CN115159604A - Evaporative crystallization method of manganese sulfate - Google Patents

Evaporative crystallization method of manganese sulfate Download PDF

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Publication number
CN115159604A
CN115159604A CN202210873577.8A CN202210873577A CN115159604A CN 115159604 A CN115159604 A CN 115159604A CN 202210873577 A CN202210873577 A CN 202210873577A CN 115159604 A CN115159604 A CN 115159604A
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CN
China
Prior art keywords
solution
container
manganese sulfate
reverse osmosis
osmosis membrane
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Pending
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CN202210873577.8A
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Chinese (zh)
Inventor
康凯
汪朝武
任莹
顾尚波
李晓雨
唐三川
罗文宗
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Guizhou Jinrui New Material Co ltd
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Guizhou Jinrui New Material Co ltd
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Priority to CN202210873577.8A priority Critical patent/CN115159604A/en
Publication of CN115159604A publication Critical patent/CN115159604A/en
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • C01G45/10Sulfates
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/441Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis

Abstract

The invention relates to the technical field of manganese sulfate preparation, and discloses an evaporative crystallization method of manganese sulfate, which comprises the following steps: the method comprises the following steps: the manganese sulfate solution after purification treatment is placed in a container with a reverse osmosis membrane in the middle, the solution is completely placed in the container on one side of the reverse osmosis membrane, then the upper part of the container is sealed, and a booster pump is arranged to enable a boosting port of the booster pump to be communicated with the interior of the container on one side of the solution. According to the invention, the container with the reverse osmosis membrane in the middle is arranged, so that the solution can be placed in the container on one side of the reverse osmosis membrane, the container is sealed, then the container on one side of the solution is pressurized and heated, water molecules in the solution permeate to the other side to be removed in a high-heat motion state, meanwhile, the solution can be subjected to preheating treatment, and then the preheated solution with more water removed is subjected to heating evaporation crystallization treatment, so that the solution can be evaporated and crystallized by consuming less energy, the crystallization speed is increased, and energy is saved.

