CN115180756A - Acetonitrile waste liquid purification and recovery device and method - Google Patents
Acetonitrile waste liquid purification and recovery device and method Download PDFInfo
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- CN115180756A CN115180756A CN202210651277.5A CN202210651277A CN115180756A CN 115180756 A CN115180756 A CN 115180756A CN 202210651277 A CN202210651277 A CN 202210651277A CN 115180756 A CN115180756 A CN 115180756A
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 title claims abstract description 316
- 239000007788 liquid Substances 0.000 title claims abstract description 159
- 239000002699 waste material Substances 0.000 title claims abstract description 47
- 238000011084 recovery Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000746 purification Methods 0.000 title claims description 27
- 238000002156 mixing Methods 0.000 claims abstract description 47
- 238000010992 reflux Methods 0.000 claims abstract description 42
- 239000012535 impurity Substances 0.000 claims abstract description 36
- 238000009833 condensation Methods 0.000 claims abstract description 34
- 230000005494 condensation Effects 0.000 claims abstract description 34
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 20
- 238000012216 screening Methods 0.000 claims abstract description 10
- 238000005496 tempering Methods 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000007790 scraping Methods 0.000 claims description 16
- 238000010791 quenching Methods 0.000 claims description 12
- 230000000171 quenching effect Effects 0.000 claims description 12
- 239000011550 stock solution Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000008878 coupling Effects 0.000 claims 1
- 238000010168 coupling process Methods 0.000 claims 1
- 238000005859 coupling reaction Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 23
- 239000002351 wastewater Substances 0.000 abstract description 14
- 150000003839 salts Chemical class 0.000 abstract description 9
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- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 description 19
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 6
- 235000017491 Bambusa tulda Nutrition 0.000 description 6
- 241001330002 Bambuseae Species 0.000 description 6
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 6
- 239000011425 bamboo Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
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- 230000007613 environmental effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
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- 239000000203 mixture Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 239000013618 particulate matter Substances 0.000 description 2
- 229920000447 polyanionic polymer Polymers 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N Hydrocyanic acid Natural products N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
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- 238000010533 azeotropic distillation Methods 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Abstract
The invention discloses a device and a method for purifying and recovering acetonitrile waste liquid, belongs to the technical field of acetonitrile waste liquid treatment, and aims to solve the problems of poor recovery effect and high energy consumption in the process of recovering and treating acetonitrile waste water; according to the invention, the mixing tank is used for mixing the acetonitrile waste water and the salt-containing neutralization solution, the impurities in the acetonitrile waste water are subjected to lifting spiral separation, and the impurities are subjected to screening treatment through the plurality of sieve plates again, so that the impurity removal effect in the acetonitrile mixed solution is greatly improved, the quality of acetonitrile recovery treatment is effectively improved, the acetonitrile mixed solution is subjected to rectification treatment through the rectification tower, and continuous rectification treatment is formed through the reflux action of the reboiling cylinder and the condensation cylinder, so that the sufficiency of the rectification treatment of the acetonitrile mixed solution is greatly improved.
Description
Technical Field
The invention belongs to the technical field of acetonitrile waste liquid treatment, and particularly relates to a device and a method for purifying and recovering acetonitrile waste liquid.
Background
Acetonitrile is also called as methyl nitrile, is colorless liquid, is extremely volatile, has special odor similar to ether, has excellent solvent performance, can dissolve various organic, inorganic and vapor substances, is infinitely mutually soluble with water and alcohol, and has certain toxicity; acetonitrile is an important chemical raw material and has wide application.
Acetonitrile is widely used as an important medical intermediate solvent. Therefore, a large amount of acetonitrile waste liquid can be generated in the production process of a medicine intermediate, heavy environmental protection pressure is brought to production, the price of an acetonitrile solvent is high, the treatment of the large amount of acetonitrile waste liquid discharged after reaction is always a big problem, because the acetonitrile and water are azeotropic and can be mutually dissolved at random, the direct distillation of the waste liquid to recover the acetonitrile is quite difficult, and the acetonitrile in the waste liquid can be recovered as far as possible only by adopting modes of salting out, adding a water carrying agent to perform azeotropic distillation and the like, but when the acetonitrile is recovered by adopting the mode, the following defects still exist:
(1) because the components of the acetonitrile waste liquid are complex, when the acetonitrile waste liquid is directly recovered by a solvent or salts, a large amount of solvent or salt raw materials are consumed, and the quality of the acetonitrile in recovery is influenced;
(2) when the acetonitrile waste liquid carries out recovery processing, easily contain partial acetonitrile in its rectification back waste liquid, it is not good to carry out the recovery effect to the acetonitrile in the waste water to directly discharge it and later can lead to COD value in these waste waters higher, be not conform to energy-concerving and environment-protective theory.
