Energy-saving and environment-friendly treatment process for dangerous waste liquid generated in preparation of trimethyl aluminum and microreactor

Abstract

The invention belongs to the technical field of waste liquid treatment, and particularly relates to an energy-saving and environment-friendly treatment process and a microreactor for dangerous waste liquid generated in preparation of trimethylaluminum, and the microreactor comprises a reaction kettle, a filling assembly and a transmission assembly; the filling assembly comprises a sliding sleeve, a liquid injection piece and a water injection piece, and the transmission assembly is installed on the filling assembly. In the process of pushing the water injection piece to move towards the outside of the sliding sleeve through the cam, a small amount of pure water is injected into the reaction kettle through the small-capacity liquid storage cavity, instant excessive contact of reactants can be avoided, explosive release of heat and hydrogen is reduced, and the risk of liquid splashing is reduced; along with the reaction of water in the small-capacity liquid storage cavity and waste liquid, the concentration of trimethyl aluminum is gradually reduced; under the action of a cam, pure water in a large-capacity liquid storage cavity is injected into the reaction kettle, and a large amount of water is injected into the reaction kettle through the large-capacity liquid storage cavity, so that thorough reaction is ensured, explosive release of heat and hydrogen is further reduced, and the treatment safety is improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of waste liquid treatment, and particularly relates to an energy-saving and environment-friendly treatment process for hazardous waste liquid prepared from trimethylaluminum and a micro-reactor. BACKGROUND

[0002] Trimethylaluminum is an important organic aluminum compound and is widely used in the fields of semiconductor thin film deposition and olefin polymerization catalysis, and is usually prepared by Grignard reagent method or aluminum powder-sodium reduction method. During the preparation of trimethylaluminum, hazardous waste liquid is left in the reaction kettle, which mainly contains hydrocarbon solvents, sodium chloride byproducts, aluminum powder, a small amount of trimethylaluminum, and trace amounts of metallic sodium and other chemical components. The waste liquid needs to be discharged after treatment.

[0003] Trimethylaluminum in the waste liquid reacts violently with water. By injecting water into the waste liquid, trimethylaluminum in the waste liquid reacts with water to generate aluminum hydroxide and methane, thereby inactivating the waste liquid. Other substances in the waste liquid are separated out through multiple filtration processes, thereby achieving treatment of the waste liquid.

[0004] In the waste liquid treatment process, the following technical problems exist. Since trimethylaluminum reacts violently with water, if a large amount of water is injected at one time, the two substances will fully contact at the moment, the reaction will be violent, a large amount of hydrogen gas and heat will be generated rapidly, and liquid splashing and local overheating may occur, which poses a high safety risk. SUMMARY

[0005] The present application aims to solve the technical problems in the prior art by providing an energy-saving and environment-friendly treatment process for hazardous waste liquid prepared from trimethylaluminum and a micro-reactor.

[0006] The technical problems can be solved by the following technical solution. An energy-saving and environment-friendly treatment micro-reactor for hazardous waste liquid prepared from trimethylaluminum comprises a reaction kettle, a fixed plate fixedly installed on the reaction kettle, an injection assembly placed on the fixed plate, a water injection pipe and a liquid injection pipe connected to the injection assembly, a liquid outlet installed at the bottom of the reaction kettle, and a gas outlet installed at the top of the reaction kettle. The injection assembly comprises a sliding sleeve, a liquid injection member and a water injection member slidingly installed on both sides of the sliding sleeve, the water injection pipe is connected to the water injection member, the liquid injection pipe is connected to the liquid injection member, the water injection member and the liquid injection member are connected to the sliding sleeve through springs, a transmission assembly is installed on the injection assembly, the transmission assembly comprises a cam, and the cam is rotated to sequentially drive the liquid injection member and the water injection member to move outward from the sliding sleeve. The water injection member is internally provided with a small-capacity liquid storage cavity, a large-capacity liquid storage cavity, and a standby cavity, and the water injection pipe injects pure water into the small-capacity liquid storage cavity and the large-capacity liquid storage cavity.

