CN218280573U - Concentration device for zirconium oxychloride aqueous solution - Google Patents

Abstract

The utility model belongs to the technical field of metal mineral development and treatment, and particularly discloses a concentration device of a zirconium oxychloride aqueous solution, which comprises a feeding unit, a preheating unit, an evaporation concentration unit, a gas washing unit, a steam compression unit and a discharging unit; the feeding unit is used for carrying the material to the district in, preheats the unit and is used for preheating the zirconium oxychloride aqueous solution that the feeding unit provided, and the evaporation concentration unit is used for carrying out evaporation concentration to the zirconium oxychloride aqueous solution after preheating the unit, and the scrubbing unit is used for carrying out the scrubbing to the secondary steam that produces in the evaporation concentration unit clean, and the steam compression unit is used for carrying out steam compression to the secondary steam after the scrubbing in the scrubbing unit. The utility model discloses for single-effect evaporation scheme, MVR's introduction can the significantly reduced raw steam's consumption, reduces the running cost, for indirect MVR evaporation scheme, can make full use of steam temperature rise, the heat transfer area and the equipment quantity that significantly reduce.

Description

Concentration device for zirconium oxychloride aqueous solution

Technical Field

The utility model relates to a metal mineral development and processing technology field, in particular to a enrichment facility of dichloro zirconia aqueous solution.

Background

Zirconium oxychloride is widely used in the fields of medicine, chemical industry, lubricating grease, additives, water-proofing agents, refractory materials, ceramics, electronics, optical glass and the like. It can be used as raw material for cosmetics and zirconium salt, and also can be used as raw material for making water-proofing and weight-increasing of textile, for making vapour-light gauze mask, for making colour lake and toner of acid and basic dyes, as additive of lubricating grease and analytical reagent, etc., as rubber additive and paint drying agent, etc.

At present, the production of zirconium oxychloride mainly comprises an alkali dissolution method and a chlorination method.

Alkali fusion method: the zircon is used as a raw material, sodium zirconate and calcium zirconate are obtained by decomposing caustic soda or soda ash or calcium oxide, then the zircon is acidified by hydrochloric acid to remove silicon impurities, and the zircon is concentrated and crystallized to obtain the zircon.

A chlorination method: mixing zircon sand and carbon, directly chlorinating by chlorine gas at high temperature to generate zirconium tetrachloride, dissolving by water to generate zirconium oxychloride, and concentrating and crystallizing to obtain the zirconium oxychloride. The chlorination method has the advantages of short flow, high product quality and the like, but has high investment and more complex process control; the manufacturers mainly adopt an alkali fusion method, and mainly comprise the following procedures: alkali fusion, hydrolysis, water washing, acidification leaching, filtration separation, concentration, crystallization, separation washing and the like.

Whether the alkali fusion method or the chlorination method is adopted, the concentration step is carried out in a graphite evaporation kettle, and the steam heating evaporation is adopted, so that the defect of high energy consumption is caused.

In recent years, the MVR (vapor recompression) technology is introduced domestically, the energy consumption can be greatly reduced by the MVR technology, but the zirconium oxychloride solution and secondary vapor generated by evaporation of the zirconium oxychloride solution contain a large amount of hydrochloric acid, so that the indirect compression technology mainly adopted by the MVR technology at present is adopted, the indirect evaporation technology not only needs a vapor compressor with large temperature rise, but also needs a group of evaporators compared with the conventional direct MVR evaporation, and meanwhile, the heat exchange area of each group of evaporators is large, so that the operation energy consumption is high, and the equipment investment is also large.

SUMMERY OF THE UTILITY MODEL

The utility model aims to overcome the defects in the prior art, and provides a concentration device for a zirconium oxychloride aqueous solution, which is low in cost and can reduce the concentrated energy consumption of the zirconium oxychloride aqueous solution.

