CN218786562U

CN218786562U - Device for improving quality and zero discharge of anhydrous sodium sulphate

Info

Publication number: CN218786562U
Application number: CN202221586612.XU
Authority: CN
Inventors: 王首锋; 周新文; 冉建军; 刘佳妮
Original assignee: Guangdong Jiana Energy Technology Co Ltd; Qingyuan Jiazhi New Materials Research Institute Co Ltd; Jiangxi Jiana Energy Technology Co Ltd
Current assignee: Guangdong Jiana Energy Technology Co Ltd; Qingyuan Jiazhi New Materials Research Institute Co Ltd; Jiangxi Jiana Energy Technology Co Ltd
Priority date: 2022-06-23
Filing date: 2022-06-23
Publication date: 2023-04-04
Anticipated expiration: 2032-06-23

Abstract

A device for improving the quality and zero discharge of anhydrous sodium sulphate comprises an ammonia still, an inclined tube sedimentation tank, a microporous filter, a forced circulation evaporator and a centrifugal machine. The ammonia still passes through three pipeline respectively with pipe chute sedimentation tank, ternary mother liquor pond and aqueous ammonia collecting pit, the pipe chute sedimentation tank is provided with two imports and two exports, and two imports are connected with heat exchanger, ammonia still respectively, and two exports are connected with microporous filter, dense slurry tank respectively, pass through the pipe connection between microporous filter and the dense slurry tank, the dense slurry tank passes through the pipeline and is connected with the pressure filter, centrifuge passes through the pipeline and is connected with crystal separator, heat exchanger, drying bed respectively, the drying bed passes through pipeline and baling press intercommunication. This promote anhydrous sodium sulphate quality and zero release's device utilizes mother liquor production anhydrous sodium sulphate after the ternary mother liquor deamination, and wherein concentrated impurity is kept apart and is shunted, makes output anhydrous sodium sulphate quality more stable, and the zero release is also realized to waste water.

Description

Device for improving quality and zero discharge of anhydrous sodium sulphate

Technical Field

The utility model belongs to the technical field of anhydrous sodium sulphate technique and specifically relates to a promote anhydrous sodium sulphate quality and zero release's device and method thereof.

Background

The anhydrous sodium sulfate refers to sodium sulfate, which is salt formed by combining sulfate radical and sodium ion, and has a chemical formula of Na ₂ SO ₄ Sodium sulfate is soluble in water, the solution of which is mostly neutral, soluble in glycerol and insoluble in ethanol. Anhydrous sodium sulphate, white, odorless, bitter crystals or powder, and has hygroscopicity. Is mainly used for manufacturing water glass, enamel, analytical chemical reagents, pharmaceuticals, feed and the like, sodium sulfate can be converted into hexagonal crystals at 241 ℃, and sodium sulfate is the most commonly used sodium sulfate in organic synthesis laboratoriesAnd (6) treating the drying agent.

The patent of China CN201910461691.8 discloses a process for treating ternary precursor wastewater, which comprises the following steps: carrying out steam stripping treatment on a mother solution generated in the preparation process of the ternary precursor to obtain anhydrous sodium sulphate; performing multi-stage reverse osmosis membrane treatment on washing water generated in the preparation process of the ternary precursor, combining concentrated solution generated in the multi-stage reverse osmosis membrane treatment into the mother solution for continuous treatment, and reusing dialyzate generated in the multi-stage reverse osmosis membrane treatment for production to realize the cyclic treatment of the ternary precursor wastewater; the recovery of ammonia and heavy metals in the wastewater is realized; the mother liquor is subjected to stripping treatment and then deamination treatment and MVR evaporation, the produced ammonia water and distilled water can be reused for production, and the anhydrous sodium sulphate as a byproduct is sold as a chemical raw material; the full-scale circulation of wastewater treatment and zero discharge are realized. China CN202021710784.4 discloses a ternary wastewater resource treatment system, and large granular impurities in the ternary wastewater can be effectively removed by performing pre-precipitation through a pre-precipitation tank; the method comprises the steps of forming hydroxide precipitates from heavy metal ions by arranging a first reaction tank and adding sodium hydroxide into the first reaction tank, and filtering and removing flocculent precipitates generated in a second reaction tank by arranging a second reaction tank and adding a heavy metal capturing agent and a flocculating agent into the second reaction tank through a ceramic membrane device; by arranging the gaseous membrane device, the wastewater and the absorption liquid flow at two sides of the hollow fiber microporous hydrophobic membrane, the ammonia nitrogen is removed, and a high-concentration ammonium salt solution is byproduct; by arranging the SWRO device and the BWRO device, the sodium sulfate can be separated from the ternary wastewater, and sodium sulfate crystals can be obtained by the freezing and crystallizing device, so that the recovery of salt resources is fully realized.

