CN111977672A - Ammonium sulfate solution evaporation crystallization method - Google Patents
Ammonium sulfate solution evaporation crystallization method Download PDFInfo
- Publication number
- CN111977672A CN111977672A CN202010775107.9A CN202010775107A CN111977672A CN 111977672 A CN111977672 A CN 111977672A CN 202010775107 A CN202010775107 A CN 202010775107A CN 111977672 A CN111977672 A CN 111977672A
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- Prior art keywords
- ammonium sulfate
- evaporation
- sulfate solution
- cooling
- crystallizing
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- 238000001704 evaporation Methods 0.000 title claims abstract description 56
- 230000008020 evaporation Effects 0.000 title claims abstract description 55
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 49
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 49
- 238000002425 crystallisation Methods 0.000 title claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000000498 cooling water Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000012452 mother liquor Substances 0.000 claims abstract description 5
- 238000004094 preconcentration Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 39
- 239000012047 saturated solution Substances 0.000 claims description 4
- 238000004134 energy conservation Methods 0.000 abstract 1
- 239000003337 fertilizer Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003898 horticulture Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
An evaporation crystallization method of an ammonium sulfate solution comprises the following steps of carrying out primary evaporation through an evaporation tank, converting water in the ammonium sulfate solution into steam to be discharged, controlling that crystallization cannot be carried out, and achieving the purpose of preconcentration of the solution; performing secondary evaporation, concentration and crystallization to facilitate solid-liquid separation; meanwhile, the third-stage preheating tank absorbs heat in the steam condensate water of the first-stage evaporation tank; cooling and crystallizing in a cooling crystallization kettle, introducing cooling water into a jacket of the crystallization kettle, crystallizing and separating out the ammonium sulfate solution in a supersaturated state through the change of temperature from high to low, balancing the crystallization and separation out due to no temperature change after cooling to room temperature, finishing the cooling and crystallizing process, returning the separated crystal to the first step, and evaporating and concentrating mother liquor; washing with a small amount of clear water to obtain the ammonium sulfate solution crystal. The method has the advantages of simple operation, energy conservation and improved yield of the crystallized ammonium sulfate.
Description
Technical Field
The invention relates to the field of evaporative crystallization methods, in particular to an evaporative crystallization method for an ammonium sulfate solution.
Background
Ammonium sulfate is an odorless, colorless crystal or white particle. Decomposing at 280 deg.C or higher. The solubility in water was 70.6g at 0 ℃ and 103.8g at 100 ℃. Insoluble in ethanol and acetone. The pH of the 0.1mol/L aqueous solution was 5.5. The relative density was 1.77. Refractive index 1.521. Ammonium sulfate is mainly used as a fertilizer and is suitable for various soils and crops. It can also be used in textile, leather, medicine, etc.
Ammonium sulfate is useful as a fertilizer, for example in agriculture, horticulture or forestry. It is usually applied as a crystalline material. The size of the crystals is important and determines utility and value. Thus, ammonium sulfate crystals of the desired size are typically present. A common method of preparing crystalline ammonium sulfate in a continuous process is to start with a saturated or supersaturated solution.
Because the solubility of the ammonium sulfate is not changed greatly along with the temperature, the vapor enthalpy of different pressure sections can be utilized to carry out multistage heating evaporation, and the influence of the combined action of the temperature and the pressure on evaporation crystallization is often ignored during preparation in the prior art, so that the crystallization rate is low.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the defects of the prior art are overcome, the steam enthalpy of different pressure sections is fully utilized to carry out multistage heating evaporation, the supersaturated ammonium sulfate solution and the crystal produced in the ammonium sulfate solution evaporation concentration process are cooled, and the ammonium sulfate is crystallized from the solution so as to prepare the ammonium sulfate fertilizer.
The technical scheme adopted by the invention for solving the technical problems is as follows: an evaporation crystallization method of ammonium sulfate solution comprises the following steps,
s1, performing primary evaporation through an evaporation tank, converting water in the ammonium sulfate solution into steam to be discharged, controlling that crystallization cannot be generated, and achieving the aim of preconcentration of the solution;
s2, performing secondary evaporation, concentration and crystallization to facilitate solid-liquid separation; meanwhile, the three-stage preheating tank absorbs heat in the steam condensate water of the first-stage evaporation tank, so that energy is saved;
s3, cooling and crystallizing in a cooling and crystallizing kettle, introducing cooling water into a jacket of the crystallizing kettle, crystallizing and separating out the ammonium sulfate solution in a supersaturated state through the change of temperature from high to low, after the ammonium sulfate solution is cooled to room temperature, because of no temperature change, the crystal separation is balanced, the cooling and crystallizing process is finished, the separated crystal is the ammonium sulfate, and the mother liquor returns to S1 to be evaporated and concentrated;
s4, washing with a small amount of clear water to obtain the ammonium sulfate solution crystal.
