle inactivation device 5.

[0056] The fine particle inactivation device 5 includes a vertically arranged spiral quartz glass tube 5-1 that is airtightly connected to the air outlet of the cyclone separator 3, an infrared heating device 5-2 located near the periphery of the spiral quartz glass tube 5-1, and an inactivating agent inlet located near the material inlet of the spiral quartz glass tube 5-1, thereby providing sufficient inactivating agent in the fine particle inactivation device 5.

[0057] Preferably, the axial length of the spiral quartz glass tube 5-1 is 5-10 meters, the diameter of the spiral shape is 0.1-0.3m, and the angle between the spiral shape and the horizontal is above 45 degrees, so as to ensure that fine particles are not easily trapped inside the quartz glass tube.

[0058] When the fine particulate slurry powder enters the inlet of the spiral quartz glass tube 5-1, the gaseous inactivating agent is also introduced into the spiral quartz glass tube 5-1 through the air inlet pipe near the inlet. The flow rate ratio of the gaseous inactivating agent to the air flow rate of the fine particulate slurry powder is 1:1. The chemical formula of the gaseous inactivating agent is X-NH-Y, where X and Y are substances selected from the same or different combinations of groups H, CnH2n+1 (n=1-10), or phenyl. Preferably, the chemical formula of the inactivating agent is NH3, CH3-NH-CH3, NH2-CH3, NH2-C6H5, etc. The inactivating agent is vaporized and purified before being introduced into the spiral quartz glass tube 5-1. The spiral quartz glass tube 5-1 is uniformly heated by an infrared heating device 5-2 located near its periphery, maintaining the internal temperature of the spiral quartz glass tube 5-1 at 150-180 degrees Celsius, thereby ensuring a full reaction between the fine particulate slurry powder and the inactivating agent.

[0059] Because of the large specific surface area of ​​the fine slurry powder, it can react more fully with the inactivating agent during all the paths of the spiral quartz glass tube 5-1, thus achieving complete inactivation.

[0060] The coarse particle slurry powder discharged from the bottom of the cyclone separator 3 is conveyed to the coarse particle inactivation device 4. This coarse particle inactivation device 4 is a plasma treatment device, in which the coarse particle slurry powder is placed in the plasma treatment chamber, and a gaseous inactivating agent with the chemical formula X-NH-Y is introduced, where X and Y are substances selected from the group consisting of H, CnH2n+1 (n=1-10), or phenyl groups, either in the same or different combinations. Preferably, the chemical formula of the inactivating agent is NH3 or CH3-NH-CH3. The coarse particle slurry powder is inactivated through a plasma-enhanced reaction.

[0061] The specific process is as follows: the back vacuum degree is 0.6 mbar, the radio frequency power is 50W, the volume ratio of gaseous inactivator to inert ambient gas N2 is 3:5, the total gas flow rate is controlled between 200 sccm and 500 sccm, the mass of the coarse particle slurry powder added is controlled at 500g, and the plasma treatment time is 20-30min.

[0062] Specifically, a mixture of inactivating agent gas and N2 is introduced into the inactivation chamber, and plasma is applied simultaneously for plasma treatment, thereby enhancing the passivation effect of N atoms on the coarse-particle slurry. Under the enhanced effect of plasma, nitrogen atoms form stable complexes with copper ions through coordination interactions. Coordination interaction refers to the formation of coordinate bonds. This process can encapsulate copper ions, inhibiting their activity, thereby "passivating" or "inactivating" the copper catalyst and reducing the risk of spontaneous combustion. For high-boiling substances, which contain reactive functional groups (such as carbonyl and carboxyl groups), amines can react with them through addition reactions, condensation reactions, etc., to form more stable, less volatile, or less reactive derivatives.

