CN113968778B - Device and process for continuous water-out extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid by one-step method - Google Patents
Device and process for continuous water-out extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid by one-step method Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000000605 extraction Methods 0.000 title claims abstract description 35
- JZFDKGFWNSQAHU-UHFFFAOYSA-N 2-(4-ethylbenzoyl)benzoic acid Chemical compound C1=CC(CC)=CC=C1C(=O)C1=CC=CC=C1C(O)=O JZFDKGFWNSQAHU-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000005191 phase separation Methods 0.000 title claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 142
- 238000000926 separation method Methods 0.000 claims abstract description 84
- 238000002156 mixing Methods 0.000 claims abstract description 57
- 239000002253 acid Substances 0.000 claims abstract description 48
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
- 239000002699 waste material Substances 0.000 description 11
- 238000005406 washing Methods 0.000 description 9
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- 239000007787 solid Substances 0.000 description 5
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- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 4
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- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
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- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 2
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- 239000003513 alkali Substances 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The application relates to the technical field of 2-ethyl anthraquinone synthesis, in particular to a device and a process for separating phases by continuous water-out extraction of 2- (4' -ethyl benzoyl) benzoic acid closed-loop liquid by a one-step method. The device mainly comprises a water separation kettle with an inner cylinder and an outer cylinder, an outer circulating pump and a heat exchanger. Continuously introducing closed-loop liquid, an extractant and process water into an inner barrel of a relatively independent elutriation kettle from different positions for mixing, standing the mixed liquid in an outer barrel of the elutriation kettle, and overflowing layered extract liquid from the elutriation kettle, and cooling and refluxing layered acid water to the inner barrel of the elutriation kettle after circulating heat exchange. The invention realizes continuous feeding and discharging, shortens the process flow, reduces the number of production equipment, saves the construction cost, and has the advantages of more convenient operation, higher production efficiency and environmental protection.
Description
Technical Field
The invention relates to the technical field of 2-ethyl anthraquinone synthesis, in particular to a device and a process for separating phases by continuous water-out extraction of 2- (4' -ethyl benzoyl) benzoic acid closed-loop liquid by a one-step method.
Background
The 2-ethyl anthraquinone is light yellow powder or bright yellow scale-shaped solid, is an important fine chemical raw material, and is mainly used for preparing hydrogen peroxide. 2-ethyl anthraquinone is also used to prepare photosensitive compounds, and is a sensitizer for photopolymerization or polymerization inhibition-grade polymerization; and also used for preparing dyes, light screen resin and agricultural chemical fertilizers. In recent years, 2-ethyl anthraquinone has also been found to have a tumor inhibiting effect, and is an effective medical intermediate.
The current general method for industrially producing 2-ethyl anthraquinone is to react ethylbenzene with phthalic anhydride, mainly due to the rapid development of petrochemical industry, so as to provide sufficient raw materials for the reaction. The industrial production method of 2-ethyl anthraquinone mainly comprises the following two steps:
(1) Preparation of 2- (4' -ethylbenzoyl) benzoic acid (BE acid for short)
Takes ethylbenzene and phthalic anhydride as raw materials, and takes Friedel-Crafts reaction in organic solvent under the catalysis of aluminum trichloride to synthesize 2- (4' -ethylbenzoyl) aluminum benzoate double salt. The 2- (4' -ethyl benzoyl) aluminum benzoate double salt is hydrolyzed in an acidic aqueous solution to generate an organic solution of BE acid, and the reaction solvent is removed to obtain pure BE acid.
(2) Preparation of 2-ethyl anthraquinone
And (3) dehydrating and closing the loop by BE acid under the catalysis of concentrated sulfuric acid or fuming sulfuric acid to obtain a closed loop liquid. Then, by utilizing the property that 2-ethyl anthraquinone is dissolved in concentrated sulfuric acid but not dissolved in dilute sulfuric acid, the closed-loop liquid is diluted by process water, and after water separation, two treatment methods are generally adopted: (2.1) directly filtering to separate out a solid 2-ethyl anthraquinone crude product; and (2.2) diluting the ring-closed liquid to a certain concentration, adding an organic solvent, extracting the 2-ethyl anthraquinone into an organic solvent phase, layering to obtain an extract and acid wastewater, and removing the solvent from the extract to obtain a solid 2-ethyl anthraquinone crude product.
