Multi-stage reaction device as well as multi-stage acid preparation equipment and multi-stage acid dissolution equipment thereof

Through the design of multi-stage reaction devices and acid dispensing equipment, the low efficiency and impurity generation problems of the acid dissolution process in the rare earth magnesium salt enrichment process are solved, and more efficient material preparation and temperature control are achieved, impurity generation is reduced, and impurity generation is improved. Production efficiency and product quality.

CN222196903UActive Publication Date: 2024-12-20GANZHOU RARE EARTH LONGNAN SMELTING & SEPARATION CO LTD
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Patent Information

Application Number
CN202420711445.X
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-04-08
Publication Date
2024-12-20
Estimated Expiration
2034-04-08

AI Technical Summary

Technical Problem

In the rare earth magnesium salt enrichment process, the traditional acid-soluble process has problems with excessive heat generation, long configuration time and difficult to filter gel ‘impurities’, which seriously affects production efficiency and product quality.

Method used

A multi-stage reaction device is designed, including multiple reaction intervals and connected reaction tanks, equipped with temperature sensors and cooling mechanisms, and through multi-stage acid and acid dissolving equipment, the step-by-step replenishment and regulation of materials is achieved, and the temperature is controlled. Acidity reduces impurity generation.

Benefits of technology

It effectively reduces the preparation time of material, improves process efficiency, and reduces the generation of impurities through temperature control, improving production efficiency and product quality.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a multistage reaction device and multistage acid preparation equipment and multistage acid dissolution equipment thereof, the multistage reaction device comprises a plurality of reaction sections which are sequentially arranged along the material transfer direction, a reaction tank is arranged in each reaction section, the reaction tanks of two adjacent reaction sections are communicated, and the reaction tanks are communicated with the reaction sections. The feeding end of the first-stage reaction tank is communicated with feeding pipelines for feeding two materials in pairs, the other stages of reaction tanks are communicated with supplementing pipes, and the discharging end of the last-stage reaction tank is communicated with a storage tank; temperature sensors for detecting the temperature of materials in the storage tank and the reaction tanks are mounted on the storage tank and the reaction tanks, and cooling mechanisms for cooling the materials in the reaction tanks during reaction are matched with the reaction tanks, so that the material preparation time can be shortened, the process efficiency can be improved, the temperature can be effectively controlled, and impurities can be reduced.
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Description

Technical Field

[0001] The utility model relates to the technical field of multi-stage reaction devices, in particular to a multi-stage reaction device and multi-stage acid preparation equipment and multi-stage acid dissolution equipment thereof. Background Art

[0002] The mining of ionic rare earth ores using the ammonium sulfate leaching-ammonium carbonate precipitation process faces the problem of excessive ammonia nitrogen in the mining area water. For this reason, the magnesium sulfate leaching-magnesium oxide enrichment precipitation mining process was developed. This process uses magnesium sulfate leaching, and the leaching mother liquor is enriched and precipitated with magnesium oxide to produce a mixed rare earth primary product - rare earth magnesium salt enrichment. The rare earth magnesium salt enrichment is then purified and processed in the industrial park, and after pulping, acid dissolution, extraction transformation and slag washing, rare earth products suitable for separation and extraction are produced.

[0003] In the acid dissolution section of the purification process, 98% of industrial concentrated sulfuric acid needs to be configured into dilute sulfuric acid with a mass fraction of 49% and 30%. The traditional configuration process has problems such as excessive heat generation, long configuration time, and the generation of difficult-to-filter colloidal "impurities", which seriously restricts production efficiency and introduces harmful factors to the production process. Utility Model Content

[0004] The purpose of the utility model is to provide a multi-stage reaction device and multi-stage acid preparation equipment and multi-stage acid dissolution equipment to solve the problems existing in the above-mentioned prior art, which can reduce the time of material preparation to increase process efficiency, and effective temperature control can reduce the generation of impurities.

[0005] To achieve the above-mentioned purpose, the utility model provides the following scheme: The utility model provides a multi-stage reaction device, comprising a plurality of reaction zones arranged in sequence along the material transfer direction, each of the reaction zones is provided with a reaction tank, the reaction tanks of two adjacent reaction zones are connected, the feed ends of the first-stage reaction tanks are connected in pairs with feed pipes for respectively feeding two materials, the reaction tanks of the remaining stages are connected with supplementary pipes, and the discharge end of the last-stage reaction tank is connected with a storage tank;

[0006] The storage tank and each of the reaction tanks are equipped with a temperature sensor for detecting the temperature of the material inside them, and each of the reaction tanks is equipped with a cooling mechanism for cooling the material inside during the reaction.

