CN112758966A - Production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment - Google Patents
Production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment Download PDFInfo
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- CN112758966A CN112758966A CN202011601698.4A CN202011601698A CN112758966A CN 112758966 A CN112758966 A CN 112758966A CN 202011601698 A CN202011601698 A CN 202011601698A CN 112758966 A CN112758966 A CN 112758966A
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- sulfate heptahydrate
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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
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
- B01F33/822—Combinations of dissimilar mixers with moving and non-moving stirring devices in the same receptacle
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/99—Heating
Abstract
The application relates to a production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment, and particularly discloses a production process of magnesium sulfate heptahydrate, which comprises the following process steps: s1, mixing magnesium sulfate mother liquor, magnesium oxide powder and sulfamic acid waste acid for reaction, and continuously introducing compressed air into the reaction liquid in the reaction process; and S2, cooling and crystallizing the reaction liquid after the reaction is finished to obtain a finished magnesium sulfate heptahydrate product. The utility model provides a magnesium sulfate heptahydrate production facility for implement aforementioned production technology of magnesium sulfate heptahydrate, includes the reaction tank, still includes the compressed air pipeline, and compressed air pipeline one end lets in the reaction tank, and the other end intercommunication has the air compressor machine. The problem that the reaction liquid solidifies when sulfamic acid waste acid is used for producing magnesium sulfate heptahydrate is solved, and in addition, the method has the advantage of reducing the production cost.
Description
Technical Field
The application relates to the field of preparation of magnesium sulfate heptahydrate, in particular to a production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment.
Background
Magnesium sulfate heptahydrate is often used in the fields of leather making, explosives, fertilizers, paper making, porcelain, dye printing, lead storage batteries and the like in industry. The traditional magnesium sulfate heptahydrate production process comprises a sulfuric acid method, a gas phase method, a bittern recrystallization method and other methods, wherein the sulfuric acid method can select industrial waste sulfuric acid as a raw material to produce the magnesium sulfate heptahydrate, so that the method is environment-friendly, can save the production cost of enterprises, and is one of the main methods for producing the magnesium sulfate heptahydrate by the enterprises. At present, when an enterprise adopts industrial waste sulfuric acid to produce magnesium sulfate heptahydrate, the used waste sulfuric acid usually contains more than 70 percent of sulfuric acid.
Since about 2.5 tons of waste acid are produced per 1 ton of sulfamic acid produced, a large amount of sulfamic acid waste acid is difficult to handle, and thus enterprises seek to produce magnesium sulfate heptahydrate using sulfamic acid waste acid as a raw material. The sulfuric acid concentration in the sulfamic acid waste acid is only 50-55%, and the inventor finds that in actual production, when the sulfamic acid waste acid is directly used as a raw material to produce magnesium sulfate heptahydrate, reaction can not be fully carried out, so that reaction liquid is solidified.
In order to solve the problems, enterprises generally adopt a method of converting waste acid into concentrated sulfuric acid, but the method still needs a large amount of concentrated sulfuric acid, and the production cost is relatively high.
Disclosure of Invention
In order to solve the problem that reaction liquid is solidified when sulfamic acid waste acid is used for producing magnesium sulfate heptahydrate, the application provides a production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment.
In a first aspect, the application provides a production process of magnesium sulfate heptahydrate, which adopts the following technical scheme:
a production process of magnesium sulfate heptahydrate comprises the following process steps:
s1, mixing magnesium sulfate mother liquor, magnesium oxide powder and sulfamic acid waste acid for reaction, and continuously introducing compressed air into the reaction liquid in the reaction process;
and S2, cooling and crystallizing the reaction liquid after the reaction is finished to obtain a finished magnesium sulfate heptahydrate product.
By adopting the technical scheme, on one hand, the reaction liquid can be rolled by increasing the volume of the compressed air after the compressed air enters the reaction tank, so that the raw materials can be fully reacted, and the problem of solidification of the reaction liquid can be solved without preparing waste acid into concentrated sulfuric acid; on the other hand, the sulfamic acid waste acid is used as a raw material, so that the sulfamic acid waste acid which is difficult to treat is treated, the magnesium sulfate heptahydrate can be prepared without using concentrated sulfuric acid, and the production cost of the magnesium sulfate heptahydrate is reduced.