[0007] As a further optimization or improvement of this solution, the filling component also includes a cylinder, a screw is fixedly installed on the water injection component, the output end of the cylinder is connected to a push plate, and the push plate is connected to a sliding plate through a spring; a sliding groove is opened on the side wall of the large-capacity liquid storage chamber near the spare chamber, a liquid delivery box is slidably installed inside the sliding groove, a through hole is opened at the bottom of the liquid delivery box, a perforated plate is slidably installed on the liquid delivery box, and the perforated plate is connected to the sliding plate through a push rod.

[0008] As a further optimization or improvement of this solution, an electromagnetic chuck is installed on the push plate, and a magnetic block is installed on the slide plate, with the electromagnetic chuck adsorbing the magnetic block; a rubber pad is installed on the inner wall of the slide, and there is sliding damping between the liquid delivery box and the slide.

[0009] As a further optimization or improvement of this solution, the transmission assembly also includes a motor 1 and a motor 2 installed on the top of the reactor. The output ends of motor 1 and motor 2 are respectively equipped with a driving gear 1 and a driving gear 2. A rotating shaft is rotatably installed on the reactor. A driven gear, a sun gear, and a cam are coaxially installed on the rotating shaft. The driven gear meshes with the driving gear 2. An internal gear ring is installed on the top of the sliding sleeve. The sun gear is located inside the internal gear ring. A planetary gear is connected between the sun gear and the internal gear ring. The driven gear ring is connected to the planetary gear and meshes with the driving gear 1.

[0010] As a further optimization or improvement of this solution, an adjusting block is installed inside the injection component, and a drive connecting screw is connected to the injection component, with the screw connected to the adjusting block.

[0011] As a further optimization or improvement to this solution, a volume scale is installed on the injection component, and an indicator scale is installed on the adjustment block.

[0012] An energy-saving and environmentally friendly process for treating hazardous waste liquid prepared from trimethylaluminum, wherein the process is applied to the microreactor described above, and the process includes the following steps: Step S1: The waste liquid is transported to the liquid injection unit through the liquid injection pipe, and then the waste liquid is transported to the reaction vessel through the liquid injection unit. Next, pure water is transported to the water injection unit through the water injection pipe, and then the pure water is transported to the reaction vessel through the water injection unit. The waste liquid and water undergo a violent chemical reaction in the reaction vessel. Step S2: The waste liquid reacts violently with water, i.e., deactivation treatment. The deactivated liquid after the mixed reaction is sent to the deactivation collection tank through the drain port. The hydrogen and methane produced in the reaction are introduced into the exhaust port. When the gas passes through the combustion structure at the end of the exhaust port, the hydrogen and methane are burned and then discharged. Step S3: The deactivation liquid inside the deactivation collection tank is separated from the organic solvent and hydrocarbon solvent by oil-water separation technology. After the organic solvent is purified, it is recycled back to the process of preparing trimethylaluminum for use. Step S4: the waste liquid after oil-water separation is sent into a solid-liquid separation tank, and the aluminum hydroxide in the waste liquid is separated out through a solid-liquid separation technology, at this time, the mixed liquid is mainly sodium chloride aqueous solution; Step S5: the sodium chloride aqueous solution is sent into an evaporation device, and pure water and sodium chloride are obtained through evaporation, the pure water is connected to a water feeding pipe and recycled to the reaction kettle to participate in the inactivation treatment of the waste liquid.