In order to solve the technical problem, the utility model discloses a technical scheme does: a concentration device for a zirconium oxychloride aqueous solution comprises a feeding unit, a preheating unit, an evaporation concentration unit, a gas washing unit, a steam compression unit and a discharging unit; the feeding unit, the preheating unit, the evaporation concentration unit, the gas washing unit, the steam compression unit and the discharging unit are connected through pipelines; the gas washing unit comprises a water washing tower, a water washing circulating pump, an alkali washing tower and an alkali washing circulating pump; the water washing tower is respectively connected with the evaporation concentration unit, the water washing circulating pump, the alkaline washing tower and the water washing circulating pump through pipelines, and the alkaline washing tower is respectively connected with the steam compression unit and the alkaline washing circulating pump through pipelines; the water washing tower is provided with a first liquid phase supplementing pipeline, the water washing circulating pump is provided with a second liquid phase discharging pipeline, the alkaline washing tower is provided with a first liquid phase supplementing pipeline, and the alkaline washing circulating pump is provided with a second liquid phase discharging pipeline. Preferably, the zirconium content of the feeding unit of the zirconium oxychloride aqueous solution is 6 to 10 percent, and the zirconium content of the discharging unit of the zirconium oxychloride aqueous solution is about 15 percent.

The gas washing unit can achieve the purpose of removing acid gas and salt solution foam carried in secondary steam from the evaporation concentration unit, wherein the water washing tower absorbs hydrogen chloride in the secondary steam by relying on the principle of gas-liquid two-phase balance, and the alkali washing tower performs neutralization reaction with the residual hydrogen chloride by relying on the principle of acid-base neutralization to remove free acid in the secondary steam.

The utility model is further provided with that the feeding unit comprises a raw material tank and a feeding pump; the head tank is connected with a feed pump pipeline, and the feed pump is connected with a preheating unit pipeline. The feeding unit plays the role of a raw material caching and inputting system, and the feeding pump is used for pumping the aqueous solution in the raw material tank to the preheating unit.

The utility model discloses further set up as, preheat the unit and include secondary steam condensate water pre-heater and/or give birth to the steam pre-heater.

The utility model is further provided with that the evaporation concentration unit comprises a falling film evaporator, a falling film separator and a falling film circulating pump; the falling film evaporator is respectively connected with the preheating unit, the falling film separator, the falling film circulating pump, the steam compression unit and the discharging unit through pipelines, and the falling film separator is connected with the falling film circulating pump and the washing tower through pipelines. The evaporation concentration unit plays a role in separating gas and liquid of part of water in the gasification raw material, the falling film evaporator can play a role in exchanging heat with steam to gasify the material liquid, the falling film separator can play a role in separating secondary steam gasified in the falling film evaporator from the material, and the falling film circulating pump can play a role in enhancing material fluidity and improving the total heat transfer coefficient of the heat exchanger.

The utility model discloses further set up to, the vapor compression unit includes compressor unit and hydrops pump, and compressor unit and evaporative concentration unit, caustic wash tower and hydrops pump pipe connection, hydrops pump and ejection of compact unit pipe connection. The steam compression unit can improve the enthalpy value of the steam, and the subsequent recovery and utilization of the heat enthalpy of the steam are facilitated.

The utility model is further provided with a discharging unit which comprises a distilled water tank, a distilled water pump and a discharging pump; the distilled water tank is connected with the evaporation concentration unit and the steam compression unit through pipelines, and the discharge pump is connected with the evaporation concentration unit through a pipeline. The discharging unit can achieve the purpose of conveying finished materials in the system out of the boundary area of the device.

The utility model is further provided with a vacuum unit which comprises a vacuum pump and a non-condensable gas cooler; the vacuum pump is connected with the pipeline of the non-condensable gas cooler, the non-condensable gas cooler is connected with the pipeline of the evaporation concentration unit, and the vacuum unit can achieve the purpose of adjusting the vacuum degree and the evaporation temperature of the system.

By adopting the technical scheme, compared with a single-effect evaporation scheme, the introduction of MVR can greatly reduce the consumption of raw steam and reduce the operation cost; and acid gas and salt liquid foam which are harmful to the compressor in secondary steam are removed by adopting secondary washing of water and alkali, the steam after washing can be directly compressed, the requirement on the temperature rise of the compressor is greatly reduced, the operation energy consumption is reduced, and the heat exchange area can be reduced.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.

FIG. 1 is a schematic structural diagram of an apparatus for concentrating an aqueous solution of zirconium oxychloride as disclosed in the present embodiment;

FIG. 2 is a schematic flow chart of a method for concentrating an aqueous solution of zirconium oxychloride disclosed in this example.

