CN115089998A - Organic matter static extraction device - Google Patents
Organic matter static extraction device Download PDFInfo
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- CN115089998A CN115089998A CN202210616504.0A CN202210616504A CN115089998A CN 115089998 A CN115089998 A CN 115089998A CN 202210616504 A CN202210616504 A CN 202210616504A CN 115089998 A CN115089998 A CN 115089998A
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- 238000000605 extraction Methods 0.000 title claims abstract description 139
- 230000003068 static effect Effects 0.000 title claims abstract description 39
- 239000005416 organic matter Substances 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 82
- 150000003934 aromatic aldehydes Chemical class 0.000 claims abstract description 71
- 239000002351 wastewater Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007921 spray Substances 0.000 claims abstract description 25
- 239000000284 extract Substances 0.000 claims abstract description 22
- 238000005507 spraying Methods 0.000 claims abstract description 19
- 239000002667 nucleating agent Substances 0.000 claims abstract description 16
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 10
- 239000000600 sorbitol Substances 0.000 claims abstract description 10
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 9
- -1 sorbitol acetal Chemical class 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 239000002699 waste material Substances 0.000 claims description 65
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 39
- 239000000945 filler Substances 0.000 claims description 32
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 23
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 23
- 239000003208 petroleum Substances 0.000 claims description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
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- 239000011521 glass Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
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- 239000004575 stone Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 29
- 238000011084 recovery Methods 0.000 abstract description 20
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004945 emulsification Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
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- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012259 ether extract Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
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- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N ortho-diethylbenzene Natural products CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
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Abstract
The invention provides an organic matter extraction device, and particularly relates to a static extraction and recovery device for aromatic aldehyde in organic waste liquid generated by preparing a sorbitol acetal nucleating agent. It includes the following subassembly: an extraction vessel: the extraction device comprises a lower water layer space with a preset height and an upper extractant layer space with a preset height, wherein the lower water layer space is filled with water, and the upper extractant space is filled with an extractant; the spray header is arranged at the top of the extraction container and is used for spraying and introducing the extract liquor to be extracted to the extractant layer; an extractant introducing port assembly arranged at the top of the extraction container and communicated with the upper extractant layer space and used for introducing an extractant into the extraction container to a preset height; and a discharge port assembly for discharging the extracted wastewater and/or extract phase from the extraction vessel. The organic matter extraction device overcomes the problem of incomplete emulsification and extraction agent and water separation caused by dynamic extraction without introducing a power pump and a power stirring device, and achieves the effects of safety, energy conservation, environmental protection and energy consumption reduction.
Description
Technical Field
The invention relates to an organic matter extraction device, in particular to a static extraction and recovery device for aromatic aldehyde in organic waste liquid generated by preparing sorbitol acetal nucleating agent.
Background
The extraction method is an effective separation and extraction method for obtaining a single organic matter from a mixed solution of organic matters. The principle of extraction separation is to transfer substances from one solvent to another by using the difference in solubility or partition coefficient of the substances in two mutually insoluble (or slightly soluble) solvents. And extracting most target compounds repeatedly. The existing extraction device basically improves the extraction efficiency by physical means such as stirring, centrifugation and the like in an auxiliary way.
In the existing chemical field, when preparing sorbitol acetal compounds, aromatic aldehyde and sorbitol are used as raw materials to carry out condensation reaction, and in the process, because the reactant aromatic aldehyde has incomplete reaction, the waste liquid after the reaction contains a certain amount of aromatic aldehyde residues. The existing extraction scheme cannot quickly and effectively separate and recover residual aromatic aldehyde in the waste liquid. Therefore, when green production is vigorously promoted in the whole society, research and development of a simple and efficient separation apparatus for recovering aromatic aldehydes in waste liquid for reuse are urgently required.
Disclosure of Invention
The invention provides a simple and efficient static extraction device for recycling aromatic aldehyde, aiming at the technical problem that the existing organic matter extraction device cannot effectively separate and recycle a large amount of unreacted aromatic aldehyde during the production of a sorbitol acetal compound nucleating agent, and solving the technical problems of waste of production raw materials, environmental pollution and the like.