The 2-ethyl anthraquinone ring-closing liquid contains a large amount of fuming sulfuric acid, so that heat is released strongly during water separation, and in the traditional water separation process, the generated heat cannot be removed in time, so that the local overheating phenomenon is serious, and further, the reaction in the production process is uncontrollable, and byproducts such as sulphonates, cokes and the like are inevitably generated.
Chinese patent publication No.: CN102050716B, entitled: a method for separating and purifying 2-ethyl anthraquinone from sulfuric acid includes such steps as slowly adding the concentrated sulfuric acid solution of 2-ethyl anthraquinone obtained by ring-closing reaction to water for water separation, extracting, separating, alkaline washing, water washing, separating again, and distilling to obtain 2-ethyl anthraquinone with high purity. The preparation method has long reaction time, low production efficiency and poor heat transfer effect, and is not suitable for the current industrial production.
Chinese patent publication No.: CN110790656a, entitled: an acid separation technology for closed-loop liquid of 2-ethyl anthraquinone features that an acid separation external circulation system is composed of acid separation reactor, acid separation external circulation pump, external circulation cooler and mixer, so improving the mass and heat transfer effect in the acid separation process of closed-loop liquid. Although the method improves the efficiency of the ring-closure reaction to a certain extent, the process flow is longer, a large amount of 2-ethyl anthraquinone solid is suspended in the water-separation finished liquid, and the pipeline is easy to be blocked when overflowed into the extraction process.
Chinese patent publication No.: CN211463172U, entitled: the utility model provides an acid-out reation kettle is used in 2-ethyl anthraquinone production, its disclosed water-out reation kettle adopts dual heat transfer medium to carry out the heat transfer, has strengthened mixing and heat transfer effect, but its equipment structure is comparatively complicated, is limited by the equipment type, and total heat transfer area is limited, and the solid that separates out is very easy deposit in equipment in addition, is inconvenient for washing and inspection maintenance.
Disclosure of Invention
The water separation, extraction and phase separation of the 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid in the prior art are divided into a plurality of steps, and the technical problems of multiple and complex equipment and longer production flow exist.
In one aspect, the application provides a device for continuous water-out extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid by a one-step method, which comprises a water-out kettle, a circulating pump and a heat exchanger which are connected with the water-out kettle, wherein the water-out kettle comprises a cylindrical water-out kettle cylinder body with an opening at the upper part and a mixing cylinder, the lower end of the mixing cylinder extends into the inner cavity of the water-out kettle cylinder body through the opening of the water-out kettle cylinder body, and the mixing cylinder is communicated with the inner cavity of the water-out kettle cylinder body; the first pipeline is communicated with a first outlet formed in the bottom of the water separation kettle cylinder body and a third outlet formed in the upper part of the water separation kettle cylinder body to control the gas-liquid internal balance of the water separation kettle cylinder body, and an acid water outflow pipeline is arranged in the first pipeline to control the liquid level in the water separation kettle to be higher than the lower end face of the mixing cylinder; a second outlet formed in the middle lower part of the water separation kettle cylinder body and a circulating liquid inlet formed in the mixing cylinder far away from the lower end surface are communicated through a second pipeline so as to enable liquid in the water separation kettle to circularly flow, and a heat exchanger and a circulating pump are connected in the second pipeline so as to timely remove heat generated in the closed loop reaction process; the middle upper part of the water separation kettle barrel is also provided with a fifth outlet for overflow discharge of layered extract, and the mixing barrel is further provided with a closed-loop liquid inlet far away from the lower end surface; adding priming circulating liquid into a circulating liquid inlet of a mixing drum in advance, stopping the circulating liquid flowing out of the acid water outflow pipeline, sealing the acid water outflow pipeline, continuously adding the circulating liquid, closed-loop liquid and extractant, mixing in the mixing drum, entering a water separation kettle barrel, standing, separating and layering an organic phase and a water phase, discharging an extract liquid obtained by separating and separating the layers from each other by overflow of a fifth outlet, entering a subsequent refining step to prepare 2-ethyl anthraquinone, timely removing heat generated in a closed-loop reaction process by the circulating liquid obtained by separating and separating the layers from the second pipeline, and circularly refluxing to the mixing drum.