[0007] Preferably, each of the supplementary pipes is connected to the feed end of the corresponding reaction tank.

[0008] Preferably, the temperature sensor is installed at the discharge end of the reaction tank.

[0009] Preferably, the cooling mechanism comprises a heat exchange tube uniformly surrounding the outer circumference of the inner cavity of the reaction tank, a heat exchange medium is passed through the heat exchange tube, and the heat exchange tube is connected to a heat exchange medium supply mechanism located outside the reaction tank.

[0010] Preferably, the heat exchange medium supply mechanism is an air cooling mechanism or a water cooling mechanism, the air cooling mechanism introduces cooling air into the heat exchange tube, and the water cooling mechanism introduces cooling water into the heat exchange tube.

[0011] Preferably, the storage tanks are connected in pairs with compensation pipes for respectively replenishing the two materials.

[0012] Preferably, the storage tank is equipped with an air pipeline for introducing normal temperature air into the interior thereof, and the outlet end of the air pipeline extends into the interior of the storage tank and is close to the bottom wall thereof.

[0013] Preferably, at least the first-stage reaction tank and the storage tank are provided with a pH sensor for detecting the pH value therein.

[0014] A multi-stage acid distribution device is also provided, wherein each of the supplementary pipes, one of the feed pipes and one of the compensation pipes are connected to a concentrated sulfuric acid supply mechanism, and another of the feed pipes and another of the compensation pipes are connected to a water supply mechanism.

[0015] A multi-stage acid dissolution device is also provided, wherein each of the supplementary pipes, one of the feed pipes and one of the compensation pipes are connected to a dilute sulfuric acid supply mechanism, and another of the feed pipes and another of the compensation pipes are connected to an enrichment or neutralized slag liquid supply mechanism.

[0016] Compared with the prior art, the utility model has achieved the following technical effects:

[0017] It can reduce the time of material preparation to increase process efficiency, and effective temperature control can reduce the generation of impurities. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0019] Figure 1 This is a schematic diagram of the overall structure of the multi-stage reaction device of the utility model;

[0020] Among them, 1-feed pipe, 2-reaction tank, 3-reaction zone, 4-PH sensor, 5-temperature sensor, 6-supplementary pipe, 7-heat exchange pipe, 8-heat exchange medium supply mechanism, 9-storage tank, 10-compensation pipe, 11-air pipeline. DETAILED DESCRIPTION

[0021] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0022] The purpose of the utility model is to provide a multi-stage reaction device and multi-stage acid preparation equipment and multi-stage acid dissolution equipment to solve the problems existing in the above-mentioned prior art, which can reduce the time of material preparation to increase process efficiency, and effective temperature control can reduce the generation of impurities.

[0023] In order to make the above-mentioned purposes, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0024] like Figure 1 As shown, this embodiment provides a multi-stage reaction device, including a plurality of reaction zones 3 arranged in sequence along the material transfer direction, each reaction zone 3 is provided with a reaction tank 2, the reaction tanks 2 of two adjacent reaction zones 3 are connected to each other so that the material can be transferred along the reaction tanks 2 of each stage of the reaction zones 3, the feeding end of the first stage reaction tank 2 is connected in pairs with a feeding pipe 1 for feeding two materials respectively, so that the two materials can be simultaneously introduced into the reaction tank 2 for reaction, the other stages of the reaction tank 2 are connected with a replenishing pipe 6 so that the corresponding amount of material can be replenished step by step, and the discharge end of the last stage reaction tank 2 is connected with a storage tank 9 to store the material after the reaction is completed;

[0025] Among them, the storage tank 9 and each reaction tank 2 are equipped with a temperature sensor 5 for detecting the temperature of the internal materials. The temperature of the materials in each reaction tank 2 and the storage tank 9 is tested by the temperature sensor 5, and each reaction tank 2 is equipped with a cooling mechanism for cooling the internal materials during the reaction. Then, according to the temperature value measured by the corresponding temperature sensor 5, the reaction tank 2 is cooled by the cooling mechanism until the material in the reaction tank 2 reaches the required temperature.

[0026] Preferably, each replenishing pipe 6 is connected to the feed end of the corresponding reaction tank 2, so that after the material after reaction in the first-stage reaction tank 2 is passed into the next-stage reaction tank 2, the replenished material can be directly introduced into the feed end thereof, thereby achieving a full reaction.