The invention provides a static extraction device for organic matters, which comprises the following components:
an extraction vessel: the extraction device comprises a lower water layer space with a preset height and an upper extractant layer space with a preset height, wherein the lower water layer space is filled with water, and the upper extractant space is filled with an extractant;
the spray header is arranged at the top of the extraction container and is used for spraying and introducing the extract liquor to be extracted to the extractant layer;
an extractant introducing port assembly arranged at the top of the extraction container and communicated with the upper extractant layer space and used for introducing an extractant into the extraction container to a preset height;
and the discharge port assembly is used for discharging the extracted wastewater and/or the extracted phase out of the extraction container.
Preferably, the mass ratio of the preset amount of the extractant filled in the upper extractant space to the extract liquid to be extracted is more than or equal to 1%.
Furthermore, the preset height of the extracting agent is more than one time of the depth of the extract liquid to be washed into.
Preferably, the preset height of the water filled in the lower water layer space is more than one time of the height of the turbulent layer formed at the discharge port when the waste water is discharged by the discharge port assembly.
Preferably, a porous support plate is arranged at the joint of the lower water layer space and the upper extractant layer space in the extraction container.
Further, the upper extractant layer space above the porous support plate is filled with a filler.
Furthermore, the particle size of the filler is 2-50mm, and the filler is filled in sequence from small to large according to the particle size of the filler to form at least two filler layers with gradually increasing particle sizes from bottom to top; in order to ensure that the packing does not leak through the porous support plate, the porous support plate is a multi-layer perforated plate with a pore size of less than 2 mm.
Further, the filler is one or a combination of a plurality of porcelain balls, porcelain rings, stainless steel wire meshes, sand or stones.
Preferably, the outer side wall of the extraction container is provided with a glass liquid level meter for observing the liquid level in the container.
Particularly preferably, the extract to be extracted is waste liquid containing aromatic aldehyde generated in the preparation of the sorbitol acetal nucleating agent.
Furthermore, one reagent or more than one mixed reagent of petroleum ether, normal hexane, ether, benzene and cyclohexane is filled in the extractant layer in advance to serve as the extractant.
Compared with the prior art, the organic matter static extraction device provided by the invention has the following beneficial effects:
(1) the inventor creatively designs the water layer and the extractant layer, achieves the aim of absorbing aromatic aldehyde by the natural flow of waste liquid in the extraction container through the waste water liquid level difference, overcomes the problems of emulsification of aromatic aldehyde and incomplete separation of the extractant and water introduced by dynamic extraction without introducing a power pump and a power stirring device, and achieves the effects of safety, energy conservation, environmental protection and energy consumption reduction.
(2) The inventor creatively preferably adopts a waste liquid spraying mode to enter the static extractant layer, and the waste liquid is uniformly sprayed on the surface of the extractant in a form of atomizing into small liquid drops, so that the effective contact area of the waste water and the extractant is greatly increased, and the extraction rate is improved.
(3) The inventor creatively adds the filler into the upper extractant layer, on one hand, the sinking time of the waste liquid fog drops in the extractant layer is prolonged, the contact time of the waste water and the extractant is prolonged, and thus the extraction rate is improved; on the other hand, atomized waste liquid fog drops gradually form large liquid drops when passing through the packing layer, the impulsive force of the waste liquid to the extractant layer is reduced, and the problem that the extractant containing aromatic aldehyde and water form serious emulsification and cannot be layered is avoided;
drawings
FIG. 1 is a schematic view of an apparatus for static extraction of organic substances according to the present invention;
FIG. 2 is a flow diagram of a process for aromatic aldehyde recovery and reproduction in the static extraction unit of FIG. 1;
FIG. 3 is a flow chart of a preferred process of the process flow chart of FIG. 2.
Detailed Description
The static extraction device for organic substances provided by the present invention is further described below with reference to the accompanying drawings, and it should be noted that the technical solution and design principle of the present invention are described in detail below with only one optimized technical solution.
