Waste tert-butyl lithium treatment system

Abstract

The utility model relates to the technical field of hazardous waste treatment, and particularly discloses a waste tert-butyl lithium treatment system which comprises an inert gas supply device, a reaction frame, a combustion device and a recovery device, a reagent bottle is placed on the reaction frame, the reagent bottle is connected with the inert gas supply device, the reagent bottle is connected with a feeding port of the combustion device through a material conveying pipe, and the height of the material conveying pipe in the reagent bottle is adjustable; a plurality of layers of fire-retardant nets are arranged above the feeding hole in the combustion device; the mesh density of the lower layer of fire-retardant net is greater than that of the upper layer of fire-retardant net; the top of the combustion device is connected with an exhaust device; a discharge port is formed in the bottom of the combustion device and is connected with the recovery device; and the combustion device is also connected with an air supply device. The waste tert-butyl lithium treatment device can be well used for treating waste tert-butyl lithium, the treatment cost is reduced, the operation convenience and safety are improved, and the lithium element is fully recycled.

Description

Technical Field

[0001] The utility model relates to the technical field of hazardous waste treatment, in particular to a waste tert-butyl lithium disposal system. Background Art

[0002] Tert-butyl lithium is an important organic lithium compound, mainly used in the polymer industry. Tert-butyl lithium is a colorless, flammable liquid with strong reducing properties and metal activity. It is usually used as a strong base reagent and reducing agent in organic synthesis, or used to generate carbon anions. Due to its high activity and flammability, special attention should be paid to safety when using it. Waste butyl lithium is easily generated during the production, use and storage of tert-butyl lithium, and since fires and explosions caused by tert-butyl lithium are not uncommon, the disposal of waste tert-butyl lithium has always been a problem that has plagued researchers.

[0003] In the prior art, the common treatment of waste tert-butyl lithium is either to react tert-butyl lithium with tetrahydrofuran, ethanol and other chemical reagents under air-tight and ice-bath conditions below 0°C, and then quench the reaction, and discharge it after the properties are stable. This treatment method is suitable for the case where the amount of waste tert-butyl lithium is small; or when the amount of waste tert-butyl lithium is large, special cold chain transportation equipment is used, and a special hazardous waste disposal center is used for disposal using a special transportation workshop for hazardous chemicals. The Chinese patent with publication number CN212618353 U discloses a waste n-butyl lithium device, which mainly treats n-butyl lithium under nitrogen environment conditions. However, its operation is complicated, the safety is not high, it cannot be fully treated, and the lithium element cannot be effectively recovered. Therefore, the utility model aims to provide a safer, more effective and resource-based waste tert-butyl lithium chemical reagent disposal system. Utility Model Content

[0004] The technical problem solved by the utility model is to provide a waste tert-butyl lithium disposal system which is safe, environmentally friendly, easy to operate and can recover lithium elements.

[0005] The technical problem solved by the utility model is achieved by the following technical solutions:

[0006] A waste tert-butyl lithium disposal system comprises an inert gas supply device, a reaction rack, a combustion device and a recovery device; a reagent bottle is placed on the reaction rack, the reagent bottle is connected to the inert gas supply device, the reagent bottle is connected to the feed port of the combustion device through a feed pipe, and the height of the feed pipe in the reagent bottle is adjustable; a multi-layer fire-blocking net is arranged above the feed port in the combustion device, and the mesh density of the lower fire-blocking net is greater than the mesh density of the upper fire-blocking net; the top of the combustion device is connected to the exhaust device; a discharge port is arranged at the bottom of the combustion device, and the discharge port is connected to the recovery device; the combustion device is also connected to a gas supply device.

[0007] Furthermore, the inert gas supply device includes a gas supply pipe, and the gas replenishment device includes a gas replenishment pipe, and regulating valves are provided on the gas supply pipe and the gas replenishment pipe.

[0008] Furthermore, the feed port is connected to the feed pipe, the feed pipe and the air supply pipe both extend into the combustion device, and the tail end of the air supply pipe is sleeved on the outside of the feed pipe.