Preferably, the weight ratio of the magnesium oxide powder to the sulfamic acid waste acid is 4: (15-21).
By adopting the technical scheme, the purity of the prepared magnesium sulfate heptahydrate is higher.
Preferably, the weight ratio of the magnesium oxide powder to the sulfamic acid waste acid is 4: (17-19).
By adopting the technical scheme, the purity of the prepared magnesium sulfate heptahydrate is higher.
Preferably, the temperature of the reaction liquid in the step S2 is reduced to 45-48 ℃, and the magnesium sulfate heptahydrate finished product is prepared through crystallization.
By adopting the technical scheme, the yield of magnesium sulfate heptahydrate is higher when the temperature is reduced to 45-48 ℃.
In a second aspect, the application provides a production facility for magnesium sulfate heptahydrate, which adopts the following technical scheme:
the production equipment for magnesium sulfate heptahydrate comprises a reaction tank and a compressed air pipeline, wherein one end of the compressed air pipeline is introduced into the reaction tank, and the other end of the compressed air pipeline is communicated with an air compressor.
Through adopting above-mentioned technical scheme, compressed air gets into volume grow can make reaction liquid roll behind the reaction tank, makes the raw materials fully react, need not to prepare the waste acid into concentrated sulfuric acid finally and can solve the problem that reaction liquid solidifies.
Preferably, the compressed air pipeline comprises a plurality of branch pipelines, the branch pipelines are tightly attached to the inner side wall of the reaction tank, and the end parts, far away from the air compressor, of the branch pipelines are different from the bottom of the reaction tank in distance.
By adopting the technical scheme, the range of compressed air introduced into the reaction tank is increased, and the possibility of solidification of the reaction liquid is further reduced.
Preferably, be equipped with agitating unit in the reaction tank, agitating unit includes (mixing) shaft and stirring vane, and stirring vane fixed connection is in the (mixing) shaft, and the end connection of (mixing) shaft has and is used for driving the rotatory motor of (mixing) shaft.
Through adopting above-mentioned technical scheme, motor drive (mixing) shaft is rotatory, makes stirring vane stir the material in to the reaction tank, has improved the mobility of material, has reduced the possibility that reaction liquid solidifies.
Preferably, the stirring blade and the stirring shaft are both hollow, the stirring blade is provided with a plurality of air outlets communicated with the inner cavity of the stirring shaft, and the compressed air pipeline is communicated with the inner cavity of the stirring shaft.
Through adopting above-mentioned technical scheme, the interior pipeline of axle passes through (mixing) shaft and stirring vane, can let in compressed air to the reaction liquid that is located blade department, has increased the scope that lets in compressed air, has further reduced the possibility that reaction liquid solidifies.
Preferably, still include filter-pressing jar and crystallizer, be connected with first conveyer pipe between reaction tank and the filter-pressing jar, be connected with the second conveyer pipe between filter-pressing jar and the crystallizer, be connected with the circulating pipe between crystallizer and the reaction tank, between reaction tank and the filter-pressing jar, between filter-pressing jar and the crystallizer, all through force pump conveying material between crystallizer and the reaction tank, first conveyer pipe overcoat is equipped with the heat transfer jacket, be connected with first water pump on the heat transfer jacket, the heat transfer jacket is connected with the delivery port of first water pump, the water inlet of first water pump is connected with the water tank, the circulating pipe overcoat is equipped with preheating jacket, be connected with the insulating tube on the heat transfer jacket, insulating tube and heat transfer jacket intercommunication, be connected with the drain pipe on preheating jacket.
By adopting the technical scheme, because the sulfuric acid reacts with the magnesium oxide to release a large amount of heat, the temperature of the reaction liquid is still high when the reaction liquid enters the filter-pressing tank, and a large amount of heat is wasted. The water with lower temperature is introduced into the heat exchange jacket to exchange heat with the reaction liquid, so that the temperature of the water in the heat exchange jacket is increased, then the water with increased temperature enters the preheating jacket through the heat preservation pipe, and the magnesium sulfate mother liquor in the circulating pipe is preheated, so that the possibility of solidification of the reaction liquid during material reaction can be further reduced, and the energy utilization rate is improved.
