Interval extraction device

Abstract

The utility model relates to the technical field of extraction, and discloses a clearance extraction device which comprises an extraction assembly, a washing assembly and a reverse extraction assembly, the extraction assembly comprises an extraction tower, an extraction agent feeding piece and a sulfonated material feeding piece, the discharge end of the extraction agent feeding piece is communicated with the extraction tower, and the extraction tower is provided with a first light liquid outlet and a first heavy liquid outlet; the washing assembly comprises a washing tower, the washing tower is communicated with the first light liquid outlet, and the washing tower is provided with a water inlet, a second light liquid outlet and a second heavy liquid outlet; the reverse extraction assembly comprises a reverse extraction tower communicated with the second light liquid outlet and an ammonia water feeding piece with the discharging end communicated with the reverse extraction tower, and the reverse extraction tower is provided with a third light liquid outlet and a third heavy liquid outlet. Through the device, extraction, washing and reverse extraction processes in a K acid production process can be realized.

Description

Technical Field

[0001] This utility model relates to the field of interstitial extraction technology, and specifically to an interstitial extraction device. Background Technology

[0002] 2-Amino-3,6,8-naphthalenetrisulfonic acid (K acid) is a light brown powder, slightly soluble in hot water, soluble in soda ash or caustic soda solution, and reacts with ferric oxide to produce a yellow-green color. It is mainly used in the preparation of azo reactive dyes, acid dyes, and organic synthetic pigments. The traditional synthesis process of K acid mainly uses 2-naphthol as raw material, and performs monosulfonation with sulfuric acid and fuming sulfuric acid to obtain G acid, R acid, and Scheffler acid. The amino G salt is then separated by potassium chloride salting out. The amino G salt is then aminated, acidified, and dried to obtain amino G acid. The amino G acid is then disulfonated with 65% fuming sulfuric acid, and finally diluted and centrifuged to obtain the finished K acid.

[0003] Publication No. CN111909061B discloses a production process for 2-amino-3,6,8-naphthalenetrisulfonic acid, characterized by the following steps: 2-naphthol undergoes a first sulfonation reaction to obtain a sulfonated material; the sulfonated material is diluted, and then an extractant is added for extraction to obtain dilute sulfuric acid and a first organic phase; during the dilution of the sulfonated material, the mass ratio of the sulfonated material to water is 1:(0.3~0.5), and the temperature is 70~85℃; during the extraction process, the extractant is a C8~C12 alkyl tertiary amine extractant, and the mass ratio of the extractant to the diluted sulfonated material is 1:( 1.0~1.2); the extraction temperature is controlled at 70~90℃; the first organic phase is washed, allowed to stand and separate into layers to obtain wash water and a second organic phase, then ammonia water is added to the second organic phase until the pH is 8~10, allowed to stand and separate into layers to obtain back-extraction liquid; the concentration of ammonia water used in obtaining back-extraction liquid is 10%~20%; ammonium bisulfite solution is added to the back-extraction liquid, and liquid ammonia is introduced at the same time to carry out ammoniation, after ammoniation is completed, deammoniation is carried out; the deammoniation material is acidified, and then separated into solid and liquid to obtain mixed dry powder; the mixed dry powder is subjected to a second sulfonation reaction to obtain 2-amino-3,6,8-naphthalenetrisulfonic acid.

[0004] The extraction, washing, and back-extraction processes of sulfonated materials were not disclosed in terms of the equipment used, making it impossible to clearly understand the structure of the extraction, washing, and back-extraction equipment for sulfonated materials. Utility Model Content

[0005] The purpose of this invention is to overcome the above-mentioned technical deficiencies and propose an intermittent extraction device to solve the technical problem that the structure of the extraction, washing, and back-extraction devices for sulfonated materials in the prior art is unclear.

[0006] To achieve the above-mentioned technical objectives, the present invention adopts the following technical solution:

[0007] This utility model provides an intermittent extraction device, including an extraction component, a washing component, and a back-extraction component. The extraction component includes an extraction tower and an extractant feeder and a sulfonated material feeder connected to the extraction tower at the discharge end. The extraction tower has a first light liquid outlet and a first heavy liquid outlet. The washing component includes a washing tower connected to the first light liquid outlet and has a water inlet, a second light liquid outlet, and a second heavy liquid outlet. The back-extraction component includes a back-extraction tower connected to the second light liquid outlet and an ammonia water feeder connected to the back-extraction tower at the discharge end. The back-extraction tower has a third light liquid outlet and a third heavy liquid outlet.

