Alkali washing tank and process for producing high-purity germane by using same

Abstract

The invention discloses an alkali washing tank and a process for producing high-purity germane by using the alkali washing tank, and relates to the technical field of alkali washing purification, the alkali washing tank comprises an alkali washing assembly, the alkali washing assembly comprises a tank body, a partition plate is fixed in the tank body, a one-way spray pipe is fixed on one side of the partition plate, a gas conveying sleeve is arranged in the tank body, and a gas conveying pipe and a gas collecting hood are embedded in the top of the tank body; the adjusting assembly is arranged at the top of the tank body and comprises a homogenizing part, the homogenizing part is located at the top of the tank body, and a conveying part is arranged on one side of the homogenizing part. The device has the beneficial effects that through the arrangement of the alkali washing assembly and the adjusting assembly, waste gas can flow into alkali liquor in a separated manner after an alkali washing reaction is carried out for a period of time; along with further alkali washing, alkali liquor is supplemented through the guide pipe, while the alkali liquor is supplemented, waste gas is still subjected to continuous purification reaction, the overall reaction rate is guaranteed, manual or electrical equipment intervention is not needed, and the actual use cost and the subsequent maintenance cost are effectively reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of caustic washing and purification, in particular to a caustic washing tank and a process for producing high-purity germane using the same. Background Art

[0002] The preparation of high-purity germanium usually involves a chlorination reaction, which releases acidic gases such as hydrogen chloride and chlorine. By means of caustic washing, more than 99.5% of the hydrogen chloride and more than 90% of the chlorides in the waste gas can be removed to ensure compliance with emissions standards. A caustic washing tank, a commonly used treatment device, is used in the caustic washing process.

[0003] In the existing caustic washing tanks, as the purification treatment progresses, the concentration of the alkali solution inside gradually decreases. While maintaining the continuous introduction of waste gas, the reaction rate between the waste gas and the alkali solution gradually decreases, affecting the overall caustic washing treatment efficiency. At the same time, after the alkali solution is gradually consumed and the concentration drops to a certain range, manual control is generally used for liquid replenishment treatment, and the overall operation efficiency is low. Summary of the Invention

[0004] In view of the problems existing in the existing caustic washing tanks for producing high-purity germane, the present invention is proposed.

[0005] Therefore, the problems to be solved by the present invention are that in the existing caustic washing tanks, while maintaining the continuous introduction of waste gas, the reaction rate between the waste gas and the alkali solution gradually decreases, affecting the overall caustic washing treatment efficiency. At the same time, after the alkali solution is gradually consumed, manual control is required for liquid replenishment treatment, and the overall operation efficiency is average.

[0006] To solve the above technical problems, the present invention provides the following technical solution: A caustic washing tank, comprising, A caustic washing assembly, including a tank body, a partition is fixed inside the tank body, a one-way spray pipe is fixed on one side of the partition, an air delivery sleeve is arranged inside the tank body, and an air delivery pipe and a gas collection hood are embedded at the top of the tank body; and, An adjustment assembly, arranged at the top of the tank body, including a homogenizing member, the homogenizing member is located at the top of the tank body, a transmission member is arranged on one side of the homogenizing member, a control member is arranged between the homogenizing member and the transmission member, the control member includes a floating plate and a bearing seat, the floating plate is arranged inside the tank body, the bearing seat is fixed at the top of the tank body, a floating rod is fixed on the top of the floating plate, a first pressing plate and a second pressing plate are rotatably connected to the bearing seat, a transmission member is arranged on the tank body, the transmission member includes a receiving sleeve, the receiving sleeve is located at the top of the tank body, a spring and a displacement seat are arranged inside the receiving sleeve, cross bars are rotatably connected to both ends of the displacement seat, and a transmission plate is rotatably connected to the other end of the cross bar.

[0007] As a preferred solution of the caustic washing tank of the present invention, wherein: First and second dial blocks are fixed on the outer circumference of the floating rod.

[0008] As a preferred embodiment of the caustic scrubbing tank of the present invention, one end of the first abutting plate is fixed with a first rotating block, a first inclined groove is formed at one end of the first abutting plate, and a first positioning block is fixed on the other side of the first rotating block.

[0009] As a preferred embodiment of the caustic scrubbing tank of the present invention, one end of the second abutting plate is fixed with a second rotating block, a second positioning block is fixed on the second rotating block, a second inclined groove is formed at one end of the second abutting plate, a convex block is fixed at one end of the second abutting plate, and a third inclined groove is formed at one end of the convex block.

[0010] As a preferred embodiment of the caustic scrubbing tank of the present invention, the homogenizing member includes a four-way pipe, which is connected between the gas transmission pipe and the gas collecting hood. A butterfly valve is fixed at the bottom of the four-way pipe, a first valve rod handle is arranged on one side of the butterfly valve, and a vertical pipe is fixed at the bottom of the butterfly valve.