Above-mentioned technique of current preparation anhydrous sodium sulphate adopts the plate frame direct filtration after the deamination, and wherein free nickel can not reach the requirement, leads to impurity enrichment in the MVR system, and output anhydrous sodium sulphate quality is unstable, can not evaporate in making the system, leads to concentrated water to return or need increase equipment recovery impurity salt toward the front end to still can output waste water, just can discharge after needing filtration treatment, increased manufacturing cost. Similar Chinese patent also discloses a near zero emission treatment system and a near zero emission treatment process for ternary precursor material production wastewater, wherein a precipitation method is adopted to recover heavy metals, and a two-stage MVR (mechanical vapor recompression) method is adopted to perform resource recovery on water, ammonia gas and sodium sulfate in the wastewater. The ammonia water generated after the ammonia gas volatilized and escaped from the waste water heating and heavy metal deposition clarification process is recovered is reused for production, water vapor and ammonia gas are generated in the MVR primary evaporation concentration separation process, the ammonia gas is recovered for producing the ammonia water while condensed water is recovered, the integration technology for simultaneously recovering the water and the ammonia replaces the existing steam stripping ammonia recovery technology with high energy consumption in a single process, the treatment process is reduced, the operation cost is reduced, and the secondary MVR evaporation crystallization technology is adopted for recovering resource anhydrous sodium sulphate and the condensed water. The method has the advantages of protecting the environment, reducing the discharge of the wastewater with high salt content, reducing the wastewater recycling treatment cost, changing waste into valuable, generating economic benefit and realizing the near-zero discharge treatment of the wastewater. Chinese CN201910044111.5 discloses an integrated treatment system for recovering sodium sulfate from ternary precursor production wastewater, which comprises a first evaporation concentration device, a second evaporation concentration device, a thickener and a drying tower which are connected in sequence; the first evaporation concentration device comprises a first-effect heater and a first-effect separator which are connected; the second evaporation concentration device comprises a double-effect heater and a double-effect separator which are connected; the drying equipment and the crystallizing equipment of the system are integrated, the flow is short, the efficiency is high, the material conveying is convenient, the operation cost can be effectively reduced, the moisture content of the sodium sulfate dry powder obtained by using the system and the method is less than 0.5%, dust and water vapor generated by the system are re-absorbed and then return to the system for crystallization, and the system is economical and environment-friendly. For another example, chinese patent No. CN201710229153.7 discloses a treatment method and a treatment system for ternary cathode material production wastewater, wherein the treatment method firstly adopts a process flow combining membrane separation, solid-liquid separation and evaporative crystallization: firstly, using a sulfuric acid solution as an absorbent, and converting ammonia nitrogen in wastewater into ammonium sulfate by adopting membrane separation to realize deamination; because the pH value in the early stage is alkaline, a large amount of metal in the wastewater after deamination breaks the complex and forms precipitate with alkali, and heavy metal precipitate in the solution is removed by filtration; after filtration, the supernatant was crystallized by evaporation to give sodium sulfate. The treatment method disclosed by the invention is used for carrying out advanced treatment and recycling on the ternary cathode material production wastewater, effectively solving the treatment problem of the ternary cathode material production wastewater, recycling resources of ammonia, heavy metal and sodium sulfate in the wastewater, realizing high water recovery rate and realizing zero emission. Four as China CN201820051097.2 patent discloses a lithium battery nickel-cobalt-manganese ternary precursor wastewater treatment system, which comprises a pretreatment unit, an ammonia water recovery unit and a sodium sulfate crystal recovery unit. The utility model has the advantages that: 1) The problems of small operation elasticity, low treatment efficiency, poor treatment effect and short service life of equipment of the ternary precursor sewage treatment system are solved; fresh water and ammonia water generated by waste liquid treatment are recovered, and a byproduct of anhydrous sodium sulfate is removed, so that the full-component recycling of the waste water is realized; the production has strong continuous stability, reduces the cost of treating waste liquid, and ensures the continuous and stable operation of production. 2) The utility model provides a setting mode of ammonia water recovery unit and sodium sulfate crystal recovery unit in ternary precursor effluent disposal system has improved effluent treatment plant's whole operation elasticity greatly to improve effluent treatment efficiency, whole system can implement production in succession high-efficiently. For example, chinese patent No. CN201720369038.5 discloses a system for treating wastewater from ternary anode material production, comprising: the membrane separation device is used for carrying out membrane separation on the ternary cathode material production wastewater to obtain deamination wastewater; the solid-liquid separation device is used for filtering the deamination wastewater to obtain supernatant and sediment, and is communicated with the membrane separation device; and the evaporative crystallization device is used for evaporating and crystallizing the supernatant to obtain sodium sulfate, and is communicated with the solid-liquid separation device. The utility model discloses a processing system carries out the advanced treatment retrieval and utilization to ternary cathode material waste water, effectively solves the processing problem of ternary cathode material waste water, and ammonia, heavy metal and sodium sulfate resource in the recovery waste water, the water rate of recovery is high, realizes the zero release.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to provide a promote anhydrous sodium sulphate quality and device and method of zero release to solve the problem that proposes in the above-mentioned background art.