[0008] In one embodiment, the washing assembly further includes a water inlet, which includes a water storage tank and a water pump. The inlet end of the water pump is connected to the water storage tank, and the outlet end is connected to the water inlet of the washing tower.

[0009] In one embodiment, the washing assembly further includes a return water pump, the inlet of which is connected to the outlet of the third heavy liquid and the outlet of which is connected to the extraction tower.

[0010] In one embodiment, the ammonia feed unit includes an ammonia tank and an ammonia pump, wherein the inlet end of the ammonia pump is connected to the ammonia tank and the outlet end is connected to the back-extraction tower.

[0011] In one embodiment, the back-extraction assembly further includes a reflux member, the inlet of which is connected to the third light liquid outlet of the back-extraction tower, and the outlet of which is connected to the extraction tower.

[0012] In one embodiment, the reflux unit includes a reflux tank and a reflux pump. The reflux tank is connected to the third light liquid outlet of the back-extraction tower, and the inlet end of the reflux pump is connected to the reflux tank, while the outlet end is connected to the extraction tower.

[0013] In one embodiment, the extraction assembly further includes a plurality of fixed rings and a stirring element, wherein the plurality of fixed rings are built into the extraction tower and spaced apart along the axial direction of the extraction tower, and the stirring element is connected to the extraction tower and is at least partially rotatably built into the extraction tower.

[0014] In one embodiment, the stirring element includes a rotating shaft, a plurality of rotating disks, and a driving unit. The rotating shaft is rotatably connected to the extraction tower and is arranged along the axial direction of the extraction tower. The plurality of rotating disks are connected to the rotating shaft and are spaced apart along the axial direction of the rotating shaft. The driving unit is connected to the rotating shaft and the extraction tower and is used to drive the rotating shaft to rotate.

[0015] In one embodiment, the washing tower has a hollow cylindrical structure inside, and the washing tower is provided with a light liquid inlet and a heavy liquid inlet. The heavy liquid inlet is located above the light liquid inlet, the light liquid inlet is connected to the first light liquid outlet, and the heavy liquid inlet is connected to the outlet of the water pump.

[0016] In one embodiment, the washing assembly further includes a dispersion plate, which is built into the washing tower and disposed between the heavy liquid inlet and the light liquid inlet, and the dispersion plate has a plurality of spaced-apart equalization holes.

[0017] Compared with the prior art, the intermittent extraction device provided by this utility model allows the sulfonated material feeder and the extractant feeder to be fed into the extraction tower for extraction, yielding dilute sulfuric acid and a first organic phase. The dilute sulfuric acid is discharged from the first heavy liquid outlet, and the first organic phase enters the washing tower from the first light liquid outlet. Washing water is introduced into the washing tower to wash the first organic phase, yielding wash water and a second organic phase. The wash water is discharged from the second heavy liquid outlet, and the second organic phase enters the back-extraction tower from the second light liquid outlet. Ammonia water is introduced into the back-extraction tower through the ammonia water feeder, yielding back-extraction liquid and extractant. The back-extraction liquid is discharged from the third heavy liquid outlet, and the extractant is discharged from the third light liquid outlet. Through the above device, extraction, washing, and back-extraction in the K acid production process are realized. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the interstitial extraction device provided in one embodiment of the present invention;

[0019] Figure 2 This is a schematic diagram of the structure of the extraction component in an intermittent extraction device provided in an embodiment of the present invention;

[0020] Figure 3 This is a schematic diagram of the washing component in an intermittent extraction device according to an embodiment of the present invention;

[0021] Figure 4 This is a schematic diagram of the back-extraction component in an intermittent extraction device provided in an embodiment of the present invention.