[0011] As a preferred embodiment of the caustic scrubbing tank of the present invention, the transmission member includes a three-way ball valve, which is arranged at the top of the tank body. A second valve rod handle is installed on one side of the three-way ball valve, a conduit is fixed at the bottom of the three-way ball valve, and a check valve is fixed on the outer ring of the conduit.

[0012] As a preferred embodiment of the caustic scrubbing tank of the present invention, one end of the spring is fixed in the receiving sleeve, the other end of the spring is fixed on the displacement seat, and a guiding rod is slidably connected to the cross bar.

[0013] As a preferred embodiment of the caustic scrubbing tank of the present invention, the number of the transmission plates is four. One end of the transmission plate on one side is rotatably connected to the first valve rod handle, and one end of the transmission plate on the other side is rotatably connected to the second valve rod handle.

[0014] As a preferred embodiment of the caustic scrubbing tank of the present invention, the gas transmission sleeve is horizontally placed in the tank body, air holes are formed on the outer ring of the gas transmission sleeve, and a filter mesh cylinder is arranged in the gas transmission sleeve.

[0015] As a preferred embodiment of the caustic scrubbing tank of the present invention, an air inlet head is embedded on one side of the tank body, an exhaust head is embedded on the other side of the tank body, a sewage discharge valve is fixed at the bottom of the tank body, the number of the one-way spray pipes is several, and one end of the one-way spray pipe is communicated with the inner cavity of the partition plate.

[0016] The present invention also provides a process for producing high-purity germane using the above caustic scrubbing tank, including the following steps: S1. In a reaction kettle, a 15% sodium hydroxide solution is quantitatively added, and then a set amount of germanium dioxide solid and sodium borohydride solid are added. Under the stirring state, dilute sulfuric acid with a concentration of 30% is added at a set flow rate to generate germane gas; S2. Pass the germane gas generated by the reaction successively through an alkali scrubbing tank, a primary water removal tower, and a secondary water removal tower, and collect it in a collection cold trap. S3. Slowly raise the temperature of the collection cold trap to vaporize the liquid-state germane, and let it enter the primary adsorption tower and the secondary adsorption tower at a set flow rate. S4. The gas material after adsorption enters a light component removal tower, and the light components are withdrawn from the side line of the light component removal tower and enter a heavy component removal tower; and S5. Withdraw high-purity germane gas from the top of the heavy component removal tower to a filling system.

[0017] As a preferred embodiment of the process for producing high-purity germane according to the present invention, in step S1, the operating pressure of the reaction kettle is 0.1 MPa, and the operating temperature is 40 °C.

[0018] As a preferred embodiment of the process for producing high-purity germane according to the present invention, in step S2, the operating pressure of the alkali scrubbing tank is 0.1 MPa, and the operating temperature is room temperature; the operating pressure of the primary water removal tower is 0.1 MPa, and the operating temperature is 0 °C; the operating pressure of the secondary water removal tower is 0.1 MPa, and the operating temperature is -65 °C; the collection operating pressure of the collection cold trap is 0.05 MPa, and the collection operating temperature is -140 °C.

[0019] As a preferred embodiment of the process for producing high-purity germane according to the present invention, in step S3, the discharging operating pressure of the collection cold trap is 0.5 MPa, and the discharging operating temperature is -45 °C; the operating pressure of the primary adsorption tower is 0.5 MPa, and the operating temperature is room temperature; the operating pressure of the secondary adsorption tower is 0.5 MPa, and the operating temperature is room temperature.

[0020] As a preferred embodiment of the process for producing high-purity germane according to the present invention, in step S4, the operating pressure of the light component removal tower is 0.4 MPa, and the operating temperature is -53 °C.

[0021] As a preferred embodiment of the process for producing high-purity germane according to the present invention, in step S5, the operating pressure of the heavy component removal tower is 0.3 MPa, and the operating temperature is -58 °C.

[0022] As a preferred embodiment of the process for producing high-purity germane according to the present invention, a condenser is provided for the reaction kettle, and circulating water is used as the refrigerant; a condenser and a cooling coil are provided for the collection cold trap, and liquid nitrogen is used as the refrigerant; a jacket is provided for the collection cold trap, and R410A (a mixture composed of difluoromethane and pentafluoroethane) at -10 °C is used as the heat medium; condensers are provided at the tops of the light component removal tower and the heavy component removal tower, and R410A (a mixture composed of difluoromethane and pentafluoroethane) at -75 °C is used as the refrigerant, and reboilers are provided at the bottoms of the light component removal tower and the heavy component removal tower, and dichloromethane at -20 °C is used as the heat medium.

