A BP-3 tailing purification treatment device and its treatment method
The BP-3 tailing purification system addresses impurity separation issues by using a series of reactors with controlled valves and heating/cooling mechanisms, ensuring high-quality product output and efficient processing.
Patent Information
- Application Number
- CN202211699419.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-28
- Publication Date
- 2025-07-15
- Estimated Expiration
- 2042-12-28
AI Technical Summary
The existing BP-3 tail material purification and treatment equipment cannot effectively separate impurities, resulting in the tail material affecting the processing effect and quality in the synthesis, alkalinization, acidification and alkali washing processes, and reducing the efficiency and effect of the purification and treatment equipment.
The dealcoholing kettle, water washing kettle, alkalizing kettle, impurity kettle and acidification kettle are used to combine the mixing mechanism, steam engine, temperature display and exhaust gas purifier to achieve dealcoholing, water washing, alkalizing and impurity separation of the tail material. By controlling the solenoid valve to open and close regularly, the tail material is ensured smoothly transfer and processing between each kettle.
Effectively separate impurities, ensure the quality and effect of the tail material in each process, improve the use efficiency of purification and treatment equipment and product qualification rate, and meet the use needs of staff.
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Figure CN116139518B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of purification treatment equipment, and particularly to a BP-3 tailing purification treatment equipment and a treatment method thereof. Background Art
[0002] BP-3 tailings refer to BP-3 dissolved in ethanol, by-products generated in the BP-3 synthesis reaction, and BP-1 that has not reacted completely, etc. Calculated based on 6 batches of BP-3 reactions per day, the tailings to be treated per day are about 250 kg, ethanol accounts for about 60%, tailings account for about 40%, BP-3 in the tailings accounts for about 60%, impurity 1 accounts for about 20%, and others account for 20%. All of the above are weight percentages.
[0003] During the production and processing of BP-3 tailings, purification treatment equipment is often required to purify the BP-3 tailings to ensure the safety of the BP-3 tailings production and processing process. For example, a production method of ultraviolet absorber BP-3 proposed in Chinese Patent CN111302920B has the advantages of stable reaction process, controllable temperature, recovery and reuse of deionized water and solvent, achieving high product yield, reducing production costs, absorbing the generated HCL through a tail gas absorption device to make high-concentration hydrochloric acid, avoiding the generation of waste water, achieving zero discharge of waste water, using the dropwise addition method for dimethyl sulfate to improve production safety, omitting the water washing and drying links between the condensation and esterification reactions, saving costs such as labor, electricity, and transportation by omitting water washing, eliminating tail gas emission pollution during the drying process by omitting drying, avoiding fluctuations in the BP-3 synthesis reaction caused by excessive moisture during drying, and creating conditions for improving enterprise efficiency. However, this design cannot effectively separate impurities from the tailings, resulting in the influence on the processing effect and quality of the tailings during the processes of synthesis, alkalization, acidification, and alkali washing of the BP-3 tailings. Because the accumulated impurities are increasing, the purification treatment effect of the BP-3 tailings is affected, making it difficult for the purification treatment equipment to process qualified products, inconvenient to use, unable to meet the needs of the staff, and reducing the use efficiency and use effect of the purification treatment equipment. Summary of the Invention
[0004] (1) Technical Problems to be Solved
[0005] In view of the deficiencies of the prior art, the present invention provides a BP-3 tailing purification treatment device and a treatment method thereof, which have the advantages of separating impurities from tailings, etc., and solve the problem that the existing BP-3 tailing purification treatment device cannot effectively separate impurities from tailings, resulting in the influence on the processing effect and quality of tailings during the processes of synthesis, alkalization, acidification and alkali washing of BP-3 tailings. Because the accumulated impurities are increasing, the purification treatment effect of BP-3 tailings is affected, making it difficult for the purification treatment device to process qualified products, inconvenient to use, unable to meet the needs of workers, and reducing the use efficiency and use effect of the purification treatment device.
[0006] (II) Technical Solution
[0007] To achieve the above object, the present invention provides the following technical solution: A BP-3 tailing purification treatment device includes a de-alcoholization kettle, a water washing kettle, an alkalization kettle, an impurity kettle, an acidification kettle, a first connecting pipe, a second connecting pipe, a third connecting pipe and a fourth connecting pipe. The de-alcoholization kettle and the water washing kettle are connected through the first connecting pipe, the water washing kettle and the alkalization kettle are connected through the second connecting pipe, the alkalization kettle and the impurity kettle are connected through the third connecting pipe, and the alkalization kettle and the acidification kettle are connected through the fourth connecting pipe.
[0008] Furthermore, a first solenoid valve is arranged on the outer side of the first connecting pipe, a second solenoid valve is arranged on the outer side of the second connecting pipe, a third solenoid valve is arranged on the outer side of the third connecting pipe, and a fourth solenoid valve is arranged on the outer side of the fourth connecting pipe.
[0009] Furthermore, the de-alcoholization kettle includes a first feed pipe, a first vacuum valve, a first discharge pipe, a first discharge valve, a first stirring mechanism, a condenser, a cooling water valve, a first steam engine, a first steam valve, a first temperature display, a first vent valve, a first intake pipe and a first tail gas purifier.
[0010] Furthermore, the water washing kettle includes a second feed pipe, a second vacuum valve, a second discharge pipe, a second discharge valve, a second steam engine, a second steam valve, a second temperature display, a second vent valve, a second intake pipe, a second tail gas purifier, a second stirring mechanism and a first water separator.
[0011] Furthermore, the alkalization kettle includes a third feed pipe, a third vacuum valve, a third discharge pipe, a third discharge valve, a third stirring mechanism, a third steam engine, a third steam valve, a third temperature display, a second water separator, a third vent valve, a third intake pipe and a third tail gas purifier.
[0012] Further, the impurity kettle includes a fourth feed pipe, a fourth vacuum valve, a fourth discharge pipe, a fourth discharge valve, a fourth stirring mechanism, a fourth steam engine, a fourth steam valve, a fourth temperature display, a third water separator, a storage barrel, a fourth vent valve, a fourth inlet pipe, and a fourth tail gas purifier.
[0013] Further, the acidification kettle includes a fifth feed pipe, a fifth vacuum valve, a timer, a fifth stirring mechanism, a fifth discharge pipe, and a fifth discharge valve.