Specifically, the lower end surface of the mixing drum extending into the inner cavity of the water separation kettle cylinder body is provided with a plurality of through holes, so that the mixing drum is communicated with the inner cavity of the water separation kettle cylinder body.
Specifically, the second pipeline is connected with a pipeline for introducing process water and a pipeline for introducing an extracting agent in a tapping way.
Specifically, the mixing drum is provided with an extractant inlet.
Specifically, the mixing drum is provided with a mixing device, and the mixing device is one or more groups of stirring paddles or one or more groups of static mixers.
Specifically, a fourth outlet for exhaust emission is formed in the upper portion of the water separation kettle barrel.
In another aspect, the present application proposes a process for continuous water separation and extraction phase separation using 2- (4 '-ethylbenzoyl) benzoic acid ring-closing liquid one-step method of the device according to claim 1, wherein the volume flow ratio of the ring-closing liquid for 2- (4' -ethylbenzoyl) benzoic acid ring-closing liquid water separation, extraction and phase separation, the extractant, the process water feed and the circulating liquid is in the range of 1:1.3 to 2:1 to 3.5:50 to 500.
Specifically, the temperature of the liquid in the outer cylinder of the water separation kettle is controlled to be 30-80 ℃.
Specifically, the process water is industrial water or waste water generated in the production process of 2-ethyl anthraquinone.
Specifically, the extractant is toluene.
The technical scheme has the following advantages or beneficial effects: the water separation kettle with the inner and outer barrel structures and the related equipment pipelines are specially designed, so that the water separation and extraction efficiency is improved, three procedures of water separation, extraction and automatic phase separation of an extraction liquid and waste acid water are finished in one equipment, continuous feeding and discharging are realized, the process flow is shortened, the number of production equipment is reduced, the construction cost is saved, the operation is more convenient, the production efficiency is higher, and the process is more environment-friendly.
Drawings
FIG. 1 is a schematic diagram of a 2- (4' -ethylbenzoyl) benzoic acid ring-closing liquid one-step continuous water-out extraction phase separation device of the application.
FIG. 2 is a schematic diagram of another variation of the 2- (4' -ethylbenzoyl) benzoic acid ring-closing liquid one-step continuous water-out extraction phase separation device of the present application.
Wherein, 1, a water separation kettle cylinder; 2. a mixing drum; 3. an inner cavity of the water separation kettle cylinder body; 4. a through hole; 5. an inner cavity of the mixing drum; 6. a first outlet; 7. a second outlet; 8. a third outlet; 9. a fourth outlet; 10. a first pipe; 11. acid water outflow pipe; 12. a circulating liquid inlet; 13. a second pipe; 14. a circulation pump; 15. a heat exchanger; 16. the process water flows into the pipeline; 17. a closed loop liquid inlet; 18. an extractant inlet; 19. a mixing device; 20. and a fifth outlet.
Detailed Description
As shown in figure 1, the device for continuous water-separating extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid by one-step method comprises a water-separating kettle and a heat exchanger connected with the water-separating kettle, wherein the water-separating kettle comprises a cylindrical water-separating kettle cylinder body 1 with an upper opening and a cylindrical mixing cylinder 2, and the mixing cylinder 2 extends into a water-separating kettle cylinder body inner cavity 3 through the upper opening of the water-separating kettle cylinder body 1. The lower end surface of the mixing drum 2 is provided with a plurality of through holes 4, so that the inner cavity 5 of the mixing drum is communicated with the inner cavity 3 of the water separation kettle cylinder.