Therefore, a device and a method for purifying and recovering acetonitrile waste liquid are needed, and the problems of poor recovery effect and large energy consumption in the process of recovering and treating acetonitrile waste liquid in the prior art are solved.
Disclosure of Invention
The invention aims to provide a device and a method for purifying and recovering acetonitrile waste liquid, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a purification recovery unit of acetonitrile waste liquid, includes the rectifying column, one side of rectifying column is provided with the blending tank, the bottom surface of blending tank with the middle part surface intercommunication of rectifying column has the stoste inlet pipe, the below of stoste inlet pipe is provided with the steam pipe an that is linked together with the rectifying column surface, the top surface intercommunication of blending tank has the conveying pipe, the inner wall of blending tank is provided with quenching and tempering edulcoration subassembly, top one side that the blending tank was kept away from to the rectifying column is provided with the condensing cylinder, the top surface of rectifying column with the top surface intercommunication of condensing cylinder has the outlet duct, the inside of condensing cylinder is provided with the condensation reflux subassembly, the below of condensing cylinder is provided with the reboiling section of thick bamboo, a reboiling section of thick bamboo side with the bottom surface intercommunication of rectifying column has the raffinate feed liquor pipe, the inside of reboiling section of thick bamboo is provided with rectifying column matched with reboiling reflux subassembly.
According to the scheme, the quenching and tempering impurity removing component comprises four sieve plates distributed at equal intervals, the four sieve plates are all fixed with the inner wall of a blending tank, a flow guide ring is fixed on the top surface of each sieve plate positioned at the top, impurity removing pipes communicated with the outer surface of the blending tank are arranged on the outer side of the flow guide ring, blending pipes communicated with the outer surface of the blending tank are arranged on the periphery of each feeding pipe, a flow collecting cover fixed with the inner wall of the flow guide ring is arranged below each feeding pipe, a plurality of separating holes distributed uniformly are formed in the inner surface of the top of the flow collecting cover, a rotating shaft rotatably connected with the top surface of the blending tank is arranged inside the flow collecting cover, a quenching and tempering motor coaxially connected with the rotating shaft is installed on the top surface of the blending tank, lifting spiral pieces are fixedly sleeved on the outer surface of the rotating shaft, and scraping rods fixedly sleeved with the outer surface of the rotating shaft are arranged above the lifting spiral pieces.
As a preferred embodiment, the flow collecting hood is arranged in a funnel shape, the top end of the lifting spiral blade is higher than the height of the columnar shape of the flow collecting hood, the top surface of the scraping rod is arranged in an inclined arc surface, and the outer surface of the scraping rod and the inner surface of the top of the flow collecting hood are in matched arc surfaces.
As a preferred embodiment, a plurality of through holes are circumferentially distributed on the surface of the lifting spiral piece, the hole diameter of each through hole is smaller than that of each separation hole, and the outer surface of the flow guide ring is arranged in an arc surface.
It is worth further saying that the condensation reflux assembly includes a purification collecting pipe communicated with the outer surface of the bottom of the condensation cylinder, the air outlet pipe and the purification collecting pipe are respectively positioned at two sides of the condensation cylinder, the outer surface of the purification collecting pipe is communicated with the outer surface of the top of the rectification tower to form a condensation reflux pipe, and a condensation water pipe is fixedly penetrated through the outer surfaces of the two sides of the condensation cylinder.
It should be further noted that the reboiling reflux assembly comprises a steam reflux pipe communicated with the top surface of the reboiling barrel, the other end of the steam reflux pipe is communicated with the outer surface of the bottom of the rectifying tower, a residual liquid outlet pipe communicated with the bottom surface of the reboiling barrel is arranged below the steam reflux pipe, a steam pipe b is communicated with the outer surface of one end, far away from the residual liquid inlet pipe, of the steam tower, and two symmetrically distributed circulating water pipes are fixedly penetrated through the outer surfaces of two sides of the reboiling barrel.
In a preferred embodiment, the steam pipe b and the two circulating water pipes are distributed in an isosceles triangle, and the two circulating water pipes are respectively located outside the top axis of the residual liquid outlet pipe.