[0014] A purification treatment method for BP-3 tailings includes the following steps:
[0015] 1) Open the first vacuum valve, pour 1000 kg of tailings into the inside of the alcohol removal kettle through the first feed pipe, and then close the first vacuum valve;
[0016] 1.1) By starting the first stirring mechanism, the 1000 kg of tailings inside the alcohol removal kettle can be stirred;
[0017] 1.2) Open the cooling water valve of the condenser, put the coolant into the inside of the alcohol removal kettle, and open the first steam valve. The tailings inside the alcohol removal kettle can be heated by the first steam engine;
[0018] 1.3) When the temperature inside the alcohol removal kettle reaches ≥120 °C and there is no distillate in the alcohol removal kettle, close the first steam valve and open the first vacuum valve to make the alcohol removal kettle start to cool slowly;
[0019] 1.4) When the temperature inside the alcohol removal kettle drops to 60 °C, by opening the first solenoid valve, the tailings inside the alcohol removal kettle can be put into the inside of the water washing kettle through the first connecting pipe;
[0020] 2) By opening the second vacuum valve, 500 kg of water can be poured into the inside of the water washing kettle through the second feed pipe, and then start the second stirring mechanism to stir the tailings and water inside the water washing kettle;
[0021] 2.1) Open the second steam valve, and the tailings and water inside the water washing kettle can be heated by the second steam engine;
[0022] 2.2) When the temperature inside the water washing kettle rises to 80 °C and is stirred for 1 hour, after standing for 2 hours, the tailings and water can be stratified through the first water separator, and at the same time, the tailings and water can be filtered and purified;
[0023] 3) By opening the second solenoid valve, the lower oil layer inside the water washing kettle can be put into the inside of the alkalization kettle through the second connecting pipe. At the same time, open the third vacuum valve, and 100 kg of alkali and 1500 kg of water can be poured into the inside of the alkalization kettle through the third feed pipe;
[0024] 3.1) By starting the third stirring mechanism, the materials inside the alkalization kettle can be stirred. At the same time, by opening the third steam valve, the materials inside the alkalization kettle can be heated by the third steam engine.
[0025] 3.2) When the temperature inside the alkalization kettle rises to 65 °C, keep it warm for 1 hour and stop stirring. After standing for 2 hours, the materials inside the alkalization kettle can be stratified through the second water separator. At the same time, the materials and the water layer can be filtered and purified.
[0026] 3.3) By opening the third solenoid valve, the impurities in the lower layer inside the alkalization kettle can be put into the inside of the impurity kettle through the third connecting pipe.
[0027] 3.4) After removing the impurities, by opening the fourth solenoid valve, the remaining water layer inside the alkalization kettle can be put into the inside of the acidification kettle through the fourth connecting pipe to prepare for dropping acid.
[0028] 4) The impurities and the water layer inside the impurity kettle can be filtered and purified through the third water separator.
[0029] 4.1) Open the fourth steam valve, and the impurities inside the impurity kettle can be heated by the fourth steam engine.
[0030] 4.2) When the temperature inside the impurity kettle rises to 65 °C, open the fourth vacuum valve to pour 800 kg of water into the inside of the impurity kettle through the fourth feed pipe. Start the fourth stirring mechanism to stir and heat the impurities and water inside the impurity kettle.
[0031] 4.3) Then add 50 kg of alkali into the impurity kettle through the fourth feed pipe. After stirring for 30 minutes, use a pH test paper to test the pH value at the sampling point. When the pH reaches 14, stop heat preservation and stirring.
[0032] 4.4) Take a sample for inspection. By adjusting the fourth discharge valve, the lower layer material of the impurity kettle can be taken through the fourth discharge pipe. When BP-3 ≤ 1% or impurity 1 ≥ 85%, the material can be transferred. When BP-3 > 1% or impurity 1 < 85%, conduct an alkali wash again. By analogy, the maximum number of alkali washes does not exceed three times.
[0033] 4.5) The oil layer inside the impurity kettle can be filled into a storage barrel through the fourth discharge pipe, and the water layer can enter the third connecting pipe and be put into the inside of the alkalization kettle.
[0034] 5) By opening the fifth vacuum valve, 340 kg of hydrochloric acid can be poured into the inside of the acidification kettle through the fifth feed pipe. Then, by opening the fourth solenoid valve, the materials inside the acidification kettle can be slowly dropped into the inside of the alkalization kettle through the fourth connecting pipe, and the time is controlled to be more than 40 minutes.
[0035] 5.1) Then start the third stirring mechanism to stir the materials inside the alkalization kettle. Meanwhile, open the third steam valve to heat the materials inside the alkalization kettle through the third steam engine.
[0036] 5.2) Keep the temperature inside the alkalization kettle at 65 °C, stir for 30 minutes, and then let it stand for 2 hours.
[0037] 5.3) By opening the third discharge valve, the materials inside the alkalization kettle can be sampled and detected through the third discharge pipe. If the impurity 1 ≤ 1% and BP-3 ≥ 96%, it is considered qualified.
[0038] 5.4) The unqualified products are immediately reworked. Without stratification, start stirring, add 100 kg of flake caustic soda, stir for 30 minutes, let it stand for 2 hours and then stratify. The oil layer enters the impurity kettle, and 340 kg of hydrochloric acid is dropwise added to the water layer, stirred for 30 minutes, let it stand for 2 hours, re-sampled and detected. After passing the detection, the material layer is filled into barrels, measured, and labeled.
[0039] Furthermore, in step 1.2), by opening the first vent valve, the tail gas generated when the tail material inside the alcohol stripping kettle is heated will be discharged into the first tail gas purifier through the first inlet pipe. The first tail gas purifier can purify the tail gas. In step 2.2), by opening the second vent valve, the tail gas generated when the tail material inside the water washing kettle is heated will be discharged into the second tail gas purifier through the second inlet pipe. The second tail gas purifier can purify the tail gas.
[0040] Furthermore, in step 3.1), by opening the third vent valve, the tail gas generated when the materials inside the alkalization kettle are heated will be discharged into the third tail gas purifier through the third inlet pipe. The third tail gas purifier can purify the tail gas. In step 4.1), by opening the fourth vent valve, the tail gas generated when the impurities inside the impurity kettle are heated will be discharged into the fourth tail gas purifier through the fourth inlet pipe. The fourth tail gas purifier can purify the tail gas.