[0023] The beneficial effects of the present invention are as follows: Through the settings of the alkali washing component and the adjusting component, when the alkali washing reaction proceeds for a period of time and both the liquid level and concentration of the alkali solution decrease, the butterfly valve can be automatically controlled to open, enabling the waste gas to be shunted and introduced into the alkali solution through the one-way spray pipe; as the alkali washing further proceeds and the liquid level and concentration of the alkali solution further decrease, the three-way ball valve automatically opens, and the alkali solution is replenished through the conduit. While replenishing the alkali solution, the waste gas continues to undergo the purification reaction without interruption, ensuring the overall reaction rate, and without the need for manual or electrical equipment intervention, effectively reducing the actual use cost and subsequent maintenance cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the drawings required for use in the description of the embodiments. Obviously, the drawings in the following description are only some embodiments of the present invention, and those of ordinary skill in the art can also obtain other drawings based on these drawings without creative efforts.

[0025] Figure 1 It is a structural diagram of the alkali washing tank provided by the present invention.

[0026] Figure 2 It is a cross-sectional view of the alkali washing tank provided by the present invention.

[0027] Figure 3 It is a cross-sectional view of the alkali washing component of the alkali washing tank provided by the present invention.

[0028] Figure 4 It is a structural diagram of the adjusting component of the alkali washing tank provided by the present invention.

[0029] Figure 5 It is a structural diagram of the homogenizing part of the alkali washing tank provided by the present invention.

[0030] Figure 6 It is a structural diagram of the transmission part of the alkali washing tank provided by the present invention.

[0031] Figure 7 It is a separation diagram of the control part of the alkali washing tank provided by the present invention.

[0032] Figure 8 It is provided by the present invention for the alkali washing tank Figure 7 The enlarged view of A.

[0033] Figure 9 It is a side view of the partial structure of the control part of the alkali washing tank provided by the present invention.

[0034] Figure 10 It is a simplified process flow diagram of the process for producing high-purity germane provided by the present invention.

[0035] In the figure: 100, caustic washing assembly; 101, tank body; 102, partition board; 102a, one-way spray pipe; 103, gas transmission sleeve; 103a, air hole; 104, exhaust head; 105, gas transmission pipe; 106, gas collecting hood; 107, air inlet head; 108, sewage discharge valve; 109, filter screen cylinder; 200, adjusting assembly; 201, homogenizing part; 201a, four-way pipe; 201b, butterfly valve; 201b-1, first valve rod handle; 201c, vertical pipe; 202, transmission part; 202a, three-way ball valve; 202a-1, second valve rod handle; 202b, conduit; 202c, check valve; 203, control part; 203a, floating plate; 203a-1, floating rod; 203a-1a, first dialing block; 203a-1b, second dialing block; 203b, bearing seat; 203b-1, first abutting plate; 203b-1a, first rotating block; 203b-1b, first inclined groove; 203b-1c, first positioning block; 203b-2, second abutting plate; 203b-2a, second rotating block; 203b-2b, second inclined groove; 203b-2c, convex block; 203b-2d, third inclined groove; 203b-2e, second positioning block; 204, transmission part; 204a, receiving sleeve; 204b, spring; 204c, displacement seat; 204c-1, groove; 204d, cross bar; 204e, transmission plate; 204f, guiding rod. Detailed implementation manners

[0036] To make the above objects, features and advantages of the present invention more obvious and understandable, the following detailed description of the specific implementation manners of the present invention will be given in conjunction with the accompanying drawings of the specification.

[0037] In the following description, many specific details are set forth in order to fully understand the present invention. However, the present invention can also be implemented in other ways different from those described herein. Those skilled in the art can make similar extensions without departing from the connotation of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed below.

[0038] Secondly, the so-called "one embodiment" or "embodiment" herein refers to a specific feature, structure or characteristic that can be included in at least one implementation manner of the present invention. The phrase "in one embodiment" appearing in different places in this specification does not necessarily refer to the same embodiment, nor is it an individual or selectively exclusive embodiment with other embodiments.

[0039] Embodiment 1 Refer to Figures 1 to 7, which is the first embodiment provided by the present invention. This embodiment provides an alkali washing tank, which includes an alkali washing component 100 and an adjusting component 200. Through the settings of the alkali washing component 100 and the adjusting component 200, when the alkali washing reaction proceeds for a period of time and both the liquid level and concentration of the alkali solution decrease, the waste gas can automatically flow into the alkali solution in a branched manner to ensure the uniformity of the reaction and maintain the reaction rate; as the alkali washing further proceeds and the liquid level and concentration of the alkali solution further decrease, the alkali solution is gradually replenished, and the waste gas still undergoes a purification reaction to ensure the overall reaction rate.

[0040] Specifically, the alkali washing component 100 includes a tank body 101. A partition plate 102 is fixed inside the tank body 101. The partition plate 102 is hollow. One side of the partition plate 102 is fixed with a one-way spray pipe 102a. As a non-limiting embodiment, the number of partition plates 102 is two, and both are fixed inside the tank body 101. The presence of the partition plate 102 can divide the inside of the tank body 101 into three chambers for three-stage alkali washing and purification treatment of high-purity germane, realizing efficient acid removal treatment of the waste gas and ensuring the acid-base neutralization effect.