Reference numerals: 1. a raw material tank; 2. a feed pump; 3. a secondary steam condensate preheater; 4. a distilled water pump; 5. a raw steam preheater; 6. a distilled water tank; 7. a falling film circulating pump; 8. a falling film evaporator; 9. a falling film separator; 10. a liquid accumulation pump; 11. a discharge pump; 12. washing the circulating pump with water; 13. washing the tower with water; 14. an alkaline washing circulating pump; 15. an alkaline washing tower; 16. a compressor unit; 17. a non-condensable gas cooler; 18. a vacuum pump.

Detailed Description

The following describes the present invention with reference to the accompanying drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features related to the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "thickness", "up and down, front and back, left and right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise" indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a defined feature of "first", "second" may explicitly or implicitly include one or more features. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise. It should be noted that unless expressly specified or limited otherwise, the terms "mounted," "connected," and "coupled" are to be construed broadly and include, for example, fixed and removable connections as well as integral connections; may be mechanically connected, may be electrically connected or may be in communication with each other; either directly connected or indirectly connected through intervening media profiles, either internally or in any combination thereof. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

In order to explain the technical means of the present invention, the following description will be given by way of specific examples.

As shown in fig. 1, in an embodiment of the present invention, there is provided a concentration device for zirconium oxychloride aqueous solution, comprising a feeding unit, a preheating unit, an evaporation concentration unit, a scrubbing unit, a vapor compression unit and a discharging unit.

The feeding unit is connected with the preheating unit through a pipeline and is used for feeding the zirconium oxychloride aqueous solution. Specifically, the feed unit includes head tank 1 and charge pump 2, and charge pump 2 sets up in one side of head tank 1 and with head tank 1, preheat unit tube coupling, during the use, head tank 1 storage zirconium oxychloride aqueous solution, and charge pump 2 carries the zirconium oxychloride aqueous solution in the head tank 1 to preheating unit.

The preheating unit is connected with the feeding unit and the evaporation concentration unit through pipelines and is used for preheating the zirconium oxychloride aqueous solution. Specifically, the preheating unit includes a secondary steam condensate preheater 3 and/or a raw steam preheater 5. The preheating unit can adopt a secondary steam condensate water preheater 3 or a raw steam preheater 5 separately. The secondary steam condensate preheater 3 and the raw steam preheater 5 may be used simultaneously. In one example, the aqueous solution of zirconium oxychloride fed from the feed unit is preheated by passing through the secondary steam condensate preheater 3 and the raw steam preheater 5 in sequence and then enters the evaporative concentration unit. In one example, the secondary steam condensate preheater 3 and the raw steam preheater 5 preheat the aqueous zirconium oxychloride solution to a boiling temperature at the operating pressure.

The evaporation concentration unit is connected with the gas washing unit, the discharging unit and the steam compression unit through pipelines and is used for carrying out heat exchange evaporation on the zirconium oxychloride aqueous solution and concentrating the solution. Specifically, the evaporation concentration unit comprises a falling film evaporator 8, a falling film separator 9 and a falling film circulating pump 7; the falling film evaporator 8 is respectively connected with the preheating unit, the falling film separator 9, the falling film circulating pump 7, the steam compression unit and the discharging unit through pipelines, and the falling film separator 9 is connected with the falling film circulating pump 7 and the water washing tower 13 through pipelines. The falling film evaporator 8 receives the zirconium oxychloride aqueous solution preheated by the preheating unit, after the zirconium oxychloride aqueous solution enters the cold side of the falling film evaporator 8, the falling film circulating pump 7 pushes the zirconium oxychloride aqueous solution to circulate in the falling film evaporator 8 and continuously exchange heat with steam at the hot side of the falling film evaporator for evaporation, and when the zirconium concentration of the feed liquid of the lower device body of the falling film evaporator 8 reaches more than 15%, the feed liquid is pumped out of a boundary area by the discharging unit. The gasified zirconium oxychloride aqueous solution can escape to the falling film separator 9 and enter the water washing tower 13 through the falling film separator 9.