[0013] The beneficial effects of the present application are as follows: (1) In the process of moving the water injection part to the outside of the sliding sleeve by the cam, the pure water in the small-capacity liquid storage cavity is sent into the reaction kettle to react with the waste liquid, a small amount of pure water is added to the reaction kettle through the small-capacity liquid storage cavity, which can avoid the instantaneous excessive contact of reactants, reduce the explosive release of heat and hydrogen, and reduce the risk of liquid splashing; as the water in the small-capacity liquid storage cavity reacts with the waste liquid, the concentration of trimethylaluminum gradually decreases, and the reactivity of the waste liquid decreases; then, under the action of the cam, the pure water in the large-capacity liquid storage cavity is injected into the reaction kettle, a large amount of water is added to the reaction kettle through the large-capacity liquid storage cavity, at this time, the low-concentration trimethylaluminum in the waste liquid reacts with water, which ensures that the reaction is complete and further reduces the explosive release of heat and hydrogen, thereby improving the safety of the treatment.

[0014] (2) The small amount of pure water in the small-capacity liquid storage cavity reacts with the waste liquid in the reaction kettle, the reaction intensity is judged by observing the bubble generation speed and temperature change; if the reaction is intense, the pure water in the large-capacity liquid storage cavity is sent into the standby cavity through the liquid feeding box, the amount of pure water in the large-capacity liquid storage cavity is reduced, a small amount of pure water is injected into the reaction kettle through the large-capacity liquid storage cavity, the reaction intensity of the waste liquid is reduced, and the risk of liquid splashing is reduced. The present application adds a small amount of pure water to the small-capacity liquid storage cavity to test the reactivity, then adjusts the amount of pure water in the large-capacity liquid storage cavity through the liquid feeding box, avoids the intense reaction of the waste liquid, and improves the safety of the treatment process. BRIEF DESCRIPTION OF DRAWINGS

[0015] The present application will be further described below with reference to the accompanying drawings.

[0016] Figure 1 The present application is a schematic diagram of the overall structure.

[0017] Figure 2 The present application is a schematic diagram of the internal structure of the reaction kettle.

[0018] Figure 3 The present application is a schematic diagram of the connection structure of the transmission assembly and the injection assembly.

[0019] Figure 4 The present application is a schematic diagram of the transmission connection between the transmission assembly and the injection assembly.

[0020] Figure 5 The present application is an exploded view of the overall structure of the transmission assembly.

[0021] Figure 6 is a schematic view of the internal structure of the filling assembly.

[0022] Figure 7 is a sectional view of the overall structure of the filling assembly.

[0023] Figure 8 is a schematic view of the structure of the liquid filling member.

[0024] Figure 9 is a schematic view of the positions where the small-capacity liquid storage cavity, the large-capacity liquid storage cavity and the standby cavity are formed.

[0025] Figure 10 is Figure 9 is an enlarged view of the structure of part A.

[0026] Figure 11 is a schematic view of the connection structure of the orifice plate and the liquid delivery box.

[0027] Figure 12 is a schematic view of the structure of Example Three.

[0028] Figure 13 is a process diagram of the waste liquid treatment of the present application.