[0041] (III) Beneficial effects
[0042] Compared with the prior art, the technical solution of this application has the following beneficial effects:
[0043] 1. The BP-3 tailing purification treatment equipment and its treatment method can carry out alcohol removal treatment on the tailings through the coordinated action among the first stirring mechanism, condenser, cooling water valve, first steam engine, first steam valve, first temperature display, first vent valve, first inlet pipe and first tail gas purifier in the alcohol removal kettle. At the same time, it can cool and heat the tailings. Cooperating with the first stirring mechanism, it can uniformly cool and heat the tailings to ensure the effects of cooling and heating the tailings. And it can purify the tail gas generated during the processing of the tailings. Through the coordinated action among the second feed pipe, second vacuum valve, second steam engine, second steam valve, second temperature display, second vent valve, second inlet pipe, second tail gas purifier, second stirring mechanism and first water separator in the water washing kettle, it can carry out water washing on the tailings, stir and heat the tailings to facilitate uniform heating of the tailings. At the same time, it can layer the tailings and water, filter and purify the tailings and water, and purify the tail gas generated during the processing of the tailings. Through the coordinated action among the third feed pipe, third vacuum valve, third stirring mechanism, third steam engine, third steam valve, third temperature display, second water separator, third vent valve, third inlet pipe and third tail gas purifier in the alkalization kettle, it can carry out alkalization treatment on the tailings, stir and heat the tailings, uniformly heat the tailings. At the same time, it can layer the tailings and water, filter and purify the tailings and water, and purify the tail gas generated during the processing of the tailings. Through the coordinated action among the fourth feed pipe, fourth vacuum valve, fourth discharge pipe, fourth discharge valve, fourth stirring mechanism, fourth steam engine, fourth steam valve, fourth temperature display, third water separator, storage barrel, fourth vent valve, fourth inlet pipe and fourth tail gas purifier in the impurity kettle, it can filter and purify the impurities and water layer. At the same time, it can stir, heat and keep warm the impurities and water, layer the impurities and water again, filter and purify the impurities and water to ensure the effect of impurity detection. Through the coordinated action among the fifth feed pipe, fifth vacuum valve, timer, fifth stirring mechanism, fifth discharge pipe and fifth discharge valve in the acidification kettle, it can stir the material and slowly drip the material into the inner side of the alkalization kettle to facilitate the processing and detection of the material. The overall structure is simple and convenient to use. The BP-3 tailing purification treatment equipment can effectively separate impurities from the tailings to ensure the effects and quality of the BP-3 tailings during processes such as synthesis, alkalization, acidification and alkali washing, avoid the accumulation of more and more impurities, improve the effect of BP-3 tailing purification treatment, and the purification treatment equipment can well process qualified products, meet the needs of the staff, and improve the use efficiency and use effect of the purification treatment equipment.
[0044] 2. The BP-3 tailing purification treatment equipment and its treatment method can control the opening or closing of the first communication pipe at regular intervals by setting the first solenoid valve, so as to put the tailing inside the de-alcoholization kettle into the inside of the water washing kettle through the first communication pipe. By setting the second solenoid valve, the opening or closing of the second communication pipe can be controlled at regular intervals, so as to put the lower oil layer inside the water washing kettle into the inside of the alkalization kettle through the second communication pipe. By setting the third solenoid valve, the opening or closing of the third communication pipe can be controlled at regular intervals, so as to put the impurities in the lower layer inside the alkalization kettle into the inside of the impurity kettle through the third communication pipe. By setting the fourth solenoid valve, the remaining water layer inside the alkalization kettle can be put into the inside of the acidification kettle through the fourth communication pipe to prepare for dropping acid, or the material inside the acidification kettle can be slowly dropped into the inside of the alkalization kettle through the fourth communication pipe. BRIEF DESCRIPTION OF THE DRAWINGS
[0045] Figure 1 It is a structural equipment flow chart of the present invention;
[0046] Figure 2 It is a structural process flow chart of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0047] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0048] Please refer to Figure 1-2 , a BP-3 tailing purification treatment equipment and its treatment method in this embodiment include a de-alcoholization kettle, a water washing kettle, an alkalization kettle, an impurity kettle, an acidification kettle, a first communication pipe, a second communication pipe, a third communication pipe, and a fourth communication pipe. The de-alcoholization kettle and the water washing kettle are connected through the first communication pipe, the water washing kettle and the alkalization kettle are connected through the second communication pipe, the alkalization kettle and the impurity kettle are connected through the third communication pipe, and the alkalization kettle and the acidification kettle are connected through the fourth communication pipe.
[0049] A first solenoid valve is fixedly installed on the outside of the first communication pipe, a second solenoid valve is fixedly installed on the outside of the second communication pipe, a third solenoid valve is fixedly installed on the outside of the third communication pipe, and a fourth solenoid valve is fixedly installed on the outside of the fourth communication pipe.
[0050] In addition, by setting the first solenoid valve, the opening or closing of the first communication pipe can be controlled at regular intervals, so as to put the tailings inside the alcohol removal kettle into the inside of the water washing kettle through the first communication pipe. By setting the second solenoid valve, the opening or closing of the second communication pipe can be controlled at regular intervals, so as to put the lower oil layer inside the water washing kettle into the inside of the alkalization kettle through the second communication pipe. By setting the third solenoid valve, the opening or closing of the third communication pipe can be controlled at regular intervals, so as to put the impurities in the lower layer inside the alkalization kettle into the inside of the impurity kettle through the third communication pipe. By setting the fourth solenoid valve, the remaining water layer inside the alkalization kettle can be put into the inside of the acidification kettle through the fourth communication pipe to prepare for dropping acid, or the materials inside the acidification kettle can be slowly dropped into the inside of the alkalization kettle through the fourth communication pipe.
[0051] The alcohol removal kettle includes a first feed pipe, a first vacuum valve, a first discharge pipe, a first discharge valve, a first stirring mechanism, a condenser, a cooling water valve, a first steam engine, a first steam valve, a first temperature display, a first vent valve, a first intake pipe, and a first tail gas purifier.
[0052] Among them, the alcohol removal kettle is connected to the first feed pipe, the first vacuum valve is fixedly installed outside the first feed pipe, the alcohol removal kettle is connected to the first discharge pipe, the first discharge valve is fixedly installed outside the first discharge pipe, the first stirring mechanism is located inside the alcohol removal kettle, a cooling pipe is fixedly connected to the outlet of the condenser, and the cooling pipe is connected to the alcohol removal kettle, the condenser is fixedly installed outside the alcohol removal kettle, the cooling water valve is fixedly installed outside the cooling pipe, a first steam pipe is fixedly connected to the outlet of the first steam engine, and the first steam pipe is connected to the alcohol removal kettle, the first steam engine is fixedly installed outside the alcohol removal kettle, the first steam valve is fixedly installed outside the first steam pipe, the first temperature display is fixedly installed outside the alcohol removal kettle, the first intake pipe is connected to the alcohol removal kettle, the first vent valve is fixedly installed outside the first intake pipe, and the first tail gas purifier is fixedly installed outside the alcohol removal kettle.
[0053] In addition, by adjusting the first vacuum valve, the tailings can be poured into the inside of the alcohol removal kettle through the first feed pipe. By adjusting the first discharge valve, the materials inside the alcohol removal kettle can be discharged through the first discharge pipe. By setting the first stirring mechanism, the materials inside the alcohol removal kettle can be stirred. By setting the condenser and the cooling water valve, the materials inside the alcohol removal kettle can be cooled. By setting the first steam engine and the first steam valve, the materials inside the alcohol removal kettle can be heated. By setting the first temperature display, the temperature inside the alcohol removal kettle can be detected and displayed. By setting the first vent valve, the first intake pipe, and the first tail gas purifier, the tail gas generated during the processing of the tailings inside the alcohol removal kettle can be purified.
[0054] The water washing kettle includes a second feed pipe, a second vacuum valve, a second discharge pipe, a second discharge valve, a second steam engine, a second steam valve, a second temperature display, a second vent valve, a second intake pipe, a second tail gas purifier, a second stirring mechanism and a first water separator.
