CN112429754A - Large-particle magnesium sulfate cooling crystallization method and system - Google Patents
Large-particle magnesium sulfate cooling crystallization method and system Download PDFInfo
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- CN112429754A CN112429754A CN202011274288.3A CN202011274288A CN112429754A CN 112429754 A CN112429754 A CN 112429754A CN 202011274288 A CN202011274288 A CN 202011274288A CN 112429754 A CN112429754 A CN 112429754A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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Abstract
The invention discloses a large-particle magnesium sulfate cooling crystallization method and a system, wherein the method comprises the following steps: step S1, adding water into the neutral magnesium sulfate solution generated by the reaction of the alkylated waste acid solution and magnesium oxide for slight dilution; step S2, adding magnesium sulfate crystal nuclei to uniformly distribute the crystal nuclei in the magnesium sulfate solution; step S3, stirring in a constant-temperature water bath tank until the crystal is completely dissolved, controlling the liquid level height to be 6-10 cm, and adjusting the pH value of the magnesium sulfate solution to 3-6; step S4, placing the mixture into a constant-temperature water bath box, and stirring the mixture at a constant speed by adopting electric stirring equipment; step S5, cooling at a constant speed and gradually stopping stirring when the cooling temperature is reduced to be below 20-25 ℃; and step S6, putting the mixture into a high-speed centrifuge for crystal and mother liquor separation, and finally drying the crystals. The invention can generate magnesium sulfate crystals with regular appearance, large and uniform particle size, realizes the conversion from magnesium sulfate solution generated by waste acid solution to magnesite cooling crystallization, protects the environment and reduces the cost.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a large-particle magnesium sulfate cooling crystallization method and a system.
Background
Magnesium sulfate is an important chemical product and is widely applied to industries such as leather making, explosives, fertilizers, papermaking and the like. In recent 10 years, the magnesium sulfate industry in China has been developed rapidly. The industrial magnesium sulfate is mainly produced by chemical processes of carbon dioxide carbonized magnesium oxide, magnesium hydroxide for absorbing sulfur dioxide, purifying, separating and heating brine and the like. The application of magnesium sulfate is limited by the defects of small (0-1 mm) magnesium sulfate particles, easy agglomeration, poor flowability and the like in general industrial production. The price of the large-particle magnesium sulfate product is 3 times higher than that of the small-particle product, and the key point is that the large-particle magnesium sulfate has better fluidity in industrial application, and a regenerated product with better quality can be obtained. Therefore, it is necessary to study the particle size and morphology control of magnesium sulfate crystals.
Crystallization is an important chemical process, and is one of typical liquid-solid phase separation processes, and supersaturation is the main driving force of separation. The rate of nucleation (the number of nuclei produced per unit volume of solution per unit time), the rate of crystal growth (the amount of increase in a certain linear dimension of the crystal per unit time) and the average residence time of the crystal in the crystallizer influence mainly the rate of crystal growth and the grain size. The supersaturation of the solution can not only influence the crystal nucleus growth rate, but also has a relationship with the crystal growth rate. Therefore, the degree of supersaturation has a large influence on the particle size of the crystalline product and its distribution. Morphology control and homogeneity of crystalline products have become the focus of industrial production and scientific research today. At present, the industrial crystal products of magnesium sulfate in China have the problems of small average particle size, uneven particle size distribution and the like.
Disclosure of Invention
The invention aims to provide a method and a system for cooling and crystallizing large-particle magnesium sulfate, which optimize a magnesium sulfate cooling and crystallizing process so as to obtain magnesium sulfate crystals with larger particle size, uniform particle size distribution and higher purity.
The technical scheme of the invention is as follows:
a cooling crystallization method of large-particle magnesium sulfate comprises the following steps:
step S1, adding water into the neutral magnesium sulfate solution generated by the reaction of the alkylated waste acid solution and magnesium oxide for slight dilution;
step S2, adding magnesium sulfate crystal nuclei into the solution obtained in step S1, so that the crystal nuclei are uniformly distributed in the magnesium sulfate solution;
step S3, stirring the solution obtained in the step S2 in a constant temperature water bath tank until the crystal is completely dissolved, controlling the liquid level height within the range of 6 cm-10 cm, and adjusting the pH value of the magnesium sulfate solution to be within the range of 3-6 by adopting concentrated sulfuric acid;
step S4, placing the magnesium sulfate solution of which the pH value is adjusted in the step S3 into a constant-temperature water bath box, uniformly stirring the solution by adopting electric stirring equipment, and simultaneously controlling the temperature to be 40-55 ℃ to preserve the temperature of the magnesium sulfate solution;
step S5, cooling the magnesium sulfate solution processed in the step S4 at a constant speed within a cooling rate range of 0.1-0.5 ℃/min, and gradually stopping stirring when the cooling temperature is reduced to 20-25 ℃;
and step S6, putting the crystal pulp mixed solution processed in the step S5 into a high-speed centrifuge for crystal and mother liquor separation, and finally drying the crystals.