Preferably, one end of the drain pipe, which is far away from the preheating jacket, is connected with a second water pump, a water inlet of the second water pump is connected with the drain pipe, and a water outlet of the second water pump is connected with the water tank.
By adopting the technical scheme, the water in the preheating jacket can enter the water tank to be reused, and the water is saved.
Drawings
FIG. 1 is a first schematic structural diagram of a magnesium sulfate heptahydrate production device in the embodiment of the application;
FIG. 2 is a schematic structural view of a reaction cell in the example of the present application;
FIG. 3 is a sectional view of a reaction cell in the example of the present application;
FIG. 4 is an enlarged view of portion A of FIG. 3;
fig. 5 is a schematic structural diagram ii of a magnesium sulfate heptahydrate production device in the embodiment of the present application.
Description of reference numerals: 1. a reaction tank; 2. a filter-pressing tank; 3. a crystallization tank; 4. a first delivery pipe; 5. a second delivery pipe; 6. a circulation pipe; 7. a stirring device; 8. a stirring shaft; 9. a stirring blade; 10. a fixed seat; 11. a motor; 12. adding an acid pipe; 13. a compressed air conduit; 14. an opening; 15. an air outlet; 16. dividing pipelines; 17. an in-shaft conduit; 18. air holes; 19. a through hole; 20. coating air holes; 21. a heat exchange jacket; 22. a first water pump; 23. a water tank; 24. preheating a jacket; 25. a heat preservation pipe; 26. a drain pipe; 27. a second water pump; 28. and (5) sealing the sleeve.
Detailed Description
The present application will be described in further detail with reference to the following examples and accompanying fig. 1-5.
Examples
The sources of the raw materials used in the examples are shown in table 1 below:
TABLE 1 sources and specifications of the various feedstocks of the examples
| Raw materials | Specification of | Source |
| Magnesium oxide powder | Industrial grade | River which rises in the northeastern part of Anhui Province Co-creation chemical Co Ltd |
| Waste acid of sulfamic acid | The sulfuric acid content is 50 to 55 percent | Laizhou Zhongda Guihe Chemical Co., Ltd. |
Example 1
A production process of magnesium sulfate heptahydrate comprises the following process steps:
s1, adding 40 kg of magnesium sulfate mother liquor and 30 kg of magnesium oxide powder into a reaction tank, starting a stirring device, introducing 140 kg of sulfamic acid waste acid (sulfuric acid content is 52%) into the reaction tank through an acid adding pipe, and introducing compressed air into the reaction tank through a compressed air pipeline connected with an air compressor.
And S2, reacting for 2 hours, introducing the reaction liquid into a filter pressing tank, performing filter pressing, separating filter residues from filtrate, conveying the filtrate into a crystallization tank, cooling to 30 ℃, and crystallizing to obtain a finished magnesium sulfate heptahydrate product.
Examples 2 to 3
Examples 2 to 3 are based on example 1, and differ from example 1 only in the temperature decrease in the step S2, as shown in table 2.
TABLE 2 reaction conditions of examples 1-3
| Examples | Example 1 | Example 2 | Example 3 |
| Reaction time (h) | 2 | 3 | 4 |
| Temperature drop (. degree.C.) | 30 | 43 | 50 |
Examples 4 to 9
Examples 4 to 9 are based on example 2 and differ from example 2 only in the weight ratio of magnesium oxide powder used to sulfamic acid waste acid (sulfuric acid content 52%), see table 3.
TABLE 3 reaction conditions for examples 4-9
| Examples | Example 2 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 |
| Magnesium oxide: sulfamic acid waste acid (weight ratio) | 3:14 | 4：16 | 4：21 | 4：15 | 4：17 | 4：19 | 4：18 |
Examples 10 to 12
Examples 10 to 12 are based on example 2, and differ from example 9 only in the temperature decrease in step S2, as shown in table 4.