Preferably, in step S1, the steam pressure during the primary evaporation and the secondary evaporation is 0.4-0.6 MPA, preferably 0.5 MPA.
Preferably, in step S1, the primary evaporation concentration is 590-610 g/L.
Preferably, in step S1, the primary evaporation temperature is 60-110 ℃.
Preferably, in step S3, the room temperature is 15 ℃ to 25 ℃.
Preferably, in step S2, the secondary evaporation reduces the volume of the saturated solution by 40-60%.
The invention has the beneficial effects that: the vapor enthalpy of different pressure sections is fully utilized to carry out multi-stage heating evaporation, and the supersaturated ammonium sulfate solution and the crystal produced in the ammonium sulfate solution evaporation concentration process are cooled, so that the ammonium sulfate is crystallized from the solution; meanwhile, the heat is absorbed and recycled by adopting three stages and the hot stabs, so that the energy is saved.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1: an evaporation crystallization method of ammonium sulfate solution comprises the following steps,
s1, performing primary evaporation through an evaporation tank, converting water in the ammonium sulfate solution into steam to be discharged, controlling that crystallization cannot be generated, and achieving the aim of preconcentration of the solution;
s2, performing secondary evaporation, concentration and crystallization to facilitate solid-liquid separation; meanwhile, the three-stage preheating tank absorbs heat in the steam condensate water of the first-stage evaporation tank, so that energy is saved;
s3, cooling and crystallizing in a cooling and crystallizing kettle, introducing cooling water into a jacket of the crystallizing kettle, crystallizing and separating out the ammonium sulfate solution in a supersaturated state through the change of temperature from high to low, after the ammonium sulfate solution is cooled to room temperature, because of no temperature change, the crystal separation is balanced, the cooling and crystallizing process is finished, the separated crystal is the ammonium sulfate, and the mother liquor returns to S1 to be evaporated and concentrated;
s4, washing with a small amount of clear water to obtain the ammonium sulfate solution crystal.
In the present embodiment, in step S1, the primary evaporation and secondary evaporation process steam pressure is 05 MPA.
In the present embodiment, in step S1, the primary evaporation concentration is 590 g/L.
In the present embodiment, in step S1, the primary evaporation temperature is 80 ℃.
In the present embodiment, in step S3, the room temperature is 15 ℃.
In the present embodiment, in step S2, the secondary evaporation reduces the volume of the saturated solution by 40-60%.
Example 2: an evaporation crystallization method of ammonium sulfate solution comprises the following steps,
s1, performing primary evaporation through an evaporation tank, converting water in the ammonium sulfate solution into steam to be discharged, controlling that crystallization cannot be generated, and achieving the aim of preconcentration of the solution;
s2, performing secondary evaporation, concentration and crystallization to facilitate solid-liquid separation; meanwhile, the three-stage preheating tank absorbs heat in the steam condensate water of the first-stage evaporation tank, so that energy is saved;
s3, cooling and crystallizing in a cooling and crystallizing kettle, introducing cooling water into a jacket of the crystallizing kettle, crystallizing and separating out the ammonium sulfate solution in a supersaturated state through the change of temperature from high to low, after the ammonium sulfate solution is cooled to room temperature, because of no temperature change, the crystal separation is balanced, the cooling and crystallizing process is finished, the separated crystal is the ammonium sulfate, and the mother liquor returns to S1 to be evaporated and concentrated;
s4, washing with a small amount of clear water to obtain the ammonium sulfate solution crystal.
In the present embodiment, in step S1, the primary evaporation and secondary evaporation process steam pressure is 0.4 MPA.
In the present embodiment, in step S1, the primary evaporation concentration is 610 g/L.
In the present embodiment, in step S1, the primary evaporation temperature is 100 ℃.
In the present embodiment, in step S3, the room temperature is 23 ℃.
In the present embodiment, in step S2, the secondary evaporation reduces the volume of the saturated solution by 40-60%.
The present invention is not limited to the above embodiments, and various combinations and modifications of the above technical features may be provided for those skilled in the art, and modifications, variations, equivalents, or uses of the structure or method of the present invention in other fields without departing from the spirit and scope of the present invention are included in the protection scope of the present invention.