[0029] indicated as: 1, reaction kettle; 2, liquid discharge port; 3, gas discharge port; 4, water filling pipe; 5, liquid filling pipe; 6, fixed plate; 7, filling assembly; 701, sliding sleeve; 702, liquid filling member; 703, water filling member; 704, spring one; 705, volume scale; 706, adjusting block; 707, screw rod; 708, indicating scale; 709, small-capacity liquid storage cavity; 710, large-capacity liquid storage cavity; 711, standby cavity; 712, sliding chute; 713, liquid delivery box; 714, orifice plate; 715, push rod; 716, sliding plate; 717, air cylinder; 718, push plate; 719, magnetic suction block; 720, electromagnetic suction disc; 721, spring two; 8, transmission assembly; 801, motor one; 802, motor two; 803, driven gear two; 804, driven gear one; 805, rotating shaft; 806, driven gear ring; 807, inner gear ring; 808, planetary gear; 809, sun gear; 810, cam; 811, driven gear; 9, liquid storage bag; 10, liquid pressing plate. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0031] Embodiment one, see Figures 1-11 The application discloses a micro-reactor for energy-saving and environment-friendly treatment of trimethylaluminum hazardous waste liquid, which comprises a reaction kettle 1, a fixed plate 6 fixedly installed on the reaction kettle 1, a filling assembly 7 placed on the fixed plate 6, a water filling pipe 4 and a liquid filling pipe 5 communicated with the filling assembly 7 respectively, a liquid outlet 2 installed at the bottom of the reaction kettle 1 and a gas outlet 3 installed at the top of the reaction kettle 1; the filling assembly 7 comprises a sliding sleeve 701, a liquid injection part 702 and a water injection part 703 slidingly installed on the two sides of the sliding sleeve 701 respectively, the water filling pipe 4 is communicated with the water injection part 703, the liquid filling pipe 5 is communicated with the liquid injection part 702, the water injection part 703 and the liquid injection part 702 are connected with the sliding sleeve 701 through springs 704 respectively, a transmission assembly 8 is installed on the filling assembly 7, the transmission assembly 8 comprises a cam 810, and the liquid injection part 702 and the water injection part 703 are driven to move outwardly of the sliding sleeve 701 in sequence through rotation of the cam 810; a small-capacity liquid storage cavity 709, a large-capacity liquid storage cavity 710 and a standby cavity 711 are arranged in the water injection part 703 respectively, and the water filling pipe 4 is used for injecting pure water into the small-capacity liquid storage cavity 709 and the large-capacity liquid storage cavity 710.

[0032] Specifically, the filling assembly 7 further comprises a gas cylinder 717, a screw rod 707 is fixedly installed on the water injection part 703, a push plate 718 is connected with the output end of the gas cylinder 717, and the push plate 718 is connected with a sliding plate 716 through a spring 721; a sliding groove 712 is formed in the side wall of the large-capacity liquid storage cavity 710 close to one end of the standby cavity 711, a liquid sending box 713 is slidingly installed in the sliding groove 712, a through hole is formed in the bottom of the liquid sending box 713, a hole plate 714 is slidingly installed on the liquid sending box 713, and the hole plate 714 is connected with the sliding plate 716 through a push rod 715.

[0033] Specifically, an electromagnetic suction disc 720 is installed on the push plate 718, a magnetic suction block 719 is installed on the sliding plate 716, and the electromagnetic suction disc 720 adsorbs the magnetic suction block 719; a rubber pad is installed on the inner wall of the sliding groove 712, and the liquid sending box 713 and the sliding groove 712 have sliding damping.

[0034] It should be noted that the water filling pipe 4 is communicated with pure water, and the liquid filling pipe 5 is communicated with hazardous waste liquid.

[0035] The application has the advantages that the small-capacity liquid storage cavity 709, the large-capacity liquid storage cavity 710 and the liquid injection part 702 are filled with water and waste liquid through the water filling pipe 4 and the liquid filling pipe 5 respectively, the liquid injection part 702 and the water injection part 703 are driven to move outwardly of the sliding sleeve 701 through rotation of the cam 810 driven by the rotation of the driving gear 802, the screw rod 707 is driven to rotate and move outwardly of the water injection part 703 through the rotation of the cam 810, the liquid sending box 713 is driven to move outwardly of the sliding groove 712 through the rotation of the cam 810, the liquid sending box 713 is driven to move outwardly of the sliding groove 712 through the rotation of the cam 810, and the liquid injection part 702 is driven to move outwardly of the sliding sleeve 701 through the rotation of the cam 810. Figure 5For example, the cam 810 rotates clockwise, the cam 810 first pushes the liquid injection part 702 to move to the outside of the sliding sleeve 701, and the waste liquid inside the liquid injection part 702 is sent into the reaction kettle 1; as the cam 810 continues to rotate, the cam 810 pushes the water injection part 703 to move to the outside of the sliding sleeve 701, and as the water injection part 703 moves, the pure water in the small-capacity liquid storage cavity 709 is sent into the reaction kettle 1 to react with the waste liquid, and a small amount of pure water is added to the reaction kettle 1 through the small-capacity liquid storage cavity 709, which can avoid the instantaneous excessive contact of the reactants, reduce the explosive release of heat and hydrogen, and reduce the risk of liquid splashing; as the water in the small-capacity liquid storage cavity 709 reacts with the waste liquid, the concentration of trimethylaluminum gradually decreases, and the reactivity of the waste liquid decreases; then under the action of the cam 810, the pure water in the large-capacity liquid storage cavity 710 is injected into the reaction kettle 1, a large amount of water is added to the reaction kettle 1 through the large-capacity liquid storage cavity 710, and at this time the low-concentration trimethylaluminum in the waste liquid reacts with water, which ensures that the reaction is thorough and further reduces the explosive release of heat and hydrogen, thereby improving the safety of the treatment.