Referring to fig. 3, a schematic diagram of an optimized static organic extraction apparatus includes an extraction vessel 100: for storing an extractant and installing a functional component, the extraction vessel may be an extraction tower or a reaction kettle, a lower aqueous layer space 1 of a predetermined height is provided inside the extraction vessel 100, the lower aqueous layer space 1 is filled with water, an upper extractant space 2 of a predetermined height is connected to the lower aqueous layer space 1, and the upper extractant space 2 is filled with an extractant. The top of the extraction container 100 is provided with a spray header 3 facing the extractant layer for spraying and introducing the extract to be extracted to the extractant layer, and the top of the extraction container 100 is also provided with an extractant introduction port assembly 5 communicated with the upper extractant layer space 2 for introducing the extractant into the extraction container to a preset height. The bottom side wall of the extraction vessel 100 is provided with a drain assembly 8 for discharging waste water, and preferably, in order to maintain the height of the water filled in the lower water layer space 1 constant, the drain assembly 8 is provided with a flow control means. The filling height of the extractant in the upper extractant layer space 2 is determined and preset according to the mass of the to-be-extracted liquid, the diameter of the inner cavity of the extraction container 100 and the impact depth of the spray header 3 on the extractant when the to-be-treated liquid is introduced, and the ratio of the setting amount of the extractant to the mass of the to-be-extracted liquid is more than 1%, preferably more than 5%. The filling amount of the extracting agent and the size of the extracting container are determined, the filling heights of the extracting agent and the filler are determined according to the impact depth of the extracting agent when the extracting solution to be extracted is introduced by the spray header 3, generally, the preset height of the extracting agent is more than one time of the depth of the extracting agent to be extracted being flushed into the extracting agent, and the filler is designed to ensure that the height of the extracting agent after the filler is added is more than one time higher than the height of the extracting agent without the filler. In order to ensure the continuous and stable operation of the equipment, the preset height of the filling water in the lower water layer space is more than one time higher than the height of a turbulent layer formed at the discharge port when the wastewater is discharged by the discharge port assembly 8, so that the incomplete separation phenomenon is avoided.
Preferably, the outer side wall of the extraction vessel 100 is provided with a glass liquid level meter 6 for observing the liquid level in the column, and the side wall of the extraction vessel 100 is provided with an extract phase recovery port 9 for extracting the extract phase, wherein the extract phase recovery port 9 can be arranged on the side wall of the bottom of the extraction vessel 100, or can be arranged at the lowest position of the extractant layer 2, and the extract phase can be just extracted from the extract phase recovery port 9 by controlling the height of the lower water layer. And in the running process of the equipment, extracting the extract phase from the extract phase recovery port at regular time to detect the concentration of the extract, and recovering and reusing the extract phase.
Preferably, a porous support plate 4 is arranged between the lower water layer space 1 and the upper extractant layer space 2, the porous support plate 4 is used for supporting the filler 21 filled in the upper extractant layer 2, preferably, the filler 21 is one or a combination of a ceramic ball, a ceramic ring, a stainless steel wire net, sand and/or stone with the particle size of 2-50mm, and the filler 21 is filled sequentially from small to large according to the particle size of the filler to form at least two filler with the particle size gradients, wherein the particle sizes of the filler gradually increase from bottom to top. In order to support the packing 21, the pore size of the porous support plate 4 should be smaller than the minimum particle size of the packing in the extractant layer, and is preferably a multi-layer pore plate, although in order to ensure the stability of the porous support plate 4, a support member is provided at the lower part of the porous support plate 4. In addition, the extraction column 100 is provided with necessary conventional functional components such as an overflow port 10, a cleaning port 11, and the like.
Referring to fig. 1 and fig. 2, the process operation of the organic static extraction device for treating the waste liquid from the preparation of the sorbitol acetal compound nucleating agent provided by the invention is described in detail, and the process operation for recovering and regenerating aromatic aldehyde comprises the following steps:
s1, presetting a static extraction device, putting water with a preset height into the extraction device, and then putting an extractant with a preset height into the extraction device to form a lower water layer 1 and an upper extractant layer 2;
s2, introducing waste liquid to be treated, and introducing the waste liquid containing aromatic aldehyde to the upper surface of an extractant layer from the top of the extraction device;
s3, extracting and absorbing the waste liquid, wherein the waste liquid enters a lower water layer through an extractant layer, so that aromatic aldehyde in the waste liquid is absorbed by the extractant to form an extraction phase;
s4, recovering an extraction phase, and when the concentration of the aromatic aldehyde in the extraction phase reaches more than 18%, taking out the extraction phase for preparing the sorbitol acetal compound nucleating agent again to finish the technological process of one-time aromatic aldehyde recovery and reproduction.