[0063] Step 5: Integration and recycling of organosilicon slag slurry inactivation powder

[0064] The outlet of the fine particle inactivation device 5 and the discharge port of the coarse particle inactivation device 4 are both connected to the inlet of the inactivation powder integration and recovery device 6. The inactivation powder integration and recovery device 6 includes an upper fine particle inlet 6-2, a side upper coarse particle inlet 6-4, a middle filter plate 6-6, a bottom exhaust outlet 6-3, and a side discharge port 6-5. The middle filter plate 6-6 includes a bottom metal filter screen 6-6-1 and a fine-pore filter element 6-6-2 located on the top surface of the bottom metal filter screen 6-6-1. The fine-pore filter element 6-6-2 can be a surface-passivated porous resin or non-woven fabric, etc.

[0065] The middle filter plate 6-6 retains both inactivated coarse and fine slurry powder in its upper part, while excess waste gas flows into the lower part of the middle filter plate 6-6 and is pumped out and recovered by a pump connected to the waste gas outlet 6-3. This process collects and preserves the inactivated coarse and fine slurry powder retained on the middle filter plate 6-6.

[0066] Example 3

[0067] The present invention also provides an inactivation system for performing the above-described method for inactivating organosilicon slurry, see [link to relevant documentation]. Figure 2-5 It includes a filter separation cylinder 1, a vacuum drying drum device 2, a cyclone separator 3, a coarse particle inactivation device 4, a fine particle inactivation device 5, and an inactivated powder integration and recovery device 6, etc.

[0068] The solid discharge port of the filter separator 1 is connected to the solid feed port of the vacuum drying drum device 2, and the liquid discharge port of the filter separator 1 is connected to the waste liquid recovery device. The solid powder discharge port of the vacuum drying drum device 2 is connected to the feed port of the cyclone separator 3, and the gaseous high-boiling-point exhaust port of the vacuum drying drum device 2 is connected to the high-boiling-point recovery device. The solid powder processed by the vacuum drying drum device 2 is fed into the feed port of the cyclone separator 3. Fine-particle slurry powder is discharged with the gas from the exhaust port at the top of the cyclone separator 3, and coarse-particle slurry powder is discharged from the discharge port at the bottom of the cyclone separator 3. The fine-particle slurry powder is inactivated by the fine-particle inactivation device 5, and the coarse-particle slurry powder is inactivated by the coarse-particle inactivation device 4. The inactivated coarse-particle slurry powder and fine-particle slurry powder are then fed into the inactivated powder integration and recovery device 6 for solid filtration and mixing collection.

[0069] The reduced pressure drying mixing drum device 2 includes a drying drum 2-2, an openable sealing cover 2-1, an openable sealing bottom 2-3, and an inner stirring rod 2-4. The inner stirring rod 2-4 is provided with grinding protrusions 2-6 extending radially therefrom. Preferably, 3-5 grinding protrusions are arranged side-by-side at the same height on the inner stirring rod 2-4, and these grinding protrusions are hemispherical or irregular in shape. The drying drum 2-2 is a cylindrical component with open top and bottom surfaces. Heating components are embedded inside the sidewalls of the drying drum 2-2 to heat the material inside. A gas inlet port (not shown) is provided at the lower part of the sidewall of the drying drum 2-2, and an exhaust port (not shown) is provided at the upper part of the sidewall of the drying drum 2-2, which is connected to a vacuum pump. Furthermore, a vacuum gauge can be installed on the upper part of the sidewall of the drying drum 2-2 to measure the vacuum level inside the drum.

[0070] A sealing cover 2-1 with an openable and closable state is connected to the top surface of the drying drum 2-2. When the sealing cover is open, it can be used to add organosilicon slurry; when the sealing cover 2-1 is closed, it provides an airtight seal. A sealing bottom 2-3 is provided on the bottom surface of the drying drum 2-2. When the sealing bottom 2-3 is open, the material stored inside the drying drum 2-2 can be unloaded; when the sealing bottom 2-3 is closed, it provides an airtight seal. A drive motor 2-5 is also provided inside the sealing bottom 2-3 or on the outside of the bottom surface. The drive motor 2-5 transmits rotational motion to the inner stirring rod 2-4 through a transmission shaft 2-7. Specifically, the top end of the transmission shaft 2-7 includes a shaft connecting key 2-8. When the sealing bottom 2-3 covers the drying drum 2-2, the shaft connecting key 2-8 can be embedded into a groove of a corresponding shape in the inner stirring rod 2-4, thereby fixing the transmission shaft and the inner stirring rod relative to each other and transmitting the rotation of the drive motor 2-5 to the inner stirring rod 2-4.