TABLE 4 crystallization temperatures for examples 10-12
| Examples | Example 10 | Example 11 | Example 12 |
| Temperature drop (. degree.C.) | 48 | 45 | 46 |
To implement the foregoing examples 1-12, the present application discloses a magnesium sulfate heptahydrate production facility.
Referring to fig. 1, the production equipment of magnesium sulfate heptahydrate comprises a reaction tank 1, a filter-pressing tank 2 and a crystallization tank 3, wherein the inner walls of the reaction tank 1, the filter-pressing tank 2 and the crystallization tank 3 are coated with anticorrosive layers. A first conveying pipe 4 is connected between the reaction tank 1 and the filter-pressing tank 2, and the first conveying pipe 4 is used for conveying the reaction liquid after the reaction is finished to the filter-pressing tank 2 for filter-pressing. A second conveying pipe 5 is arranged between the filter pressing tank 2 and the crystallizing tank 3, and the second conveying pipe 5 is used for conveying filter pressed filtrate into the crystallizing tank 3. A circulating pipe 6 is connected between the crystallization tank 3 and the reaction tank 1, magnesium sulfate heptahydrate is crystallized in the crystallization tank 3, then crystals are separated out to obtain a finished magnesium sulfate heptahydrate product, and the magnesium sulfate mother liquor obtained by separation is conveyed to the reaction tank 1 through the circulating pipe 6 for recycling. Materials are conveyed between the reaction tank 1 and the filter-pressing tank 2, between the filter-pressing tank 2 and the crystallization tank 3 and between the crystallization tank 3 and the reaction tank 1 through pressure pumps.
Referring to fig. 2, a stirring device 7 for stirring reaction materials is arranged in the reaction tank 1, the stirring device 7 comprises a stirring shaft 8 and stirring blades 9, the stirring shaft 8 is located on the central axis of the reaction tank 1, the stirring blades 9 are fixed on the stirring shaft 8, the stirring blades 9 are distributed along the axial direction of the stirring shaft 8, and the stirring blades 9 are inclined towards the tank opening of the reaction tank 1. The reaction tank 1 is fixedly connected with a fixed seat 10 on the tank mouth, a motor 11 is bolted on the fixed seat 10, and the motor 11 is in driving connection with a stirring shaft 8. Be equipped with in the reaction tank 1 and add acid pipe 12, compressed air pipeline 13, the inside wall setting of reaction tank 1 is hugged closely to the outer wall of adding acid pipe 12, and compressed air pipeline 13 is used for letting in compressed air in to reaction tank 1.
Referring to fig. 3, the stirring shaft 8 and the stirring blades 9 are both hollow, and an opening 14 is formed at the end of the stirring shaft 8 close to the bottom of the reaction tank 1. The compressed air pipeline 13 comprises a plurality of branch pipelines 16 and an in-shaft pipeline 17, the branch pipelines 16 are arranged along the circumferential direction of the inner side wall of the reaction tank 1, the depth of each branch pipeline 16 extending into the reaction tank 1 is not consistent, and the outer wall of each branch pipeline 16 is tightly attached to the inner side wall of the reaction tank 1. The shaft inner pipeline 17 is provided with one, the shaft inner pipeline 17 penetrates through the stirring shaft 8 through the opening 14 of the stirring shaft 8, and the shaft inner pipeline 17 in the stirring shaft 8 is coaxial with the stirring shaft 8.
Referring to fig. 3 and 4, a plurality of sealing sleeves 28 are fixedly sleeved on the outer wall of the shaft inner pipeline 17, the positions of the sealing sleeves 28 correspond to the positions of the stirring blades 9 one by one, the outer side walls of the sealing sleeves 28 are coaxial with the inner side wall of the stirring shaft 8, and when the stirring shaft 8 rotates relative to the sealing sleeves 28, the outer wall of the sealing sleeves 28 is always attached to the inner side wall of the stirring shaft 8. The stirring blade 9 is provided with a plurality of air outlets 15 communicated with the inner cavity of the stirring blade 9, the side wall of an inner shaft pipeline 17 positioned in the stirring shaft 8 is provided with a plurality of air holes 18, and the air holes 18 are communicated with the inside of the inner shaft pipeline 17. The sealing sleeve 28 is provided with a plurality of through holes 19 which are the same as the air holes 18, and the positions of the through holes 19 correspond to the positions of the air holes 18 one by one. The stirring shaft 8 is provided with a plurality of air holes 20, the air holes 20 are communicated with the inside of the stirring blade 9 and the inside of the stirring shaft 8, and when the stirring shaft 8 rotates, the air holes 20 are communicated with the through holes 19.