In one embodiment, the mixing drum 2 is provided with a circulating liquid inlet 12, a closed-loop liquid inlet 17 and an extractant inlet 18 at a position far from the through hole 4, and specific positions of the inlets can be arranged arbitrarily. For example, the circulating liquid inlet 12 is arranged at the upper part of the mixing drum 2, and the closed-loop liquid inlet 17 and the extractant inlet 18 are arranged at the middle part of the mixing drum 2. The mixing drum 2 is internally provided with a mixing device 19, and the mixing device 19 is one or more groups of stirring paddles or static mixers, and is preferably arranged along the axial line direction of the mixing drum 2.
In a specific embodiment, the middle lower part of the water separation kettle cylinder 1 is provided with a first outlet 6, the middle upper part of the water separation kettle cylinder 1 is provided with a third outlet 8, the first outlet 6 and the third outlet 8 are communicated through a first pipeline 10, and an acid water outflow pipeline 11 is separately arranged in the first pipeline 10 to control the liquid in the water separation kettle to permeate through the end face of the mixing cylinder 2.
In a specific embodiment, the middle lower part of the water separation kettle cylinder 1 is provided with a second outlet 7, the second outlet 7 is communicated with the circulating liquid inlet 12 of the mixing cylinder 2 through a second pipeline 13, and the second pipeline 13 is provided with a circulating pump 14 and a heat exchanger 15. The liquid in the inner cavity 3 of the water separation kettle is circulated and flows through the second pipeline 13 by the action of the circulating pump 14, and the circulating pump 14 is preferably arranged externally. When the liquid in the inner cavity 3 of the water separation kettle circularly flows, heat released by water separation is taken away through heat exchange of the heat exchanger 15.
In one embodiment, the second pipe 13 is further provided with a process water inflow pipe 16, and the process water is mixed into and dilutes the circulating liquid. The middle upper part of the water separation kettle barrel 1 can be provided with a fourth outlet 9 for discharging tail gas out of the water separation kettle barrel 1 and a fifth outlet 20 for discharging extraction liquid overflowed out of the water separation kettle barrel 1.
In one embodiment, as shown in fig. 2, the mixing drum 2 is provided with a circulating fluid inlet 12 and a closed loop fluid inlet 17. The extractant is then re-introduced into the mixing drum 2 via the second conduit 13. Preferably, the extractant may be introduced into the second conduit 13 together with the process water.
Example 1
A water separation kettle is manufactured according to the mode shown in the figure 1, a device is built according to the flow in the schematic diagram, and relevant meters and control valves are arranged. Preparing a proper amount of closed-loop liquid, extracting agent toluene and industrial water.
Adding 35% acid water into the water separation kettle cylinder 1 in advance until the acid water flows out from the acid water outflow pipeline 11, and stopping adding the acid water in advanceAs priming circulation. Starting the circulation pump 14 to establish a circulation system, wherein the flow rate of the circulation liquid is about 250m 3 And/h. By adjusting the circulating water of the heat exchanger 15, the temperature of the acid water is controlled to be not higher than 55 ℃.
The mixing device 19 is started, and the closed-loop liquid inlet 17 is controlled to be 3.5m towards the inner barrel 5 of the water separation kettle 3 The flow rate/h is introduced into the closed-loop liquid, and the flow rate of the process water into the pipeline 16 is controlled to be 10m to the circulating liquid 3 The flow rate of/h is introduced into the industrial water, and the extractant inlet 18 is controlled to be 6.2m into the inner cylinder 5 of the water separation kettle 3 The flow rate of/h was continuously introduced into toluene.