In order to solve the problem, the utility model provides a promote device of anhydrous sodium sulphate quality and zero release, including ammonia still, pipe chute sedimentation tank, microfilter, thick liquid jar, pressure filter, falling film evaporation ware, forced circulation evaporimeter, crystal separator, stiff ware, centrifuge, drying bed, baling press, heat exchanger, ammonia still pass through three pipeline respectively with pipe chute sedimentation tank, ternary mother liquor pond and aqueous ammonia collecting pit, the pipe chute sedimentation tank is provided with two imports and two exports, and two imports are connected with heat exchanger, ammonia still respectively, and two exports are connected with microfilter, thick liquid jar respectively, pass through pipe connection between microfilter and the thick liquid jar, thick liquid jar passes through the pipeline and is connected with the pressure filter, microfilter, falling film evaporation ware, forced circulation evaporimeter, crystal separator, stiff ware, centrifuge pass through pipe connection between the two, crystal separator, heat exchanger, drying bed are connected with crystal separator, drying bed respectively through the pipeline, drying bed passes through pipeline and baling press intercommunication.

Further, the pipeline between the inclined tube sedimentation tank and the microporous filter is arranged at a quarter of the height above the inclined tube sedimentation tank.

Furthermore, a pipeline between the inclined tube sedimentation tank and the ammonia still is arranged above the dirt storage tank in the inclined tube sedimentation tank.

Furthermore, the cross section of the inclined tube in the inclined tube sedimentation tank is of a continuous wave structure.

Further, a sewage storage pool with an inverted trapezoidal structure is arranged at the bottom of the inner side of the inclined tube sedimentation tank.

Further, the falling film evaporator and the forced circulation evaporator are arranged in the same MVR system.

Further, the centrifuge is provided with three output pipelines which are respectively used for conveying crystallization, concentrated water with high impurities and concentrated water with low impurities.

Further, a vibrating screen is arranged on the drying bed.