The use method of the acetonitrile waste liquid purification and recovery device comprises the following steps:
s1, quenching and tempering and impurity removal: the acetonitrile waste liquid and the neutralization liquid are respectively sent into a blending tank for neutralization reaction through an acetonitrile waste liquid feeding pump and a neutralization liquid feeding pump, the acetonitrile waste liquid and the neutralization liquid are spirally mixed and neutralized in the blending tank through the driving of a tempering motor, and screening and impurity removing are carried out through four sieve plates;
s2, steam rectification: the mixed liquor subjected to neutralization, screening and impurity removal in the step S1 enters a rectifying tower through a stock solution feeding pipe, and is subjected to stripping and rectifying treatment through steam entering in a steam pipe a, so that the mixed liquor residual enters a reboiling cylinder through a residual liquor inlet pipe, and mixed liquor rectifying gas enters a condensation cylinder along with the steam through a gas outlet pipe for condensation treatment, so that the steam rectifying treatment on the mixed liquor is completed;
s3, reflux rectification:
1) Heating the mixed liquid residual liquid in the step S2 through a steam pipe b, so that steam flows the residual liquid back to the bottom of the rectifying tower through the steam pipe, and rectifying the residual liquid again;
2) The mixed liquid rectification gas is cooled through a condensate pipe, the liquid subjected to condensation treatment is guided through a purification collecting pipe, the acetonitrile waste liquid is primarily purified and recovered, and part of the liquid enters the top of the rectification tower through a condensation reflux pipe to be rectified again.
Compared with the prior art, the device and the method for purifying and recovering the acetonitrile waste liquid provided by the invention at least have the following beneficial effects:
(1) Carry out hybrid processing to acetonitrile waste water and contain salt neutralization solution through the blending tank, and promote the spiral separation to its inside impurity, and screen through a plurality of sieves once more and handle, thereby improve the impurity removal effect in the mixed liquid of acetonitrile greatly, thereby effectively improve the quality that carries out recovery processing to the acetonitrile, and carry out the rectification processing to it through the rectifying column, through the reflux effect of reboiling a section of thick bamboo and a condensation cylinder, make it form continuous rectification processing, thereby improve the sufficiency that the mixed liquid of acetonitrile carries out the rectification processing greatly, effectively avoid containing the acetonitrile composition in the mixed liquid raffinate, accord with the environmental protection theory.
(2) The steam entering the steam pipe b can be matched with the steam entering the steam pipe a, so that the stripping effect of the bottom end of the rectifying tower on the acetonitrile mixed liquid can be improved, and the use energy consumption of the rectifying tower is reduced to a certain extent.
(3) The packing has the molecular sieve granule between two sieve boards that are located the bottom, and it has the active carbon granule to be located to fill between two sieve boards at top, and it has polyanion cellulose adsorption material to be located to fill between two sieve boards at central point, through the filler material between four sieve boards, cooperates the screening effect step by step of four sieve boards, can further improve the impurity removal effect in the mixed liquid of acetonitrile.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of the structure of the circulating water pipe according to the present invention;
FIG. 3 is a schematic view of the internal structure of the blending tank of the present invention;
FIG. 4 is an enlarged view of the area A in FIG. 3 according to the present invention;
fig. 5 is a schematic view of a partial structure of a deflector ring according to the present invention;
fig. 6 is an enlarged structural schematic diagram of the area B in fig. 5 according to the present invention.
In the figure: 1. a rectifying tower; 2. a blending tank; 3. a stock solution feeding pipe; 4. a steam pipe a; 5. a feed pipe; 6. a tempering and impurity removing component; 61. a sieve plate; 62. a flow guide ring; 63. an impurity removal pipe; 64. a mixing pipe; 65. a flow-collecting hood; 66. a separation well; 67. a rotating shaft; 68. a tempering motor; 69. lifting the spiral sheet; 610. a scraping rod; 7. a condensing cylinder; 8. an air outlet pipe; 9. a condensing reflux assembly; 91. purifying the collecting pipe; 92. a condensing reflux pipe; 93. a condensate pipe; 10. reboiling the barrel; 11. a raffinate inlet pipe; 12. a reboiling reflux assembly; 121. a steam return pipe; 122. a residual liquid outlet pipe; 123. a steam pipe b; 124. a circulating water pipe; 13. and a through hole.
Detailed Description
The present invention will be further described with reference to the following examples.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the technical solutions of the embodiments of the present invention will be described below with reference to the drawings of the embodiments of the present invention, it is obvious that the described embodiments are some embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative work based on the described embodiments of the present invention belong to the protection scope of the present invention.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The conditions in the embodiments may be further adjusted according to specific conditions, and simple modifications of the method of the present invention based on the concept of the present invention are all within the scope of the present invention as claimed.