[0022] Explanation of reference numerals in the attached figures:

[0023] Extraction component 1;

[0024] Extraction tower 11;

[0025] First light liquid outlet 11a;

[0026] First heavy liquid outlet 11b;

[0027] Extractant feed unit 12;

[0028] Extractant storage tank 121;

[0029] First injection pump 122;

[0030] 13. Sulfonated material feeder;

[0031] Sulfonated material storage tank 131;

[0032] Second injection pump 132;

[0033] Retaining ring 14;

[0034] Mixing component 15;

[0035] Shaft 151;

[0036] Turntable 152;

[0037] Drive unit 153;

[0038] Washing component 2;

[0039] Scrubber 21;

[0040] Inlet 21a;

[0041] Second light liquid outlet 21b;

[0042] Second heavy liquid outlet 21c;

[0043] Water inlet component 22;

[0044] Water storage tank 221;

[0045] Water pump 222;

[0046] Return water pump 23;

[0047] Distributed plate 24;

[0048] Back-extraction component 3;

[0049] Anti-extraction tower 31;

[0050] Third light liquid outlet 31a;

[0051] Third heavy liquid outlet 31b;

[0052] Ammonia feeder 32;

[0053] Ammonia tank 321;

[0054] Ammonia pump 322;

[0055] Return component 33;

[0056] Return box 331;

[0057] Reflux pump 332. Detailed Implementation

[0058] To make the objectives, technical solutions, and advantages of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present utility model and are not intended to limit the present utility model.

[0059] To address the technical problem of unclear structure of extraction, washing, and back-extraction devices for sulfonated materials, this utility model provides an intermittent extraction device capable of extracting, washing, and back-extracting sulfonated materials.

[0060] It should be noted that the intermittent extraction device described in this utility model is used for, but not limited to, extraction, washing, and back-extraction processes in the production of ketonic acid. For ease of explanation, this utility model only uses the application of the intermittent extraction device in the extraction, washing, and back-extraction processes in the production of ketonic acid as an example. The principle of the intermittent extraction device applied to other types of equipment is essentially the same as that applied to compound preparation, and will not be elaborated here.

[0061] Please see Figure 1 , Figure 1 This is a schematic diagram of the intermittent extraction device in one embodiment of the present invention. The intermittent extraction device includes an extraction component 1, a washing component 2, and a back-extraction component 3. The extraction component 1 includes an extraction tower 11 and an extractant feed 12 and a sulfonated material feed 13 connected to the extraction tower 11 at the discharge end. The extraction tower 11 has a first light liquid outlet 11a and a first heavy liquid outlet 11b. The washing component 2 includes a washing tower 21 connected to the first light liquid outlet 11a. The washing tower 21 has a water inlet 21a, a second light liquid outlet 21b, and a second heavy liquid outlet 21c. The back-extraction component 3 includes a back-extraction tower 31 connected to the second light liquid outlet 21b and an ammonia water feed 32 connected to the back-extraction tower 31 at the discharge end. The back-extraction tower 31 has a third light liquid outlet 31a and a third heavy liquid outlet 31b.

[0062] Sulfonated material feed 13 and extractant feed 12 respectively feed the sulfonated material and extractant into extraction tower 11 for extraction, yielding dilute sulfuric acid and a first organic phase. The dilute sulfuric acid is discharged from the first heavy liquid outlet 11b, and the first organic phase enters the washing tower 21 from the first light liquid outlet 11a. Washing water is introduced into the washing tower 21 to wash the first organic phase, yielding wash water and a second organic phase. The wash water is discharged from the second heavy liquid outlet 21c, and the second organic phase enters the back-extraction tower 31 from the second light liquid outlet 21b. Ammonia water is introduced into the back-extraction tower 31 through ammonia water feed 32, yielding back-extraction liquid and extractant. The back-extraction liquid is discharged from the third heavy liquid outlet 31b, and the extractant is discharged from the third light liquid outlet 31a. Through the above device, extraction, washing, and back-extraction in the K acid production process are realized. Moreover, in this invention, both extraction and back-extraction adopt intermittent extraction, which can produce intermittently according to the required product, providing high flexibility and allowing adjustment according to different production conditions.