In one embodiment, the saturation degree of the neutral magnesium sulfate solution in the step S1 is in the range of 1-1.25%.
In one embodiment, in step S2, magnesium sulfate crystal nuclei are added in an amount of 1 to 3g per 1000ml of the solution obtained in step S1.
In one embodiment, in step S3, the temperature of the constant temperature water bath is within a range of 75 ℃ to 79 ℃. In one embodiment, in step S4, the stirring speed of the electric stirring device is 500 to 800 rpm.
In one embodiment, in step S4, the temperature of the magnesium sulfate solution is stabilized to 40 ℃ to 55 ℃ and then kept for 2h to 3 h.
In one embodiment, in step S5, after the stirring is gradually stopped when the cooling temperature is reduced to 20 to 25 ℃, the crystals are further cooled for 16 to 24 hours.
In one embodiment, in step S6, the centrifugal speed of the high-speed centrifuge ranges from 5000r/min to 8000 r/min.
In one embodiment, in step S6, the crystal drying temperature is 45 ℃ to 75 ℃, and the crystal drying time is 20min to 40 min.
A large granular magnesium sulfate cooling crystallization system for implementing the above-mentioned large granular magnesium sulfate cooling crystallization method, the system comprising: crystal nucleus growth system and cooling system, crystal nucleus growth system includes electronic stirring rake, constant temperature water bath, beaker and sealing film, cooling system includes the controllable refrigerator of temperature.
The invention has the following beneficial effects: the large-particle magnesium sulfate cooling crystallization method and the large-particle magnesium sulfate cooling crystallization system provided by the invention can generate magnesium sulfate crystals with regular appearance, large and uniform particle size, increase the product particle size, facilitate product screening, greatly improve the product purity, ensure that the product particle size is uniformly distributed, are more suitable for agricultural and industrial applications, realize the conversion from magnesium sulfate solution generated by waste acid solution to magnesite cooling crystallization, protect the environment and reduce the cost.
Drawings
FIG. 1 is a flow chart of a cooling crystallization method of large-particle magnesium sulfate provided by the invention.
FIG. 2 is a schematic diagram of a large-particle magnesium sulfate cooling crystallization system provided by the invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
Spatially relative terms, such as "above … …," "above … …," "above … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial relationship to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary term "above … …" can include both an orientation of "above … …" and "below … …". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The terms "first," "second," and the like in the description and in the claims of the present application and in the above-described drawings are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein.
Detailed Description
The method for cooling and crystallizing large particle magnesium sulfate according to the present invention will be described in detail with reference to several specific examples:
example 1: controlling the saturation degree of a magnesium sulfate solution generated by waste acid and magnesium oxide (MgO) to be 1%, controlling the addition amount of crystal nuclei to be 2g/1000ml, controlling the pH value to be 3, and controlling the stirring speed to be 500 rmp/min; keeping the temperature of the magnesium sulfate solution at constant temperature for 2h by controlling the water temperature in the water bath tank to be adjusted to 40 ℃, controlling the liquid level height to be within 6cm, finally cooling the magnesium sulfate solution at a constant speed at a cooling rate of 0.1 ℃/min, and gradually stopping stirring when the cooling temperature is reduced to be below 20 ℃; the cooling crystallization time is 16 h. After crystal pulp is separated by centrifugation at 5000r/min, the drying temperature of the crystal is 45 ℃ and the drying time is 20 min. Magnesium sulfate crystal particles with uniform size and regular shape and the diameter range of 5-7 mm are prepared.