[0071] In this vacuum drying process, the organosilicon slurry is heated to 180-200 degrees Celsius. Under the combined action of low pressure and high temperature, the high-boiling materials in the slurry are more fully vaporized and recovered. In the initial stage, most of the high-boiling components are removed, reducing the possibility of spontaneous combustion of the slurry and reducing the consumption of inactivating agents by high-boiling materials in subsequent processing.

[0072] In the aforementioned vacuum drying process, most of the high-boiling-point components are first separated physically through a low-pressure and high-temperature environment. Furthermore, during vacuum drying, the slurry is subjected to gravity and centrifugal force, resulting in thorough contact between the slurry and the grinding portions of the internal stirring rods 2-4 inside the vacuum drying cylinder. This grinding of the solid slurry significantly reduces its particle size, which is beneficial for subsequent reactions.

[0073] Inside the cyclone separator 3, coarse slurry powder is thrown towards the inner wall of the separator by centrifugal force and falls vertically into the coarse particle collector below the separator. Fine slurry powder flows with the airflow, and after the airflow spirals to the bottom of the separator, it flows upward, and finally flows out from the air outlet at the top of the cyclone separator. In this way, the separation of powder slurry particles of different sizes is achieved. Preferably, fine particles refer to particles with a diameter of less than 10 micrometers, and coarse particles refer to particles with a diameter of more than 10 micrometers.

[0074] The coarse particle inactivation device 4 includes a cavity 4-1, a radio frequency induction coil 4-2, an air inlet pipe 4-3, a gas spray head 4-4, a feed port 4-5, a discharge port 4-6, and a lower electrode support plate 4-7. The radio frequency induction coil 4-2 and the lower electrode support plate 4-7 are respectively connected to a radio frequency power supply to generate plasma. The air inlet pipe 4-3 includes an inlet pipe for gaseous inactivating agent and inert gas. After the gaseous inactivating agent and inert gas are mixed, they flow into the sealed cavity through the spray head 4-4. Under the enhanced effect of the plasma, nitrogen atoms form stable complexes with copper ions through coordination. Coordination refers to the formation of coordinate bonds. This process can encapsulate copper ions, inhibiting their activity, thereby "passivating" or "inactivating" the copper catalyst and reducing the risk of spontaneous combustion. For high-boiling substances, which contain reactive functional groups (such as carbonyl and carboxyl groups), amines can react with them through addition reactions, condensation reactions, etc., to form more stable, less volatile, or less reactive derivatives.

[0075] The fine particle inactivation device 5 includes a vertically arranged spiral quartz glass tube 5-1 that is airtightly connected to the air outlet of the cyclone separator 3, an infrared heating device 5-2 located near the periphery of the spiral quartz glass tube 5-1, and an inactivating agent inlet located near the material inlet of the spiral quartz glass tube 5-1, thereby providing sufficient inactivating agent in the fine particle inactivation device 5.

[0076] Preferably, the axial length of the spiral quartz glass tube 5-1 is 5-10 meters, the diameter of the spiral shape is 0.1-0.3m, and the angle between the spiral shape and the horizontal is above 45 degrees, so as to ensure that fine particles are not easily trapped inside the quartz glass tube.

