CN1554595A - Method for treating magnesium sulfate mather slution after producing boric acid by sulfuric acid method - Google Patents
Method for treating magnesium sulfate mather slution after producing boric acid by sulfuric acid method Download PDFInfo
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- CN1554595A CN1554595A CNA2003101208422A CN200310120842A CN1554595A CN 1554595 A CN1554595 A CN 1554595A CN A2003101208422 A CNA2003101208422 A CN A2003101208422A CN 200310120842 A CN200310120842 A CN 200310120842A CN 1554595 A CN1554595 A CN 1554595A
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- mother liquor
- ammonium sulfate
- magnesium
- sulfuric acid
- boric acid
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Abstract
The technological scheme of the present invention is the magnesium sulfate mother solution treating process including: heating the mother solution to 95-100 deg.c, adding solid ammonium sulfate into the mother solution to produce magnesium ammonium sulfate with the weight ratio between ammonium sulfate and magnesium sulfate being 1-1.4, filtering the produced solution, lowering the temperature to crystallize and separate magnesium ammonium sulfate, and drying. The said process needs no concentration while extracting over 80% of magnesium sulfate, and has fast production speed, low power consumption and low cost. In addition, the said process has reduced loss of barium and less environmental pollution. The produced magnesium ammonium sulfate is one excellent fertilizer with nitrogen, magnesium and sulfur.
Description
Technical field
The present invention relates to the treatment process of sal epsom mother liquor behind a kind of Production By Sulfuric Acid Process boric acid.
Background technology
Boric acid is a kind of purposes Chemicals very widely.At present, the industrial Production By Sulfuric Acid Process boric acid that generally uses is about to the boron magnesium slag and adds sulfuric acid and directly produce boric acid, also claims " single stage method ".In addition, big industrial production is also used " two-step approach " usually, promptly earlier produces borax (Na with boron ore powder
2B
4O
7.10H
2And then add sulfuric acid with borax and produce boric acid O)." two-step approach " complex process equipment, to produce investment big, and only propose the boron in the boron rock, and other compositions 80% or more become the slag public hazards entirely in the boron rock, both contaminate environment, and boron rock causes the cost height again less than comprehensive utilization, competitive power decline.Use sulfuric acid process to produce that boric acid technology is simple, less investment, scale is changeable, not only can propose the boron in the boron rock, and the magnesium oxide up to 40% that contains in the magnesium borate ore can be proposed, and slag is reduced in a large number, thereby can reduce cost greatly.
Yet using the topmost problem of Production By Sulfuric Acid Process boric acid is to produce a large amount of sal epsom mother liquors.At present, these mother liquors of industrial processing are generally used method of enrichment, whenever concentrate a mother liquor volume and subtract 1/3rd approximately, promptly need spissated sal epsom mother liquor to be real three times of producing the mother liquor amount.Therefore, the main man-hour of Production By Sulfuric Acid Process boric acid, institute's consuming electric power, heat energy and the hold facility overwhelming majority are to be used in the processing of sal epsom mother liquor.So the treatment process of sal epsom mother liquor is very big to the popularization influence of Production By Sulfuric Acid Process boric acid technology, also directly influences economic return.
Summary of the invention
Purpose of the present invention overcomes exactly uses more difficult this topmost problem of sal epsom mother liquor in the Production By Sulfuric Acid Process boric acid process, and the new treatment process of sal epsom mother liquor behind a kind of Production By Sulfuric Acid Process boric acid is provided.
The technical solution used in the present invention is: handle sal epsom mother liquor behind the Production By Sulfuric Acid Process boric acid by following technological process: at first described mother liquor is warming up to 95 ℃-105 ℃, an amount of solid ammonium sulfate (NH that adds in mother liquor
4)
2SO
4, the weight ratio of sal epsom is 1 in ammonium sulfate and the mother liquor: 1-1.4: 1, and make its dissolving and reaction generate ammonium sulfate magnesium (NH
4)
2SO
4MgO.6H
2O lowers the temperature behind the liquid filtering that reaction is generated, the ammonium sulfate magnesium (NH that crystallization is separated out
4)
2SO
4MgO.6H
2O dries and dries processing.
The treatment process beneficial effect of sal epsom mother liquor is behind this Production By Sulfuric Acid Process boric acid provided by the invention:
1. production rate is fast, consumption coal, little power consumption.