Description

Evaporative crystallization method of manganese sulfate
Technical Field
The invention relates to the technical field of manganese sulfate preparation, in particular to an evaporative crystallization method of manganese sulfate.
Background
Manganese sulfate is a traditional manganese salt product and is widely applied to the fields of chemical fertilizers, feeds, paints, pesticides and the like, a domestic manganese sulfate production process mainly takes pyrolusite as a raw material and comprises two reduction leaching process technologies of carbon fire reduction and wet reduction acid leaching, potassium and sodium are removed through jarosite, iron is removed through oxidative hydrolysis, heavy metals are removed through sulfides, calcium and magnesium are removed through fluorides, a manganese sulfate solution after impurity removal and purification is obtained through standing, precipitation and filtration, and crystals of manganese sulfate are obtained after evaporation and crystallization of the manganese sulfate solution after impurity removal and purification.
In the evaporation crystallization method in the prior art, the purified solution is directly placed in a crystallization vessel, and then the solution is heated at a high temperature, so that the water in the solution is evaporated, and manganese sulfate crystals are formed. Therefore, we propose a method for the evaporative crystallization of manganese sulfate.
Disclosure of Invention
The invention aims to provide an evaporative crystallization method of manganese sulfate, which is characterized in that a container with a reverse osmosis membrane in the middle is arranged, a solution can be placed in the container on one side of the reverse osmosis membrane to seal the container, then the container on one side of the solution is pressurized and heated to enable water molecules in the solution to permeate to the other side to be removed in a high-heat motion state, meanwhile, the solution can be preheated, and then the preheated solution with more water removed is heated, evaporated and crystallized, so that less energy can be consumed to evaporate and crystallize the solution, the crystallization speed is improved, the energy is saved, and the problems in the background art are solved.
In order to achieve the purpose, the invention provides the following technical scheme: the evaporative crystallization method of manganese sulfate comprises the following steps:
the method comprises the following steps: putting the purified manganese sulfate solution into a container with a reverse osmosis membrane in the middle, and putting the solution into the container on one side of the reverse osmosis membrane, then sealing the upper part of the container, arranging a booster pump to enable a boosting port of the booster pump to be communicated with the interior of the container on one side with the solution, and enabling an air suction port of the booster pump to be communicated with the interior of the container on the side without the solution;
step two: starting a booster pump to pressurize the interior of the container at the side with the solution, enabling the interior of the container at the side without the solution to be in a negative pressure state, heating the solution, increasing the thermal motion of water molecules in the solution and preheating the solution, and under the influence of the pressurization and the thermal motion of the solution, more easily enabling the water molecules to enter the container at the other side through a reverse osmosis membrane, and leaving a small part of water molecules and manganese sulfate ions in the solution;
step three: stopping the work of a booster pump, releasing the sealing state of a container, putting the treated solution into a vessel for evaporation crystallization, heating the vessel to evaporate water and finally precipitate manganese sulfate crystals, and crushing the generated crystals to obtain manganese sulfate;
step four: adding purified water into one side of the container which is not filled with the solution, sealing the container again, heating the interior of the container filled with the purified water by utilizing a booster pump in the reverse connection mode, forming negative pressure on the other side of the container, enabling the purified water to reversely flow to reversely flush the reverse osmosis membrane, and enabling ions adsorbed on the reverse osmosis membrane to be flushed into the container filled with the solution;
step five: and (4) removing the seal of the container again, taking out the purified water which is added in the step and does not permeate to the other side, adding the treated manganese sulfate solution into the container which is originally added into one side of the solution, and repeating the steps from the first step to the fifth step to continue the evaporation crystallization of manganese sulfate.
In a preferred embodiment of the present invention, the reverse osmosis membrane in the first step can only pass water molecules, but cannot pass manganese sulfate ions.
In a preferred embodiment of the present invention, a heating device is installed in the container on the side of the manganese sulfate solution in the second step, and the solution is heated by the heating device.
In a preferred embodiment of the present invention, a stirring structure may be further installed in the container on the side where the solution is filled in the second step, so as to further increase the movement speed of water molecules.
In a preferred embodiment of the present invention, the rotation speed of the stirring structure installed inside the container is at least 60r/min.
In a preferred embodiment of the present invention, in the third step, when the solution is heated, evaporated and crystallized, the solution needs to be slowly stirred to ensure the evaporation rate of water.
In a preferred embodiment of the present invention, in the third step, the crystallized manganese sulfate may be crushed by a crusher or a grinder, and before crushing, the crystallized manganese sulfate may be dried.
As a preferred embodiment of the invention, the adding height of the purified water in the fourth step is required to be greater than that of the solution in the first step, so as to ensure the complete flushing of the reverse osmosis membrane.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the container with the reverse osmosis membrane in the middle is arranged, so that the solution can be placed in the container on one side of the reverse osmosis membrane, the container is sealed, then the container on one side of the solution is pressurized and heated, water molecules in the solution permeate to the other side to be removed in a high-heat motion state, meanwhile, the solution can be subjected to preheating treatment, and then the preheated solution with more water removed is subjected to heating evaporation crystallization treatment, so that the solution can be evaporated and crystallized by consuming less energy, the crystallization speed is increased, and energy is saved.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a flow chart of the evaporative crystallization method of manganese sulfate.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Referring to fig. 1, the present invention provides a technical solution: the evaporative crystallization method of manganese sulfate comprises the following steps:
the method comprises the following steps: putting the purified manganese sulfate solution into a container with a reverse osmosis membrane in the middle, and putting the solution into the container on one side of the reverse osmosis membrane, then sealing the upper part of the container, arranging a booster pump to enable a boosting port of the booster pump to be communicated with the interior of the container on one side with the solution, and enabling an air suction port of the booster pump to be communicated with the interior of the container on the side without the solution;
step two: starting a booster pump to pressurize the interior of the container at the side with the solution, enabling the interior of the container at the side without the solution to be in a negative pressure state, heating the solution, increasing the thermal motion of water molecules in the solution and preheating the solution, and under the influence of the pressurization and the thermal motion of the solution, more easily enabling the water molecules to enter the container at the other side through a reverse osmosis membrane, and leaving a small part of water molecules and manganese sulfate ions in the solution;
step three: stopping the work of a booster pump, releasing the sealing state of a container, putting the treated solution into a vessel for evaporating crystals, heating the vessel to evaporate water and finally separate manganese sulfate into crystals, and crushing the generated crystals to obtain manganese sulfate;
step four: adding purified water into one side of the container which is not filled with the solution, sealing the container again, heating the interior of the container filled with the purified water by utilizing a booster pump in the reverse connection mode, forming negative pressure on the other side of the container, enabling the purified water to reversely flow to reversely flush the reverse osmosis membrane, and enabling ions adsorbed on the reverse osmosis membrane to be flushed into the container filled with the solution;
step five: and releasing the sealing of the container again, taking out the purified water which is added in the step and does not permeate to the other side, adding the treated manganese sulfate solution into the container which is originally added into one side of the solution, and repeating the steps from the first step to the fifth step to continue the evaporation crystallization of manganese sulfate.
Furthermore, the reverse osmosis membrane in the first step can only allow water molecules to pass through, and cannot allow manganese sulfate ions to pass through.
Furthermore, a heating device is installed in the container at the side, where the manganese sulfate solution is filled, in the second step, and the solution is heated through the heating device.
Furthermore, a stirring structure can be arranged in the container at the side where the solution is filled in the step two, so that the movement speed of water molecules can be further increased.
Further, the rotating speed of the stirring structure arranged in the container is at least 60r/min.
Furthermore, in the third step, when the solution is heated, evaporated and crystallized, the solution needs to be slowly stirred to ensure the speed of water evaporation.
Furthermore, in the third step, a crusher or a grinder can be used for crushing the crystallized manganese sulfate, and the crystallized manganese sulfate is dried before crushing.
Furthermore, the adding height of the purified water in the fourth step is greater than that of the solution in the first step, so that the comprehensive washing of the reverse osmosis membrane is ensured.
Data parameters of the conventional crystallization method and the crystallization method of the examples are shown in table 1 below:
test items Quality of the product Crystallization rate
Conventional crystallization method Good wine 97.59%
EXAMPLES crystallization method Superior food 99.39%
When the evaporation crystallization method of manganese sulfate is used, the manganese sulfate solution after purification treatment is placed in a container with a reverse osmosis membrane in the middle, the solution is completely positioned in the container on one side of the reverse osmosis membrane, then the upper part of the container is sealed, a booster pump is arranged to enable a boosting port of the booster pump to be communicated with the interior of the container on one side with the solution, and an air suction port of the booster pump is communicated with the interior of the container on the side without the solution; starting a booster pump to pressurize the interior of the container at the side with the solution, enabling the interior of the container at the side without the solution to be in a negative pressure state, heating the solution, increasing the thermal motion of water molecules in the solution and preheating the solution, and under the influence of the pressurization and the thermal motion of the solution, more easily enabling the water molecules to enter the container at the other side through a reverse osmosis membrane, and leaving a small part of water molecules and manganese sulfate ions in the solution; stopping the work of a booster pump, releasing the sealing state of a container, putting the treated solution into a vessel for evaporating crystals, heating the vessel to evaporate water and finally separate manganese sulfate into crystals, and crushing the generated crystals to obtain manganese sulfate; adding purified water into one side of the container which is not filled with the solution, sealing the container again, heating the interior of the container filled with the purified water by utilizing a booster pump in the reverse connection mode, forming negative pressure on the other side of the container, enabling the purified water to reversely flow to reversely flush the reverse osmosis membrane, and enabling ions adsorbed on the reverse osmosis membrane to be flushed into the container filled with the solution; and releasing the sealing of the container again, taking out the purified water which is added in the step and does not permeate to the other side, adding the treated manganese sulfate solution into the container which is originally added into one side of the solution, and repeating the steps from the first step to the fifth step to continue the evaporation crystallization of manganese sulfate.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.