[0041] An air delivery sleeve 103 is arranged inside the tank body 101. An exhaust head 104, an air delivery pipe 105, a gas collecting hood 106, an air inlet head 107, and a sewage discharge valve 108 are embedded on the tank body 101. Among them, the exhaust head 104 is located on one side of the tank body 101, while the air inlet head 107 is located on the other side of the tank body 101. The sewage discharge valve 108 is fixed at the bottom of the tank body 101 and is communicated with the tank body 101.

[0042] The bottom end of the air delivery pipe 105 is communicated with the inner cavity of the air delivery sleeve 103 for inputting the waste gas into the air delivery sleeve 103. The bottom end of the gas collecting hood 106 is designed in an inverted funnel shape to increase the bottom air inlet space and is conducive to the transmission of the waste gas. Through the settings of the exhaust head 104, the air delivery pipe 105, the gas collecting hood 106, and the air inlet head 107, the waste gas circulation treatment can be completed. After the waste gas is input, it is discharged after three-stage purification. Through the setting of the sewage discharge valve 108, the waste liquid inside the tank body 101 can be discharged when it is in the open state.

[0043] Specifically, the adjusting component 200 is arranged on the top of the tank body 101 and includes a homogenizing member 201. The homogenizing member 201 is located on the top of the tank body 101. A transmission member 202 is arranged on one side of the homogenizing member 201. A control member 203 is arranged between the homogenizing member 201 and the transmission member 202. The control member 203 includes a floating plate 203a and a bearing seat 203b. The floating plate 203a is arranged inside the tank body 101, and the bearing seat 203b is fixed on the top of the tank body 101. A floating rod 203a-1 is fixed on the top of the floating plate 203a.

[0044] A first pressing plate 203b-1 and a second pressing plate 203b-2 are rotatably connected to the bearing seat 203b. Among them, the first pressing plate 203b-1 and the second pressing plate 203b-2 are both separately provided, and the first pressing plate 203b-1 and the second pressing plate 203b-2 are symmetrically connected to the bearing seat 203b. A transmission member 204 is provided on the tank body 101. The transmission member 204 includes a receiving sleeve 204a. The receiving sleeve 204a is located at the top of the tank body 101. A spring 204b and a displacement seat 204c are provided in the receiving sleeve 204a. One end of the spring 204b is fixed in the receiving sleeve 204a, and the other end of the spring 204b is fixed on the displacement seat 204c. Cross bars 204d are rotatably connected to both ends of the displacement seat 204c. The other end of each cross bar 204d, that is, the outer end, is rotatably connected to a transmission plate 204e.

[0045] Through the settings of the homogenizing member 201 and the transmission member 204, the transmission member 204 can drive the homogenizing member 201 to act to complete the opening or closing operation. In the open state, it is used to divert and input waste gas into the lye to ensure the rate of acid-base reaction.

[0046] Through the settings of the transmission member 202 and the transmission member 204, the transmission member 204 can drive the transmission member 202 to act to complete the opening or closing operation, and is used to realize the liquid supplement operation or the cleaning operation.

[0047] Embodiment 2 Refer to Figures 2 to 9 , which is the second embodiment of the present invention. This embodiment is based on the previous embodiment.

[0048] Specifically, a first dial block 203a-1a and a second dial block 203a-1b are fixed to the outer circumference of the floating rod 203a-1. The first dial block 203a-1a and the second dial block 203a-1b are designed with a dislocation, that is, the first dial block 203a-1a is located on one side of the floating rod 203a-1, while the second dial block 203a-1b is located on the other side of the floating rod 203a-1. At the same time, the first dial block 203a-1a and the second dial block 203a-1b are designed with different heights, and the first dial block 203a-1a is lower than the height of the second dial block 203a-1b.

[0049] One end of the first pressing plate 203b-1 is fixed with a first rotating block 203b-1a. One end of the first pressing plate 203b-1 is provided with a first inclined groove 203b-1b. The other side of the first rotating block 203b-1a is fixed with a first positioning block 203b-1c. The number of the first positioning blocks 203b-1c is two, and the side of the first pressing plate 203b-1 adjacent to the first inclined groove 203b-1b is a flat surface.

[0050] When the floating plate 203a and the floating rod 203a-1 descend, the first shifting block 203a-1a will descend accordingly and contact the first positioning block 203b-1c, thereby shifting the first pressing plate 203b-1 to rotate. Through the settings of the first inclined groove 203b-1b and the displacement seat 204c, when the first pressing plate 203b-1 is in a rotating state, the first inclined groove 203b-1b can contact the displacement seat 204c to drive the displacement seat 204c to generate displacement until the flat surface on the first pressing plate 203b-1 contacts the displacement seat 204c, ensuring the stability of the position where the displacement seat 204c is located.