Referring to fig. 3 and 4, when compressed air is introduced into the compressed air pipe 13, the branch pipes 16 are engaged with the in-shaft pipe 17, and compressed air can be introduced into various positions in the reaction cell 1. After the compressed air enters the reaction tank 1, the volume is increased, the reaction liquid is rolled, the raw materials can fully react, the problem of solidification of the reaction liquid can be solved without adding concentrated sulfuric acid into the reaction liquid, and the cost for producing the magnesium sulfate heptahydrate is reduced.
Referring to fig. 5, a heat exchange jacket 21 is sleeved outside the first conveying pipe 4, the heat exchange jacket 21 is coaxial with the first conveying pipe 4, one end of the heat exchange jacket 21 close to the reaction tank 1 is connected with a first water pump 22, and the heat exchange jacket 21 is connected with a water outlet of the first water pump 22. A water tank 23 is connected to an inlet of the first water pump 22, and the water tank 23 is used for placing cold water. A preheating jacket 24 is coaxially sleeved outside the circulating pipe 6, one end of the heat exchange jacket 21 close to the pressure filtration tank 2 and one end of the preheating jacket 24 close to the crystallization tank are connected with a heat preservation pipe 25, and one end of the preheating jacket 24 close to the reaction tank 1 is connected with a drain pipe 26. One section of the drain pipe 26 far away from the preheating jacket 24 is connected with a second water pump 27, the water inlet of the water pump is connected with the drain pipe 26, and the water outlet of the second water pump 27 is communicated with the water tank 23.
Referring to fig. 5, sulfuric acid reacts with magnesium oxide to release a large amount of heat, the temperature of the reaction solution is still high when the reaction solution enters the pressure filtration tank 2, cold water is introduced into the heat exchange jacket 21 to exchange heat with the reaction solution, so that the temperature of the water in the heat exchange jacket 21 is raised, the water with the raised temperature enters the preheating jacket 24 through the heat preservation pipe 25 to exchange heat with the magnesium sulfate mother solution in the circulating pipe 6, the heat of the water is absorbed by the magnesium sulfate mother solution, and the cooled water is transmitted back to the water tank 23 again. The temperature of the magnesium sulfate mother liquor is higher, so that the possibility of coagulation of the reaction liquid is further reduced during the reaction.
The implementation principle of the production equipment for magnesium sulfate heptahydrate in the embodiment of the application is as follows: magnesium sulfate mother liquor is preheated through a heat exchange jacket 21, a heat preservation pipe 25 and the like, magnesium oxide powder, the preheated magnesium sulfate mother liquor and sulfamic acid waste acid are introduced into a reaction tank 1, a stirring device 7 is used for stirring materials, compressed air is introduced into the reaction tank 1 through a compressed air pipeline 13, reaction liquid is enabled to be boiled in a rolling mode, and therefore solidification of the reaction liquid is prevented.
Comparative example
Comparative example 1
Comparative example 1 is based on example 1 and differs from example 1 only in that: compressed air is not introduced into the reaction tank in the reaction process, and the reaction liquid in the reaction tank is solidified after the reaction is carried out for 20 minutes.
Comparative example 2
Comparative example 2 is based on comparative example 1 and differs from comparative example 1 only in that: the magnesium sulfate heptahydrate is prepared by using sulfuric acid with the concentration of 70% as a raw material.
Detection method
And (3) purity testing: a Waters e2695 model HPLC, comprising 515 high pressure pump, 2487 detector and 7725i manual injection valve; a chromatography workstation; microsyringe: 200 μ L.