As shown in connection with fig. 3, the process operations may preferably include:
s1.1, arranging a porous support plate 4 at the joint of a lower water layer 1 and an upper extractant layer 2 in an extraction device;
s1.2, putting water with a preset height into an extraction device, and then putting an extracting agent with a preset height into the extraction device to form a lower water layer 1 and an upper extracting agent layer 2;
s1.3 packing 21 with the grain diameter of 2-50mm is filled above the porous support plate 4, namely in the extractant layer.
S2, the waste liquid containing aromatic aldehyde is introduced into the upper surface of the extractant layer 2 from the top of the extraction device through the spray header 3 in a spraying mode.
S3.1, the waste liquid enters a lower water layer through an extractant layer 2 to form a waste water layer 1, so that aromatic aldehyde in the waste liquid is absorbed by the extractant to form an extraction phase;
s3.2, adjusting the height of the waste water layer 1 to keep the height of the lower waste water layer 1 to be basically the preset height.
Preferably, S3.2 is to maintain the height of the lower wastewater layer 1 at substantially the preset height by discharging the clear wastewater at the lower portion of the wastewater layer 1 in real time.
Preferably, the aromatic aldehyde content in the discharged clear wastewater is less than 200 mg/L. More preferably, the aromatic aldehyde content in the discharged clear wastewater is less than 100 mg/L.
And S4, when the concentration of the aromatic aldehyde in the extraction phase reaches more than 18%, taking out the extraction phase for preparing the sorbitol acetal compound nucleating agent, and completing the primary recovery process flow of the aromatic aldehyde.
In order to better implement the technical solution of the present invention, preferably, in the process, the porous support plate 4 is a multi-layer pore plate with a pore diameter smaller than the minimum particle diameter of a filler in the extractant layer, and the extractant is one reagent or a mixture of more than one reagent selected from petroleum ether, n-hexane, diethyl ether, benzene and cyclohexane. Preferably, the mass ratio of the preset amount of the extracting agent to the treated waste liquid containing aromatic aldehyde is more than or equal to 1%. Preferably, the mass ratio of the preset amount of the extracting agent to the treated waste liquid containing aromatic aldehyde is more than or equal to 5%.
When the process for recovering aromatic aldehyde is completed, the static extraction apparatus is required to be preset again for the next process for recovering aromatic aldehyde, and it should be noted that when the static extraction apparatus is preset, some steps are not necessary, for example, S1.1 is provided with a porous support plate 4, which may be assembled already at the time of manufacturing the apparatus. In addition, when the aromatic aldehyde is recycled, a person skilled in the art can select whether to empty the lower wastewater layer or not according to needs when the static extraction device is preset, and when the extraction phase discharge port is arranged at the lower part of the upper extractant layer, namely the upper part of the lower wastewater layer, the extractant with the preset height is only put in again under the condition of not emptying the lower wastewater layer, so that the effect of the aromatic aldehyde recycling process is basically not influenced.
The organic matter static extraction device provided by the invention is technically verified by the following specific embodiments:
example 1
1) Selecting an extraction tower with the height of 500mm and the diameter of 60mm as a static extraction device, arranging a porous support plate 4 with the pore diameter of less than 2mm in the extraction tower at a position 200mm away from the bottom of a container, firstly putting water with the height of 200mm into the extraction tower, and then putting cyclohexane with the height of 200mm as an extracting agent to form a lower water layer 1 and an upper extracting agent layer 2;
2) adding a filler with the diameter of 2-50mm into the upper cyclohexane extractant layer 2, and sequentially filling according to the particle size of the filler from small to large;
3) the waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extracting agent layer 2 through the spray header 3 in a spraying mode, attention needs to be paid to the fact that the spraying force needs to be reasonably controlled so as to control the spraying waste liquid not to be sprayed to the inner wall of the extracting tower, otherwise, the waste liquid rapidly passes through the extracting agent layer 2 along the inner wall and enters a waste water layer due to the diversion effect of the inner wall of the extracting tower, and the technical problem of insufficient extraction can be caused.
4) When the weight ratio of the preset cyclohexane to the spray waste liquid reaches 1 percent and the waste liquid completely passes through the cyclohexane extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is measured by HPLC to be 150mg/L, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid after static extraction reaches 85 percent. The cyclohexane extract phase containing aromatic aldehyde can be directly used as a production raw material of the nucleating agent for standby.