[0063] It should be understood that in the K acid production process, after the back-extraction solution is formed, it still needs to undergo ammoniation, deammoniation, acidification, and solid-liquid separation. These processes are carried out in a reactor or microreactor, deammoniation in the middle of the distillation column, acidification in a reactor or microreactor, and solid-liquid separation in a solid-liquid separator. The reactor, distillation column, and solid-liquid separator are connected in sequence to process the back-extraction solution sequentially. This process is existing technology and will not be described in detail in this application.

[0064] It should be understood that the washing water can flow into the washing tower 21 spontaneously under the action of gravity, or it can be actively pumped into the washing tower 21. Specifically, in one embodiment, the washing assembly 2 also includes a water inlet 22, which includes a water storage tank 221 and a water pump 222. The inlet end of the water pump 222 is connected to the water storage tank 221, and the outlet end is connected to the water inlet of the washing tower 21.

[0065] When it is necessary to wash the first organic phase with washing water, the water pump 222 is started, and the water pump 222 pumps the washing water into the washing tower 21 to wash the first organic phase in the washing tower 21.

[0066] The sulfonated material needs to be diluted with water, and excess washing water will be generated during the operation of the washing tower 21. Therefore, in one embodiment, the washing assembly 2 also includes a return water pump 23, the inlet of which is connected to the third heavy liquid outlet 31b and the outlet is connected to the extraction tower 11.

[0067] The washing water generated during the washing process is sent back to the extraction tower 11 by the return water pump 23 to dilute the sulfonated material in the extraction tower 11, reduce the amount of dilution water used, and reuse the washing water.

[0068] It should be understood that the extractant feed 12 and the sulfonated material feed 13 can be pipes or injection pumps capable of introducing extractant and sulfonated material into the extraction tower 11. Specifically, in one embodiment, the extractant feed 12 includes an extractant storage tank 121 and a first injection pump 122, with the inlet end of the first injection pump 122 connected to the extractant storage tank 121 and the outlet end connected to the extraction tower 11; the sulfonated material feed 13 includes a sulfonated material storage tank 131 and a second injection pump 132, with the inlet end of the second injection pump 132 connected to the sulfonated material storage tank 131 and the outlet end connected to the extraction tower 11.

[0069] The first injection pump 122 adds the extractant from the extractant storage tank 121 to the extraction tower 11 according to the set amount; the second injection pump 132 adds the sulfonated material from the sulfonated material storage tank 131 to the extraction tower 11 according to the set amount.

[0070] It should be understood that ammonia water can flow spontaneously into the back-extraction tower 31 under the action of gravity, or it can be actively pumped into the back-extraction tower 31. Specifically, in one embodiment, the ammonia water feed unit 32 includes an ammonia water tank 321 and an ammonia water pump 322. The inlet end of the ammonia water pump 322 is connected to the ammonia water tank 321, and the outlet end is connected to the back-extraction tower 31.

[0071] During back-extraction, ammonia pump 322 pumps ammonia water from ammonia tank 321 into back-extraction tower 31. The ammonia water is back-extracted with the second organic phase in extraction tower 11. The pH value of the organic phase is adjusted so that the distribution coefficient of the target product and its related impurities between the organic phase and the aqueous phase changes, thereby causing the target product to transfer from the organic phase to the aqueous phase.

[0072] When the extraction tower 11 performs extraction, it needs to consume extractant. The back-extraction tower 31 will form extractant when it is working. In order to reduce the consumption and waste of extractant, in one embodiment, the back-extraction component 3 also includes a reflux member 33. The inlet end of the reflux member 33 is connected to the third light liquid outlet 31a of the back-extraction tower 31, and the outlet end is connected to the extraction tower 11.

[0073] In the back-extraction tower 31, ammonia reacts with the second organic phase to form an extractant and a back-extraction liquid. The formed extractant is fed into the extraction tower 11 under the action of the reflux element 33, realizing the recovery and utilization of the extractant and reducing the consumption of the extractant.

[0074] It should be understood that the extractant can spontaneously return to the extraction tower 11 through the pipeline under the action of gravity, or it can be returned to the extraction tower 11 by pumping. Specifically, in one embodiment, the reflux component 33 includes a reflux box 331 and a reflux pump 332. The reflux box 331 is connected to the third light liquid outlet 31a of the back-extraction tower 31. The inlet end of the reflux pump 332 is connected to the reflux box 331, and the outlet end is connected to the extraction tower 11.