[0009] Furthermore, the combustion device comprises a hollow columnar combustion chamber, and the combustion device is a corundum combustion device.

[0010] Furthermore, the ratio of the diameter to the height of the combustion device is in the range of 1:4 to 5.

[0011] Furthermore, in the combustion device, the mesh size of the lower fire-blocking net ranges from 30 to 35 meshes, the mesh size of the upper fire-blocking net ranges from 15 to 20 meshes, and the spacing between the lower fire-blocking net and the upper fire-blocking net is 5 to 10 cm.

[0012] Furthermore, the exhaust device includes an exhaust pipe and a water ring vacuum pump connected to the exhaust pipe.

[0013] A method for disposing of waste tert-butyl lithium, based on the waste tert-butyl lithium disposal system as described above, comprises the following steps:

[0014] Inert gas replacement: The reagent bottle contains waste tert-butyl lithium. Adjust the bottom of the feed pipe in the reagent bottle to be above the liquid surface. Turn on the inert gas supply device to replace the air in the treatment system.

[0015] Combustion treatment: adjust the bottom of the feed pipe in the agent bottle to be below the liquid level, open the air supply device, and allow the waste tert-butyl lithium to enter the combustion device for combustion; during the combustion process, adjust the inert gas supply device and the air supply device to keep the negative pressure in the combustion device at -10 to 0 Pa;

[0016] Exhaust gas discharge: exhaust gas after combustion is discharged through the exhaust device;

[0017] Lithium recovery: After the combustion is completed, continue the nitrogen replacement treatment, then clean the inside of the combustion device with water, collect the cleaning water and titrate it into the phosphoric acid solution to obtain lithium phosphate precipitation, and continue the evaporation treatment to obtain the lithium phosphate product.

[0018] Furthermore, at the beginning of the combustion process, the negative pressure of the exhaust device is adjusted to -45 to -55 Pa; as the combustion proceeds, the negative pressure of the exhaust device decreases, and when the difference between the negative pressure of the exhaust device and the negative pressure in the combustion device is stable and close, the combustion ends.

[0019] Furthermore, during the combustion process, the air supply device is controlled so that the actual air supply amount is 1.2 to 1.5 times the theoretical air supply amount. The air supply amount during the combustion process is extremely important. When the air supply amount is insufficient, the combustion is incomplete, and the generated lithium salt is easy to block the air outlet. When the air supply amount is too much, such as when the air supply amount is more than 2 times the theoretical air supply amount, the flame is easy to deform and split into several small fireballs, and the pressure distribution in the combustion device is affected, which poses a safety risk.

[0020] Furthermore, the collected cleaning water is configured into a lithium hydroxide solution with a concentration of 1.0-1.5 mol / L, and the lithium hydroxide solution is slowly added dropwise to a 2.5-3.5 mol / L phosphoric acid solution to obtain lithium phosphate precipitation. During the titration process, the phosphoric acid solution is maintained at 85-95° C. in a water bath, and the reaction is terminated when the system pH value is 7-8.

[0021] Beneficial effects: The waste tert-butyl lithium disposal system described in the utility model can be well used for the technical treatment of waste tert-butyl lithium. The system has low purchase and installation costs, is easy to operate, and the nodes are easy to control, and has a good prospect for promotion and application.

[0022] In the waste tert-butyl lithium disposal system described in the utility model, a unique setting is used to make the reaction process control and endpoint judgment simpler, and the safety risks and incomplete combustion caused by the dispersion and irregular movement of the tert-butyl lithium flame can be prevented during the combustion process.

[0023] Compared with the treatment system that strictly controls sub-zero reaction conditions and requires a large amount of tetrahydrofuran, ethanol and hydrogen chloride reagent consumption, the method for disposing of waste tert-butyl lithium described in the utility model has mild reaction conditions, lower reagent costs, and can obtain a single lithium salt product while being more environmentally friendly, and has lower production costs and better economic value.

[0024] The method for disposing waste tert-butyl lithium described in the utility model can fully treat the waste tert-butyl lithium and obtain lithium phosphate products with stable and safe properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a structural schematic diagram of a preferred embodiment of the utility model.