[0077] The inactivated powder integrated recycling equipment 6 includes an upper fine particle inlet 6-2, a side upper coarse particle inlet 6-4, a middle filter plate 6-6, a bottom exhaust outlet 6-3, and a side outlet 6-5. The middle filter plate 6-6 includes a bottom metal filter screen 6-6-1 and a fine-pore filter element 6-6-2 located on the top surface of the bottom metal filter screen 6-6-1. The fine-pore filter element 6-6-2 can be made of passivated porous resin or non-woven fabric, etc.

[0078] The inactivated coarse and fine slurry powders are retained in the upper part of the middle filter plate 6-6, while excess waste gas flows into the lower part of the middle filter plate 6-6 and is pumped out and recovered by a pump connected to the waste gas outlet 6-3. This process collects and preserves the inactivated coarse and fine slurry powders retained on the middle filter plate 6-6.

[0079] Furthermore, the conveying device in this system can be a conveyor belt, a robotic arm, or other conveying device familiar to those skilled in the art to achieve material transfer between equipment. As for the necessary sealing devices, pumps, and valves, those skilled in the art are familiar with their basic installation methods, and will not elaborate further here.

[0080] The present invention can achieve the following technical effects:

[0081] 1) The inactivator X-NH-Y interacts with residual high-boiling substances and elemental copper catalysts. For elemental copper catalysts, X-NH-Y is an amine compound in which the nitrogen atom forms a stable complex with copper ions through coordination. Coordination refers to the formation of coordinate bonds. This process can encapsulate copper ions, inhibiting their activity, thereby "passivating" or "inactivating" the copper catalyst and reducing the risk of spontaneous combustion. For high-boiling substances, which contain reactive functional groups (such as carbonyl and carboxyl groups), amines can react with them through addition and condensation reactions to form more stable, less volatile, or less reactive derivatives. Furthermore, amines may also prevent the spontaneous combustion tendency of high-boiling substances by providing a relatively inert environment, capturing free radicals, or inhibiting oxidation reactions. In summary, the aforementioned X-NH-Y inactivator alters the chemical properties of hazardous substances through chemical reactions, rendering them ineligible for spontaneous combustion and thus increasing the safety of material transportation.

[0082] 2) For fine particles with a very large specific surface area, fine and coarse particles are treated separately. Heat-enhanced methods are used to ensure the fine particles react fully with a high concentration of inactivating agent, while plasma-enhanced methods are used to ensure the coarse particles react fully with the inactivating agent. This reduces the amount of inactivating agent used and improves the inactivation effect.

[0083] 3) This invention uses amine inactivators, avoiding conventional hydrolysis methods. The hydrolysis products are strongly acidic, requiring a necessary neutralization step before subsequent processing, thus saving process steps in slurry treatment.

[0084] 4) Before the inactivation step, the high-boiling materials in the slurry are fully vaporized and recovered under the combined action of low pressure and high temperature. In the initial stage, most of the high-boiling components are removed, reducing the possibility of spontaneous combustion of the slurry and reducing the consumption of inactivating agent by high-boiling materials in subsequent treatment processes.

[0085] 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 deactivating organosilicon slurry, characterized in that: It uses an inactivating agent with the chemical formula X-NH-Y, where X and Y are H and C groups, respectively. n H 2n+1 Substances selected from the same or different combinations of substances composed of phenyl groups, where n = 1-10.

2. The inactivation method as described in claim 1, characterized in that: The chemical formula of the inactivating agent is NH3, CH3-NH-CH3, NH2-CH3 or NH2-C6H5.

3. The inactivation method as described in claim 2, characterized in that: The method also includes: passing a gaseous inactivating agent into organosilicon slurry powder.

4. The inactivation method as described in claim 3, characterized in that: The organosilicon slurry powder was obtained by vacuum drying.

5. The inactivation method as described in claim 4, characterized in that: Before vacuum drying, it also underwent a separation and filtration step.

6. The inactivation method as described in claim 3, characterized in that: The method includes heating while introducing a gaseous inactivating agent.

7. The inactivation method as described in claim 3, characterized in that: The method includes applying plasma while introducing a gaseous inactivating agent.

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