The circulating liquid flowing into the inner cylinder cavity 5 of the water separation kettle through the circulating liquid inlet 12 generates a large amount of heat in the process of diluting the closed-loop liquid, and the action of the mixing device 19 prevents local overheating on one hand, and on the other hand, the closed-loop liquid, the circulating liquid and the extractant which are collected into the mixing cylinder 2 can be quickly and fully mixed and then enter the inner cylinder cavity 3 of the water separation kettle through the through hole 4. Meanwhile, the circulating pump 14 acts to enable circulating liquid to flow, heat generated by a closed loop is removed in time through the heat exchanger 15, and the temperature of materials in the water separation kettle is controlled to be not more than 55 ℃ by adjusting circulating water of the heat exchanger 15 and the circulating pump 14.
As the closed-loop liquid, the extractant and the part of the heat removed circulating liquid are gradually fed into the inner cylinder cavity 5 of the relatively independent water separation kettle, the dilution process of the closed-loop liquid and the mixing of the closed-loop liquid and the extractant are synchronously carried out. The inner cavity 3 of the water separation kettle cylinder body and the inner cavity 5 of the water separation kettle inner cylinder are mutually independent to a certain extent, so that liquid in the inner cavity 3 of the water separation kettle cylinder body is gradually divided into an upper layer of extract liquid and a lower layer of waste acid water, and the extract liquid overflows and is discharged from a fifth outlet 20 at the upper part of the water separation kettle cylinder body 1 and enters the next alkaline washing process. Waste acid water flows out from the bottom of the water separation kettle through a U-shaped pipeline (not shown) and enters the subsequent acid water treatment process, so that continuous automatic phase separation is realized.
After the continuous and stable operation of this example for 8 hours, the extraction solution and the waste acid water were sampled, respectively. The extract liquid is orange red transparent liquid, and is basically consistent with the extract liquid obtained by the traditional extraction method. And (3) carrying out post-treatment on the extract, including alkali washing, water washing and toluene removal to obtain a 2-ethyl anthraquinone product, wherein the yield calculated by the input BE acid is 85.3%. The waste acid water is dark brownish red, the sulfuric acid content is 35%, the tar-like precipitate is 0.2%, and the COD value is 8500mg/L.
Example 2
In this example, similarly to example 1, acid water having a concentration of 38% was previously added to the dialysis vessel cylinder 1 until the acid water outflow pipe 11 stopped, and the resulting solution was used as a priming circulation solution. The circulation pump 14 is started to establish a circulation system, and the flow rate of the circulating liquid is about 900m 3 And/h. By adjusting the circulating water of the heat exchanger 15, the acid water temperature is controlled to be lower than 43 ℃.
The mixing device 19 was started, and the extractant inlet 18 was controlled to 7.1m into the inner drum 5 of the dialysis pot 3 Toluene is continuously introduced into the flow of/h as an extractant; at the same time, the closed-loop liquid inlet 17 is controlled to be 3.9m to the inner cylinder 5 of the water separation kettle 3 The flow rate/h is introduced into the closed-loop liquid. By controlling the process water flow into the recycle liquid through the pipe 16 at 9.5m 3 The flow rate of/h is introduced into the industrial water.
The heat generated by the dilution of the closed-loop liquid is removed by the heat exchanger 15, and the temperature of the materials in the water separation kettle is controlled to be not more than 43 ℃ by adjusting the circulating water of the heat exchanger 15 and the circulating pump 14.
Along with the gradual feeding of the extraction liquid, the closed-loop liquid and the process water into the inner cylinder cavity 5 of the elutriation kettle, the extraction liquid and the process water are stirred and mixed, and the inner cylinder cavity 3 of the elutriation kettle and the inner cylinder cavity 5 of the elutriation kettle are mutually independent to a certain extent, so that the liquid in the inner cylinder cavity 3 of the elutriation kettle is gradually divided into the extraction liquid at the upper layer and the waste acid water at the lower layer, and the extraction liquid flows out from an overflow port at the upper part of the side surface of the elutriation kettle and enters the next alkaline washing process. Waste acid water flows out from the bottom of the water separation kettle through a U-shaped pipeline and enters the subsequent acid water treatment process, so that continuous automatic phase separation is realized.