Claims (7)
1. An evaporation crystallization method of ammonium sulfate solution is characterized in that: comprises the following steps of (a) carrying out,
s1, performing primary evaporation through an evaporation tank, converting water in the ammonium sulfate solution into steam to be discharged, controlling that crystallization cannot be generated, and achieving the aim of preconcentration of the solution;
s2, performing secondary evaporation, concentration and crystallization to facilitate solid-liquid separation; meanwhile, the three-stage preheating tank absorbs heat in the steam condensate water of the first-stage evaporation tank and transmits the heat to the first-stage evaporation tank;
s3, cooling and crystallizing in a cooling and crystallizing kettle, introducing cooling water into a jacket of the crystallizing kettle, crystallizing and separating out the ammonium sulfate solution in a supersaturated state through the change of temperature from high to low, after the ammonium sulfate solution is cooled to room temperature, because of no temperature change, the crystal separation is balanced, the cooling and crystallizing process is finished, the separated crystal is the ammonium sulfate, and the mother liquor returns to S1 to be evaporated and concentrated;
s4, washing with a small amount of clear water to obtain the ammonium sulfate solution crystal.
2. The evaporative crystallization method of ammonium sulfate solution as set forth in claim 1, characterized in that: in step S1, the steam pressure in the primary evaporation and the secondary evaporation is 0.4-0.6 MPA.
3. The evaporative crystallization method of ammonium sulfate solution as set forth in claim 2, characterized in that: in step S1, the primary and secondary evaporation process steam pressure is 0.5 MPA.
4. The evaporative crystallization method of ammonium sulfate solution as set forth in claim 1, characterized in that: in step S1, the primary evaporation temperature is 60-110 ℃.
5. The evaporative crystallization method of ammonium sulfate solution as set forth in claim 1, characterized in that: in step S1, the primary evaporation concentration is 590-610 g/L.
6. The evaporative crystallization method of ammonium sulfate solution as set forth in claim 1, characterized in that: in step S2, the secondary evaporation reduces the volume of the saturated solution by 40-60%.
7. The evaporative crystallization method of ammonium sulfate solution as set forth in claim 1, characterized in that: in step S3, the room temperature is 15 ℃ to 25 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010775107.9A CN111977672A (en) | 2020-08-05 | 2020-08-05 | Ammonium sulfate solution evaporation crystallization method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010775107.9A CN111977672A (en) | 2020-08-05 | 2020-08-05 | Ammonium sulfate solution evaporation crystallization method |
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| CN111977672A true CN111977672A (en) | 2020-11-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010775107.9A Withdrawn CN111977672A (en) | 2020-08-05 | 2020-08-05 | Ammonium sulfate solution evaporation crystallization method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715966A (en) * | 2022-04-08 | 2022-07-08 | 广州市迈源科技有限公司 | Method for separating and purifying ammonium sulfate and ammonium dihydrogen phosphate in wastewater |
| CN114907149A (en) * | 2022-04-18 | 2022-08-16 | 昆明理工大学 | Method for improving quality of ammonium sulfate fertilizer by using ammonium persulfate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999326A (en) * | 2006-12-29 | 2007-07-18 | 中国天辰化学工程公司 | Production method of ammonium sulphate |
| CN101092266A (en) * | 2006-06-21 | 2007-12-26 | 中国石油化工股份有限公司 | Method for treating wastewater of dilute thiamine containing acrylonitrile |
| CN101439866A (en) * | 2008-12-24 | 2009-05-27 | 贵州省化工研究院 | Method for producing ammonium nitrate phosphate by decomposing phosphate ore using ammonium bisulfate and nitric acid |
| CN102390844A (en) * | 2011-08-08 | 2012-03-28 | 河北科技大学 | Preparation process of large-grain ammonium sulfate crystals |
| CN103496715A (en) * | 2013-10-22 | 2014-01-08 | 武汉科技大学 | Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization |
-
2020
- 2020-08-05 CN CN202010775107.9A patent/CN111977672A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092266A (en) * | 2006-06-21 | 2007-12-26 | 中国石油化工股份有限公司 | Method for treating wastewater of dilute thiamine containing acrylonitrile |
| CN100999326A (en) * | 2006-12-29 | 2007-07-18 | 中国天辰化学工程公司 | Production method of ammonium sulphate |
| CN101439866A (en) * | 2008-12-24 | 2009-05-27 | 贵州省化工研究院 | Method for producing ammonium nitrate phosphate by decomposing phosphate ore using ammonium bisulfate and nitric acid |
| CN102390844A (en) * | 2011-08-08 | 2012-03-28 | 河北科技大学 | Preparation process of large-grain ammonium sulfate crystals |
| CN103496715A (en) * | 2013-10-22 | 2014-01-08 | 武汉科技大学 | Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114715966A (en) * | 2022-04-08 | 2022-07-08 | 广州市迈源科技有限公司 | Method for separating and purifying ammonium sulfate and ammonium dihydrogen phosphate in wastewater |
| CN114907149A (en) * | 2022-04-18 | 2022-08-16 | 昆明理工大学 | Method for improving quality of ammonium sulfate fertilizer by using ammonium persulfate |
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Application publication date: 20201124 |