Example 2
Steps 1) and 2) are the same as in example 1;
3) the waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through the spray header 3 in a spraying mode.
4) When the weight ratio of the preset cyclohexane to the spray waste liquid reaches 5 percent and the waste liquid completely passes through the cyclohexane extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is determined to be 65mg/L by HPLC, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid after static extraction reaches 93.5 percent. The cyclohexane extract phase containing aromatic aldehyde can be directly used as a production raw material of the nucleating agent for standby.
Example 3
Steps 1) and 2) are the same as in example 1;
3) the waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through the spray header 3 in a spraying mode.
4) When the weight ratio of the preset cyclohexane to the spray waste liquid reaches 8 percent and the waste liquid completely passes through the cyclohexane extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is measured by HPLC to be 40mg/L, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid subjected to static extraction reaches 96 percent. The cyclohexane extract phase containing aromatic aldehyde can be directly used as a production raw material of the nucleating agent for standby.
Example 4
1) Selecting an extraction tower with the height of 500mm and the diameter of 60mm as a static extraction device, arranging a porous support plate 4 with the pore diameter smaller than 2mm in a position 200mm away from the bottom of a container in the extraction tower, firstly putting water with the height of 200mm in the extraction tower, and then putting petroleum ether with the height of 200mm as an extracting agent to form a lower water layer 1 and an upper petroleum ether extracting agent layer 2;
2) adding a filler with the diameter of 2-10mm into the upper petroleum ether extractant layer 2, and sequentially filling according to the particle size of the filler from small to large;
3) waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through a spray header 3 in a spraying manner.
4) When the weight ratio of the preset petroleum ether to the spray waste liquid reaches 8 percent and the waste liquid completely passes through the petroleum ether extracting agent layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is determined to be 100mg/L by HPLC, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid after static extraction reaches 90 percent. The petroleum ether extract phase containing aromatic aldehyde can be directly used as a production raw material of the nucleating agent for later use.
Example 5
1) Selecting an extraction tower with the height of 500mm and the diameter of 60mm as a static extraction device, arranging a porous support plate 4 with the aperture smaller than 2mm at a position 200mm away from the bottom of a container in the extraction tower, firstly putting water with the height of 200mm in the extraction tower, and then putting n-hexane with the height of 200mm as an extracting agent to form a lower water layer 1 and an upper n-hexane extracting agent layer 2;
2) adding a filler with the diameter of 2-10mm into the n-hexane extractant layer 2 at the upper layer, and sequentially filling according to the particle size of the filler from small to large;
3) the waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through the spray header 3 in a spraying mode.
4) When the weight ratio of the preset normal hexane to the spray waste liquid reaches 8 percent and the waste liquid completely passes through the petroleum ether extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is measured by HPLC to be 105mg/L, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid after static extraction reaches 89.5 percent. The n-hexane extract phase containing aromatic aldehyde can be directly used as a production raw material of the nucleating agent for later use.
Example 6
1) Selecting an extraction tower with the height of 500mm and the diameter of 60mm as a static extraction device, arranging a porous support plate 4 with the pore diameter smaller than 2mm in a position 200mm away from the bottom of a container in the extraction tower, firstly putting water with the height of 200mm in the extraction tower, and then putting ether with the height of 200mm as an extracting agent to form a lower water layer 1 and an upper ether extracting agent layer 2;
2) adding a filler with the diameter of 2-50mm into the ether extractant layer at the upper layer, and sequentially filling according to the particle size of the filler from small to large;
3) waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through a spray header 3 in a spraying manner.
4) When the weight ratio of the preset ether to the spray waste liquid reaches 8 percent and the waste liquid completely passes through the petroleum ether extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is measured by HPLC to be 120mg/L, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid subjected to static extraction reaches 88 percent. The ether extract phase containing aromatic aldehyde can be directly used as a raw material for producing the nucleating agent for later use.
Example 7
1) Selecting an extraction tower with the height of 500mm and the diameter of 60mm as a static extraction device, arranging a porous support plate 4 with the aperture smaller than 2mm at a position 200mm away from the bottom of a container in the extraction tower, firstly putting water with the height of 200mm in the extraction tower, and then putting benzene with the height of 200mm as an extracting agent to form a lower water layer 1 and an upper benzene extracting agent layer 2;
2) adding a filler with the diameter of 2-50mm into the benzene extractant layer at the upper layer, and sequentially filling according to the particle size of the filler from small to large;
3) waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through a spray header 3 in a spraying manner.