[0055] Among them, the water washing kettle is connected to the second feed pipe, the second vacuum valve is fixedly installed outside the second feed pipe, the water washing kettle is connected to the second discharge pipe, the second discharge valve is fixedly installed outside the second discharge pipe, the outlet of the second steam engine is fixedly connected with a second steam pipe, and the second steam pipe is connected to the water washing kettle, the second steam engine is fixedly installed outside the water washing kettle, the second steam valve is fixedly installed outside the second steam pipe, the second temperature display is fixedly installed outside the water washing kettle, the second intake pipe is connected to the water washing kettle, the second vent valve is fixedly installed outside the second intake pipe, the second tail gas purifier is fixedly installed outside the water washing kettle, the second stirring mechanism is located inside the water washing kettle, and the first water separator is fixedly installed outside the water washing kettle.
[0056] In addition, by adjusting the second vacuum valve, the material can be poured into the inside of the water washing kettle through the second feed pipe. By adjusting the second discharge valve, the material inside the water washing kettle can be discharged through the second discharge pipe. By setting the second stirring mechanism, the material inside the water washing kettle can be stirred. By setting the second steam engine and the second steam valve, the material inside the water washing kettle can be heated. By setting the second temperature display, the temperature inside the water washing kettle can be detected and displayed. By setting the second vent valve, the second intake pipe and the second tail gas purifier, the tail gas generated during the processing of the tail material inside the alcohol removal kettle can be purified. By setting the first water separator, the tail material and water can be stratified, and at the same time, the tail material and water can be filtered and purified.
[0057] The alkalization kettle includes a third feed pipe, a third vacuum valve, a third discharge pipe, a third discharge valve, a third stirring mechanism, a third steam engine, a third steam valve, a third temperature display, a second water separator, a third vent valve, a third intake pipe and a third tail gas purifier.
[0058] Among them, the alkalization kettle is connected to the third feed pipe, the third vacuum valve is fixedly installed outside the third feed pipe, the alkalization kettle is connected to the third discharge pipe, the third discharge valve is fixedly installed outside the third discharge pipe, the outlet of the third steam engine is fixedly connected with a third steam pipe, and the third steam pipe is connected to the alkalization kettle, the third steam engine is fixedly installed outside the alkalization kettle, the third steam valve is fixedly installed outside the third steam pipe, the third temperature display is fixedly installed outside the alkalization kettle, the third intake pipe is connected to the alkalization kettle, the third vent valve is fixedly installed outside the third intake pipe, the third tail gas purifier is fixedly installed outside the alkalization kettle, the third stirring mechanism is located inside the alkalization kettle, and the second water separator is fixedly installed outside the alkalization kettle.
[0059] In addition, by adjusting the third vacuum valve, the material can be poured into the inside of the alkalization kettle through the third feed pipe. By adjusting the third discharge valve, the material inside the alkalization kettle can be discharged through the third discharge pipe. By setting the third stirring mechanism, the material inside the alkalization kettle can be stirred. By setting the third steam engine and the third steam valve, the material inside the alkalization kettle can be heated. By setting the third temperature display, the temperature inside the alkalization kettle can be detected and displayed. By setting the third vent valve, the third inlet pipe and the third tail gas purifier, the tail gas generated during the processing of the tail material inside the alkalization kettle can be purified. By setting the second water separator, the tail material and water can be stratified, and at the same time, the tail material and water can be filtered and purified.
[0060] The impurity kettle includes a fourth feed pipe, a fourth vacuum valve, a fourth discharge pipe, a fourth discharge valve, a fourth stirring mechanism, a fourth steam engine, a fourth steam valve, a fourth temperature display, a third water separator, a storage bucket, a fourth vent valve, a fourth inlet pipe and a fourth tail gas purifier.
[0061] Among them, the impurity kettle is connected to the fourth feed pipe, the fourth vacuum valve is fixedly installed on the outside of the fourth feed pipe, the impurity kettle is connected to the fourth discharge pipe, the fourth discharge valve is fixedly installed on the outside of the fourth discharge pipe, the outlet of the fourth steam engine is fixedly connected with a fourth steam pipe, and the fourth steam pipe is connected to the impurity kettle. The fourth steam engine is fixedly installed on the outside of the impurity kettle, the fourth steam valve is fixedly installed on the outside of the fourth steam pipe, the fourth temperature display is fixedly installed on the outside of the impurity kettle, the fourth inlet pipe is connected to the impurity kettle, the fourth vent valve is fixedly installed on the outside of the fourth inlet pipe, the fourth tail gas purifier is fixedly installed on the outside of the impurity kettle, the fourth stirring mechanism is located inside the impurity kettle, the third water separator is fixedly installed on the outside of the impurity kettle, and the storage bucket is located below the fourth discharge valve.
[0062] In addition, by adjusting the fourth vacuum valve, the material can be poured into the inside of the impurity kettle through the fourth feed pipe. By adjusting the fourth discharge valve, the material inside the impurity kettle can be discharged through the fourth discharge pipe. By setting the fourth stirring mechanism, the material inside the impurity kettle can be stirred. By setting the fourth steam engine and the fourth steam valve, the material inside the impurity kettle can be heated. By setting the fourth temperature display, the temperature inside the impurity kettle can be detected and displayed. By setting the fourth vent valve, the fourth inlet pipe and the fourth tail gas purifier, the tail gas generated during the processing of the tail material inside the impurity kettle can be purified. By setting the third water separator, the tail material and water can be stratified, and at the same time, the tail material and water can be filtered and purified. The storage bucket is located below the fourth discharge pipe.
[0063] The acidification kettle includes a fifth feed pipe, a fifth vacuum valve, a timer, a fifth stirring mechanism, a fifth discharge pipe, and a fifth discharge valve.
[0064] Among them, the acidification kettle is communicated with the fifth feed pipe, the fifth vacuum valve is fixedly installed outside the fifth feed pipe, the acidification kettle is communicated with the fifth discharge pipe, the fifth discharge valve is fixedly installed outside the fifth discharge pipe, the fifth stirring mechanism is located inside the acidification kettle, and the timer is located outside the acidification kettle.
[0065] In addition, by adjusting the fifth vacuum valve, the material can be poured into the inside of the acidification kettle through the fifth feed pipe. By adjusting the fifth discharge valve, the material inside the acidification kettle can be discharged through the fifth discharge pipe. By setting the fifth stirring mechanism, the material inside the acidification kettle can be stirred. By setting the timer, the outside of the acidification kettle can have a timing effect to facilitate observing the time when the material inside the acidification kettle drops into the alkalization kettle.