[0051] One end of the second pressing plate 203b-2 is fixed with a second rotating block 203b-2a, and a second positioning block 203b-2e is fixed on the second rotating block 203b-2a. One end of the second pressing plate 203b-2 is provided with a second inclined groove 203b-2b, and a convex block 203b-2c is fixed at one end of the second pressing plate 203b-2. The convex block 203b-2c is located outside the second inclined groove 203b-2b, and a third inclined groove 203b-2d is provided at one end of the convex block 203b-2c. The number of the second positioning blocks 203b-2e is two. When the floating plate 203a and the floating rod 203a-1 further descend, the second shifting block 203a-1b will descend accordingly and contact the second positioning block 203b-2e, thereby shifting the second pressing plate 203b-2 to rotate.

[0052] Through the setting of the second inclined groove 203b-2b, when the second inclined groove 203b-2b contacts the displacement seat 204c, it presses the displacement seat 204c to displace. Through the setting of the groove 204c-1, the rotation space requirement of the convex block 203b-2c can be satisfied. As the second pressing plate 203b-2 further rotates, the third inclined groove 203b-2d on the convex block 203b-2c will contact the groove 204c-1, thereby pushing the displacement seat 204c to further displace.

[0053] The homogenizing member 201 includes a four-way pipe 201a, which is connected between the gas transmission pipe 105 and the gas collecting hood 106. A butterfly valve 201b is fixed at the bottom of the four-way pipe 201a. A first valve rod handle 201b-1 is arranged on one side of the butterfly valve 201b, and a vertical pipe 201c is fixed at the bottom of the butterfly valve 201b.

[0054] Through the setting of the four-way pipe 201a, the gas collecting hood 106 and the gas transmission pipe 105 can be connected to meet the normal transmission requirement of the waste gas. Through the settings of the butterfly valve 201b and the first valve rod handle 201b-1, as the first valve rod handle 201b-1 rotates, the opening and closing of the butterfly valve 201b can be completed, so that the four-way pipe 201a and the vertical pipe 201c can be flexibly connected or disconnected.

[0055] The bottom end of the vertical pipe 201c passes through the tank body 101 and is connected to the inner cavity of the partition (102). Through the setting of the vertical pipe 201c, it can be connected to the partition 102. When the butterfly valve 201b is opened, the exhaust gas is diverted and transmitted to the partition 102, and then transmitted to the alkali solution in the tank body 101 through the one-way nozzle 102a, so as to further improve the uniformity of the reaction between the gas and the alkali solution.

[0056] The transmission member 202 includes a three-way ball valve 202a, which is arranged on the top of the tank body 101. A second valve stem handle 202a-1 is installed on one side of the three-way ball valve 202a. A conduit 202b is fixed to the bottom of the three-way ball valve 202a, and a one-way valve 202c is fixed to the outer ring of the conduit 202b.

[0057] The bottom end of the conduit 202b is connected to the inner cavity of the tank 101, and the flow direction of the one-way valve 202c is from top to bottom, which is used for one-way transmission of the conveying medium to ensure the stability of system operation.

[0058] One end of the spring 204b is fixed in the storage sleeve 204a, and the other end of the spring 204b is fixed on the displacement seat 204c. The cross bar 204d is slidably connected with a guide rod 204f, and the guide rod 204f is located outside the transmission plate 204e. This design can prevent the guide rod 204f from hindering the movement of the transmission plate 204e.

[0059] The bottom end of the guide rod 204f is fixed to the top of the tank body 101. The guide rod 204f is used to guide the displacement of the cross bar 204d to improve the movement stability of the cross bar 204d. The spring 204b is configured to elastically connect with the displacement seat 204c to prevent the displacement seat 204c from being displaced randomly without external force.

[0060] There are four transmission plates 204e, that is, two transmission plates 204e are provided on each side, and the two transmission plates 204e on the same side are symmetrically arranged on the outside of the displacement seat 204c, one end of the transmission plate 204e on one side is rotatably connected to the first valve stem handle 201b-1, and one end of the transmission plate 204e on the other side is rotatably connected to the second valve stem handle 202a-1.

[0061] By setting the cross bar 204d and the transmission plate 204e, when the displacement seat 204c moves up and down, the inclination angle of the linkage transmission plate 204e can change, thereby driving the first valve stem handle 201b-1 or the second valve stem handle 202a-1 to rotate, so as to adjust the opening and closing state of the butterfly valve 201b or the three-way ball valve 202a.

[0062] The gas delivery sleeve 103 is horizontally placed in the tank body 101 . The outer ring of the gas delivery sleeve 103 is provided with air holes 103 a . There are three gas delivery sleeves 103 . A filter screen cylinder 109 is arranged inside the gas delivery sleeve 103 .

[0063] Through the arrangement of the gas transmission sleeve 103 and the air hole 103a, it can be submerged in the alkali solution. When the waste gas is introduced, the waste gas can be evenly discharged outward through the air hole 103a, the reaction uniformity is good, and the acid-base reaction rate is guaranteed.