[0036] Another use method; the present application reacts a small amount of pure water in the small-capacity liquid storage cavity 709 with the waste liquid in the reaction kettle 1, and judges the reaction intensity by observing the bubble generation speed and temperature change; if the reaction is slow, then a large amount of pure water is added to the reaction kettle 1 through the large-capacity liquid storage cavity 710; if the reaction is intense, at this time the electromagnetic suction plate 720 is powered on, the electromagnetic suction plate 720 attracts the electromagnetic suction plate 720 on the sliding plate 716, and then drives the sliding plate 716 to move close to the push plate 718, the sliding plate 716 drives the hole plate 714 to slide to the inside of the liquid sending box 713 through the push rod 715, so that the through hole on the hole plate 714 is out of position with the through hole at the bottom of the liquid sending box 713, as the cylinder 717 drives the sliding plate 716 to move, the sliding plate 716 pushes the liquid sending box 713 to move to the inside of the standby cavity 711 through the hole plate 714, then the electromagnetic suction plate 720 is disconnected, the sliding plate 716 is reset under the action of the spring two 721, at this time the sliding plate 716 drives the hole plate 714 to move to the outside of the liquid sending box 713, so that the through hole on the hole plate 714 is coincided with the through hole at the bottom of the liquid sending box 713, and the pure water in the liquid sending box 713 is sent into the standby cavity 711, reducing the amount of pure water in the large-capacity liquid storage cavity 710, and injecting a small amount of pure water into the reaction kettle 1 through the large-capacity liquid storage cavity 710, reducing the reaction intensity of the waste liquid, and reducing the risk of liquid splashing.

[0037] The present application adds a small amount of pure water to the small-capacity liquid storage cavity 709 to test the reaction activity, and then adjusts the amount of pure water in the large-capacity liquid storage cavity 710 through the liquid sending box 713, so as to avoid the violent reaction of the waste liquid and improve the safety of the treatment process. A temperature sensor and a sensor can be installed in the reaction kettle 1 to detect the bubble generation speed and temperature change during the reaction process, and then automatically judge the reaction intensity.

[0038] It should be noted that, since the waste liquid contains hydrocarbon organic solvent, after the waste liquid is injected into the reaction kettle 1, the oil liquid is prone to stratification, which affects the reaction process, therefore, the stirring assembly is installed at the bottom of the fixed plate 6, which is used for stirring the mixed waste liquid, so as to avoid the stratification phenomenon.

[0039] Referring to Figure 8 The liquid injection piece 702 is internally provided with an adjusting block 706, and a screw rod 707 is connected to the liquid injection piece 702, and the screw rod 707 is connected to the adjusting block 706.

[0040] Specifically, the liquid injection piece 702 is provided with a volume scale 705, and the adjusting block 706 is provided with an indicating scale 708.

[0041] It should be noted that, in use, the position of the adjusting block 706 is adjusted through the screw rod 707, and then the volume of the liquid injection piece 702 is adjusted.