The yield is as follows: mass of actual product material/amount of theoretical product material.
The test results of examples 1 to 12 and comparative examples 1 to 2 are shown in Table 5.
TABLE 5 purities and yields of examples 1-12 and comparative examples 1-2
| Examples | Purity (%) | Yield (%) | Examples | Purity (%) | Yield (%) |
| Example 1 | 99.54 | 98.64 | Example 8 | 99.85 | 98.92 |
| Example 2 | 99.65 | 98.73 | Example 9 | 99.89 | 98.92 |
| Example 3 | 99.55 | 98.67 | Example 10 | 99.71 | 99.12 |
| Example 4 | 99.74 | 98.84 | Example 11 | 99.73 | 99.01 |
| Example 5 | 99.78 | 98.85 | Example 12 | 99.68 | 98.97 |
| Example 6 | 99.75 | 98.87 | Comparative example 1 | 74.89 | 67.48 |
| Example 7 | 99.83 | 98.91 | Comparative example 2 | 99.46 | 96.87 |
The test results of examples 1 to 12 and comparative examples 1 to 2 were analyzed to find that:
data for comparative examples 1-3: the product of example 2 is the highest in yield and purity, so example 2 is the best example of examples 1-3, and the product of example 1 is the lowest in yield and purity.
Compared with the example 1, the difference of the comparative example 1 is that compressed air is not introduced into the reaction tank in the reaction process, the reaction liquid in the reaction tank in the comparative example 1 is solidified, and the purity and yield of the prepared magnesium sulfate heptahydrate are far lower than those of the example 1, which shows that the problem of solidification of the reaction liquid when the magnesium sulfate heptahydrate is produced by taking sulfamic acid as a raw material can be solved by introducing compressed air into the reaction tank through a compressed air pipeline connected with an air compressor.
Compared with the comparative example 1, the difference of the comparative example 2 and the comparative example 1 is only that the sulfuric acid with the concentration of 70% is used, and the purity and the yield of the magnesium sulfate heptahydrate prepared in the comparative example 2 are not much different from those of the example 1, which shows that the compressed air is introduced into the reaction tank, not only solves the problem of solidification of reaction liquid when the sulfamic acid waste acid is used for producing the magnesium sulfate heptahydrate, but also can achieve the effect of preparing the magnesium sulfate heptahydrate by using the sulfuric acid with the concentration of 70%.
Examples 4-6 differ from example 2 only in the weight ratio of magnesium oxide to sulfamic acid waste acid (sulfuric acid content 52%) used, and examples 4-6 produced magnesium sulfate heptahydrate having a higher purity than example 2, indicating that the weight ratio of magnesium oxide powder to sulfamic acid waste acid (sulfuric acid content 52%) used was 4: (15-21), the purity of the magnesium sulfate heptahydrate obtained was high.
Examples 7-9 compared to examples 4-6, differing only in the weight ratio of magnesium oxide used to the sulfamic acid waste acid (sulfuric acid content 52%), the purity of the magnesium sulfate heptahydrate produced in examples 7-9 was higher than that of the magnesium sulfate heptahydrate produced in example 2, indicating that the weight ratio of magnesium oxide powder used to sulfamic acid waste acid (sulfuric acid content 52%) was 4: (17-19), the purity of the magnesium sulfate heptahydrate obtained was high.