The gas washing unit is connected with the steam compression unit through a pipeline and is used for washing the gasified zirconium oxychloride aqueous solution to remove acid gas and salt liquid foam which are harmful to the compressor. Specifically, the gas washing unit comprises a water washing tower 13, a water washing circulating pump 12, an alkaline washing tower 15 and an alkaline washing circulating pump 14; the water scrubber 13 is respectively connected with the evaporation concentration unit, the water scrubbing circulating pump 12, the alkaline washing tower 15 and the water scrubbing circulating pump 12 through pipelines, and the alkaline washing tower 15 is respectively connected with the steam compression unit and the alkaline washing circulating pump 14 through pipelines; the washing tower 13 is provided with a first liquid phase supplementing pipeline for communicating with an external deionized water or soft water source pipeline, the washing circulating pump 12 is provided with a second liquid phase discharging pipeline for communicating with an external hydrochloric acid liquid receiving pipeline, the alkaline washing tower 15 is provided with a first liquid phase supplementing pipeline for communicating with an external NaOH aqueous solution medicament water source pipeline, and the alkaline washing circulating pump 14 is provided with a second liquid phase discharging pipeline for communicating with an external sodium chloride solution liquid receiving pipeline. The acid washing tower absorbs hydrogen chloride in the secondary steam by means of a gas-liquid two-phase balance principle, and the alkali washing tower reacts with the residual hydrogen chloride by means of an acid-base neutralization principle to raise the pH value in the secondary steam.

The steam compression unit is used for compressing secondary steam after the cleaning of the gas washing unit and returning the secondary steam to the evaporation concentration unit. Specifically, the vapor compression unit comprises a compressor unit 16 and a liquid accumulation pump 10, the compressor unit 16 is connected with the evaporation concentration unit, the alkaline tower 15 and the liquid accumulation pump 10 through pipelines, and the liquid accumulation pump 10 is connected with the discharge unit through a pipeline. The secondary steam that the scrubbing unit escaped passes through the process pipeline and gets into compressor unit 16, heats up after compressing and steps up, carries to the evaporation concentration unit afterwards, and hydrops pump 10 is arranged in taking out the hydrops that compressor unit 16 produced in the course of the work, carries to in the distilled water jar 6.

The discharging unit is connected with the evaporation and concentration unit and the steam compression unit through pipelines. Specifically, the discharging unit comprises a distilled water tank 6, a distilled water pump 4 and a discharging pump 11; the distilled water tank 6 is connected with a steam compression unit pipeline of the evaporation concentration unit, and the discharge pump 11 is connected with the evaporation concentration unit pipeline.

In this embodiment, the apparatus for concentrating an aqueous solution of zirconium oxychloride further comprises a vacuum unit comprising a vacuum pump 18 and a non-condensable gas cooler 17; the vacuum pump 18 is connected with the noncondensable gas cooler 17 through a pipeline, and the noncondensable gas cooler 17 is connected with the evaporation and concentration unit through a pipeline.

The utility model discloses a concentration device of dichloro zirconia aqueous solution, preheat the dichloro zirconia aqueous solution that the unit provided the feeding unit through preheating, the evaporative concentration unit carries out evaporative concentration to the aqueous solution after preheating the unit, the secondary steam that the scrubbing unit produced in to the evaporative concentration unit carries out the washing and removes the foam, the secondary steam after the steam compression unit washed gas in to the scrubbing unit compresses, discharge unit is used for discharging the dichloro zirconia aqueous solution after the concentration, and then provides a concentration device of dichloro zirconia aqueous solution, the convenience is concentrated discharge zirconium concentration's dichloro zirconia aqueous solution about 12%.

More specifically, one side of charge pump 2 is provided with head tank 1, the opposite side of charge pump 2 is provided with flash steam condensate water preheater 3, live steam preheater 5 follows behind flash steam condensate water preheater 3, and be connected with falling film evaporator 8, flash steam condensate water preheater 3 links to each other through cold side import and export with live steam preheater 5 each other, 3 hot side imports of flash steam condensate water preheater link to each other with distilled water pump 4 exports, 5 hot side imports of live steam preheater link to each other with public engineering live steam supply pipe, 5 hot side exports of live steam preheater links to each other with distilled water tank 6.

The upper end of the falling film evaporator 8 is connected with an outlet of the falling film circulating pump 7, the lower device body of the falling film evaporator 8 is connected with a falling film separator 9, the lower end of the falling film separator 9 is connected with an inlet of the falling film circulating pump 7 to form a loop, the falling film separator 9 is arranged behind the falling film evaporator 8, and the upper part of the falling film evaporator 8 is connected with a gas phase inlet of a water washing tower 13.