[0042] In the second embodiment, referring to Figures 4-11 The transmission assembly 8 further comprises a motor one 801 and a motor two 802 installed at the top of the reaction kettle 1, and the output ends of the motor one 801 and the motor two 802 are respectively provided with a driving gear one 804 and a driving gear two 803; the reaction kettle 1 is rotatably provided with a rotating shaft 805, and the rotating shaft 805 is coaxially provided with a driven gear 811, a sun gear 809 and a cam 810; the driven gear 811 is engaged with the driving gear two 803; the top of the sliding sleeve 701 is provided with an inner ring gear 807, and the sun gear 809 is located inside the inner ring gear 807; the sun gear 809 and the inner ring gear 807 are drivingly connected with a planetary gear 808, and the driven gear ring 806 is connected with the planetary gear 808, and the driven gear ring 806 is engaged with the driving gear one 804.

[0043] It should be noted that the rotating shaft 805 is coaxially provided with the driven gear 811, the sun gear 809 and the cam 810 from top to bottom, and the motor two 802 drives the rotating shaft 805 and the cam 810 to rotate through the engagement of the driven gear 811 and the driving gear two 803; the planetary gear 808 is connected with the driven gear ring 806, and the motor one 801 drives the planetary gear 808 to rotate through the engagement of the driven gear ring 806 and the driving gear one 804. The inner ring gear 807, the planetary gear 808 and the sun gear 809 form a planetary gear set, and when the motor one 801 drives the driven gear ring 806 to rotate, the driven gear ring 806 drives the rotating shaft 805 and the cam 810 to move at a reduced speed through the planetary gear 808.

[0044] The application drives the liquid injection part 702 to move to the outside of the sliding sleeve 701 by the motor two 802 driving the cam 810, so as to realize the delivery of the waste liquid; the water injection part 703 is pushed to move to the outside of the sliding sleeve 701 by the motor two 802 driving the cam 810, so as to realize the delivery of the pure water; since the motor two 802 drives the cam 810 to move at a reduced speed, the pure water injection speed of the water injection part 703 is reduced, so that the pure water is not injected too fast, the reaction is not accelerated sharply in a short time, a large amount of hydrogen gas is not generated and accumulated rapidly, and the huge heat released by the reaction cannot be dissipated in time, so that the system pressure is suddenly increased, and explosion is caused.

[0045] It should be noted that the motor one 801 and the motor two 802 are connected with the driving gear one 804 and the driving gear two 803 respectively through the one-way transmission structure, for example, the ratchet structure. Advantage one: since the motor one 801 and the motor two 802 are alternately operated, when the motor two 802 drives the rotating shaft 805 to rotate through the driving gear two 803, the rotating shaft 805 does not interfere with the motor one 801; the same is true when the motor one 801 operates. Advantage two: the motor one 801 drives the rotating shaft 805 and the cam 810 to move clockwise through the ratchet structure, so that the motor one 801 preferentially pushes the liquid injection part 702, and then pushes the water injection part 703, so as to ensure that the waste liquid is injected first, then the pure water is injected, and then the water is injected, so that the water is not excessive, the reaction intensity of the trimethylaluminum and water is controlled; the motor one 801 cannot drive the cam 810 to rotate counterclockwise through the ratchet structure, so that the water is not injected first, then the waste liquid is injected, the water is excessive, and then when the trimethylaluminum is dropped into the water, the excessive water contacts the trimethylaluminum, so that the reaction is sharply caused instantaneously, a large amount of bubbles (hydrogen gas) is generated, and the safety hidden danger in the experiment or production is increased.

[0046] Example three, see Figure 12 The difference from the above-mentioned example two is that the pure water is injected into the liquid storage bag 9, the liquid discharge pipe of the liquid storage bag 9 is directed to the bottom of the reaction kettle 1, the liquid storage bag 9 is extruded by the liquid pressing plate 10 driven by the motor two 802 driving the cam 810, so as to realize the delivery of the pure water, and since the motor two 802 drives the cam 810 to move at a reduced speed, the injection speed of the pure water in the liquid storage bag 9 is reduced.