In the production beginning, the operation method of the utility model comprises the following steps:

(1) Deaminating the ternary mother liquor by an ammonia still, sending the deaminated liquor into an inclined tube sedimentation tank for weight removal, and simultaneously sending ammonia water to a production workshop through a pipeline;

(2) Sending supernatant in the inclined tube sedimentation tank into a microporous filter through a pipeline, enabling effluent to enter an MVR raw water bucket, and performing microporous filtration again after impurity enrichment and front-end cooling in the MVR operation process, so as to reduce impurities in a system and ensure stable operation of the system;

(3) The impurity salt part separated by the centrifuge is in large particles, crystals pass through a drying bed and enter a vibrating screen through a fluidized bed, coarse particles of oversize products can be discharged and packaged independently, the stable quality of the anhydrous sodium sulphate is ensured, and zero emission is achieved after MVR runs for a long time.

Further, the MVR operation process of the step (2) specifically includes the following steps:

after being filtered by a microporous filter, the high-impurity concentrated water is sequentially fed into a falling film evaporator and a forced circulation evaporator through pipelines, then is fed into a crystallization separator, is separated and then is fed into a thickener, and then is separated by a centrifugal machine to obtain high-impurity concentrated water and low-impurity concentrated water, the high-impurity concentrated water is fed into an inclined tube sedimentation tank for treatment after passing through a heat exchanger, and the low-impurity concentrated water is fed into the crystallization separator for secondary separation treatment.

The utility model utilizes the mother liquor after the ternary mother liquor is deaminated to produce anhydrous sodium sulphate, wherein the concentrated impurities are isolated and shunted, so that the quality of the produced anhydrous sodium sulphate is more stable, and the zero discharge of the waste water is realized; removing weight of the ternary mother liquor after deamination in an inclined tube sedimentation tank, feeding supernatant into a microporous filter, feeding effluent into an MVR raw water bucket, and performing microporous filtration again after impurity enrichment and front-end cooling in the MVR operation process to reduce impurities in a system and ensure stable operation of the system; and the impurity salt part is in the large granule, and the crystallization is through fluidized bed entering shale shaker, and oversize thing coarse grain can be discharged the packing alone, can guarantee anhydrous sodium sulphate stable quality like this, and MVR long-time operation reaches the zero release.

Drawings

Fig. 1 is a connection diagram, i.e., a production flow diagram, of the equipment system of the present invention.

Detailed Description

The technical solutions of the present invention will be described in detail and completely with reference to the accompanying drawings, and it is to be understood that the described embodiments are only some embodiments of the present invention, rather than all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

Example one

Referring to fig. 1, the present invention provides a technical solution: a device for improving the quality and zero emission of anhydrous sodium sulphate and a method thereof are disclosed, comprising an ammonia distillation tower, an inclined tube sedimentation tank, a microporous filter, a thick liquid tank, a filter press, a falling film evaporator, a forced circulation evaporator, a crystallization separator, a thickener, a centrifuge, a drying bed, a packing machine and a heat exchanger, wherein the ammonia distillation tower is respectively connected with the inclined tube sedimentation tank, a ternary mother liquid tank and an ammonia water collecting tank through three pipelines, the inclined tube sedimentation tank is provided with two inlets and two outlets, the two inlets are respectively connected with the heat exchanger and the ammonia distillation tower, the two outlets are respectively connected with the microporous filter and the thick liquid tank, the microporous filter is connected with the thick liquid tank through a pipeline, the thick liquid tank is connected with the filter press through a pipeline, the microporous filter, the falling film evaporator, the forced circulation evaporator, the crystallization separator, the thickener and the centrifuge are respectively connected with the crystallization separator, the heat exchanger and the drying bed through pipelines, and the drying bed is communicated with the packing machine through a conveying pipeline.

Example two

Referring to fig. 1, the pipeline between the inclined tube sedimentation tank and the microporous filter is arranged at a quarter of the height above the inclined tube sedimentation tank; the pipeline between the inclined tube sedimentation tank and the ammonia still is arranged above the internal dirt storage tank of the inclined tube sedimentation tank; the cross section of the inclined tube in the inclined tube sedimentation tank is of a continuous wave-folded structure; a dirt storage tank with an inverted trapezoidal structure is arranged at the bottom of the inner side of the inclined tube sedimentation tank; the falling film evaporator and the forced circulation evaporator are arranged in the same MVR system; the centrifugal machine is provided with three output pipelines which are respectively used for conveying crystallization, high-impurity concentrated water and low-impurity concentrated water; the drying bed is provided with a vibrating screen.

