An integrated processing system for silicone waste bodies

Abstract

This utility model discloses an integrated treatment system for waste silicone catalysts, comprising a hydrolysis tank, a gas distributor at the bottom of the hydrolysis tank, a stirrer above the hydrolysis tank, and an exhaust pipe connected to the top of the hydrolysis tank. The outlet of a nitrogen pipeline is connected to the inlet of the gas distributor via a pipe; the outlet of a waste catalyst conveying pipeline is connected to the inlet of the hydrolysis tank; and the outlet of a dilute hydrochloric acid pipeline and the outlet of a water pipeline are both connected to the inlet of the hydrolysis tank. Beneficial effects: This utility model has a simple connection structure, is easy to implement, shortens the processing cycle, reduces material loss, and thus reduces equipment and labor costs; it also reduces safety hazards, improves copper leaching rate, can be directly adapted to the waste catalyst treatment needs of existing silicone monomer workshops, has low equipment modification difficulty, and is easy to promote.

Description

Technical Field

[0001] This utility model relates to the field of solid waste treatment technology in organosilicon monomer production, and in particular to an integrated treatment system for organosilicon waste catalysts. Background Technology

[0002] In the industrial production of organosilicon monomers, silicon powder and chloromethane react in a fluidized bed reactor under the action of a copper-based catalyst. A large amount of waste catalyst is generated in the later stages of the reaction. The main components of this waste catalyst include: unreacted silicon powder, deactivated copper-based catalyst, organic carbon generated during the reaction, metalloid chlorides carried over from the silicon raw material, and chloromethane residue. Actual production operation has verified that the aforementioned waste catalyst has reached a relatively fine particle size due to the continuous fluidization effect during the fluidized bed reaction process, and can meet the specific surface area requirements of the subsequent leaching reaction without additional grinding. If the waste catalyst is directly piled up or landfilled without proper treatment, it will not only waste copper resources in copper-based catalysts, but also cause soil acidification and excessive heavy metals in groundwater due to the strong acidity and water solubility of metalloid chlorides. The current industry generally adopts the traditional treatment process of "resource recycling + solid waste compliance". The core steps of this process are: hydrolysis pretreatment → pressure filtration separation → ball milling → stirring and mixing → leaching → secondary pressure filtration → sponge copper extraction → solid waste neutralization and disposal. However, this traditional process has significant drawbacks: 1. The production process still includes a ball milling step, without taking into account the actual production situation that "the waste catalyst has a fine particle size and does not require grinding". The sequence of first pressing and then ball milling is difficult to crush because the filter cake is compacted. As a result, the copper catalyst is coated and the leaching rate is not high. Moreover, the redundant ball milling, stirring and mixing and soaking leaching steps result in high material transfer losses. It also requires an additional 2 to 3 operators, increases the number of equipment failure points, increases costs, and the existing processing technology is cumbersome and inefficient.

[0003] 2. Currently, nitrogen is added to the hydrolysis tank through a pipeline at the top. Since the venting pipeline is also at the top and the venting system is under slight negative pressure, the added nitrogen will be directly discharged from the hydrolysis tank through the venting pipeline. This does not effectively dilute the hydrogen, causing the trace amounts of hydrogen produced by the silicon powder hydrolysis reaction to easily accumulate at the top of the hydrolysis tank where the nitrogen cannot reach. This poses a significant safety risk and a major safety hazard. To address the aforementioned shortcomings, there is an urgent need to design a waste catalyst treatment solution that integrates functions, optimizes processes, and balances safety and efficiency, in order to solve the pain points of traditional processes. Utility Model Content

[0004] The main purpose of this utility model is to provide an integrated treatment system for waste silicone catalysts, which shortens the treatment cycle, reduces material loss, and thus reduces equipment and labor costs; it also reduces safety hazards, increases copper leaching rate, and can be directly adapted to the waste catalyst treatment needs of existing silicone monomer workshops. The equipment is easy to modify and promote. To achieve the above objectives, the technical solution adopted by this utility model is as follows: an integrated treatment system for organosilicon waste catalysts, comprising a hydrolysis tank, a gas distributor installed at the bottom of the hydrolysis tank, a stirrer installed above the hydrolysis tank, and an exhaust pipe connected to the top of the hydrolysis tank; the outlet of a nitrogen pipeline is connected to the inlet of the gas distributor via a pipe; the outlet of a waste catalyst conveying pipeline is connected to the inlet of the hydrolysis tank; the outlet of a dilute hydrochloric acid pipeline and the outlet of a water conveying pipeline are both connected to the inlet of the hydrolysis tank; the outlet of the hydrolysis tank is connected to the inlet of a first filter press; the outlet of the first filter press is connected to the inlet of a sponge copper tank; the outlet of an iron powder silo is connected to the inlet of the sponge copper tank; the outlet of the first filter press is connected to the inlet of a solid waste storage tank; and the outlet of the sponge copper tank is connected to the inlet of a second filter press.