4) When the weight ratio of the preset benzene to the spraying waste liquid reaches 8 percent; and after the waste liquid completely passes through the petroleum ether extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is determined to be 110mg/L by adopting HPLC, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid subjected to static extraction reaches 89%. The benzene extraction phase containing aromatic aldehyde can be directly used as a production raw material of the nucleating agent for later use.
Comparative example 1
Reference example 1, steps 1) and 2), except that a filler was not added to the cyclohexane layer;
3) waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through a spray header 3 in a spraying manner.
4) When the weight ratio of the preset cyclohexane to the spray waste liquid reaches 1 percent and the waste liquid completely passes through the petroleum ether extractant layer and enters the waste water layer, the aromatic aldehyde concentration in the waste water layer is determined to be 400mg/L by HPLC, and the extraction recovery rate of the aromatic aldehyde-containing waste liquid after static extraction is only 60 percent.
Comparative example 2
Reference example 1, steps 1) and 2), except that no aqueous layer was introduced into the extraction apparatus;
3) the waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extractant layer 2 through the spray header 3 in a spraying mode.
4) When the weight ratio of the preset cyclohexane to the spray waste liquid reaches 8%, the aromatic aldehyde concentration in the waste water layer is determined to be 650mg/L by HPLC, the extraction recovery rate of the aromatic aldehyde-containing waste liquid subjected to static extraction is only 35%, the waste water layer and the cyclohexane extraction layer are not completely separated, the effluent waste water is turbid and not clear, the cyclohexane loss is large, and the utilization rate is low.
Comparative example 3
1) Selecting an extraction tower with the height of 500mm and the diameter of 60mm as a static extraction device, and directly adding cyclohexane into the extraction tower as an extracting agent;
2) waste liquid containing aromatic aldehyde with the concentration of 1000mg/L is introduced to the upper surface of the extracting agent in a spraying mode through a spray header 3.
3) And (3) centrifugally stirring cyclohexane and waste liquid in the extraction tower for 30min by adopting a centrifugal stirring mode, standing for 2h, and not layering, wherein the waste liquid and a cyclohexane layer are seriously emulsified, so that the layering of a cyclohexane extraction phase and waste water is difficult to achieve, and the effective extraction and recovery of the waste liquid containing aromatic aldehyde cannot be realized.
Compared with the experiments of the comparative examples 1 to 3, the process method for recovering and regenerating the aromatic aldehyde can realize high extraction recovery rate of the aromatic aldehyde-containing waste liquid, and the extracted aromatic aldehyde-containing extract phase can be directly used as a production raw material of the nucleating agent without a rectification process, so that the process method is simple to operate, energy-saving and environment-friendly.
The above are only preferred embodiments of the present invention, and it should be noted that the above preferred embodiments should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that several modifications, substitutions, improvements and embellishments of the steps can be made without departing from the spirit and scope of the invention, and these modifications, substitutions, improvements and embellishments should also be construed as the scope of the invention.
Claims (12)
1. An organic matter static extraction device comprises the following components:
an extraction vessel: the extraction device comprises a lower water layer space with a preset height and an upper extractant layer space with a preset height, wherein the lower water layer space is filled with water, and the upper extractant space is filled with an extractant;
the spray header is arranged at the top of the extraction container and is used for spraying and introducing the extract liquor to be extracted to the extractant layer;
an extractant introducing port assembly arranged at the top of the extraction container and communicated with the upper extractant layer space and used for introducing an extractant into the extraction container to a preset height;
and a discharge port assembly for discharging the extracted wastewater and/or extract phase from the extraction vessel.
2. The static extraction device for organic matters as claimed in claim 1, wherein the mass ratio of the preset amount of the extractant filled in the upper extractant space to the liquid to be extracted is more than or equal to 1%.
3. The apparatus of claim 2, wherein the predetermined height of the extractant is more than one time of the depth of the liquid to be extracted.
4. The static extraction apparatus for organic substances as claimed in claim 1, wherein the predetermined height of the water filled in the lower water layer space is more than one time greater than the height of the turbulent flow layer formed at the discharge port when the waste water is discharged by the discharge port assembly.