The washing circulating pump 12 sets up in washing tower 13 rear, the import and the export of washing circulating pump 12 link to each other with washing tower 13 liquid phase export and import respectively and form the return circuit, alkaline washing circulating pump 14 sets up in alkaline washing tower 15 rear, alkaline washing circulating pump 14's import and export link to each other with alkaline washing tower 15 liquid phase export and import respectively and form the return circuit, alkaline washing tower 15 sets up in washing tower 13 rear, the gaseous phase import of alkaline washing tower 15 top links to each other with the gaseous phase export at washing tower 13 middle part, the gaseous phase export at alkaline washing tower 15 middle part links to each other with compressor unit 16 import.

The liquid accumulation pump 10 is positioned below the compressor unit 16, an inlet of the liquid accumulation pump 10 is connected with a volute of the compressor unit 16 through a pipeline, and an outlet of the compressor unit 16 is connected with a hot-side inlet of the falling film evaporator 8.

The distilled water tank 6 is respectively connected with the inlet of the distilled water pump 4 and the outlet of the effusion pump 10.

In this embodiment, the present invention is suitable for treating zirconium oxychloride aqueous solution with a temperature of about 38 ℃, a zirconium mass fraction of 7-8%, an evaporation capacity of 16000kg/h and a design pressure of 0.32bar. The compressor train 16 of the vapor compression unit may raise the vapor temperature by 16 deg.c.

In this embodiment, the feed pump 2, the distilled water pump 4 and all are variable frequency pumps, and the operation flow rate thereof can be adjusted by variable frequency.

In the present embodiment, the secondary steam generated by the falling film evaporator 8 is mixed steam of hydrogen chloride and water, and the hydrogen chloride content is about 9.5%.

In this example, the gas phase discharge from the water scrubber 13 was 15650kg/h of mixed steam of hydrogen chloride and water with a hydrogen chloride content of about 0.51%, the liquid phase feed to the water scrubber 13 was 12400kg/h of process soft water, and the discharge was 12750kg/h of an aqueous solution of hydrogen chloride and water with a hydrogen chloride content of about 11.3%.

In this example, the gas phase discharge from the caustic tower 15 was 15670kg/h of secondary steam, the hydrogen chloride content was about trace, the liquid phase feed from the caustic tower 15 was 550kg/h 10% NaOH solution, and the discharge was 530kg/h 15.2% NaCl solution.

As shown in fig. 1 and fig. 2, the process of the present invention is as follows: the raw material of the raw material tank 1 enters a secondary steam condensate water preheater 3 and a raw steam preheater 5 through a feed pump 2 for preheating, the temperature of the raw material after being preheated by the raw steam preheater 5 is about 74 ℃, the raw material enters a falling film evaporator 8, a solution is circulated in the falling film evaporator 8 under the circulation pushing of a falling film circulating pump 7 and continuously exchanges heat with a hot side for evaporation, the evaporation temperature of the falling film evaporator 8 is 70 ℃, the temperature of a feed liquid is about 77.5 ℃, the pressure is 32kPa, the generated secondary steam is escaped to a falling film separator 9 through a connecting pipeline, then sequentially passes through a water washing tower 13 and an alkali washing tower 15, and then enters a compressor unit 16, the temperature and the pressure of the secondary steam after being heated and boosted is about 86 ℃, the pressure is 60kPa, the secondary steam returns to the hot side of the falling film evaporator 8 again as a heating heat source, and is liquefied into secondary steam condensate water after heat utilization and flows into a distillation water tank 6; secondary steam condensate water in the distilled water tank 6 is pumped out by the distilled water pump 4 and is pumped into a secondary condensate water preheater to exchange heat with the raw materials for preheating; when the zirconium concentration of the feed liquid of the lower device body of the falling-film evaporator 8 reaches more than 12%, the feed liquid is pumped out by the discharge pump 11 and is pumped out of a boundary area; the feed liquid contains a small amount of dissolved air or the device has a small amount of air leakage, non-condensed steam can be formed in the evaporation process, and the vacuum pump 18 for adjusting the vacuum degree of the system is used for pumping and discharging the material out of a system boundary area after being preliminarily cooled by the non-condensed steam cooler 17 with circulating cooling water.