Referring to fig. 1-6, the invention provides a device for purifying and recovering acetonitrile waste liquid, comprising a rectifying tower 1, a blending tank 2 is arranged at one side of the rectifying tower 1, a raw liquid feeding pipe 3 is communicated with the bottom surface of the blending tank 2 and the outer surface of the middle part of the rectifying tower 1, a steam pipe a4 communicated with the outer surface of the rectifying tower 1 is arranged below the raw liquid feeding pipe 3, a feeding pipe 5 is communicated with the outer surface of the top part of the blending tank 2, a tempering and impurity removing component 6 is arranged on the inner wall of the blending tank 2, a condensing cylinder 7 is arranged at one side of the rectifying tower 1 far away from the top part of the blending tank 2, an air outlet pipe 8 is communicated with the top surface of the condensing cylinder 7 and the top part of the rectifying tower 1, a condensing reflux component 9 is arranged inside the condensing cylinder 7, a reboiling cylinder 10 is arranged below the condensing cylinder 7, a liquid inlet pipe 11 is communicated with the bottom surface of the rectifying tower 1 at one side of the reboiling cylinder 10, a reboiling reflux component 12 matched with the rectifying tower 1 is arranged inside the reboiling cylinder 10, acetonitrile waste water is sent into a blending tank 2 through an acetonitrile waste liquid feeding pump, neutralization treatment is carried out on the acetonitrile waste water through a tempering impurity removal component 6, impurities in the acetonitrile waste water are removed through certain screening, the acetonitrile waste water enters the middle part of a rectifying tower 1 through a feeding pipe 5, heated steam is sent through a steam pipe a4, so that the acetonitrile mixed liquid is subjected to stripping rectification treatment, mixed liquid residual liquid is sent into a reboiling cylinder 10 through a residual liquid feeding pipe 11, acetonitrile in the residual liquid is heated and reboiled through a reboiling reflux component 12 and flows back to the bottom of the rectifying tower 1, acetonitrile raw liquid with the top subjected to primary rectification enters a condensation cylinder 7 through an air outlet pipe 8 for condensation treatment, so that the acetonitrile mixed liquid subjected to rectification treatment is subjected to separation and partial reflux treatment through a condensation reflux component 9, and full continuous rectification treatment on the acetonitrile mixed liquid is formed, greatly improving the effect of rectifying the acetonitrile.
Further as shown in fig. 3, 4, 5 and 6, it is worth concretely explaining that the quenching and tempering impurity removing assembly 6 includes four sieve plates 61 distributed at equal intervals, the four sieve plates 61 are all fixed with the inner wall of the tempering tank 2, a flow guide ring 62 is fixed on the top surface of the sieve plate 61 positioned at the top, impurity removing pipes 63 communicated with the outer surface of the tempering tank 2 are arranged outside the flow guide ring 62, a tempering pipe 64 communicated with the outer surface of the tempering tank 2 is arranged on the periphery of the feed pipe 5, a flow collecting cover 65 fixed with the inner wall of the flow guide ring 62 is arranged below the feed pipe 5, a plurality of separating holes 66 distributed uniformly are arranged on the inner surface of the top of the flow collecting cover 65, a rotating shaft 67 rotatably connected with the top surface of the tempering tank 2 is arranged inside the flow collecting cover 65, a quenching and tempering motor 68 coaxially connected with the rotating shaft 67 is arranged on the top surface of the tempering tank 2, a lifting spiral sheet 69 is tightly sleeved on the outer surface of the rotating shaft 67, promote the top of flight 69 and be provided with the scraping bar 610 that cup joints with the outer surface fastening of pivot 67, drive through quenching and tempering motor 68, make promotion flight 69 spiral upward movement in mass flow cover 65, and drive scraping bar 610 in step and carry out reciprocating motion, thereby make and get into in tempering tank 2 acetonitrile waste water and contain salt neutralization solution and carry out spiral lifting hybrid processing, and make the impurity in the mixed liquid promote through the spiral that promotes flight 69, make granular impurity enter into the inside to the kuppe through the separation hole 66 at mass flow cover 65 top, thereby improve the separation effect to the particulate matter of mixed liquid in the mass flow cover 65 greatly, and reciprocating motion through scraping bar 610, effectively avoid mass flow cover 65 top separation hole 66 to take place blocking phenomenon, and sieve through four sieve plates 61, further improve the edulcoration effect to mixed liquid.