[0064] The left end of the filter screen cartridge 109 is solid in design, in sliding contact with the tank body 101 and sealed. Its core is fixed to the tank body 101 by a sealing bolt. Through the setting of the filter screen cartridge 109, when the exhaust gas passes into the filter screen cartridge 109, the particulate impurities in the exhaust gas can be intercepted and filtered to avoid blockage. With the completion of the alkaline washing reaction, the sealing bolts can be removed, the filter screen cartridge 109 can be moved out, and the internal impurities can be cleaned.

[0065] There are several one-way nozzles 102a, and one end of the one-way nozzle 102a is connected to the inner cavity of the partition 102. The flow direction of the one-way nozzle 102a is from the partition 102 to the tank body 101. When the gas is diverted, the waste gas can be diverted and injected into the waste liquid in the tank body 101 to improve the reaction uniformity.

[0066] When in use, the exhaust gas enters through the air inlet head 107, is filtered by the filter mesh cylinder 109, enters the air delivery sleeve 103 and is discharged through the air hole 103a. After the gas reacts evenly with the alkali solution, it is transmitted through the gas collecting hood 106, the four-way pipe 201a and the air delivery pipe 105, enters the air delivery sleeve 103 and the air hole 103a of another level, and undergoes a secondary reaction. Similarly, a tertiary reaction is performed again. Finally, the gas after alkali washing is discharged from the exhaust head 104.

[0067] As the waste gas purification process proceeds, the alkali solution in the tank 101 is gradually consumed and its concentration decreases. The liquid level in the tank 101 decreases, and the floating plate 203a is driven by gravity to move the floating rod 203a-1 downward, thereby causing the first shifting block 203a-1a and the second shifting block 203a-1b to move downward.

[0068] When the alkali solution is consumed to a certain extent, the concentration of the alkali solution decreases, while the unit gas volume and speed of the exhaust gas remain unchanged, and the acid-base reaction rate decreases to a certain extent. As the float rod 203a-1 moves, the first shift block 203a-1a will contact the first positioning block 203b-1c in advance, and then drive the first abutment plate 203b-1 to rotate, and the first inclined groove 203b-1b contacts the displacement seat 204c, so that the corresponding displacement seat 204c moves downward, and the spring 204b is compressed.

[0069] When the cross bar 204d and the transmission plate 204e are connected, the first valve stem handle 201b-1 rotates, the butterfly valve 201b opens, and the exhaust gas transmitted through the four-way pipe 201a is diverted to the vertical pipe 201c, and evenly diffused into the alkaline solution in the tank body 101 through the partition 102 and the one-way nozzle 102a, further improving the acid-base reaction rate and ensuring the overall purification treatment efficiency.

[0070] As the lye is further consumed, its concentration will further decrease, causing the floating plate 203a and the floating rod 203a-1 to move further downward. At this time, the second shifting block 203a-1b moves downward and contacts the second positioning block 203b-2e to shift the second pressing plate 203b-2 to rotate. The second inclined groove 203b-2b contacts the displacement seat 204c to push the corresponding displacement seat 204c to displace. At this time, the convex block 203b-2c enters the groove 204c-1.

[0071] The displacement of the corresponding displacement seat 204c drives the rotation of the second valve rod handle 202a-1, causing the bottom end of the three-way ball valve 202a to open. The lye is replenished into the tank body 101 through the conduit 202b. At this time, with the cooperation of the one-way valve 202c, the waste gas will not backflush and escape through the conduit 202b, and the liquid replenishment operation is completed while ensuring the normal acid-base reaction between the waste gas and the lye.

[0072] As the liquid replenishment operation progresses, the lye liquid level in the tank body 101 rises, driving the floating plate 203a and the floating rod 203a-1 to move upward and reset. The first rotating block 203b-1a and the second shifting block 203a-1b move upward, and cooperate with the first positioning block 203b-1c and the second positioning block 203b-2e to shift the second pressing plate 203b-2 and the first pressing plate 203b-1 to rotate. The flat surfaces on the first pressing plate 203b-1 and the second pressing plate 203b-2 no longer contact the displacement seat 204c. At this time, under the elastic support of the spring 204b, the first pressing plate 203b-1 and the second pressing plate 203b-2 are well reset.

[0073] After the caustic washing is completed, when it is necessary to clean the inside of the tank body 101, the sewage discharge valve 108 is opened to discharge the waste liquid, and then the floating rod 203a-1 is actively driven to move downward. After the second pressing plate 203b-2 contacts and presses against the transmission part 204, the second pressing plate 203b-2 rotates further, and the third inclined groove 203b-2d contacts the displacement seat 204c, causing the corresponding transmission part 204 to displace further, so that the side end of the second valve rod handle 202a-1 opens and the bottom end is closed.