[0066] A method for purifying and treating BP-3 tailings includes the following steps:
[0067] 1) Open the first vacuum valve, pour 1000 kg of tailings into the inside of the alcohol stripping kettle through the first feed pipe, and then close the first vacuum valve;
[0068] 1.1) By starting the first stirring mechanism, the 1000 kg of tailings inside the alcohol stripping kettle can be stirred;
[0069] 1.2) Open the cooling water valve of the condenser, put the coolant into the inside of the alcohol stripping kettle, and open the first steam valve. The first steam engine can heat the tailings inside the alcohol stripping kettle. By opening the first vent valve, the tail gas generated when the tailings inside the alcohol stripping kettle are heated will be put into the inside of the first tail gas purifier through the first intake pipe, and the first tail gas purifier can purify the tail gas;
[0070] 1.3) When the temperature inside the alcohol stripping kettle reaches ≥120 °C and there is no distillate observed in the alcohol stripping kettle, close the first steam valve and open the first vacuum valve to make the alcohol stripping kettle start to cool slowly;
[0071] 1.4) When the temperature inside the alcohol stripping kettle drops to 60 °C, by opening the first solenoid valve, the tailings inside the alcohol stripping kettle can be put into the inside of the water washing kettle through the first connecting pipe;
[0072] 2) By opening the second vacuum valve, 500 kg of water can be poured into the inside of the water washing kettle through the second feed pipe, and then start the second stirring mechanism to stir the tailings and water inside the water washing kettle;
[0073] 2.1) Open the second steam valve to heat the tailings and water inside the water washing kettle through the second steam engine;
[0074] 2.2) When the temperature inside the water-washing kettle rises to 80 °C and is stirred for 1 hour, after standing for 2 hours, the tailings and water can be stratified through the first water separator, and at the same time, the tailings and water can be filtered and purified. By opening the second vent valve, the tail gas generated when the temperature of the tailings inside the water-washing kettle rises will be discharged into the second tail gas purifier through the second inlet pipe, and the second tail gas purifier can purify the tail gas;
[0075] 3) By opening the second solenoid valve, the lower oil layer inside the water-washing kettle can be put into the alkalization kettle through the second connecting pipe. At the same time, by opening the third vacuum valve, 100 kg of alkali and 1500 kg of water can be poured into the alkalization kettle through the third feed pipe;
[0076] 3.1) By opening the third stirring mechanism, the materials inside the alkalization kettle can be stirred. At the same time, by opening the third steam valve, the materials inside the alkalization kettle can be heated by the third steam engine. By opening the third vent valve, the tail gas generated when the temperature of the materials inside the alkalization kettle rises will be discharged into the third tail gas purifier through the third inlet pipe, and the third tail gas purifier can purify the tail gas;
[0077] 3.2) When the temperature inside the alkalization kettle rises to 65 °C, keep it warm for 1 hour and stop stirring. After standing for 2 hours, the materials inside the alkalization kettle can be stratified through the second water separator, and at the same time, the materials and the water layer can be filtered and purified;
[0078] 3.3) By opening the third solenoid valve, the impurities in the lower layer inside the alkalization kettle can be put into the impurity kettle through the third connecting pipe;
[0079] 3.4) After removing the impurities, by opening the fourth solenoid valve, the remaining water layer inside the alkalization kettle can be put into the acidification kettle through the fourth connecting pipe to prepare for dropping acid;
[0080] 4) The impurities and water layer inside the impurity kettle can be filtered and purified through the third water separator;
[0081] 4.1) Open the fourth steam valve, and the impurities inside the impurity kettle can be heated by the fourth steam engine. By opening the fourth vent valve, the tail gas generated when the temperature of the impurities inside the impurity kettle rises will be discharged into the fourth tail gas purifier through the fourth inlet pipe, and the fourth tail gas purifier can purify the tail gas;
[0082] 4.2) When the temperature inside the impurity kettle rises to 65 °C, open the fourth vacuum valve to pour 800 kg of water into the impurity kettle through the fourth feed pipe, and open the fourth stirring mechanism to stir and heat the impurities and water inside the impurity kettle;
[0083] 4.3) Then add 50 kg of alkali into the impurity kettle through the fourth feed pipe. After stirring for 30 minutes, use a pH test paper to test the pH value at the sampling point. When the pH reaches 14, stop heat preservation and stirring;
[0084] 4.4) Take samples for inspection. By adjusting the fourth discharge valve, the lower layer of the material in the impurity kettle can be taken through the fourth discharge pipe. Transfer of materials is allowed only when BP-3 ≤ 1% or impurity 1 ≥ 85%. If BP-3 > 1% or impurity 1 < 85%, perform alkali washing again. By analogy, the maximum number of alkali washings is three times;
[0085] 4.5) The oil layer inside the impurity kettle can be filled into a storage barrel through the fourth discharge pipe, and the water layer can enter the third connecting pipe and be put into the inside of the alkalization kettle;
[0086] 5) By opening the fifth vacuum valve, 340 kg of hydrochloric acid can be poured into the inside of the acidification kettle through the fifth feed pipe. Then, by opening the fourth solenoid valve, the material inside the acidification kettle can be slowly dripped into the inside of the alkalization kettle through the fourth connecting pipe, and the time is controlled to be more than 40 minutes;
[0087] 5.1) Then start the third stirring mechanism to stir the material inside the alkalization kettle. At the same time, open the third steam valve to heat the material inside the alkalization kettle through the third steam engine;
[0088] 5.2) Keep the temperature inside the alkalization kettle at 65 °C, stir for 30 minutes, and then let it stand for 2 hours;
[0089] 5.3) By opening the third discharge valve, the material inside the alkalization kettle can be sampled and detected through the third discharge pipe. When impurity 1 ≤ 1% and BP-3 ≥ 96%, it is considered qualified later;
[0090] 5.4) Non-conforming products are immediately reworked. Without stratification, start stirring, add 100 kg of caustic soda flakes, stir for 30 minutes, let it stand for 2 hours and then stratify. The oil layer enters the impurity kettle, and 340 kg of hydrochloric acid is added dropwise to the water layer, stir for 30 minutes, let it stand for 2 hours, re-sample and detect. After the detection is qualified, the material layer is filled into a barrel, weighed, and labeled.
[0091] Preparations before feeding:
[0092] 1) Check whether the status labels of the operation site, equipment, and containers meet the requirements and are clean;
[0093] 2) Check whether the measuring instruments, platform scales, etc. meet the requirements and are clean;
[0094] 3) Check whether the power systems such as water, electricity, steam, and air pressure are normal, and check whether the electrical instruments are normal;
[0095] 4) Check whether the enamel inside the reaction kettle and tank is intact, and check whether the bottom valve is closed;
[0096] 5) Check whether all the required raw materials are ready;
[0097] 6) Check whether the tools are complete;
[0098] 7) Check whether the connection of the feed pipeline of the reactor is secure;
[0099] 8) Wear labor protection articles as required.
[0100] In case of emergency stop:
[0101] 1) Close all the heating valves of the reactor, open the vent valve, disconnect the power supply of the stirring motor, and the stop procedure is completed;
[0102] 2) In case of normal stop, the stop sequence of each kettle is opposite to the start-up sequence. Close each valve in turn and disconnect the power supply of the stirring motor;
[0103] 3) Remove the barreled materials, and do not leave a single unlabeled barrel on site;
[0104] 4) When starting up after emergency stop, there is no phenomenon of heat accumulation and sudden escape of a large amount of gas in the processes of alkalization, acidification, alkali washing, impurity purification and water washing. After emergency stop and start-up, just start the stirring, and other operations refer to the normal start-up procedure.