When an enterprise uses sulfuric acid with the concentration of 70% as a raw material to produce magnesium sulfate heptahydrate, at least 1.2 tons of sulfuric acid are needed for producing 1 ton of magnesium sulfate heptahydrate; when enterprises use sulfamic acid waste acid (50% -55% of sulfuric acid) as a raw material to produce magnesium sulfate heptahydrate, at least 1.5 tons of sulfamic acid waste acid is needed for producing 1 ton of magnesium sulfate heptahydrate. If enterprises prepare the sulfamic acid waste acid into concentrated acid with the concentration of 70%, at least 0.78 ton of concentrated sulfuric acid with the concentration of 98% is needed for producing 1 ton of magnesium sulfate heptahydrate, and each ton of concentrated sulfuric acid with the concentration of 98% is about 600 RMB, so that the enterprises need to purchase the concentrated sulfuric acid with the concentration of 98% by about 500 RMB. When the air compressor is used for introducing compressed air, the air compressor with the pressure of 75kw at most is needed, when 1 ton of magnesium sulfate heptahydrate is produced by taking sulfamic acid waste acid as a raw material, the power consumption of the air compressor is about 150 degrees, the electricity cost is about 200 RMB, and the cost is reduced by about 60%.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A production process of magnesium sulfate heptahydrate is characterized in that: the method comprises the following process steps:
s1, mixing magnesium sulfate mother liquor, magnesium oxide powder and sulfamic acid waste acid for reaction, and continuously introducing compressed air into the reaction liquid in the reaction process;
and S2, cooling and crystallizing the reaction liquid after the reaction is finished to obtain a finished magnesium sulfate heptahydrate product.
2. The process for producing magnesium sulfate heptahydrate according to claim 1, wherein: the weight ratio of the magnesium oxide powder to the sulfamic acid waste acid is 4: (15-21).
3. The process for producing magnesium sulfate heptahydrate according to claim 1, wherein: the weight ratio of the magnesium oxide powder to the sulfamic acid waste acid is 4: (17-19).
4. The process for producing magnesium sulfate heptahydrate according to claim 1, wherein: and cooling the reaction liquid in the step S2 to 45-48 ℃, and crystallizing to obtain a finished magnesium sulfate heptahydrate product.
5. A production facility of magnesium sulfate heptahydrate for implementing a production process of magnesium sulfate heptahydrate according to claim 1, comprising a reaction tank (1), characterized in that: still include compressed air pipeline (13), compressed air pipeline (13) one end lets in reaction tank (1), and the other end intercommunication has the air compressor machine.
6. The apparatus for producing magnesium sulfate heptahydrate according to claim 5, wherein: the compressed air pipeline (13) comprises a plurality of branch pipelines (16), the branch pipelines (16) are tightly attached to the inner side wall of the reaction tank (1), and the end parts, far away from the air compressor, of the branch pipelines (16) are different from the tank bottom of the reaction tank (1) in distance.
7. The apparatus for producing magnesium sulfate heptahydrate according to claim 6, wherein: be equipped with agitating unit (7) in reaction tank (1), agitating unit (7) include (mixing) shaft (8) and stirring vane (9), stirring vane (9) fixed connection in (mixing) shaft (8), and the end connection of (mixing) shaft (8) has motor (11) that are used for driving (mixing) shaft (8) rotation.
8. The apparatus for producing magnesium sulfate heptahydrate according to claim 7, wherein: the stirring blades (9) and the stirring shaft (8) are both hollow, a plurality of air outlets (15) communicated with the inner cavity of the stirring shaft (8) are arranged on the stirring blades (9), and the compressed air pipeline (13) is communicated with the inner cavity of the stirring shaft (8).
9. The apparatus for producing magnesium sulfate heptahydrate according to claim 5, wherein: the device also comprises a filter-pressing tank (2) and a crystallization tank (3), a first conveying pipe (4) is connected between the reaction tank (1) and the filter-pressing tank (2), a second conveying pipe (5) is connected between the filter-pressing tank (2) and the crystallization tank (3), a circulating pipe (6) is connected between the crystallization tank (3) and the reaction tank (1), materials are conveyed between the reaction tank (1) and the filter-pressing tank (2), between the filter-pressing tank (2) and the crystallization tank (3), and between the crystallization tank (3) and the reaction tank (1) through pressure pumps, a heat exchange jacket (21) is sleeved outside the first conveying pipe (4), a first water pump (22) is connected on the heat exchange jacket (21), the heat exchange jacket (21) is connected with a water outlet of the first water pump (22), a water tank (23) is connected with a water inlet of the first water pump (22), a preheating jacket (24) is sleeved outside the circulating pipe (6), a heat preservation pipe (25) is connected on the heat, the heat preservation pipe (25) is communicated with the heat exchange jacket (21), and the preheating jacket (24) is connected with a drain pipe (26).