[0075] The extractant formed during the back-extraction process is collected in the reflux box 331, and then pumped into the extraction tower 11 by the reflux pump 332.

[0076] To ensure thorough mixing of the extractant and the sulfonated material, in one embodiment, the extraction assembly 1 further includes a plurality of fixed rings 14 and a stirring element 15. The plurality of fixed rings 14 are built into the extraction tower 11 and are spaced apart along the axial direction of the extraction tower 11. The stirring element 15 is connected to the extraction tower 11 and is at least partially rotatably built into the extraction tower 11.

[0077] By setting multiple fixed rings 14, the flow path of the extractant and sulfonated material can be restricted. By setting a stirrer 15, the water in the extraction tower 11 can be stirred to promote full contact between the extractant and the sulfonated material. After stirring, the stirrer 15 is turned off, and the dilute sulfuric acid and the first organic phase are allowed to settle and separate.

[0078] In order to achieve sufficient dispersion of materials, in one embodiment, the retaining ring 14 is provided with multiple through holes (not shown in the figure) along the axial direction, so that the materials can be dispersed through the through holes.

[0079] The stirring component 15 can be a stirring paddle, a stirring pump, etc. Specifically, in one embodiment, the stirring component 15 includes a rotating shaft 151, a plurality of rotating disks 152 and a driving unit 153. The rotating shaft 151 is rotatably connected to the extraction tower 11 and is arranged along the axial direction of the extraction tower 11. The plurality of rotating disks 152 are connected to the rotating shaft 151 and are spaced apart along the axial direction of the rotating shaft 151. The driving unit 153 is connected to the rotating shaft 151 and the extraction tower 11 and is used to drive the rotating shaft 151 to rotate.

[0080] When stirring is required, the drive unit 153 is activated, which drives the rotating shaft 151 to rotate. The rotating shaft 151 drives multiple rotating disks 152 to rotate, and the rotating disks 152 stir the solution in the extraction tower 11.

[0081] The drive unit 153 can be a combination of a motor and a reducer, or a combination of a hydraulic motor and a reducer.

[0082] It should be understood that, in order to promote the full mixing of ammonia and the second organic phase in the back-extraction tower 31, the back-extraction tower 31 is also equipped with the same number of fixed rings and stirring elements as the extraction tower 11.

[0083] It should be understood that the washing tower 21 can be a vertical washing tower 21, a horizontal washing tower 21, a hollow washing tower 21, etc. Specifically, in one embodiment, the washing tower 21 has a hollow cylindrical structure inside. The washing tower 21 is provided with a light liquid inlet and a heavy liquid inlet. The heavy liquid inlet is located above the light liquid inlet. The light liquid inlet is connected to the first light liquid outlet 11a, and the heavy liquid inlet is connected to the outlet of the water pump 222.

[0084] The first organic phase is introduced into the bottom of the washing tower 21 from the first light liquid outlet 11a, and the washing water enters the top of the washing tower 21 from the heavy liquid inlet. The first organic phase flows upward and the washing water flows downward. The two flow in countercurrent contact, which can wash the first organic phase with water.

[0085] In order to promote the full dispersion of the first organic phase and the washing water during the washing process, in one embodiment, the washing assembly 2 further includes a dispersion disk 24, which is built into the washing tower 21 and disposed between the heavy liquid inlet and the light liquid inlet. The dispersion disk 24 has a plurality of spaced-apart equalization holes.

[0086] During the process of the first organic phase rising and the washing water falling, both must pass through the equalization holes of the dispersion disk 24 to fully disperse the first organic phase and the washing water, so that the first organic phase and the washing water can come into full contact.

[0087] It should be understood that in this utility model, valves are provided at both the light liquid outlet and the first heavy liquid outlet during the extraction and back-extraction processes. At this time, the valves are closed. After the organic phase and aqueous phase have settled and separated, the valve at the light liquid outlet is opened, and the organic phase overflows from the light liquid outlet. Then, the valve at the heavy liquid outlet is opened, and the aqueous phase is discharged from the heavy liquid outlet.