[0105] Abnormal handling:
[0106] 1) When the barrel leaks during heating of the raw materials, immediately stop heating and report to the production department for guidance on handling;
[0107] 2) When the raw materials expand and overflow during heating, immediately stop heating and report to the production department for guidance on handling;
[0108] 3) When the pot overflows during alkali addition, immediately stop adding alkali, stop heating, stop stirring, report to the production department for guidance on handling, and evacuate the personnel;
[0109] 4) When sudden power failure occurs, close all the heating valves of the reactor, open the vent valve, disconnect the power supply of the stirring motor, and the stop procedure is completed;
[0110] 5) When running material occurs during alcohol removal, stop the vacuum, stop heating and open the vent valve. When the temperature drops below 80 °C, then turn on the vacuum, turn on the stirring and turn on the heating in sequence;
[0111] 6) When the layers are disordered during layering, stop layering, stir for 30 minutes, and let it stand for 2 hours before layering again.
[0112] Environmental protection measures:
[0113] 1) Handle the materials with care when moving;
[0114] 2) When heating the materials, lay two layers of filter cloth under the bottom of the barrel;
[0115] 3) When transferring materials, operate in a filtration tank lined with filter cloth;
[0116] 4) If leakage is found in any link of the operation, stop the machine immediately and report to the production department for guidance on handling.
[0117] Example 1: The experimental detection method for the tailings of BP-3 includes the following steps:
[0118] 1) Feeding: 150 g of impurities (comprehensive sample), 250 g of dichloroethane, 105 °C at normal pressure, and 50 g of distillation solvent;
[0119] 2) Sampling and detection: BP-3: 30%, impurities: 37%, BP-1: 20%, and moisture: 0.1%;
[0120] 3) Put the sample into a 500 ml isobaric dropping funnel;
[0121] 4) Add a magnetic sleeve thermometer, a reflux pipe, 50 g of aluminum trichloride (containing 30% aluminum hydroxide), and 100 g of dichloroethane to a 1000 ml three-necked flask. Heat up to an internal temperature of 40 °C and start dropping the sample from the isobaric dropping funnel, controlling the internal temperature at 38 - 40 °C. Finish dropping in 1 hour and keep the reaction at a constant temperature for 1 hour, totaling 2 hours;
[0122] 5) Add 500 ml of water to a 1000 ml wide-mouth beaker. Slowly pour the reacted material in the 1000 ml three-necked flask into the 1000 ml wide-mouth beaker. After hydrolysis for 20 minutes, the hydrolysis is completed. Stir for 30 minutes, let it stand for 1 hour and then layer. The water is at the bottom layer and the material is at the upper layer. After separating the water layer, sample and detect the material: BP-3: 40%, impurities 10%, and BP-1: 50%.
[0123] Example 2: The experimental detection method for the tailings of BP-3 includes the following steps:
[0124] 1) Feeding: 150 g of impurities (separately packaged sample), 250 g of dichloroethane, 105 °C at normal pressure, and 50 g of distillation solvent;
[0125] 2) Sampling and detection: BP-3: 7.8%, impurities: 91.9%, BP-1: 0%, and moisture: 0.3%;
[0126] 3) Put the sample into a 500 ml isobaric dropping funnel;
[0127] 4) Add a magnetic sleeve thermometer, a reflux pipe, 50 g of aluminum trichloride (containing 30% aluminum hydroxide), and 100 g of dichloroethane to a 1000 ml three-necked flask. Heat up to an internal temperature of 40 °C and start dropping the sample from the isobaric dropping funnel, controlling the internal temperature at 38 - 40 °C. Finish dropping in 1 hour and keep the reaction at a constant temperature for 1 hour, totaling 2 hours;
[0128] 5) Hydrolyze in 1000 ml of water pre-cooled to 25 °C. Slowly pour in the material to prevent splashing and overheating during hydrolysis. When the temperature rises to 50 °C, immediately stop pouring. When the temperature drops to around 25 °C, start hydrolysis again. After the transfer hydrolysis is completed, stir for 30 minutes, let it stand for 1 hour and then layer. The water is in the lower layer and the material is in the upper layer. After separating the water layer, take a sample of the material for testing: BP-3: 52% and BP-1: 48%.
[0129] Experimental conclusion: Take 25 g of the sample in Example 1. According to the absolute content of BP-1 being 50%, add sodium carbonate and dimethyl sulfate to synthesize 20.5 g of crude BP-3. Take 25 g of the sample in Example 2. According to the absolute content of BP-1 being 50%, add sodium carbonate and dimethyl sulfate to synthesize 15.2 g of crude BP-3. Impurity 1 can be completely converted into BP-1. The BP-1 converted from impurity 1 can be used to synthesize BP-3. The original BP-3 contained in impurity 1 is basically not affected during the conversion and synthesis process.
[0130] Example 3: Experimental detection method for BP-3 tailings, including the following steps:
[0131] 1) Feeding: 50 g of refined residue (containing alcohol), 250 g of dichloroethane, at normal pressure of 105 °C and 50 g of distillation solvent:
[0132] 2) Sampling and testing: BP-3: 60%, impurities: 15%, BP-1: 1% and moisture: 0.2%;
[0133] 3) Put the sample into a 500 ml equal-pressure dropping funnel;
[0134] 4) Add a magnetic sleeve thermometer to a 1000 ml three-necked flask, add a reflux pipe, add 50 g of aluminum chloride (containing 30% aluminum hydroxide), add 100 g of dichloroethane, heat up to an internal temperature of 40 °C and start dropping the sample from the equal-pressure dropping funnel. Finish dropping in 1 hour, keep the temperature for reaction for 1 hour, hydrolyze. The weight of the hydrolysis water is 500 g, the water temperature is at room temperature, and after hydrolysis, it is ≤ 50 °C. Heat up to 80 °C, stir for 30 minutes, let it stand for 1 hour and then layer. The water is in the lower layer. Take a sample of the material layer after separating the water layer for testing: BP-3: 50%, impurities: 0% and BP-1: 20%.
[0135] Experimental conclusion:
[0136] 1. For the standing residue with a BP-3 content less than 60%, or the residue with a higher BP-3 content, without first separating the impurities, aluminum chloride containing aluminum hydroxide from Qianjia can be used to remove the two methoxy groups in the impurities without removing the methoxy group at the 4th position in the original BP-3.
[0137] 2. For safety, on the basis of protecting the methoxy group at the 4th position in BP-3, use aluminum chloride containing aluminum hydroxide to remove the two methoxy groups on impurity 1.
[0138] 3. Aluminum chloride containing aluminum hydroxide has a strong attacking ability on the 2nd and 4th methoxy groups on the benzene ring, but it loses its effect on BP-3 with a hydroxyl group at the 2nd position and a methoxy group at the 4th position.