It is to add ammonium sulfate behind the sal epsom mother liquor elevated temperature, and dissolving finishes and can decrease temperature crystalline go out ammonium sulfate magnesium, puies forward the magnesium rate up to more than 80%, and the solution that will carry again behind the magnesium returns reactor as decomposing breeze.No longer adopt the traditional method of concentrated vitriol mother liquid of magnesium, accelerated production rate, economize coal, power saving, reduced cost.
2. the mother liquor treatment capacity is few.
Compare with method of enrichment, the sal epsom mother liquor amount that its is handled has not only improved production rate less than half of method of enrichment, has also saved equipment.
3. crystallization velocity is fast.
What use the method for enrichment output is sal epsom, can generate supersaturated solution in the concentration process, make crystallization slowly, not thorough, often will adds crystal seed for this reason and prolong crystallization time, and there are not the problems referred to above in the method for using the present invention to carry magnesium.
4. mistake boron is few, pollution is few.
Boron is very easy in the steam volatilization, and the present invention puies forward the magnesium method does not need concentrated mother liquor, does not have the mistake boron and the pollution of this respect.
5. owing to do not concentrate, it is big not to be afraid of the mother liquor amount, so can be fully used in a large amount of low-grade boron magnesium ore deposit.
6. the ammonium sulfate magnesium (NH that obtains after the sal epsom mother liquor is handled
4)
2SO
4MgO.6H
2O is a good nitrogen, magnesium amd sulphur fertilizer on a kind of agricultural
Embodiment:
Under room temperature (20-25 ℃) condition, general pH value is 2-2.5 with the sal epsom mother liquor that produces behind the Production By Sulfuric Acid Process boric acid, and the sulfur acid magnesium density is 270-315kg/m
3, boron oxide B
2O
3Content is 14kg/m
3
Embodiment 1:
Use the sulfur acid magnesium density to be 315kg/m
3The sal epsom mother liquor, adopt following processing step to handle:
(1) at first with described mother liquor heat temperature raising to 95 ℃;
(2) add solid ammonium sulfate in described mother liquor, the weight ratio of ammonium sulfate and sal epsom is 1: 1, makes its dissolving back stand-by;
(3) liquid that step (2) is generated uses plate-and-frame filter press to filter under normal pressure, removes impurity, and filtration temperature is 95 ℃;
(4) with the aforesaid liquid cooling, ammonium sulfate magnesium is separated out in crystallization;
The ammonium sulfate magnesium of (5) crystallization being separated out dries and dries processing, after the drying crystalline ammonium sulfate magnesium is packed;
(6) will remain the reactor that mother liquor returns Production By Sulfuric Acid Process boric acid.
Experiment shows that the extraction yield of sal epsom is 69% under these conditions.
Embodiment 2:
Use the sulfur acid magnesium density to be 270kg/m
3The sal epsom mother liquor, adopt following processing step to handle:
(1) at first with described mother liquor heat temperature raising to 98 ℃;
(2) add solid ammonium sulfate in described mother liquor, the weight ratio of ammonium sulfate and sal epsom is 1.2: 1, makes its dissolving back stand-by;
(3) liquid that step (2) is generated uses plate-and-frame filter press to filter under normal pressure, removes impurity, and filtration temperature is 96 ℃;
(4) with the aforesaid liquid cooling, ammonium sulfate magnesium is separated out in crystallization;
The ammonium sulfate magnesium of (5) crystallization being separated out dries and dries processing, after the drying crystalline ammonium sulfate magnesium is packed;
(6) will remain the reactor that mother liquor returns Production By Sulfuric Acid Process boric acid.
Experiment shows that the extraction yield of sal epsom is 83% under these conditions.
Embodiment 3:
Use the sulfur acid magnesium density to be 276kg/m
3The sal epsom mother liquor, adopt following processing step to handle:
(1) at first with described mother liquor heat temperature raising to 100 ℃;
(2) add solid ammonium sulfate in described mother liquor, the weight ratio of ammonium sulfate and sal epsom is 1.4: 1, makes its dissolving back stand-by;
(3) liquid that step (2) is generated uses plate-and-frame filter press to filter under normal pressure, removes impurity, and filtration temperature is 98 ℃;
(4) with the aforesaid liquid cooling, ammonium sulfate magnesium is separated out in crystallization;
The ammonium sulfate magnesium of (5) crystallization being separated out dries and dries processing, after the drying crystalline ammonium sulfate magnesium is packed;
(6) will remain the reactor that mother liquor returns Production By Sulfuric Acid Process boric acid.