[0074] At this time, the butterfly valve 201b is also in an open state, and the cleaning liquid and the clean gas can both be introduced through the four-way pipe 201a and the conduit 202b, and cooperate with the partition plate 102 and the one-way spray pipe 102a, the air delivery sleeve 103 and the air holes 103a to complete the uniform cleaning treatment of the inner wall of the tank body 101.

[0075] Embodiment 3 Referring to Figures 1 to 9 , this is the third embodiment of the present invention, and this embodiment is based on the first two embodiments.

[0076] Specifically, the upper end of the three-way ball valve 202a is a normally open end. The side end and the bottom end of the three-way ball valve 202a will be opened or closed with the movement of the second valve stem handle 202a-1. The upper end of the three-way ball valve 202a is connected to an external three-way valve, an external alkali liquid source, and an external cleaning source. Both the external alkali liquid source and the external cleaning source are driven by a centrifugal pump. The external cleaning source includes a special cleaning liquid for the alkali washing tank and a clean gas source, and can be used to separately introduce alkali liquid, cleaning liquid, or clean gas source.

[0077] In summary, compared with the prior art, through the settings of the alkali washing assembly 100 and the adjustment assembly 200, according to the reaction degree of acidic substances in the waste gas with the alkali liquid, the uniform jetting treatment can be automatically completed to ensure the overall reaction rate. As the reaction progresses further, the liquid supplement operation can be automatically completed without manual observation and manual intervention, and it is also convenient for subsequent uniform cleaning treatment.

[0078] Example 4 As Figure 10 shown, quantitatively add 15% sodium hydroxide solution to the alkali batching tank, then add germanium dioxide solid and sodium borohydride solid, stir evenly and add them to the reaction kettle. Configure 30% dilute sulfuric acid in the dilute sulfuric acid batching tank and add it to the reaction kettle at a set flow rate. As the dilute sulfuric acid is added, germane gas begins to be generated. The reaction equation is as follows: GeO 2 +NaOH+NaBH 4 +H 2 SO 4 =GeH 4 +B(OH) 3 +Na 2 SO 4 The reaction residue enters the purification kettle. After purifying and recovering the germane gas, it is treated as waste liquid.

[0079] Then, the germane gas generated by the reaction and the germane gas purified and recovered by the purification kettle are successively passed through the alkali washing tank and the water removal tower, and then collected in the collection cold trap.

[0080] Next, slowly raise the temperature of the collection cold trap to vaporize the liquid-state germane, and enter the primary adsorption tower and the secondary adsorption tower at a set flow rate to remove carbon dioxide and water impurities.

[0081] Subsequently, the adsorbed gas material enters the light component removal tower. Light components such as nitrogen and oxygen are taken out from the top of the light component removal tower to the three-waste cold trap to recover germane, and the non-condensable gas is vented to the three-waste system. The side-line of the light component removal tower takes out the light component removal and enters the heavy component removal tower.

[0082] High-purity germane gas is taken out from the top of the heavy component removal tower to the filling system, and the heavy components are taken out from the bottom of the heavy component removal tower to the three-waste cold trap. The crude germane that can still be recovered is also in the three-waste cold trap.

[0083] In the specific production process, the operating pressure of the reaction kettle is 0.1 MPa, and the operating temperature is 40 °C; the operating pressure of the alkali washing tank is 0.1 MPa, and the operating temperature is room temperature; the operating pressure of the first-stage water removal tower is 0.1 MPa, and the operating temperature is 0 °C; the operating pressure of the second-stage water removal tower is 0.1 MPa, and the operating temperature is -65 °C; the operating pressure of the collection cold trap for collection is 0.05 MPa, and the collection operating temperature is -140 °C; the operating pressure of the purification kettle is 0.05 MPa, and the operating temperature is 60 °C; the operating pressure of the collection cold trap for discharging is 0.5 MPa, and the discharging operating temperature is -45 °C; the operating pressure of the first-stage adsorption tower is 0.5 MPa, and the operating temperature is room temperature; the operating pressure of the second-stage adsorption tower is 0.5 MPa, and the operating temperature is room temperature; the operating pressure of the light component removal tower is 0.4 MPa, and the operating temperature is -53 °C; the operating pressure of the heavy component removal tower is 0.3 MPa, and the operating temperature is -58 °C; the operating pressure of the three-waste cold trap for collection is 0.05 MPa, and the operating temperature is -140 °C; the operating pressure of the three-waste cold trap for gas compression is 0.5 MPa, and the operating temperature is -45 °C.

[0084] Using the alkali washing tank provided by the present invention and the above process steps, the purity of the germane produced is ≥99.9995%.

[0085] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention, and they should all be covered within the scope of the claims of the present invention.