Similar to example 1, the extract and the spent acid water were sampled after eight hours of continuous stable operation of this example. The extract was an orange-red transparent liquid and the yield of 2-ethyl anthraquinone was 87%. The waste acid water is brownish red, the sulfuric acid content is 38%, the tar-like precipitate is 0.1%, and the COD value is 8650mg/L.
Example 3
As in example 1, a water separation kettle was manufactured in the manner shown in FIG. 1, and the apparatus was set up according to the flow scheme in the schematic diagram, and associated meters and control valves were provided. The difference between this example and example 1 is that the point of introduction of the extractant is located on the pipe between the outlet of the circulation pump and the heat exchanger. And preparing a proper amount of closed-loop liquid, toluene and wastewater generated by washing the extract.
Acid water with the concentration of 48% is added into the water separation kettle cylinder body 1 in advance until the outflow of the acid water is stopped at an acid water port, and the mixture is used as priming circulation liquid. Starting the circulation pump 14 to establish a circulation system, wherein the flow rate of the circulation liquid is about 550m 3 And/h. By adjusting the circulating water of the heat exchanger 15, the temperature of the acid water is controlled to be lower than 40 ℃.
The mixing device 19 is started, and the extractant inlet 18 is controlled to be 8.6m into the inner cylinder 5 of the water separation kettle 3 Toluene is continuously introduced into the flow of/h as an extractant; simultaneously controlling the closed-loop liquid inlet 17 to be 5.8m to the inner cylinder 5 of the water separation kettle 3 The flow rate/h is introduced into the closed-loop liquid. By controlling the process water flow into the circulation liquid through the pipeline 16 at 14m 3 The flow rate of/h is introduced into the industrial water.
The heat generated by the dilution of the closed-loop liquid is removed by the heat exchanger 15, and the temperature of the materials in the water separation kettle is controlled to be not more than 40 ℃ by adjusting the circulating water of the heat exchanger 15 and the circulating pump 14.
Along with the gradual feeding of the extraction liquid, the closed-loop liquid and the process water into the inner cylinder cavity 5 of the elutriation kettle, the extraction liquid and the process water are stirred and mixed, and the inner cylinder cavity 3 of the elutriation kettle and the inner cylinder cavity 5 of the elutriation kettle are mutually independent to a certain extent, so that the liquid in the inner cylinder cavity 3 of the elutriation kettle is gradually divided into the extraction liquid at the upper layer and the waste acid water at the lower layer, and the extraction liquid flows out from an overflow port at the upper part of the side surface of the elutriation kettle and enters the next alkaline washing process. Waste acid water flows out from the bottom of the water separation kettle through a U-shaped pipeline and enters the subsequent acid water treatment process, so that continuous automatic phase separation is realized.
Similar to example 1, the extract and the spent acid water were sampled after eight hours of continuous stable operation of this example. The extract was an orange-red transparent liquid with a 2-ethyl anthraquinone yield of 85%. The waste acid water is brownish red, the sulfuric acid content is 38%, the tar-like precipitate is 0.1%, and the COD value is 8700mg/L.
All the devices and components in the above embodiments are correspondingly provided with accessories such as control valves and meters, and the specific setting modes of the above accessories are well known to those skilled in the art, and are not described herein.
The present embodiment is only for explanation of the present invention and is not to be construed as limiting the present invention, and modifications to the present embodiment, which may not creatively contribute to the present invention as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present invention.