The other structures are the same as those in the first embodiment.

EXAMPLE III

A method for improving the quality and zero emission of anhydrous sodium sulphate comprises the following steps:

(1) Deaminating the ternary mother liquor by an ammonia still, sending the deaminated liquor to an inclined tube sedimentation tank for weight removal, and meanwhile sending ammonia water to a production workshop through a pipeline;

(2) Sending supernatant in the inclined tube sedimentation tank into a microporous filter through a pipeline, enabling outlet water to enter an MVR raw water bucket, filtering by the microporous filter, sequentially sending the filtered supernatant into a falling film evaporator and a forced circulation evaporator through the pipeline, then inputting the filtered supernatant into a crystallization separator, sending the separated supernatant into a thickener after separation, then separating out concentrated water with high impurities and concentrated water with low impurities through a centrifuge, enabling the concentrated water with high impurities to pass through a heat exchanger and then input into the inclined tube sedimentation tank for treatment, sending the concentrated water with low impurities into the crystallization separator for secondary separation treatment, and returning the temperature to the front end after the impurities are enriched in the MVR operation process and then filtering through micropores again, so that the impurities in the system are reduced, and the stable operation of the system is ensured;

(3) The impurity salt part separated by the centrifuge is in large particles, crystals pass through the drying bed and enter the vibrating screen through the fluidized bed, coarse particles of oversize products can be discharged and packed independently, the stable quality of anhydrous sodium sulphate is ensured, and zero emission is achieved by MVR long-time operation.

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

1. The utility model provides a promote anhydrous sodium sulphate quality and device of zero release, includes ammonia still, pipe chute sedimentation tank, microporous filter, thick liquid jar, pressure filter, falling film evaporator, forced circulation evaporimeter, crystallization separator, stiff ware, centrifuge, drying bed, baling press, heat exchanger, its characterized in that: the ammonia still communicates with pipe chute sedimentation tank, ternary mother liquor pond and aqueous ammonia collecting pit respectively through three pipeline, the pipe chute sedimentation tank is provided with two imports and two exports, and two imports communicate with heat exchanger, ammonia still respectively, and two exports communicate with microporous filter, thick liquid jar respectively, pass through the pipe connection between microporous filter and the thick liquid jar, thick liquid jar passes through the pipeline and is connected with the pressure filter, microporous filter, falling film evaporation ware, forced circulation evaporimeter, crystal separator, thickener, centrifuge are adjacent pass through the pipe connection between the two, centrifuge passes through the pipeline and is connected with crystal separator, heat exchanger, drier bed respectively, the drier bed passes through pipeline and baling press intercommunication.

2. The apparatus of claim 1, wherein the apparatus comprises: and the pipeline between the inclined tube sedimentation tank and the microporous filter is arranged at a quarter of the height above the inclined tube sedimentation tank.

3. The apparatus as claimed in claim 1, wherein the apparatus comprises: and the pipeline between the inclined tube sedimentation tank and the ammonia still is arranged above the sewage storage tank in the inclined tube sedimentation tank.

4. The apparatus as claimed in claim 1, wherein the apparatus comprises: the cross section of the inclined tube in the inclined tube sedimentation tank is of a continuous wave structure.

5. The apparatus of claim 1, wherein the apparatus comprises: and a dirt storage tank with an inverted trapezoidal structure is arranged at the bottom of the inner side of the inclined tube sedimentation tank.

6. The apparatus as claimed in claim 1, wherein the apparatus comprises: the falling film evaporator and the forced circulation evaporator are arranged in the same MVR system.

7. The apparatus as claimed in claim 1, wherein the apparatus comprises: the centrifuge is provided with three output pipelines which are respectively used for conveying crystallization, concentrated water with high impurities and concentrated water with low impurities.

8. The apparatus of claim 1, wherein the apparatus comprises: and a vibrating screen is arranged on the drying bed.