Example 2: controlling the saturation degree of a magnesium sulfate solution generated by waste acid and magnesium oxide (MgO) to be 1.25%, controlling the addition amount of crystal nuclei to be 1g/1000ml, controlling the pH value to be 6 and controlling the stirring speed to be 600 rmp/min; and the magnesium sulfate solution is kept at a constant temperature for 3 hours by controlling the water temperature in the water bath tank to be adjusted to 50 ℃, meanwhile, the liquid level height is controlled within 10cm, and finally, the magnesium sulfate solution is cooled at a constant speed at a cooling rate of 0.5 ℃/min. Gradually stopping stirring when the cooling temperature is reduced to below 23 ℃; the cooling crystallization time is 20 h. After crystal pulp is separated by centrifugation of 6500r/min, the drying temperature of the crystal is 60 ℃, and the drying time is 20 min. Magnesium sulfate crystal particles with uniform size and regular shape and the diameter range of 5-7 mm are prepared.
Example 3: controlling the saturation degree of a magnesium sulfate solution generated by waste acid and magnesium oxide (MgO) to be 1.15%, controlling the crystal nucleus addition amount to be 3g/1000ml, controlling the pH value to be 5 and controlling the stirring speed to be 800 rmp/min; and the magnesium sulfate solution is kept at the constant temperature for 2.5h by controlling the water temperature in the water bath box to be adjusted to 55 ℃, meanwhile, the liquid level height is controlled within the range of 8cm, and finally, the magnesium sulfate solution is cooled at a constant speed at the cooling rate of 0.3 ℃/min. Gradually stopping stirring when the cooling temperature is reduced to below 25 ℃; the cooling crystallization time is 24 h. After crystal pulp is separated by centrifugation at 8000r/min, the drying temperature of the crystal is 75 ℃, and the drying time is 40 min. Magnesium sulfate crystal particles with uniform size and regular shape and the diameter range of 5-7 mm are prepared.
Comparative example 1: referring to example 1, the process was identical to that of example 1 except that the step of allowing the magnesium sulfate mother liquor to stand in the incubator for 2 hours was omitted. The specific process is described in detail as follows: controlling the saturation degree of a magnesium sulfate solution generated by waste acid and magnesium oxide (MgO) to be 1%, controlling the addition amount of crystal nuclei to be 2g/1000ml, controlling the pH value to be 3, and controlling the stirring speed to be 500 rmp/min; controlling the liquid level height within 6cm, finally cooling the magnesium sulfate solution at a constant speed at a cooling rate of 0.1 ℃/min, and gradually stopping stirring when the cooling temperature is reduced to below 20 ℃; the cooling crystallization time is 16 h. After crystal pulp is separated by centrifugation at 5000r/min, the drying temperature of the crystal is 45 ℃ and the drying time is 20 min. Magnesium sulfate crystal particles with uniform size and regular shape with the diameter range of 2-3 mm are prepared.
Comparative example 2: referring to example 1, the process was identical to that of example 1 except that the step of adding crystal nuclei of magnesium sulfate mother liquor in an amount of 2g/1000ml was omitted. The specific process is described in detail as follows: controlling the saturation degree of magnesium sulfate solution generated by waste acid and magnesium oxide (MgO) to be 1%, the pH value to be 3, and the stirring speed to be 500 rmp/min; keeping the temperature of the magnesium sulfate solution at constant temperature for 2h by controlling the water temperature in the water bath tank to be adjusted to 40 ℃, controlling the liquid level height to be within 6cm, finally cooling the magnesium sulfate solution at a constant speed at a cooling rate of 0.1 ℃/min, and gradually stopping stirring when the cooling temperature is reduced to be below 20 ℃; the cooling crystallization time is 16 h. After crystal pulp is separated by centrifugation at 5000r/min, the drying temperature of the crystal is 45 ℃ and the drying time is 20 min. Magnesium sulfate crystal particles with uniform size and regular shape with the diameter range of 2-3 mm are prepared.
Therefore, the large-particle magnesium sulfate cooling crystallization method provided by the invention can generate magnesium sulfate crystals with regular appearance, large and uniform particle size, increases the product particle size, is beneficial to product screening, greatly improves the product purity, is more suitable for agricultural and industrial application due to uniform product particle size distribution, realizes the conversion from magnesium sulfate solution generated by waste acid solution to magnesite cooling crystallization, protects the environment and reduces the cost.