By adopting the technical scheme, the vacuum of different systems can be respectively controlled to a set value by interlocking the pressure of the systems through the vacuum pump 18, the pressure sensor and the regulating valve, so that the automatic control of the operating pressure is realized, and the automatic control of the feeding can be realized by interlocking the liquid level of the falling film evaporator 8 with the frequency converter of the feeding pump 2; the whole automatic control system can realize high automation degree.

In this embodiment, the condensed liquid generated by the compressor unit 16 during the operation process flows into the liquid accumulation pipeline of the compressor and is connected to the inlet of the liquid accumulation pump 10, and the liquid accumulation pump 10 pumps the liquid accumulated in the compressor into the distilled water tank 6 to participate in the subsequent preheating and discharging.

Compared with a single-effect evaporation scheme, the MVR is introduced, so that the consumption of generated steam can be greatly reduced, and the operation cost is reduced; and acid gas and salt liquid foam which are harmful to the compressor in secondary steam are removed by adopting secondary washing of water and alkali, the steam after washing can be directly compressed, the requirement on the temperature rise of the compressor is greatly reduced, the operation energy consumption is reduced, and the heat exchange area can be reduced.

As shown in fig. 2, the utility model also discloses a method for concentrating the zirconium oxychloride aqueous solution, which is applied to the device for concentrating the zirconium oxychloride aqueous solution, and comprises the following steps:

s1: preheating the zirconium oxychloride aqueous solution, and preheating the zirconium oxychloride aqueous solution to the boiling point temperature under the operating pressure through the working of a preheating unit. Specifically, the stock solution in the stock tank 1 is pumped out by the feed pump 2, introduced into the preheater, respectively flows through the secondary steam condensate water preheater 3 and the raw steam preheater 5, respectively exchanges heat with the secondary steam condensate water and the raw steam for preheating, and is introduced into the falling film evaporator 8 after being preheated to the boiling point temperature (74 ℃) under the operating pressure.

S2: and (4) evaporating and concentrating, namely evaporating and concentrating the preheated zirconium oxychloride aqueous solution by using an evaporation and concentration unit to work, and gasifying the zirconium oxychloride aqueous solution to form secondary steam with acid liquid foam and salt liquid foam inside. Specifically, after the material is introduced into the cold side of the falling film evaporator 8, the material is subjected to heat exchange evaporation with steam at the hot side of the falling film evaporator, part of the material is gasified, the purpose of solution concentration is achieved, the remaining unevaporated material liquid is remained in the lower body of the falling film evaporator 8 and is pumped out by the falling film circulating pump 7, and the material liquid is introduced into the top of the falling film evaporator 8 and participates in falling film evaporation circulation together with the preheated raw material; the compressed secondary steam at the hot side of the falling-film evaporator 8 is condensed into secondary steam condensate water after heat exchange with the cold feed liquid, and then flows into the distilled water tank 6.

S3: and secondary steam washing, namely removing and cleaning the secondary steam through a washing unit to remove acid liquid foam and salt liquid foam in the secondary steam. Specifically, the material steam gasified in the falling film evaporator 8 escapes to the falling film separator 9, is discharged from the upper part of the falling film separator 9 and then enters the water scrubber 13, secondary steam is preliminarily washed and absorbed under the flow of circulating liquid pushed by the water scrubber circulating pump 12, is discharged from the middle part of the water scrubber 13 and enters the alkaline tower 15, neutralization is carried out under the flow of circulating liquid pushed by the alkaline washing circulating pump 14, hydrochloric acid contained in the secondary steam is reacted, and then, is discharged from the middle part of the alkaline tower 15.

S4: and (3) vapor recompression, wherein the secondary vapor after removal and cleaning is compressed by the vapor compression unit and is returned to the evaporation concentration unit to provide an evaporation heat source of the evaporation concentration unit, and the vapor compression unit generates effusion in the compression process. Specifically, the secondary steam escaping from the middle part of the alkaline tower 15 enters the compressor unit 16 through a process pipeline, is heated and pressurized after being compressed, and then is conveyed to the hot side of the evaporation concentration unit falling film evaporator 8, and the effusion pump 10 can pump out effusion generated in the working process of the compressor unit 16 and convey the effusion into the distilled water tank 6.

S5: and heat recovery is carried out, accumulated liquid generated by the vapor compression unit is collected through the recovery unit, and the accumulated liquid is conveyed to the preheating unit to provide a preheated heat source.