[0139] Comprehensive opinion: Change the disposal method of BP-3 tailings. Change the disposal method of adding alkali and then dripping back with acid to remove impurities to directly converting impurities into BP-1 with aluminum chloride, then adding alkali and synthesizing BP-3 with dimethyl sulfate.
[0140] Taking every 100 kg of impurities treated as an example, the absolute content of impurities is 50%. For 100 kg of impurities, the water consumption in the process: 15 kg, aluminum chloride added: 100 kg, hydrolysis with water added: 1000 kg. Ignoring the water consumption of 15 kg in the process, after the 100 kg of impurities 1 + BP-3 undergoes treatment with aluminum chloride HOU, the reaction products are: 100 kg of BP-1 + BP-3.
[0141] After the aluminum chloride-containing wastewater is reused once, the pH value is adjusted to 7 with sodium hydroxide and then distilled. The distillate is reused continuously, and the distillation bottom residue is basic aluminum chloride, which can be used as a flocculant for sewage treatment.
[0142] The working principle of the above embodiments is as follows:
[0143] (1) Through the cooperative action among the first stirring mechanism, condenser, cooling water valve, first steam engine, first steam valve, first temperature display, first vent valve, first inlet pipe, and first tail gas purifier in the de-alcoholization kettle, the tailings can be de-alcoholized, and at the same time, the tailings can be cooled and heated. Cooperating with the first stirring mechanism, the tailings can be evenly cooled and heated to ensure the cooling and heating effects of the tailings, and the tail gas generated during the processing of the tailings can be purified.
[0144] (2) Through the cooperative action among the second feed pipe, second vacuum valve, second steam engine, second steam valve, second temperature display, second vent valve, second inlet pipe, second tail gas purifier, second stirring mechanism, and first water separator in the water washing kettle, the tailings can be washed with water, and the tailings can be stirred and heated to facilitate uniform heating of the tailings. At the same time, the tailings and water can be stratified, the tailings and water can be filtered and purified, and the tail gas generated during the processing of the tailings can be purified.
[0145] (3) Through the combined action among the third feed pipe, the third vacuum valve, the third stirring mechanism, the third steam engine, the third steam valve, the third temperature display, the second water separator, the third vent valve, the third intake pipe and the third tail gas purifier in the alkalization kettle, the tail material can be alkalized, stirred and heated, heated evenly, and at the same time, the tail material and water can be stratified, filtered and purified, and the tail gas generated during the processing of the tail material can be purified.
[0146] (4) Through the combined action among the fourth feed pipe, the fourth vacuum valve, the fourth discharge pipe, the fourth discharge valve, the fourth stirring mechanism, the fourth steam engine, the fourth steam valve, the fourth temperature display, the third water separator, the storage barrel, the fourth vent valve, the fourth intake pipe and the fourth tail gas purifier in the impurity kettle, the impurities and water layer can be filtered and purified, and at the same time, the impurities and water can be stirred, heated and kept warm, and the impurities and water can be stratified again, and the impurities and water can be filtered and purified to ensure the effect of impurity detection.
[0147] (5) Through the combined action among the fifth feed pipe, the fifth vacuum valve, the timer, the fifth stirring mechanism, the fifth discharge pipe and the fifth discharge valve in the acidification kettle, the material can be stirred and slowly dropped into the inner side of the alkalization kettle for processing and detection of the material.
[0148] (6) By setting the first solenoid valve, the first connecting pipe can be controlled to be opened or closed regularly, so as to put the tail material inside the de-alcoholization kettle into the inner side of the water washing kettle through the first connecting pipe. By setting the second solenoid valve, the second connecting pipe can be controlled to be opened or closed regularly, so as to put the lower oil layer inside the water washing kettle into the inner side of the alkalization kettle through the second connecting pipe.
[0149] (7) By setting the third solenoid valve, the third connecting pipe can be controlled to be opened or closed regularly, so as to put the impurities in the lower layer inside the alkalization kettle into the inner side of the impurity kettle through the third connecting pipe. By setting the fourth solenoid valve, the remaining water layer inside the alkalization kettle can be put into the inner side of the acidification kettle through the fourth connecting pipe to prepare for dropping acid, or the material inside the acidification kettle can be slowly dropped into the inner side of the alkalization kettle through the fourth connecting pipe.
[0150] Compared with the prior art, the overall structure is simple and convenient to use. The BP-3 tail material purification treatment equipment can effectively separate impurities from the tail material to ensure the effect and quality of the BP-3 tail material during processes such as synthesis, alkalization, acidification and alkali washing, avoid the accumulation of more and more impurities, improve the purification treatment effect of the BP-3 tail material, and the purification treatment equipment can well process qualified products, meet the needs of the staff, and improve the use efficiency and use effect of the purification treatment equipment.
[0151] It should be noted that in this text, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprising", "including" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements not only includes those elements but also includes other elements not expressly listed, or further includes elements inherent to such process, method, article or device. Without further limitation, an element defined by the statement "comprising an..." does not exclude the presence of additional identical elements in the process, method, article or device comprising the element.
[0152] Although embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A purification treatment device for BP-3 tailings, comprising a de-alcoholization kettle, a water-washing kettle, an alkalization kettle, an impurity kettle, an acidification kettle, a first connecting pipe, a second connecting pipe, a third connecting pipe and a fourth connecting pipe, characterized in that: The de-ethanolization kettle and the water-washing kettle are connected through a first connecting pipe, the water-washing kettle and the alkalization kettle are connected through a second connecting pipe, the alkalization kettle and the impurity kettle are connected through a third connecting pipe, and the alkalization kettle and the acidification kettle are connected through a fourth connecting pipe.
2. The purification treatment equipment for the BP-3 tailings according to claim 1, wherein: A first solenoid valve is arranged on the outer side of the first connecting pipe, a second solenoid valve is arranged on the outer side of the second connecting pipe, a third solenoid valve is arranged on the outer side of the third connecting pipe, and a fourth solenoid valve is arranged on the outer side of the fourth connecting pipe.
3. The BP-3 tailing purification treatment equipment according to claim 2, characterized in that: The de-ethanolization kettle includes a first feed pipe, a first vacuum valve, a first discharge pipe, a first discharge valve, a first stirring mechanism, a condenser, a cooling water valve, a first steam engine, a first steam valve, a first temperature display, a first vent valve, a first inlet pipe, and a first tail gas purifier.
4. A BP-3 tailing purification treatment device according to claim 3, characterized in that: The water-washing kettle includes a second feed pipe, a second vacuum valve, a second discharge pipe, a second discharge valve, a second steam engine, a second steam valve, a second temperature display, a second vent valve, a second inlet pipe, a second tail gas purifier, a second stirring mechanism, and a first water separator.
5. A BP-3 tailing purification treatment device according to claim 4, characterized in that: The alkalization kettle includes a third feed pipe, a third vacuum valve, a third discharge pipe, a third discharge valve, a third stirring mechanism, a third steam engine, a third steam valve, a third temperature display, a second water separator, a third vent valve, a third inlet pipe, and a third tail gas purifier.