[0026] Figure 2 for Figure 1 Schematic diagram of the enlarged structure of part A.

[0027] Among them: 1. Inert gas supply device; 2. Reaction rack; 3. Reagent bottle; 4. Combustion device; 5. Water ring vacuum pump; 6. Air supply pipe; 7. Air supply pipe; 8. Feed pipe; 9. Feed inlet; 10. Lower fire-blocking net; 11. Upper fire-blocking net; 12. Exhaust pipe; 13. Recovery device. DETAILED DESCRIPTION

[0028] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further described below with reference to specific illustrations.

[0029] like Figure 1 The waste tert-butyl lithium disposal system shown includes an inert gas supply device 1, a reaction frame 2, a combustion device 4 and a recovery device 13.

[0030] The inert gas supply device 1 is preferably a nitrogen supply device, and the inert gas supply device 1 includes a gas supply pipe 6, on which a regulating valve is provided, and the regulating valve preferably includes a pressure reducing valve and a switch valve, so as to facilitate pressure control and switch control; a reagent bottle 3 is placed on the reaction rack 2, such as Figure 1 As shown, the reagent bottle 3 is fixed on the reaction rack 2, and the outside of the reagent bottle 3 is detachably fixedly connected to the reaction rack 2 through a clamp, so as to facilitate the replacement of different reagent bottles 3. The reagent bottle 3 is connected to the inert gas supply device 1, and the reagent bottle 3 is also connected to the feed port 9 of the combustion device 4 through a feed pipe 8, and the height of the feed pipe 8 in the reagent bottle 3 is adjustable. In the preferred scheme, the feed pipe 8 is preferably a hard feed pipe 8, and a rubber plug is provided on the top of the reagent bottle 3. The feed pipe 8 passes through the rubber plug on the top of the reagent bottle 3, and the rubber plug forms a clamping effect on the feed pipe 8, thereby preventing the feed pipe 8 from sliding freely after the height adjustment in the reagent bottle 3.

[0031] In a preferred embodiment, the combustion device 4 includes a hollow cylindrical combustion chamber, and the ratio of the combustion chamber diameter to the height is in the range of 1:4 to 5. The position of the feed port 9 of the combustion chamber is set so that the combustion time after feeding is greater than 2s to ensure sufficient combustion. The combustion device 4 is preferably a corundum combustion device 4. The top of the combustion device 4 is connected to an exhaust device, and the exhaust device includes an exhaust pipe 12 and a negative pressure device connected to the exhaust pipe 12. The negative pressure device is preferably a water ring vacuum pump; a discharge port is set at the bottom of the combustion device 4, and the discharge port is connected to the recovery device 13. The rising airflow generated by the flame of the combustion of the waste tert-butyl lithium and the negative pressure formed by the negative pressure device at the top keep the flame in a certain flame-upward long strip shape.

[0032] In a preferred embodiment, the combustion chamber is a transparent combustion chamber or has a transparent observation window.

[0033] like Figure 1As shown, a multi-layer fire-blocking net is arranged above the feed port 9 in the combustion device 4. The fire-blocking net is preferably arranged horizontally, and the fire-blocking net is detachably fixedly connected to the inner wall of the combustion device 4. The fire-blocking net has two layers, and both are steel wire meshes, wherein the mesh density of the lower fire-blocking net 10 is greater than the mesh density of the upper fire-blocking net 11; since the burning flame of the waste tert-butyl lithium is easily split into multiple drifting small fireballs during the combustion process, it is easy to escape everywhere, resulting in low safety and incomplete combustion. The setting of the fine lower fire-blocking net 10 can well adhere to the small fireballs and prevent the small fireballs from escaping, so that the tert-butyl lithium adheres to the steel wire mesh for full combustion, and the upper fire-blocking net 11 can further prevent the escaping flame from entering the subsequent pipeline, further ensuring the effect of full combustion. In a preferred embodiment, in the combustion device, the mesh size of the lower fire-blocking net 10 is in the range of 30-35 meshes, the mesh size of the upper fire-blocking net 11 is in the range of 15-20 meshes, and the distance between the lower fire-blocking net 10 and the upper fire-blocking net 11 is 5-10 cm.