S6: and discharging, namely discharging the concentrated zirconium oxychloride aqueous solution through a discharging unit, and discharging the zirconium oxychloride aqueous solution from the evaporation concentration unit through the discharging unit when the concentration of the zirconium oxychloride aqueous solution in the evaporation concentration unit reaches 15 ℃.

In the method and the device for concentrating the zirconium oxychloride aqueous solution disclosed by the embodiment, an energy-saving mechanical vapor recompression technology is adopted, and compared with the traditional rectification without adopting the mechanical vapor recompression technology, the process has high thermal efficiency and low power consumption, and can save about 1.1 ton of steam compared with single-effect evaporation of each ton of water; the secondary steam compression is adopted as a circulating heat source, so that the dependence of a boiler can be reduced, the energy consumption is reduced, pollutants are reduced, the environmental pollution is reduced, and the energy-saving and environment-friendly effects are achieved; compared with an indirect evaporation concentration process, the process has the advantages that the equipment investment cost and the operation energy consumption are lower, and the operation is more stable compared with a compressor with lower temperature rise; the device has the advantages of simple process flow, easy realization, high automation degree and low operation cost, meets the requirement of sustainable development, and can be widely applied to the actual industrial production process.

The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in the embodiments without departing from the principles and spirit of the invention, and these embodiments are still within the scope of the invention.

Claims (7)

1. The device for concentrating the zirconium oxychloride aqueous solution is characterized by comprising a feeding unit, a preheating unit, an evaporation concentration unit, a gas washing unit, a steam compression unit and a discharging unit;

the feeding unit, the preheating unit, the evaporation concentration unit, the gas washing unit, the steam compression unit and the discharging unit are connected through pipelines;

the gas washing unit comprises a water washing tower, a water washing circulating pump, an alkaline washing tower and an alkaline washing circulating pump; the water washing tower is respectively connected with the evaporation concentration unit, the water washing circulating pump, the alkaline washing tower and the water washing circulating pump through pipelines, and the alkaline washing tower is respectively connected with the steam compression unit and the alkaline washing circulating pump through pipelines;

the water washing tower is provided with a first liquid phase supplementing pipeline, the water washing circulating pump is provided with a second liquid phase discharging pipeline, the alkaline washing tower is provided with a first liquid phase supplementing pipeline, and the alkaline washing circulating pump is provided with a second liquid phase discharging pipeline.

2. The apparatus for concentrating an aqueous solution of zirconyl chloride of claim 1 wherein said feed unit comprises a feed tank and a feed pump;

the raw material tank is connected with the feed pump through a pipeline, and the feed pump is connected with the preheating unit through a pipeline.

3. The apparatus for the concentration of an aqueous solution of zirconium oxychloride according to claim 1, wherein the preheating unit comprises a secondary steam condensate preheater and/or a raw steam preheater.

4. The apparatus for concentrating an aqueous solution of zirconium oxychloride according to claim 1, wherein the evaporation concentration unit comprises a falling film evaporator, a falling film separator and a falling film circulation pump;

the falling film evaporator is respectively connected with the preheating unit, the falling film separator, the falling film circulating pump, the steam compression unit and the discharging unit through pipelines, and the falling film separator is connected with the falling film circulating pump and the washing tower through pipelines.

5. The apparatus for concentrating an aqueous solution of zirconium oxychloride as claimed in claim 1, wherein the vapor compression unit comprises a compressor unit and a liquid accumulation pump, the compressor unit is connected with the evaporation concentration unit, the caustic tower and the liquid accumulation pump through pipelines, and the liquid accumulation pump is connected with the discharge unit through a pipeline.

6. The apparatus for concentrating an aqueous solution of zirconium oxychloride according to claim 1, wherein the discharge unit comprises a distilled water tank, a distilled water pump and a discharge pump;

the distilled water tank is connected with the evaporation concentration unit and the vapor compression unit through pipelines, and the discharge pump is connected with the evaporation concentration unit through a pipeline.

7. The apparatus for concentrating an aqueous solution of zirconium oxychloride according to claim 1 further comprising a vacuum unit comprising a vacuum pump and a non-condensable gas cooler;

the vacuum pump is connected with the pipeline of the non-condensable gas cooler, and the non-condensable gas cooler is connected with the pipeline of the evaporation concentration unit.

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