[0005] Furthermore, the gas distributor adopts a multi-group concentric ring pipe structure, and several gas outlet holes are opened at the bottom of the gas distributor facing the hydrolysis tank. Adjacent concentric ring pipes are connected by connecting pipes.

[0006] Furthermore, the spacing between adjacent air outlets is 180-380mm, and the diameter of the air outlet is 1-3mm.

[0007] Furthermore, it also includes a mixing tank, the outlet of the solid waste storage tank is connected to the inlet of the mixing tank, the outlet of the dilute hydrochloric acid pipeline is connected to the inlet of the mixing tank, and the outlet of the mixing tank is connected to the inlet of the first filter press.

[0008] Furthermore, it also includes a calcium oxide silo, the outlet of which is connected to the inlet of the solid waste storage tank.

[0009] This utility model has the following beneficial effects: 1. The connection structure of this utility model is simple and easy to implement. The hydrolysis tank integrates hydrolysis and soaking functions, eliminating redundant ball mills and soaking tanks, reducing material transfer links, shortening the processing cycle, reducing material loss, and thus reducing equipment and labor costs. 2. This utility model sets up a gas distributor at the bottom of the hydrolysis tank, and then uses nitrogen bubbling to dilute and remove trace amounts of hydrogen, reducing safety hazards, and also enhances material mixing and improves the copper leaching rate. Based on the actual production design of "fine particle size of waste catalyst that does not require grinding", it can be directly adapted to the waste catalyst treatment needs of existing organosilicon monomer workshops. The equipment is easy to modify and promote. Attached Figure Description To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0010] Figure 1 This is a schematic diagram of the overall structure of an integrated treatment system for organosilicon waste catalysts according to the present invention.

[0011] Figure 2 for Figure 1 A cross-sectional view of section AA.

[0012] In the diagram: 1. Hydrolysis tank; 2. Gas distributor; 21. Concentric ring pipe; 22. Gas outlet; 23. Connecting pipe; 3. Agitator; 4. Exhaust pipe; 5. Nitrogen pipeline; 6. Waste catalyst conveying pipeline; 7. Dilute hydrochloric acid pipeline; 8. Water pipeline; 9. First filter press; 10. Sponge copper tank; 11. Iron powder silo; 12. Solid waste storage tank; 13. Second filter press; 14. Agitator; 15. Calcium oxide silo. Detailed Implementation

[0013] The following is in conjunction with the appendix Figure 1-2 The principles and features of this utility model are described, making the technical means, creative features, and achieved objectives of this utility model easy to understand, and further elaborating on this utility model.

[0014] In the description of this utility model, it should be noted that the terms "upper," "lower," "inner," "front end," "rear end," "both ends," "one end," and "the other end," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0015] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installed," "equipped with," and "connected," etc., should be interpreted broadly. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be a connection within two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0016] like Figure 1-2 As shown, the technical solution adopted by this utility model is as follows: an integrated treatment system for organosilicon waste catalyst, comprising a hydrolysis tank 1, a gas distributor 2 installed at the bottom of the hydrolysis tank 1, a stirrer 3 installed above the hydrolysis tank 1, and an exhaust pipe 4 connected to the top of the hydrolysis tank 1; the outlet end of a nitrogen pipeline 5 is connected to the inlet end of the gas distributor 2 via a pipe, the outlet end of a waste catalyst conveying pipeline 6 is connected to the inlet of the hydrolysis tank 1, and a dilute salt... The outlet of acid pipeline 7 and the outlet of water pipeline 8 are both connected to the inlet of hydrolysis tank 1. The outlet of hydrolysis tank 1 is connected to the inlet of first filter press 9. The outlet of first filter press 9 is connected to the inlet of sponge copper tank 10. The outlet of iron powder silo 11 is connected to the inlet of sponge copper tank 10. The outlet of first filter press 9 is connected to the inlet of solid waste storage 12. The outlet of sponge copper tank 10 is connected to the inlet of second filter press 13.

[0017] The gas distributor 2 adopts a multi-group concentric ring pipe structure. Several gas outlet holes 22 are opened at the bottom of the gas distributor 2 facing the hydrolysis tank 1. Adjacent concentric ring pipes 21 are connected by connecting pipes 23. The distance between adjacent gas outlet holes 22 is 180-380mm, and the diameter of the gas outlet hole 22 is 1-3mm.

[0018] The discharge port of the solid waste storage 12 is connected to the inlet of the mixing tank 14, the liquid outlet of the dilute hydrochloric acid pipeline 7 is connected to the liquid inlet of the mixing tank 14, and the liquid outlet of the mixing tank 14 is connected to the liquid inlet of the first filter press 9; the discharge port of the calcium oxide silo 15 is connected to the inlet of the solid waste storage 12.