[0088] It should be understood that in this application, the first organic phase enters the washing tower 21, the washing water enters the extraction tower 11, the second organic phase enters the back-extraction tower 31, and the extractant returns to the extraction tower 11. This return can be achieved by gravity flow or by pumping. Specifically, in one embodiment...

[0089] To facilitate the flow of liquids, the first organic phase flows out from the first light liquid outlet 11a and is then pumped into the washing tower 21. In the washing tower 21, the washing water flows out from the second heavy liquid outlet 21c and is then pumped into the extraction tower 11. The second organic phase flows out from the second light liquid outlet 21b and enters the back-extraction tower 31 under the action of a pump.

[0090] The specific embodiments of this utility model described above do not constitute a limitation on the scope of protection of this utility model. Any other corresponding changes and modifications made based on the technical concept of this utility model should be included within the scope of protection of the claims of this utility model.

Claims

1. A gap extraction device, characterized in that, The device comprises: an extraction assembly comprising an extraction column and an extractant feeding device and a sulfonated material feeding device connected to the extraction column, the extraction column having a first light liquid outlet and a first heavy liquid outlet; a washing assembly comprising a washing column connected to the first light liquid outlet, the washing column having a water inlet, a second light liquid outlet and a second heavy liquid outlet; and a reverse extraction assembly comprising a reverse extraction column connected to the second light liquid outlet and an ammonia water feeding device connected to the reverse extraction column, the reverse extraction column having a third light liquid outlet and a third heavy liquid outlet.

2. The gap extraction device according to claim 1, wherein: the washing assembly further comprises a water feeding device, the water feeding device comprising a water storage tank and a water pump, the water pump having a liquid inlet connected to the water storage tank and a liquid outlet connected to the water inlet of the washing column.

3. The gap extraction device according to claim 2, wherein: the washing assembly further comprises a backwater pump, the backwater pump having a liquid inlet connected to the third heavy liquid outlet and a liquid outlet connected to the extraction column.

4. The gap extraction device according to claim 1, wherein: the ammonia water feeding device comprises an ammonia water tank and an ammonia water pump, the ammonia water pump having a liquid inlet connected to the ammonia water tank and a liquid outlet connected to the reverse extraction column.

5. The gap extraction device according to claim 1, wherein: the reverse extraction assembly further comprises a backflow device, the backflow device having a liquid inlet connected to the third light liquid outlet of the reverse extraction column and a liquid outlet connected to the extraction column.

6. The gap extraction device according to claim 5, wherein: the backflow device comprises a backflow tank and a backflow pump, the backflow tank being connected to the third light liquid outlet of the reverse extraction column, the backflow pump having a liquid inlet connected to the backflow tank and a liquid outlet connected to the extraction column.

7. The gap extraction device according to claim 6, wherein: the extraction assembly further comprises a plurality of fixed rings and a stirring device, the fixed rings being arranged in the extraction column and spaced along the axial direction of the extraction column, the stirring device being connected to the extraction column and at least partially rotating in the extraction column.

8. The gap extraction device according to claim 7, wherein: the stirring device comprises a rotating shaft, a plurality of rotating discs and a driving part, the rotating shaft being rotatably connected to the extraction column and arranged along the axial direction of the extraction column, the rotating discs being connected to the rotating shaft and spaced along the axial direction of the rotating shaft, the driving part being connected to the rotating shaft and the extraction column and configured to drive the rotating shaft to rotate.

9. The gap extraction device according to claim 2, wherein: the washing column has a hollow cylindrical structure, the washing column being provided with a light liquid inlet and a heavy liquid inlet, the heavy liquid inlet being located above the light liquid inlet, the light liquid inlet being connected to the first light liquid outlet, and the heavy liquid inlet being connected to the water outlet of the water pump.

10. The gap extraction device according to claim 9, wherein: The washing assembly further comprises a dispersion disc which is built in the washing tower and arranged between the heavy liquid inlet and the light liquid inlet, and the dispersion disc is provided with a plurality of evenly distributed liquid equalizing holes.

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