5. The apparatus of claim 1, wherein a porous support plate is disposed in the extraction container at the junction of the lower aqueous layer space and the upper extractant layer space.
6. The static extraction device for organic substances according to claim 5, characterized in that the space of the upper extractant layer above the porous support plate is filled with filler.
7. The static extraction device for organic substances according to claim 6, characterized in that the grain diameter of the filler is 2-50 mm.
8. The apparatus of claim 7, wherein the packing is sequentially filled according to the sizes of the packing from small to large, so as to form at least two packing layers with gradually increasing sizes from bottom to top.
9. The static extraction device for organic matter as claimed in any one of claims 6 to 8, wherein the filler is one or more of ceramic balls, ceramic rings, stainless steel wire meshes, sand or stones.
10. The apparatus of claim 1, wherein the outer sidewall of the extraction vessel is provided with a glass level gauge for observing the liquid level in the vessel.
11. The apparatus of claim 1, wherein the extraction liquid is a waste liquid containing aromatic aldehyde generated in the preparation of sorbitol acetal nucleating agent.
12. The apparatus of claim 11, wherein the extractant layer is pre-filled with one or more of petroleum ether, n-hexane, ether, benzene and cyclohexane as an extractant.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB717725A (en) * | 1951-07-25 | 1954-11-03 | Universal Oil Prod Co | Improvements in or relating to the separation of mixtures of organic compounds |
| GB743039A (en) * | 1952-11-18 | 1956-01-04 | Koppers Co Inc | Improvements in or relating to method and apparatus for absorbing naphthalene or other substance present in a liquid by contacting the liquid with another immiscible liquid of different density |
| GB902763A (en) * | 1957-08-26 | 1962-08-09 | Sven Olof Osterman | Method of extracting alkaloidal constituents from plant material |
| US4842745A (en) * | 1986-06-04 | 1989-06-27 | Passavant-Werke Ag & Co. Kg | Process for separating organic compounds from water by extraction |
| CN2090288U (en) * | 1991-05-16 | 1991-12-11 | 清华大学 | Honeycomb grid structured packing extraction tower |
| US5965784A (en) * | 1995-09-12 | 1999-10-12 | Total Raffinage Distribution S.A. | Process and apparatus for extracting aromatic compounds contained in a hydrocarbon feedstock |
| CN202410231U (en) * | 2012-02-16 | 2012-09-05 | 齐学辉 | Extraction equipment for petrochemical industry |
| CN103845924A (en) * | 2012-12-07 | 2014-06-11 | 厦门大学 | Parallel flow falling film extraction process and equipment |
| JP2021147364A (en) * | 2020-03-23 | 2021-09-27 | 三菱ケミカル株式会社 | Method for producing acrylic acid |
-
2022
- 2022-06-01 CN CN202210616504.0A patent/CN115089998B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB717725A (en) * | 1951-07-25 | 1954-11-03 | Universal Oil Prod Co | Improvements in or relating to the separation of mixtures of organic compounds |
| GB743039A (en) * | 1952-11-18 | 1956-01-04 | Koppers Co Inc | Improvements in or relating to method and apparatus for absorbing naphthalene or other substance present in a liquid by contacting the liquid with another immiscible liquid of different density |
| GB902763A (en) * | 1957-08-26 | 1962-08-09 | Sven Olof Osterman | Method of extracting alkaloidal constituents from plant material |
| US4842745A (en) * | 1986-06-04 | 1989-06-27 | Passavant-Werke Ag & Co. Kg | Process for separating organic compounds from water by extraction |
| CN2090288U (en) * | 1991-05-16 | 1991-12-11 | 清华大学 | Honeycomb grid structured packing extraction tower |
| US5965784A (en) * | 1995-09-12 | 1999-10-12 | Total Raffinage Distribution S.A. | Process and apparatus for extracting aromatic compounds contained in a hydrocarbon feedstock |
| CN202410231U (en) * | 2012-02-16 | 2012-09-05 | 齐学辉 | Extraction equipment for petrochemical industry |
| CN103845924A (en) * | 2012-12-07 | 2014-06-11 | 厦门大学 | Parallel flow falling film extraction process and equipment |
| JP2021147364A (en) * | 2020-03-23 | 2021-09-27 | 三菱ケミカル株式会社 | Method for producing acrylic acid |
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