[0047] Please refer to Figure 1 , Figure 2 and Figure 13 , the application is a kind of trimethylaluminum preparation hazardous waste liquid energy saving and environmental protection processing technology, the process is applied to the microreactor as described in the above-mentioned example, the process comprises the following steps: Step S1: the waste liquid is delivered to the liquid injection part 702 through the liquid inlet pipe 5, then the waste liquid is delivered to the reaction kettle 1 by the liquid injection part 702, then the pure water is delivered to the water injection part 703 through the water inlet pipe 4, and then the pure water is delivered to the reaction kettle 1 by the water injection part 703, and the waste liquid and water react sharply in the reaction kettle 1. Step S2: the waste liquid and water react violently, i.e. deactivation treatment, the mixed reaction deactivation liquid is sent into the deactivation collection tank through the liquid outlet 2, the hydrogen and methane generated in the reaction are discharged through the exhaust port 3, when the gas passes through the combustion structure at the end of the exhaust port 3, the hydrogen and methane are combusted and discharged; Step S3: the deactivation liquid in the deactivation collection tank is separated from the organic solvent hydrocarbon solvent by oil-water separation technology, the organic solvent is purified and treated, and then recycled to the process of preparing trimethyl aluminum for use; Step S4: the waste liquid after oil-water separation is sent into the solid-liquid separation tank, and the aluminum hydroxide is separated out by solid-liquid separation technology, at this time, the mixed liquid is mainly sodium chloride aqueous solution; Step S5: the sodium chloride aqueous solution is sent into the evaporation equipment, pure water and sodium chloride are obtained by evaporation, the pure water is connected to the water inlet pipe 4, and then recycled to the reaction kettle 1 to participate in the deactivation treatment of the waste liquid.

[0048] The above shows and describes the basic principles, main features and advantages of the present application. It should be understood by those skilled in the art that the present application is not limited to the above embodiments, and the above embodiments and descriptions in the specification are only to illustrate the principles of the present application, and various changes and improvements can be made without departing from the spirit and scope of the present application, and these changes and improvements all fall within the scope of the present application.

Claims

1. A microreactor for the energy-saving and environmentally friendly treatment of hazardous waste liquid prepared from trimethylaluminum, characterized in that: The utility model provides a kind of reaction kettle, comprising reaction kettle (1), reaction kettle (1) is fixedly installed fixed plate (6), fixed plate (6) is placed and fills component (7), and fills component (7) respectively communicates water pipe (4) and liquid pipe (5), reaction kettle (1) bottom installs liquid outlet (2), top installs exhaust port (3); The filling component (7) includes a sliding sleeve (701), and the sliding sleeve (701) is slidably installed with a liquid injection member (702) and a water injection member (703) on both sides, respectively; the water pipe (4) is connected to the water injection member (703), and the liquid pipe (5) is connected to the liquid injection member (702); the water injection member (703) and the liquid injection member (702) are connected to the sliding sleeve (701) through a spring (704), respectively; a transmission assembly (8) is installed on the filling component (7), and the transmission assembly (8) includes a cam (810); the cam (810) is rotated to drive the liquid injection member (702) and the water injection member (703) to move outwardly from the sliding sleeve (701) in sequence.

2. The trimethylaluminum preparation hazardous waste liquid energy-saving and environmentally friendly treatment microreactor according to claim 1, characterized in that: The water injection member (703) is internally provided with a small-capacity liquid storage cavity (709), a large-capacity liquid storage cavity (710), and a standby cavity (711), respectively; and the water pipe (4) injects pure water into the small-capacity liquid storage cavity (709) and the large-capacity liquid storage cavity (710).

3. The trimethylaluminum preparation hazardous waste liquid energy-saving and environmentally friendly treatment micro-reactor according to claim 2, characterized in that: The filling component (7) further includes a pneumatic cylinder (717), and the water injection member (703) is fixedly installed with a screw rod (707); the output end of the pneumatic cylinder (717) is connected to a push plate (718); and the push plate (718) is connected to a sliding plate (716) through a spring (721).