Claims (8)
1. The utility model provides a 2- (4 '-ethylbenzoyl) benzoic acid closed loop liquid one-step method continuous water separation extraction phase separation's device, includes water separation cauldron and circulating pump and heat exchanger that links to each other with it, its characterized in that:
the water separation kettle comprises a cylindrical water separation kettle barrel (1) with an upper opening and a mixing barrel (2), wherein the lower end of the mixing barrel extends into an inner cavity (3) of the water separation kettle barrel through the upper opening of the water separation kettle barrel, a through hole is formed in the lower end face of the mixing barrel so as to be communicated with the inner cavity of the water separation kettle barrel, and a mixing device (19) is arranged on the mixing barrel;
a first outlet (6) formed in the bottom of the water separation kettle cylinder body and a third outlet (8) formed in the upper part of the water separation kettle cylinder body are communicated through a first pipeline (10) for controlling the gas-liquid internal balance of the water separation kettle cylinder body, and an acid water outflow pipeline (11) is arranged in the first pipeline for controlling the liquid level height in the water separation kettle to be less than the lower end face of the mixing cylinder;
a second outlet (7) formed in the middle lower part of the water separation kettle cylinder body and a circulating liquid inlet (12) formed in the mixing cylinder far away from the lower end surface are communicated through a second pipeline (13) so as to enable liquid in the water separation kettle to circularly flow, and a heat exchanger (15) and a circulating pump (14) are connected in the second pipeline so as to timely remove heat generated in the closed loop reaction process;
the middle upper part of the water separation kettle barrel is also provided with a fifth outlet (8) for overflow discharge of layered extract, and the mixing barrel is further provided with a closed-loop liquid inlet (17) far away from the lower end surface;
the mixing cylinder is provided with an extractant inlet (18) or the extractant enters the mixing cylinder again through a second pipeline (13);
and (3) adding priming circulating liquid into a circulating liquid inlet of a mixing cylinder in advance until circulating liquid flows out of the acid water outflow pipeline, stopping, sealing the acid water outflow pipeline, continuously adding circulating liquid, closed-loop liquid and an extracting agent, mixing in the mixing cylinder, standing and layering in a water separation kettle cylinder, discharging the extracting liquid obtained by layering separation into a subsequent refining step through overflow of a fifth outlet to prepare 2-ethyl anthraquinone, timely removing heat generated in the closed-loop reaction process from the circulating liquid obtained by layering separation through a second pipeline, and circularly refluxing to the mixing cylinder.
2. The apparatus for continuous aqueous extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid one-step method according to claim 1, wherein: the second pipeline is connected with a pipeline for introducing process water and a pipeline for introducing an extracting agent in a tapping way.
3. The apparatus for continuous aqueous extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid one-step method according to claim 1, wherein: the mixing device is one or more groups of stirring paddles or one or more groups of static mixers.
4. The apparatus for continuous aqueous extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid one-step method according to claim 1, wherein: the upper part of the water separation kettle cylinder body is provided with a fourth outlet (9) for discharging tail gas.
5. A process for continuous aqueous extraction phase separation using the apparatus of claim 1 in a closed loop liquid one-step process of 2- (4' -ethylbenzoyl) benzoic acid, characterized in that: the volume flow ratio of the closed-loop liquid, the extractant and the process water feed to the circulating liquid used for the water separation, the extraction and the phase separation of the closed-loop liquid of the 2- (4' -ethylbenzoyl) benzoic acid is 1:1.3 to 2:1 to 3.5:50 to 500.
6. The process for continuous aqueous extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid one-step method according to claim 5, wherein the process is characterized in that: the temperature of the liquid in the water separation kettle is controlled at 30-80 ℃.
7. The process for continuous aqueous extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid ring-closing liquid one-step method according to claim 5, wherein: the process water is industrial water or waste water generated in the production process of 2-ethyl anthraquinone.
8. The process for continuous aqueous extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid ring-closing liquid one-step method according to claim 5, wherein: the extractant is toluene.
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| CN202111387370.1A CN113968778B (en) | 2021-11-22 | 2021-11-22 | Device and process for continuous water-out extraction phase separation of 2- (4' -ethylbenzoyl) benzoic acid closed-loop liquid by one-step method |
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