10. The apparatus for producing magnesium sulfate heptahydrate according to claim 9, wherein: one end of the drain pipe (26) far away from the preheating jacket (24) is connected with a second water pump (27), a water inlet of the second water pump (27) is connected with the drain pipe (26), and a water outlet of the second water pump (27) is connected with the water tank (23).
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| JPH06191831A (en) * | 1992-12-28 | 1994-07-12 | Kawasaki Steel Corp | Production of granular ammonium sulfate |
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| CN202766389U (en) * | 2012-09-26 | 2013-03-06 | 湖南湘牛环保实业有限公司 | Novel sewage biological reaction and membrane purification device |
| CN103387247A (en) * | 2012-05-09 | 2013-11-13 | 中节能六合天融环保科技有限公司 | Process for preparing magnesium sulfate heptahydrate and liquid sulfur dioxide by comprehensively utilizing magnesium desulfurization byproducts |
| CN104118893A (en) * | 2014-07-31 | 2014-10-29 | 四川龙蟒钛业股份有限公司 | Method for producing industrial-grade magnesium sulfate by using titanium white waste acid |
| CN109135831A (en) * | 2018-10-31 | 2019-01-04 | 上海电气集团股份有限公司 | A kind of pyrolysis cylinder conveying device of internal heating type biomass gasifying furnace |
| CN209259849U (en) * | 2018-12-28 | 2019-08-16 | 湖南谊诚科技有限公司 | A kind of dilute sulfuric acid waste water treatment system |
| CN110980782A (en) * | 2019-12-31 | 2020-04-10 | 盘锦泓实环保科技有限公司 | Method for producing high-purity magnesium sulfate by using alkylation waste sulfuric acid and application thereof |
| CN211462268U (en) * | 2019-12-26 | 2020-09-11 | 广东也乐新材料制造有限公司 | Vacuum suction filtration integrated device |
| CN111847491A (en) * | 2020-07-31 | 2020-10-30 | 山东泓瑞医药科技股份公司 | Treatment method of amantadine production waste acid |
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2020
- 2020-12-30 CN CN202011601698.4A patent/CN112758966B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06191831A (en) * | 1992-12-28 | 1994-07-12 | Kawasaki Steel Corp | Production of granular ammonium sulfate |
| CN101367533A (en) * | 2007-08-16 | 2009-02-18 | 苏州麒麟医药化学研发有限公司 | Process for preparing magnesium sulphate heptahydrate in treatment of industrial waste sulphuric acid liquid |
| CN103387247A (en) * | 2012-05-09 | 2013-11-13 | 中节能六合天融环保科技有限公司 | Process for preparing magnesium sulfate heptahydrate and liquid sulfur dioxide by comprehensively utilizing magnesium desulfurization byproducts |
| CN202766389U (en) * | 2012-09-26 | 2013-03-06 | 湖南湘牛环保实业有限公司 | Novel sewage biological reaction and membrane purification device |
| CN104118893A (en) * | 2014-07-31 | 2014-10-29 | 四川龙蟒钛业股份有限公司 | Method for producing industrial-grade magnesium sulfate by using titanium white waste acid |
| CN109135831A (en) * | 2018-10-31 | 2019-01-04 | 上海电气集团股份有限公司 | A kind of pyrolysis cylinder conveying device of internal heating type biomass gasifying furnace |
| CN209259849U (en) * | 2018-12-28 | 2019-08-16 | 湖南谊诚科技有限公司 | A kind of dilute sulfuric acid waste water treatment system |
| CN211462268U (en) * | 2019-12-26 | 2020-09-11 | 广东也乐新材料制造有限公司 | Vacuum suction filtration integrated device |
| CN110980782A (en) * | 2019-12-31 | 2020-04-10 | 盘锦泓实环保科技有限公司 | Method for producing high-purity magnesium sulfate by using alkylation waste sulfuric acid and application thereof |
| CN111847491A (en) * | 2020-07-31 | 2020-10-30 | 山东泓瑞医药科技股份公司 | Treatment method of amantadine production waste acid |
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