4. The trimethylaluminum preparation hazardous waste liquid energy-saving and environmentally friendly treatment microreactor according to claim 1, characterized in that: A sliding groove (712) is formed on the side wall of the large-capacity liquid storage cavity (710) near one end of the standby cavity (711); a liquid delivery box (713) is slidably installed in the sliding groove (712); a through hole is formed in the bottom of the liquid delivery box (713); a hole plate (714) is slidably installed on the liquid delivery box (713); and the hole plate (714) is connected to the sliding plate (716) through a push rod (715). An electromagnetic suction disc (720) is installed on the push plate (718), and a magnetic suction block (719) is installed on the sliding plate (716); the electromagnetic suction disc (720) is used to adsorb the magnetic suction block (719); a rubber pad is installed on the inner wall of the sliding groove (712); and the liquid delivery box (713) and the sliding groove (712) have sliding damping. The transmission assembly (8) further includes a motor (801) and a motor (802) installed on the top of the reaction kettle (1); the output ends of the motor (801) and the motor (802) are installed with a driving gear (804) and a driving gear (803), respectively; a rotating shaft (805) is rotatably installed on the reaction kettle (1); the rotating shaft (805) is coaxially installed with a driven gear (811), a sun gear (809), and a cam (810), respectively; the driven gear (811) is engaged with the driving gear (803); an inner gear ring (807) is installed on the top of the sliding sleeve (701); the sun gear (809) is located inside the inner gear ring (807); the sun gear (809) and the inner gear ring (807) are transmissionally connected with a planetary gear (808); a driven gear ring (806) is connected with the planetary gear (808); and the driven gear ring (806) is engaged with the driving gear (804).

5. The trimethylaluminum preparation hazardous waste liquid energy-saving and environmentally friendly treatment microreactor according to claim 1, characterized in that: The injection liquid piece (702) is internally provided with an adjusting block (706), and the injection liquid piece (702) is provided with a screw rod (707) in a driving connection mode, and the screw rod (707) is connected with the adjusting block (706).

6. The trimethylaluminum preparation hazardous waste liquid energy-saving and environmentally friendly treatment microreactor according to claim 5, characterized in that: The injection liquid piece (702) is provided with a volume scale (705), and the adjusting block (706) is provided with an indicating scale (708).

7. A process for preparing hazardous waste liquid of trimethylaluminum, characterized in that, The process is applied to the micro-reactor as claimed in any one of claims 1-6, and the process comprises the following steps: Step S1: the waste liquid is delivered to the injection liquid piece (702) through the liquid feeding pipe (5), and then the waste liquid is delivered to the reaction kettle (1) by the injection liquid piece (702), then the pure water is delivered to the water injection piece (703) through the water feeding pipe (4), and then the pure water is delivered to the reaction kettle (1) by the water injection piece (703), and the waste liquid and water are subjected to a violent chemical reaction in the reaction kettle (1); Step S2: the waste liquid and water are subjected to a violent reaction, i.e. deactivation treatment, and the mixed reaction deactivation liquid is sent to the deactivation collection tank through the liquid outlet (2), wherein the hydrogen and methane generated in the reaction are discharged through the exhaust port (3), and when the gas passes through the combustion structure at the end of the exhaust port (3), the hydrogen and methane are burned and discharged; Step S3: the deactivation liquid in the deactivation collection tank is separated from the organic solvent hydrocarbon solvent by oil-water separation technology, and after the organic solvent is purified, it is recycled to the process of preparing trimethyl aluminum for use; Step S4: the waste liquid after oil-water separation is sent to the solid-liquid separation tank, and the aluminum hydroxide is separated out by solid-liquid separation technology, at this time the mixed liquid is mainly sodium chloride aqueous solution; Step S5: the sodium chloride aqueous solution is sent to the evaporation equipment, and pure water and sodium chloride are obtained by evaporation, the pure water is connected to the water feeding pipe (4), and then recycled to the reaction kettle (1) to participate in the deactivation treatment of the waste liquid.

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