6. The BP-3 tailing purification treatment equipment according to claim 5, wherein: The impurity kettle includes a fourth feed pipe, a fourth vacuum valve, a fourth discharge pipe, a fourth discharge valve, a fourth stirring mechanism, a fourth steam engine, a fourth steam valve, a fourth temperature display, a third water separator, a storage bucket, a fourth vent valve, a fourth inlet pipe, and a fourth tail gas purifier.
7. The BP-3 tailing purification treatment equipment according to claim 6, characterized in that: The acidification kettle includes a fifth feed pipe, a fifth vacuum valve, a timer, a fifth stirring mechanism, a fifth discharge pipe, and a fifth discharge valve.
8. A purification treatment method for BP-3 tailings, based on a BP-3 tailings purification treatment device as described in claim 7, characterized in that, It includes the following steps: 1) Open the first vacuum valve, pour 1000 kg of tailings into the inner side of the de-ethanolization kettle through the first feed pipe, and then close the first vacuum valve; 1.1) By starting the first stirring mechanism, the 1000 kg of tailings inside the de-ethanolization kettle can be stirred; 1.2) Open the cooling water valve of the condenser, put the coolant into the inner side of the de-ethanolization kettle, and open the first steam valve. The tailings inside the de-ethanolization kettle can be heated by the first steam engine; 1.3) When the temperature inside the de-ethanolization kettle reaches ≥120 °C and there is no distillate observed in the de-ethanolization kettle, close the first steam valve and open the first vacuum valve to make the de-ethanolization kettle start to cool down slowly; 1.4) When the temperature inside the de-ethanolization kettle drops to 60 °C, by opening the first solenoid valve, the tailings inside the de-ethanolization kettle can be put into the inner side of the water-washing kettle through the first connecting pipe; 2) By opening the second vacuum valve, 500 kg of water can be poured into the inner side of the water-washing kettle through the second water inlet pipe, and then start the second stirring mechanism to stir the tailings and water inside the water-washing kettle; 2.1) Open the second steam valve, and the tailings and water inside the water-washing kettle can be heated by the second steam engine; 2.2) When the temperature inside the water-washing kettle rises to 80 °C and is stirred for 1 hour, after standing for 2 hours, the tailings and water can be stratified through the first water separator, and at the same time, the tailings and water can be filtered and purified; 3) By opening the second solenoid valve, the lower oil layer inside the water-washing kettle can be put into the inside of the alkalization kettle through the second connecting pipe. At the same time, by opening the third vacuum valve, 100 kg of alkali and 1500 kg of water can be poured into the inside of the alkalization kettle through the third feed pipe; 3.1) By opening the third stirring mechanism, the materials inside the alkalization kettle can be stirred. At the same time, by opening the third steam valve, the materials inside the alkalization kettle can be heated by the third steam engine; 3.2) When the temperature inside the alkalization kettle rises to 65 °C, keep it warm for 1 hour and stop stirring. After standing for 2 hours, the materials inside the alkalization kettle can be stratified through the second water separator, and at the same time, the materials and the water layer can be filtered and purified; 3.3) By opening the third solenoid valve, the impurities in the lower layer inside the alkalization kettle can be put into the inside of the impurity kettle through the third connecting pipe; 3.4) After removing the impurities, by opening the fourth solenoid valve, the remaining water layer inside the alkalization kettle can be put into the inside of the acidification kettle through the fourth connecting pipe to prepare for dropping acid; 4) The impurities and the water layer inside the impurity kettle can be filtered and purified through the third water separator; 4.1) Open the fourth steam valve, and the impurities inside the impurity kettle can be heated by the fourth steam engine; 4.2) When the temperature inside the impurity kettle rises to 65 °C, open the fourth vacuum valve to pour 800 kg of water into the inside of the impurity kettle through the fourth feed pipe. Open the fourth stirring mechanism to stir and heat the impurities and water inside the impurity kettle; 4.3) Then add 50 kg of alkali to the impurity kettle through the fourth feed pipe. After stirring for 30 minutes, use a pH test paper to test the pH value at the sampling point. When the pH reaches 14, stop heat preservation and stirring; 4.4) Take a sample for inspection. By adjusting the fourth discharge valve, the lower layer of the impurity kettle can be taken through the fourth discharge pipe. When BP-3 ≤ 1% or impurity 1 ≥ 85%, it can be transferred. When BP-3 > 1% or impurity 1 < 85%, alkali wash it again, and so on, with a maximum of no more than three alkali washes; 4.5) The oil layer inside the impurity kettle can be filled into the storage barrel through the fourth discharge pipe, and the water layer can enter the third connecting pipe and be put into the inside of the alkalization kettle; 5) By opening the fifth vacuum valve, 340 kg of hydrochloric acid can be poured into the inside of the acidification kettle through the fifth feed pipe. Then, by opening the fourth solenoid valve, the materials inside the acidification kettle can be slowly dropped into the inside of the alkalization kettle through the fourth connecting pipe, and the time is controlled to be more than 40 minutes; 5.1) Then open the third stirring mechanism to stir the materials inside the alkalization kettle. At the same time, open the third steam valve to heat the materials inside the alkalization kettle by the third steam engine; 5.2) Keep the temperature inside the alkalization kettle at 65 °C, stir for 30 minutes, and then stand for 2 hours; 5.3) By opening the third discharge valve, the materials inside the alkalization kettle can be sampled and detected through the third discharge pipe. When impurity 1 ≤ 1% and BP-3 ≥ 96%, it is qualified; 5.4) Nonconforming products shall be reworked immediately. Without delamination, start stirring, add 100 kg of caustic soda flakes, stir for 30 minutes, let stand for 2 hours and then delaminate. The oil layer shall be put into the impurity kettle, and 340 kg of hydrochloric acid shall be added dropwise to the water layer, stir for 30 minutes, let stand for 2 hours, take a new sample for testing. After passing the test, the material layer shall be filled into barrels, measured, and labeled.
9. A purification treatment method for BP-3 tailings according to claim 8, characterized in that: In step 1.2), by opening the first vent valve, the tail gas generated when the tail material inside the alcohol stripping kettle is heated will be discharged into the inside of the first tail gas purifier through the first intake pipe, and the first tail gas purifier can purify the tail gas. In step 2.2), by opening the second vent valve, the tail gas generated when the tail material inside the water washing kettle is heated will be discharged into the inside of the second tail gas purifier through the second intake pipe, and the second tail gas purifier can purify the tail gas.
10. A method for purifying the tailings of BP-3 according to claim 8, characterized in that: In step 3.1), by opening the third vent valve, the tail gas generated when the material inside the alkalization kettle is heated will be discharged into the inside of the third tail gas purifier through the third intake pipe, and the third tail gas purifier can purify the tail gas. In step 4.1), by opening the fourth vent valve, the tail gas generated when the impurities inside the impurity kettle are heated will be discharged into the inside of the fourth tail gas purifier through the fourth intake pipe, and the fourth tail gas purifier can purify the tail gas.
Citation Information
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