Further shown in fig. 4, it is worth specifically explaining that the mass flow cover 65 is funnel-shaped, the top height of the lifting spiral piece 69 is higher than the height of the column shape of the mass flow cover 65, the top surface of the scraping rod 610 is inclined to form an arc surface, the outer surface of the scraping rod 610 and the inner surface of the top of the mass flow cover 65 are adaptive to form an arc surface, the height of the lifting spiral piece 69 is set, the lifting spiral piece 69 is convenient to lift impurities of mixed liquid to the separation hole 66 of the mass flow cover 65 in a spiral manner to perform separation treatment, the shape of the scraping rod 610 is convenient to perform full scraping treatment on the separation hole 66 of the mass flow cover 65, and therefore the separation effect of the mass flow cover 65 is guaranteed.
Further as shown in fig. 4 and fig. 6, it is worth specifically explaining that a plurality of through holes 13 distributed circumferentially are formed in the surface of the lifting spiral piece 69, the hole diameter of each through hole 13 is smaller than that of the separation hole 66, the outer surface of the flow guide ring 62 is arranged in an arc surface, and the through holes 13 are arranged, so that impurities with smaller specifications can spirally rise along with the lifting spiral piece 69, and the mixed liquid in the flow collecting cover 65 is sufficiently screened through the sieve plate 61.
Further as shown in fig. 1, fig. 3 and fig. 5, it is worth specifically explaining that, the condensing and refluxing component 9 includes a purification collecting pipe 91 communicated with the outer surface of the bottom of the condensation cylinder 7, the air outlet pipe 8 and the purification collecting pipe 91 are respectively located at two sides of the condensation cylinder 7, the outer surface of the purification collecting pipe 91 is communicated with the outer surface of the top of the rectification tower 1 to form a condensing and refluxing pipe 92, a condensing water pipe 93 is fixed on the outer surface of two sides of the condensation cylinder 7, the condensing water pipe 93 is externally connected with a circulating water pump and a cooling water supply device, and is used for condensing and recovering the acetonitrile mixed liquid subjected to the preliminary rectification treatment in the condensation cylinder 7, and collecting and recovering the acetonitrile mixed liquid through the purification collecting pipe 91, and part of the acetonitrile mixed liquid returns to the top of the rectification tower 1 through the condensing and refluxing pipe 92 to perform the rectification treatment again.
As further shown in fig. 1, fig. 2, fig. 3 and fig. 5, it should be specifically noted that the reboiling reflux assembly 12 includes a steam reflux pipe 121 communicated with the top surface of the reboiling barrel 10, the other end of the steam reflux pipe 121 is communicated with the outer surface of the bottom of the rectification column 1, a residual liquid outlet pipe 122 communicated with the bottom surface of the reboiling barrel 10 is disposed below the steam reflux pipe 121, a steam pipe b123 is communicated with the outer surface of one end of the steam column far away from the residual liquid inlet pipe 11, two symmetrically distributed circulation water pipes 124 are fixedly penetrated through the outer surfaces of both sides of the reboiling barrel 10, the circulation water pipes 124 are used for cooling the acetonitrile residual liquid mixed solution, so that most of the residual liquid is collected through the residual liquid outlet pipe 122, thereby forming a sufficient removal treatment of the acetonitrile mixed solution, the circulation water pipe 124 is externally connected with a cooling water supply device for providing a certain condensation effect in the reboiling barrel 10, and so that a part of the residual liquid mixed solution flows back the acetonitrile remaining in the residual liquid to the bottom of the rectification column 1 through the steam reflux pipe 121.
Further as shown in fig. 2, it is worth specifically explaining that the steam pipe b123 and the two circulating water pipes 124 are distributed in an isosceles triangle, the two circulating water pipes 124 are respectively located outside the top axis of the residual liquid outlet pipe 122, and the arrangement of the circulating water pipes 124 enables the residual liquid of the mixed liquid entering through the residual liquid inlet pipe 11 to be directly condensed and enter into the residual liquid outlet pipe 122 for diversion collection treatment under the action of the circulating water pipes 124.