Claims

1. An alkali washing tank, characterized in that: include: The alkali washing component (100) and the regulating component (200) are as follows: The alkali cleaning assembly (100) comprises a tank body (101), a partition (102) is fixed inside the tank body (101), a one-way nozzle (102a) is fixed on one side of the partition (102), a gas supply sleeve (103) is arranged inside the tank body (101), and a gas supply pipe (105) and a gas collecting hood (106) are embedded on the top of the tank body (101); and, The regulating assembly (200) comprises a homogenizing member (201), the homogenizing member (201) being located at the top of the tank body (101), a transmission member (202) being arranged on one side of the homogenizing member (201), a control member (203) being arranged between the homogenizing member (201) and the transmission member (202), the control member (203) comprising a floating plate (203a) and a bearing seat (203b), the floating plate (203a) being arranged in the tank body (101), the bearing seat (203b) being fixed to the top of the tank body (101), and a control member (203b) being arranged on the bearing seat (203b). A first abutment plate (203b-1) and a second abutment plate (203b-2) are rotatably connected, a transmission member (204) is provided on the tank body (101), the transmission member (204) comprises a storage sleeve (204a), the storage sleeve (204a) is located at the top of the tank body (101), a spring (204b) and a displacement seat (204c) are provided in the storage sleeve (204a), both ends of the displacement seat (204c) are rotatably connected to a cross bar (204d), and the other end of the cross bar (204d) is rotatably connected to a transmission plate (204e).

2. The alkali cleaning tank according to claim 1, characterized in that: A floating rod (203a-1) is fixed on the top of the floating plate (203a), and a first shifting block (203a-1a) and a second shifting block (203a-1b) are fixed on the outer ring of the floating rod (203a-1).

3. The alkali cleaning tank according to claim 2, characterized in that: A first rotating block (203b-1a) is fixed to one end of the first abutment plate (203b-1), a first inclined groove (203b-1b) is provided at one end of the first abutment plate (203b-1), and a first positioning block (203b-1c) is fixed to the other side of the first rotating block (203b-1a).

4. The alkali cleaning tank according to claim 3, characterized in that: A second rotating block (203b-2a) is fixed to one end of the second abutment plate (203b-2), a second positioning block (203b-2e) is fixed to the second rotating block (203b-2a), a second inclined groove (203b-2b) is provided at one end of the second abutment plate (203b-2), a convex block (203b-2c) is fixed to one end of the second abutment plate (203b-2), and a third inclined groove (203b-2d) is provided at one end of the convex block (203b-2c).

5. The alkali cleaning tank according to claim 1, characterized in that: The homogenizing element (201) comprises a four-way pipe (201a) connected between the gas transmission pipe (105) and the gas collecting hood (106); a butterfly valve (201b) is fixed at the bottom of the four-way pipe (201a); a first valve stem handle (201b-1) is provided on one side of the butterfly valve (201b); and a vertical pipe (201c) is fixed at the bottom of the butterfly valve (201b).

6. The alkali cleaning tank according to claim 1, characterized in that: The transmission component (202) comprises a three-way ball valve (202a) arranged on the top of the tank body (101), a second valve stem handle (202a-1) being installed on one side of the three-way ball valve (202a), a conduit (202b) being fixed at the bottom of the three-way ball valve (202a), and a one-way valve (202c) being fixed on the outer ring of the conduit (202b).

7. The alkali cleaning tank according to claim 1, characterized in that: One end of the spring (204b) is fixed in the storage sleeve (204a), the other end of the spring (204b) is fixed on the displacement seat (204c), and a guide rod (204f) is slidably connected to the crossbar (204d).

8. The alkali cleaning tank according to claim 5 or 6, characterized in that: There are four transmission plates (204e), one end of a transmission plate (204e) on one side is rotatably connected to the first valve stem handle (201b-1), and one end of a transmission plate (204e) on the other side is rotatably connected to the second valve stem handle (202a-1).

9. The alkali cleaning tank according to claim 1, characterized in that: The gas transmission sleeve (103) is placed horizontally in the tank body (101); an air hole (103a) is provided on the outer ring of the gas transmission sleeve (103); and a filter screen cylinder (109) is arranged in the gas transmission sleeve (103).

10. A process for producing high-purity germane, using the alkali washing tank according to any one of claims 1 to 9, characterized in that: The steps include: S1. In a reaction kettle, 15% sodium hydroxide solution is quantitatively added, and then a set amount of germanium dioxide solid and sodium borohydride solid are added. Under stirring, 30% dilute sulfuric acid is added at a set flow rate to generate germane gas; S2, the germane gas generated by the reaction passes through the alkali washing tank, the primary dehydration tower and the secondary dehydration tower in sequence, and is collected in a collection cold trap; S3, slowly increase the temperature of the collection cold trap to vaporize the liquid germane and enter the primary adsorption tower and the secondary adsorption tower at a set flow rate; S4, the gas material after adsorption enters the light removal tower, and the light components are taken out from the side line of the light removal tower and enter the heavy removal tower; as well as S5. High-purity germane gas is extracted from the top of the deweighting tower and fed to the filling system.

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