[0027] Moreover, the temperature sensor 5 is installed at the discharge end of the reaction tank 2 so as to intuitively measure the temperature of the material after full reaction in the reaction tank 2, thereby ensuring the accuracy of the measured data results.

[0028] Further, the cooling mechanism includes a heat exchange tube 7 uniformly surrounding the outer peripheral side of the inner cavity of the reaction tank 2, a heat exchange medium is passed into the heat exchange tube 7, and the heat exchange tube 7 is connected to a heat exchange medium supply mechanism 8 located outside the reaction tank 2. Among them, the heat exchange medium supply mechanism 8 is an air cooling mechanism or a water cooling mechanism, the air cooling mechanism passes cooling air into the heat exchange tube 7, and the water cooling mechanism passes cooling water into the heat exchange tube 7. The corresponding cooling medium can be passed into the heat exchange tube 7 through the air cooling mechanism or the water cooling mechanism, thereby cooling the reaction tank 2.

[0029] Preferably, the storage tanks 9 are connected in pairs with compensation pipes 10 for respectively replenishing the two materials, and then the corresponding materials are introduced into the storage tanks 9 through the compensation pipes 10 to adjust the concentration of the final desired product.

[0030] Among them, the storage tank 9 is equipped with an air pipe 11 for introducing normal temperature air into the interior thereof. The outlet end of the air pipe 11 extends into the interior of the storage tank 9 and is close to the bottom wall thereof, thereby introducing normal temperature air to cool the product in the storage tank 9 and achieve a stirring effect.

[0031] Furthermore, a pH sensor 4 for detecting the internal pH value is provided at least at the first-stage reaction tank 2 and the storage tank 9, so as to know the pH value of the material in the first-stage reaction tank 2 and then adjust the replenished material accordingly. By detecting the pH value of the material in the storage tank 9, the pH value of the final product can be obtained, and the material can be replenished according to the measured pH value.

[0032] As a preferred embodiment of the present invention, a multi-stage acid preparation device is also provided, wherein each supplementary pipe 6 and a feed pipe 1 and a compensation pipe 10 are connected to a concentrated sulfuric acid supply mechanism, and another feed pipe 1 and another compensation pipe 10 are connected to a water supply mechanism, so as to prepare dilute sulfuric acid using concentrated sulfuric acid.

[0033] According to the required final concentrated sulfuric acid acidity, the required amount of sulfuric acid and the amount of clean water are calculated. According to the ratio of the two, the clean water is first injected into the reactor 2 in the primary reaction interval 3 at the flow rate Q0, and then the concentrated sulfuric acid feed amount Q1 is controlled according to the temperature feedback value of the reactor 2 in the primary reaction interval 3. The size of Q1 is controlled according to the temperature change trend so that the temperature in the reactor 2 does not exceed the set value. PID control can be used here, mainly related to the concentrated sulfuric acid flow rate and the temperature of the reactor 2. In the same way, the Q0+Q1 mixed liquid enters the reactor 2 in the secondary reaction interval 3, and the concentrated sulfuric acid flow rate Q2 is supplemented according to the temperature change, and the reaction is sequentially n levels. During the process, the total flow rate of concentrated sulfuric acid (Q1+Q2+...+Qn) and the amount of clean water Q0 are controlled to be the pre-calculated ratio value. Finally, the acidity is tested in the storage tank 9. If there is an error, concentrated sulfuric acid and clean water can be supplemented through the compensation tube 10 for regulation, and the corresponding dilute sulfuric acid is finally obtained.