The scheme has the following working processes: acetonitrile waste liquid feed pump and neutralization liquid feed pump send the acetonitrile waste liquid and neutralization liquid into the inside of blending tank 2 respectively to carry out neutralization reaction, through the drive of tempering motor 68, make the acetonitrile waste liquid and contain salt neutralization liquid carry out the spiral mixing neutralization treatment in blending tank 2, make promotion flight 69 upwards move in the spiral of mass flow cover 65, and drive scraping rod 610 to carry out reciprocating motion in step, thereby make the acetonitrile waste water and the neutralization liquid that contains salt in getting into blending tank 2 carry out the spiral promotion mixing treatment, and make impurity in the mixed liquid through the spiral promotion of promotion flight 69, make granular impurity enter into the inside of kuppe through the separation hole 66 at the top of mass flow cover 65, thereby improve the particulate matter separation effect to the mixed liquid in the mass flow cover 65 greatly, and through the reciprocating motion of scraping rod 610, effectively avoid the separation hole 66 at the top of mass flow cover 65 to take place the jam phenomenon, and the mixed liquid after neutralization treatment enters the middle part of the rectifying tower 1 through the stock solution feeding pipe 3, the mixed liquid is subjected to stripping and rectifying treatment through the steam entering in the steam pipe a4, so that the mixed liquid residual liquid enters the reboiling cylinder 10 through the residual liquid inlet pipe 11, the mixed liquid rectifying gas enters the condensing cylinder 7 through the steam outlet pipe 8 along with the steam to be subjected to condensing treatment, the steam rectifying treatment on the mixed liquid is completed, meanwhile, the mixed liquid residual liquid enters the reboiling cylinder 10 through the residual liquid inlet pipe 11, most of the mixed liquid residual liquid is directly guided out from the residual liquid outlet pipe 122, the acetonitrile component contained in the mixed liquid residual liquid enters the bottom of the rectifying tower 1 through the steam return pipe 121 to be subjected to stripping and rectifying treatment through the action of the heating steam of the steam pipe b123, and the acetonitrile mixed liquid is effectively prevented from directly flowing out from the residual liquid outlet pipe 122, the rectification effect and the sufficiency to the acetonitrile waste liquid have been improved greatly, and the mixed liquid of 1 top rectification processing through rectifying column enters into condensation cylinder 7 in through outlet duct 8, carries out condensation processing to it through condensate pipe 93 to make the acetonitrile of condensation derive through purification collecting pipe 91, the gaseous acetonitrile of partial condensation passes through condensation reflux pipe 92 and reentries into the rectification end of rectifying column 1 and carries out rectification processing once more.
According to the working process, the following steps are known: carry out hybrid processing through blending tank 2 to acetonitrile waste water and contain salt neutralization solution, and promote the spiral separation to its inside impurity, and carry out the screening processing through four sieve plates 61 once more, thereby improve the impurity removal effect in the mixed liquid of acetonitrile greatly, thereby effectively improve the quality that carries out recovery processing to the acetonitrile, and carry out rectification treatment to it through rectifying column 1, through the reflux action of reboiling a section of thick bamboo 10 and condenser tube 7, make it form continuous rectification processing, thereby improve the sufficiency that the mixed liquid of acetonitrile carries out rectification processing greatly, effectively avoid containing the acetonitrile composition in the mixed liquid raffinate, accord with the environmental protection theory, and the steam that gets into in the steam pipe b123 can cooperate the steam that gets into in steam pipe a4, can improve the stripping effect of the bottom of rectifying column 1 to the mixed liquid of acetonitrile, its use energy consumption has been reduced to a certain extent.
The use method of the acetonitrile waste liquid purification and recovery device comprises the following steps:
s1, quenching and tempering and impurity removal: the acetonitrile waste liquid and the neutralization liquid are respectively sent into the interior of the blending tank 2 through an acetonitrile waste liquid feeding pump and a neutralization liquid feeding pump for neutralization reaction, the acetonitrile waste liquid and the neutralization liquid are spirally mixed and neutralized in the blending tank 2 through the driving of a tempering motor 68, and screening and impurity removing treatment is carried out through four screen plates 61;
the top that is located the sieve 61 of bottom and stoste inlet pipe 3 is in the laminating state, thereby improve the isolation removal effect to stoste inlet pipe 3 department mixed liquid, it has the molecular sieve granule to be located to fill between two sieves 61 of bottom, it has the activated carbon particle to be located to fill between two sieves 61 at top, it has polyanion cellulose adsorption material to be located to fill between two sieves 61 of central point, through the filler material between four sieves 61, can further improve the impurity removal effect to in the acetonitrile mixed liquid.