[0034] The combustion device 4 is also connected to an air supply device, which includes an air supply pipe 7. A regulating valve is arranged on the air supply pipe 7. The regulating valve includes a switch valve and a flow valve for adjusting the air supply flow and size. The feed port 9 of the combustion device 4 is connected to the feed pipe. The feed pipe and the air supply pipe 7 both extend into the combustion device 4. Figure 2 As shown, the tail end of the air supply pipe 7 is sleeved outside the feed pipe, and the tail end of the feed pipe is longer than the air supply pipe 7. The setting of the air supply pipe 7 can well supplement air, which is conducive to ensuring the sufficiency of combustion, and can blow off the ignited waste gas tert-butyl lithium liquid from the pipe mouth of the feed pipe to prevent the generated lithium salt from clogging the pipe mouth, thereby ensuring the long-term high efficiency and stable operation of waste gas tert-butyl lithium recovery.

[0035] During use of the system, after combustion is completed, the inner wall of the combustion device and the fire-blocking net are cleaned with hot water, and the cleaning water is recovered through the recovery device 13.

[0036] As an improvement to the utility model, the recovery device can be connected to the titration device, or the recovery device can be subjected to a titration reaction treatment alone, and a lithium phosphate product is generated in the titration device, so that the lithium element is fully recovered.

[0037] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0038] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the present utility model, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0039] In the present utility model, unless otherwise clearly stipulated and limited, the terms such as "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense. For example, it 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, or it can be the internal connection of two elements.

[0040] The above contents are further detailed descriptions of the present invention in combination with specific implementation methods, and it cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, several simple deductions or substitutions can be made without departing from the concept of the present invention.

Claims

1. A waste tert-butyl lithium disposal system, It is characterized in that It comprises an inert gas supply device, a reaction frame, a combustion device and a recovery device; a reagent bottle is placed on the reaction frame, the reagent bottle is connected to the inert gas supply device, the reagent bottle is connected to the feed port of the combustion device through a feed pipe, and the height of the feed pipe in the reagent bottle is adjustable; a multi-layer fire-blocking net is arranged above the feed port in the combustion device, and the mesh density of the lower layer of the fire-blocking net is greater than the mesh density of the upper layer of the fire-blocking net; the top of the combustion device is connected to the exhaust device; a discharge port is arranged at the bottom of the combustion device, and the discharge port is connected to the recovery device; the combustion device is also connected to the air supply device.

2. The waste tert-butyl lithium disposal system according to claim 1, It is characterized in that The inert gas supply device comprises a gas supply pipe, and the gas replenishment device comprises a gas replenishment pipe. Both the gas supply pipe and the gas replenishment pipe are provided with regulating valves.

3. The waste tert-butyl lithium disposal system according to claim 2, It is characterized in that The feed port is connected to the feed pipe, the feed pipe and the air supply pipe both extend into the combustion device, and the tail end of the air supply pipe is sleeved on the outside of the feed pipe.

4. The waste tert-butyl lithium disposal system according to claim 1, It is characterized in that The combustion device comprises a hollow columnar combustion chamber, and the combustion device is a corundum combustion device.

5. The waste tert-butyl lithium disposal system according to claim 4, It is characterized in that The ratio of the diameter to the height of the combustion device is in the range of 1:4-5.

6. The waste tert-butyl lithium disposal system according to claim 1, It is characterized in that In the combustion device, the mesh aperture of the lower fire-blocking net ranges from 30 to 35 meshes, the mesh aperture of the upper fire-blocking net ranges from 15 to 20 meshes, and the distance between the lower fire-blocking net and the upper fire-blocking net is 5 to 10 cm.

7. The waste tert-butyl lithium disposal system according to claim 1, It is characterized in that The exhaust device comprises an exhaust pipe and a water ring vacuum pump connected to the exhaust pipe.

Images