[0034] As a preferred embodiment of the present invention, a multi-stage acid dissolution equipment is also provided, in which each supplementary pipe 6 and a feed pipe 1 and a compensation pipe 10 are connected to a dilute sulfuric acid supply mechanism, and another feed pipe 1 and another compensation pipe 10 are connected to an enriched material or a neutralized slag liquid supply mechanism. The idea is similar to that of the multi-stage acid distribution equipment. According to the pH value required for final neutralization, dilute sulfuric acid and enriched material or neutralized slag liquid are respectively introduced through the two feed pipes 1 in a corresponding proportion. Taking the enriched material as an example: first, the enriched material is injected into the reaction tank 2 in the first-stage reaction interval 3 at a flow rate Q0, and then the dilute sulfuric acid feed amount Q1 is controlled according to the temperature feedback value of the reaction tank 2 in the first-stage reaction interval 3. The size of Q1 is controlled according to the temperature change trend so that the temperature in the reaction tank 2 does not exceed the set value. PID control can be used here, which mainly relates to three parameters: dilute sulfuric acid flow rate, pH value, and temperature of the reaction tank 2. Similarly, the Q0+Q1 mixed solution enters the reaction tank 2 in the secondary reaction interval 3, and the dilute sulfuric acid flow Q2 is supplemented according to the temperature change and the pH value, and the reaction is sequentially n levels. During the process, the total flow of dilute sulfuric acid (Q1+Q2+...+Qn) and the enriched material amount Q0 are controlled to be a pre-calculated proportional value. Finally, the acidity is tested in the storage tank 9. If there is an error, the dilute sulfuric acid and the enriched material can be supplemented by the compensation tube 10 for regulation, and the neutralized product is finally obtained. Preferably, a pH sensor 4 is set in each reaction tank 2 and the storage tank 9 to measure the pH value in the corresponding reaction tank 2 and the storage tank 9, and preferably, a pH sensor 4 is set in the first-level reaction tank 2 and the storage tank 9 to save costs.

[0035] Adaptive changes made according to actual needs are all within the protection scope of this utility model.

[0036] It should be noted that it is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or basic features of the present invention. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims are included in the present invention. Any reference numerals in the claims should not be regarded as limiting the claims involved.

[0037] The present invention uses specific examples to illustrate the principle and implementation of the present invention. The above examples are only used to help understand the method and core idea of ​​the present invention. At the same time, for those skilled in the art, according to the idea of ​​the present invention, there will be changes in the specific implementation and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A multi-stage reaction device, It is characterized in that It comprises a plurality of reaction zones arranged in sequence along the material transfer direction, each of the reaction zones is provided with a reaction tank, the reaction tanks of two adjacent reaction zones are connected, the feed ends of the first-stage reaction tanks are connected in pairs with feed pipes for feeding two materials respectively, the reaction tanks of the remaining stages are connected with replenishing pipes, and the discharge end of the last-stage reaction tank is connected with a storage tank; The storage tank and each of the reaction tanks are equipped with a temperature sensor for detecting the temperature of the material inside them, and each of the reaction tanks is equipped with a cooling mechanism for cooling the material inside during the reaction.

2. The multi-stage reaction device according to claim 1, It is characterized in that Each of the supplementary pipes is connected to the feed end of the corresponding reaction tank.

3. The multi-stage reaction device according to claim 1 or 2, It is characterized in that The temperature sensor is installed at the discharge end of the reaction tank.

4. The multi-stage reaction device according to claim 3, It is characterized in that The cooling mechanism comprises a heat exchange tube uniformly surrounding the outer peripheral side of the inner cavity of the reaction tank, a heat exchange medium is introduced into the heat exchange tube, and the heat exchange tube is connected to a heat exchange medium supply mechanism located outside the reaction tank.

5. The multi-stage reaction device according to claim 4, It is characterized in that The heat exchange medium supply mechanism is an air cooling mechanism or a water cooling mechanism. The air cooling mechanism passes cooling air into the heat exchange tube, and the water cooling mechanism passes cooling water into the heat exchange tube.

6. The multi-stage reaction device according to claim 5, It is characterized in that The storage tanks are connected in pairs with compensation pipes for respectively replenishing two kinds of materials.

7. The multi-stage reaction device according to claim 6, It is characterized in that The storage tank is equipped with an air pipeline for introducing normal temperature air into the interior thereof, and the outlet end of the air pipeline extends into the interior of the storage tank and is close to the bottom wall thereof.

8. The multi-stage reaction device according to claim 7, It is characterized in that At least the first-stage reaction tank and the storage tank are provided with a pH sensor for detecting the pH value therein.

9. A multi-stage acid preparation device using the multi-stage reaction device according to any one of claims 1 to 8, It is characterized in that Each of the supplementary pipes, one of the feed pipes and one of the compensation pipes are connected to a concentrated sulfuric acid supply mechanism, and another of the feed pipes and another of the compensation pipes are connected to a water supply mechanism.

10. A multi-stage acid dissolution device using the multi-stage reaction device according to any one of claims 1 to 8, It is characterized in that Each of the supplementary pipes, one of the feed pipes and one of the compensation pipes are connected to a dilute sulfuric acid supply mechanism, and another of the feed pipes and another of the compensation pipes are connected to an enrichment or neutralized slag liquid supply mechanism.