[0019] Working principle: Step 1: Feeding and Hydrolysis Pretreatment Waste catalyst and tap water are fed into hydrolysis tank 1 through the top inlet at a solid-liquid ratio of 1:3 to 1:5. The top agitator 3 is turned on (rotation speed 30 to 40 r / min); at the same time, a trace amount of nitrogen gas (flow rate 0.5 to 0.8 m³ / min) is introduced. 3Nitrogen gas is evenly bubbled through the outlet 22 on the gas distributor 2 at the bottom of the tank, forming a dual mixing effect of "stirring + bubbling"; at the same time, the trace amount of hydrogen gas generated in the tank is diluted and sent to the tail gas treatment device (combustion or adsorption) through the exhaust pipe 4 on the top of the tank to ensure that the hydrogen concentration in the tank is below the lower explosive limit; the temperature inside the tank is controlled at 40~60℃, and the hydrolysis reaction is carried out for 2~3 hours. During this period, the pH is sampled regularly through the sampling port (maintaining pH 2~3) until the organic carbon structure is destroyed and the dissolution rate of metalloid chloride is ≥90%. Step 2: Soaking and Extraction After hydrolysis, keep stirrer 3 running (speed adjusted to 40~60 r / min) and nitrogen bubbling (flow rate 0.8~1.0 m³ / min). 3 Add 5%~10% dilute hydrochloric acid (by mass), with the amount of dilute hydrochloric acid added controlled according to the molar ratio of copper catalyst to sulfuric acid of 1:1.2~1:1.5; leaching for 1~2 hours, during which the copper ion concentration is measured through the sampling port. When the copper ion concentration is stable (change ≤0.1g / L), the leaching is considered complete. Step 3: Pressure filtration and sponge copper extraction Turn off the agitator 3 and nitrogen, and pump the reacted solid-liquid mixture to the first filter press 9 for solid-liquid separation. The separated filtrate (containing copper ions and metalloid chlorides) is sent to the sponge copper extraction tank, and iron filings (molar ratio of iron filings to copper ions 1.1~1.2:1) are added to carry out a displacement reaction to generate sponge copper (copper purity ≥98%). The sponge copper product is obtained by filtration through the second filter press 13, and the filtrate is treated as wastewater. The filter cake (solid waste) obtained from the first filter press 9 is sampled and tested for copper content. Step 4: Secondary copper extraction and neutralization with solid waste If the copper content of the filter cake in step 3 is >0.5%, the filter cake is sent to the mixing tank 14 for secondary copper extraction. Dilute hydrochloric acid is added and mixed at a solid-liquid ratio of 1:4 to 1:6. After stirring and leaching for 1 to 1.5 hours, the filter cake is filtered again through the first filter press 9 until the copper content of the filter cake is ≤0.5%. The qualified filter cake is sent to the solid waste storage 12. Calcium oxide powder is added at 5% to 10% of the filter cake mass. The mixture is stirred until the pH of the filter cake is 6 to 8. The neutralized solid waste is then handed over to a qualified unit for disposal. The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of this utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claims. The scope of protection of this utility model is defined by the appended claims and their equivalents.

Claims

1. An integrated treatment system for organosilicon waste catalysts, characterized in that, It includes a hydrolysis tank, a gas distributor is installed at the bottom of the hydrolysis tank, an agitator is installed above the hydrolysis tank, and an exhaust pipe is connected to the top of the hydrolysis tank; the outlet of the nitrogen pipeline is connected to the inlet of the gas distributor via a pipe; the outlet of the waste catalyst conveying pipeline is connected to the inlet of the hydrolysis tank; the outlet of the dilute hydrochloric acid pipeline and the outlet of the water conveying pipeline are both connected to the inlet of the hydrolysis tank; the outlet of the hydrolysis tank is connected to the inlet of the first filter press; the outlet of the first filter press is connected to the inlet of the sponge copper tank; the outlet of the iron powder silo is connected to the inlet of the sponge copper tank; the outlet of the first filter press is connected to the inlet of the solid waste storage; and the outlet of the sponge copper tank is connected to the inlet of the second filter press.

2. The integrated treatment system for organosilicon waste catalyst according to claim 1, characterized in that, The gas distributor adopts a multi-group concentric ring pipe structure, and several gas outlet holes are opened at the bottom of the gas distributor facing the hydrolysis tank. Adjacent concentric ring pipes are connected by connecting pipes.

3. The integrated treatment system for organosilicon waste catalyst according to claim 2, characterized in that, The spacing between adjacent air outlets is 180-380mm, and the diameter of the air outlet is 1-3mm.

4. The integrated treatment system for organosilicon waste catalyst according to claim 1, characterized in that, It also includes a mixing tank, the outlet of the solid waste storage is connected to the inlet of the mixing tank, the outlet of the dilute hydrochloric acid pipeline is connected to the inlet of the mixing tank, and the outlet of the mixing tank is connected to the inlet of the first filter press.

5. The integrated treatment system for organosilicon waste catalyst according to claim 1, characterized in that, It also includes a calcium oxide silo, the outlet of which is connected to the inlet of the solid waste storage facility.

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