As shown in fig. 2, the present invention further provides a large granular magnesium sulfate cooling crystallization system, which is used for implementing the above-mentioned large granular magnesium sulfate cooling crystallization method, and the system comprises: crystal nucleus growth system and cooling system, crystal nucleus growth system includes electronic stirring rake 1, constant temperature water bath 2, beaker 3 and sealing film, cooling system includes controllable refrigerator 4 of temperature. The crystal nuclei in the magnesium sulfate solution in the beaker 3 can be nucleated and uniformly grow by the electric stirring paddle 1 and the constant-temperature water bath box 2, and the evaporated solvent is collected and refluxed into the beaker 3 by adopting a sealing film at the opening of the beaker, so that the balance of the composition ratio of the raw materials is ensured.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A cooling crystallization method of large-particle magnesium sulfate is characterized by comprising the following steps:
step S1, adding water into the neutral magnesium sulfate solution generated by the reaction of the alkylated waste acid solution and magnesium oxide for slight dilution;
step S2, adding magnesium sulfate crystal nuclei into the solution obtained in step S1, so that the crystal nuclei are uniformly distributed in the magnesium sulfate solution;
step S3, stirring the solution obtained in the step S2 in a constant temperature water bath tank until the crystal is completely dissolved, controlling the liquid level height within the range of 6 cm-10 cm, and adjusting the pH value of the magnesium sulfate solution to be within the range of 3-6 by adopting concentrated sulfuric acid;
step S4, placing the magnesium sulfate solution of which the pH value is adjusted in the step S3 into a constant-temperature water bath box, uniformly stirring the solution by adopting electric stirring equipment, and simultaneously controlling the temperature to be 40-55 ℃ to preserve the temperature of the magnesium sulfate solution;
step S5, cooling the magnesium sulfate solution processed in the step S4 at a constant speed within a cooling rate range of 0.1-0.5 ℃/min, and gradually stopping stirring when the cooling temperature is reduced to 20-25 ℃;
and step S6, putting the crystal pulp mixed solution processed in the step S5 into a high-speed centrifuge for crystal and mother liquor separation, and finally drying the crystals.
2. The method for cooling and crystallizing large particle magnesium sulfate as claimed in claim 1, wherein the supersaturation degree of the neutral magnesium sulfate solution in step S1 is in the range of 1-1.25%.
3. The method for cooling and crystallizing large particle magnesium sulfate as claimed in claim 1, wherein in step S2, 1-3 g of magnesium sulfate crystal nuclei are added per 1000ml of the solution obtained in step S1.
4. The method for cooling and crystallizing large granular magnesium sulfate as claimed in claim 1, wherein in step S3, the temperature of the constant temperature water bath is in the range of 75 ℃ to 79 ℃.
5. The method for cooling and crystallizing large granular magnesium sulfate as claimed in claim 1, wherein in step S4, the stirring speed of the electric stirring device is 500-800 rpm.
6. The method for cooling and crystallizing large granular magnesium sulfate as claimed in claim 1, wherein in step S4, the temperature of the magnesium sulfate solution is maintained at 40-55 ℃ for 2-3 h.
7. The method for cooling and crystallizing large granular magnesium sulfate as claimed in claim 1, wherein in step S5, after the stirring is gradually stopped when the cooling temperature is reduced to 20-25 ℃, the large granular magnesium sulfate is further cooled and crystallized for 16-24 h.
8. The method for cooling and crystallizing large granular magnesium sulfate as claimed in claim 1, wherein in step S6, the centrifugal speed of the high speed centrifuge is in the range of 5000r/min to 8000 r/min.
9. The method for cooling and crystallizing large granular magnesium sulfate as claimed in claim 1, wherein in step S6, the crystal drying temperature is 45-75 ℃ and the crystal drying time is 20-40 min.
10. A large-particle magnesium sulfate cooling crystallization system for realizing the large-particle magnesium sulfate cooling crystallization method of any one of claims 1 to 9, wherein the system comprises: crystal nucleus growth system and cooling system, crystal nucleus growth system includes electronic stirring rake, constant temperature water bath, beaker and sealing film, cooling system includes the controllable refrigerator of temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114146444A (en) * | 2021-12-14 | 2022-03-08 | 桐乡市思远环保科技有限公司 | Method for crystallizing magnesium sulfate |
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Application publication date: 20210302 |