S2, steam rectification: the mixed liquor subjected to neutralization, screening and impurity removal in the step S1 enters a rectifying tower 1 through a stock solution feeding pipe 3, the mixed liquor is subjected to stripping and rectifying treatment through steam entering a steam pipe a4, so that the mixed liquor residual enters a reboiling cylinder 10 through a residual liquid inlet pipe 11, the distilled gas of the mixed liquor enters a condensation cylinder 7 through a gas outlet pipe 8 along with the steam to be subjected to condensation treatment, and the steam rectifying treatment on the mixed liquor is completed;
s3, reflux rectification:
1) Heating the mixed liquid residual liquid in the step S2 through a steam pipe b123, so that steam enables the residual liquid to flow back to the bottom of the rectifying tower 1 through the steam pipe, and rectifying the residual liquid again;
2) The mixed liquid rectification gas is cooled by a condensate pipe 93, the liquid subjected to condensation treatment is guided by a purification collecting pipe 91, the acetonitrile waste liquid is subjected to primary purification and recovery treatment, and part of the liquid enters the top of the rectification tower 1 through a condensation reflux pipe 92 to be rectified again.
To sum up: carry out hybrid processing through blending tank 2 to acetonitrile waste water and contain salt neutralization solution, and promote spiral separation to its inside impurity, and again through four sieve 61 and four packing materials between the sieve 61, can further improve the impurity removal effect in the mixed liquid of acetonitrile, thereby improve the impurity removal effect in the mixed liquid of acetonitrile greatly, thereby effectively improve the quality that carries out recovery processing to the acetonitrile, and carry out rectification treatment to it through rectifying column 1, through the reflux action of reboiling section of thick bamboo 10 and condenser tube 7, make it form continuous rectification processing, thereby improve the sufficiency that the mixed liquid of acetonitrile carries out rectification processing greatly, effectively avoid containing the acetonitrile composition in the mixed liquid raffinate, accord with the environmental protection theory, and the steam that gets into in the steam pipe b123 can cooperate the steam that gets into in steam pipe a4, can improve the stripping effect of the bottom of rectifying column 1 to the mixed liquid of acetonitrile, its energy consumption of using has been reduced to a certain extent.
The tempering motor 68 is commercially available, and the tempering motor 68 is provided with a power supply, which belongs to the mature technology in the field and is fully disclosed, so repeated description is omitted in the specification.
Unless defined otherwise, technical or scientific terms used herein should be construed as commonly understood by one of ordinary skill in the art, and the use of the term "comprising" or "including" and the like in the present invention means that the element or item preceding the term covers the element or item listed after the term and its equivalents, but does not exclude other elements or items, and the term "connected" or "connected" and the like are not limited to physical or mechanical connections, but may also include electrical connections, whether direct or indirect, "upper", "lower", "left", "right", and the like, are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may be changed accordingly.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The utility model provides a purification recovery unit of acetonitrile waste liquid, includes rectifying column (1), its characterized in that, one side of rectifying column (1) is provided with blending tank (2), the bottom surface of blending tank (2) with the middle part surface intercommunication of rectifying column (1) has stoste inlet pipe (3), the below of stoste inlet pipe (3) is provided with steam pipe a (4) that are linked together with rectifying column (1) surface, the top surface intercommunication of blending tank (2) has conveying pipe (5), the inner wall of blending tank (2) is provided with quenching and tempering edulcoration subassembly (6), top one side that blending tank (2) were kept away from in rectifying column (1) is provided with condensing cylinder (7), the top surface of rectifying column (1) with the top surface intercommunication of condensing cylinder (7) has outlet duct (8), the inside of condensing cylinder (7) is provided with condensing reflux subassembly (9), the below of condensing cylinder (7) is provided with reboiling cylinder (10), a side face of reboiling cylinder (10) with the bottom surface of rectifying column (1) has feed liquor reflux subassembly (11), the inside reflux subassembly (12) that reboils with the rectifying column (1) that reboiling cooperatees.
2. The purification and recovery device of acetonitrile waste liquid according to claim 1, characterized in that: quenching and tempering edulcoration subassembly (6) including four sieve (61) that are the equidistance and distribute, four sieve (61) all with the inner wall of blending tank (2) is fixed, be located the top surface of sieve (61) is fixed with water conservancy diversion ring (62), the outside of water conservancy diversion ring (62) is provided with edulcoration pipe (63) with blending tank (2) surface intercommunication, the periphery of conveying pipe (5) be provided with blending pipe (64) of blending tank (2) surface intercommunication, the below of conveying pipe (5) be provided with water conservancy diversion ring (62) inner wall fixed mass flow cover (65), a plurality of separation holes (66) that are evenly distributed have been seted up to the top internal surface of mass flow cover (65), the inside of mass flow cover (65) be provided with the pivot (67) of blending tank (2) top surface rotation connection, the top surface of blending tank (2) install with pivot (67) coaxial coupling's quenching and tempering motor (68), the surface of pivot (67) cup joints the fastening has promotion flight (69), the top of promotion flight (69) cup joints the fastening with the surface of pivot (610) and connects the scraping rod.