Claims (8)

1. The evaporative crystallization method of manganese sulfate is characterized by comprising the following steps:
the method comprises the following steps: putting the purified manganese sulfate solution into a container with a reverse osmosis membrane in the middle, and putting the solution into the container on one side of the reverse osmosis membrane, then sealing the upper part of the container, arranging a booster pump to enable a boosting port of the booster pump to be communicated with the interior of the container on one side with the solution, and enabling an air suction port of the booster pump to be communicated with the interior of the container on the side without the solution;
step two: starting a booster pump to pressurize the interior of the container at the side with the solution, enabling the interior of the container at the side without the solution to be in a negative pressure state, heating the solution, increasing the thermal motion of water molecules in the solution and preheating the solution, and under the influence of the pressurization and the thermal motion of the solution, more easily enabling the water molecules to enter the container at the other side through a reverse osmosis membrane, and leaving a small part of water molecules and manganese sulfate ions in the solution;
step three: stopping the work of a booster pump, releasing the sealing state of a container, putting the treated solution into a vessel for evaporation crystallization, heating the vessel to evaporate water and finally precipitate manganese sulfate crystals, and crushing the generated crystals to obtain manganese sulfate;
step four: adding purified water into one side of the container which is not filled with the solution, sealing the container again, heating the interior of the container filled with the purified water by utilizing a booster pump in the reverse connection mode, forming negative pressure on the other side of the container, enabling the purified water to reversely flow to reversely flush the reverse osmosis membrane, and enabling ions adsorbed on the reverse osmosis membrane to be flushed into the container filled with the solution;
step five: and releasing the sealing of the container again, taking out the purified water which is added in the step and does not permeate to the other side, adding the treated manganese sulfate solution into the container which is originally added into one side of the solution, and repeating the steps from the first step to the fifth step to continue the evaporation crystallization of manganese sulfate.
2. The evaporative crystallization method of manganese sulfate as claimed in claim 1, wherein: the reverse osmosis membrane in the first step can only allow water molecules to pass through, but cannot allow manganese sulfate ions to pass through.
3. The evaporative crystallization method of manganese sulfate as claimed in claim 1, wherein: and in the second step, a heating device is arranged in the container at the side of the manganese sulfate solution, and the solution is heated by the heating device.
4. The evaporative crystallization method of manganese sulfate as claimed in claim 1, wherein: and a stirring structure can be arranged in the container at the side where the solution is filled in the step two, so that the movement speed of water molecules can be further increased.
5. The evaporative crystallization method of manganese sulfate as claimed in claim 4, wherein: the rotating speed of the stirring structure arranged in the container is at least 60r/min.
6. The evaporative crystallization method of manganese sulfate as claimed in claim 1, wherein: in the third step, when the solution is heated, evaporated and crystallized, the solution needs to be slowly stirred, so that the evaporation speed of water is ensured.
7. The evaporative crystallization method of manganese sulfate as claimed in claim 1, wherein: in the third step, a crusher or a grinder can be used for crushing the crystallized manganese sulfate, and the crystallized manganese sulfate is dried before crushing.
8. The evaporative crystallization method of manganese sulfate as claimed in claim 1, wherein: and in the fourth step, the adding height of the purified water is greater than that of the solution in the first step, so that the reverse osmosis membrane is comprehensively washed.
CN202210873577.8A 2022-07-23 2022-07-23 Evaporative crystallization method of manganese sulfate Pending CN115159604A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA3013043A1 (en) * 2016-01-28 2017-08-03 Nano-Green Biorefineries Inc. Production of crystalline cellulose
CN206828282U (en) * 2017-01-16 2018-01-02 泰州烯王新能源科技有限公司 Graphene production wastewater treatment system
CN108118152A (en) * 2017-12-27 2018-06-05 广东光华科技股份有限公司 A kind of method of fluorine ion in efficient removal manganese sulfate solution
CN109231399A (en) * 2018-08-28 2019-01-18 杭州轩辉环境设备有限公司 A kind of process for extracting sulfate
CN110482613A (en) * 2019-08-23 2019-11-22 安庆市长虹化工有限公司 A kind of technique preparing manganese sulfate using Waste Sulfuric Acid in DYE PRODUCTION

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA3013043A1 (en) * 2016-01-28 2017-08-03 Nano-Green Biorefineries Inc. Production of crystalline cellulose
CN206828282U (en) * 2017-01-16 2018-01-02 泰州烯王新能源科技有限公司 Graphene production wastewater treatment system
CN108118152A (en) * 2017-12-27 2018-06-05 广东光华科技股份有限公司 A kind of method of fluorine ion in efficient removal manganese sulfate solution
CN109231399A (en) * 2018-08-28 2019-01-18 杭州轩辉环境设备有限公司 A kind of process for extracting sulfate
CN110482613A (en) * 2019-08-23 2019-11-22 安庆市长虹化工有限公司 A kind of technique preparing manganese sulfate using Waste Sulfuric Acid in DYE PRODUCTION

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Title
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