3. The purification recovery unit of acetonitrile waste liquid of claim 2, characterized in that: the flow collecting cover (65) is arranged in a funnel shape, the top end of the lifting spiral sheet (69) is higher than the height of the column shape of the flow collecting cover (65), the top surface of the scraping rod (610) is arranged in an inclined arc surface, and the outer surface of the scraping rod (610) and the inner surface of the top of the flow collecting cover (65) are in matched arc surfaces.
4. The purification and recovery device of acetonitrile waste liquid according to claim 2, characterized in that: the surface of the lifting spiral piece (69) is provided with a plurality of through holes (13) distributed circumferentially, the hole diameter of each through hole (13) is smaller than that of the corresponding separation hole (66), and the outer surface of the flow guide ring (62) is arranged in an arc surface manner.
5. The purification recovery unit of acetonitrile waste liquid of claim 1, characterized in that: condensation reflux subassembly (9) include with purification collecting pipe (91) of condensing cylinder (7) bottom surface intercommunication, outlet duct (8) with purification collecting pipe (91) are located respectively the both sides of condensing cylinder (7), the surface of purification collecting pipe (91) with the top surface intercommunication of rectifying column (1) has condensate return pipe (92), the both sides external surface mounting of condensing cylinder (7) runs through condensate pipe (93).
6. The purification and recovery device of acetonitrile waste liquid according to claim 1, characterized in that: the reboiling reflux assembly (12) comprises a steam reflux pipe (121) communicated with the top surface of the reboiling cylinder (10), the other end of the steam reflux pipe (121) is communicated with the outer surface of the bottom of the rectifying tower (1), a residual liquid outlet pipe (122) communicated with the bottom surface of the reboiling cylinder (10) is arranged below the steam reflux pipe (121), a steam pipe b (123) is communicated with the outer surface of one end, far away from the residual liquid inlet pipe (11), of the steam tower, and two symmetrically-distributed circulating water pipes (124) are fixedly penetrated through the outer surfaces of two sides of the reboiling cylinder (10).
7. The apparatus for purifying and recovering the acetonitrile waste liquid according to claim 6, wherein: the steam pipe b (123) and the two circulating water pipes (124) are distributed in an isosceles triangle, and the two circulating water pipes (124) are respectively positioned on the outer sides of the top axial lines of the residual liquid outlet pipes (122).
8. A method for using the apparatus for purifying and recovering the acetonitrile waste liquid according to any one of claims 1 to 7, wherein: the method comprises the following steps:
s1, quenching and tempering and impurity removal: the acetonitrile waste liquid and the neutralization liquid are respectively sent into a blending tank (2) through an acetonitrile waste liquid feeding pump and a neutralization liquid feeding pump to carry out neutralization reaction, the acetonitrile waste liquid and the neutralization liquid are spirally mixed and neutralized in the blending tank (2) through the driving of a tempering motor (68), and screening and impurity removing treatment is carried out through four sieve plates (61);
s2, steam rectification: the mixed liquor subjected to neutralization, screening and impurity removal in the step S1 enters a rectifying tower (1) through a stock solution feeding pipe (3), the mixed liquor is subjected to stripping and rectifying treatment through steam entering a steam pipe a (4), so that the mixed liquor residual liquid enters a reboiling cylinder (10) through a residual liquid inlet pipe (11), the rectified gas of the mixed liquor enters a condensing cylinder (7) through a gas outlet pipe (8) along with the steam for condensation treatment, and the steam rectifying treatment on the mixed liquor is completed;
s3, reflux rectification:
1) Heating the mixed liquid residual liquid in the step S2 through a steam pipe b (123), so that steam flows the residual liquid back to the bottom of the rectifying tower (1) through the steam pipe, and rectifying the residual liquid again;
2) The mixed liquid rectification gas is cooled through a condensate pipe (93), the liquid subjected to condensation treatment is guided through a purification collecting pipe (91), the acetonitrile waste liquid is subjected to primary purification and recovery treatment, and part of liquid enters the top of the rectification tower (1) through a condensation return pipe (92) to be rectified again.
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|---|---|---|---|
| CN202210651277.5A CN115180756A (en) | 2022-06-10 | 2022-06-10 | Acetonitrile waste liquid purification and recovery device and method |
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| CN202210651277.5A CN115180756A (en) | 2022-06-10 | 2022-06-10 | Acetonitrile waste liquid purification and recovery device and method |
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