Experiment shows that the extraction yield of sal epsom is 93% under these conditions.
More embodiment show, as long as the sal epsom mother liquor behind the Production By Sulfuric Acid Process boric acid is heated more than 95 ℃, in mother liquor, add solid ammonium sulfate, the weight ratio of ammonium sulfate and sal epsom is 1: 1-1.4.: 1, filtration temperature is not less than 95 ℃, in case crystallization before filtering all can obtain the sal epsom extraction yield in the better result more than 80%.Under the constant situation of the processing condition of using such as sal epsom mother liquor sulfur acid magnesium density, mother liquor Heating temperature and filtration temperature, suitably increase the ratio that adds solid ammonium sulfate, the sal epsom extraction yield increases to some extent, certainly, too much strengthen the ratio that adds solid ammonium sulfate, then can cause the waste of ammonium sulfate raw material and man-hour and equipment.
Claims (3)
1. the treatment process of sal epsom mother liquor behind the Production By Sulfuric Acid Process boric acid is characterized in that comprising following processing step:
(1) mother liquor behind the Production By Sulfuric Acid Process boric acid is placed in the container, heat to 95 ℃-100 ℃;
(2) add solid ammonium sulfate in described mother liquor, the weight ratio of sal epsom is 1 in ammonium sulfate and the mother liquor: 1-1.4: 1, and make its dissolving back stand-by;
(3) liquid filtering that step (2) is generated is removed impurity;
(4) with the aforesaid liquid cooling, ammonium sulfate magnesium is separated out in crystallization;
The ammonium sulfate magnesium of (5) crystallization being separated out dries and dries processing, after the drying crystalline ammonium sulfate magnesium is packed;
(6) will remain the reactor that mother liquor returns Production By Sulfuric Acid Process boric acid.
2. the treatment process of sal epsom mother liquor behind the Production By Sulfuric Acid Process boric acid according to claim 1 is characterized in that the concentration of sal epsom mother liquor sulfur acid magnesium is 270-315kg/m behind the described Production By Sulfuric Acid Process boric acid
3
3. the treatment process of sal epsom mother liquor behind the Production By Sulfuric Acid Process boric acid according to claim 1 is characterized in that the described filtration of step (3), is to carry out under normal pressure, and the temperature of liquid must not be lower than 95 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310120842 CN1251968C (en) | 2003-12-30 | 2003-12-30 | Method for treating magnesium sulfate mather slution after producing boric acid by sulfuric acid method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310120842 CN1251968C (en) | 2003-12-30 | 2003-12-30 | Method for treating magnesium sulfate mather slution after producing boric acid by sulfuric acid method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1554595A true CN1554595A (en) | 2004-12-15 |
| CN1251968C CN1251968C (en) | 2006-04-19 |
Family
ID=34338318
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310120842 Expired - Fee Related CN1251968C (en) | 2003-12-30 | 2003-12-30 | Method for treating magnesium sulfate mather slution after producing boric acid by sulfuric acid method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232048A (en) * | 2013-05-07 | 2013-08-07 | 中国科学院青海盐湖研究所 | Process for recovering magnesium sulfate monohydrate from boron extraction mother liquor |
| CN104947154A (en) * | 2015-07-08 | 2015-09-30 | 长沙矿冶研究院有限责任公司 | Method for demagging anolyte of electrolytic manganese |
| CN105040038A (en) * | 2015-07-08 | 2015-11-11 | 长沙矿冶研究院有限责任公司 | Method for carrying out demagging on electrolytic manganese anolyte with ammonium sulfate |
| CN108164046A (en) * | 2018-01-17 | 2018-06-15 | 郑州轻工业学院 | A kind of method that high-concentration ammonia nitrogenous wastewater and recycling are handled with desulfurization wastewater |
| CN109133127A (en) * | 2017-06-17 | 2019-01-04 | 新疆丰泰化工科技有限公司 | A kind for the treatment of process of ammonia process of desulfurization waste liquid |
| CN110921691A (en) * | 2019-12-05 | 2020-03-27 | 安徽皖东树脂科技有限公司 | Treatment process of mother liquor pigment in magnesium sulfate production |
| CN116081660A (en) * | 2023-02-22 | 2023-05-09 | 西南科技大学 | Preparation method of hydrated ammonium sulfate salt |
-
2003
- 2003-12-30 CN CN 200310120842 patent/CN1251968C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232048A (en) * | 2013-05-07 | 2013-08-07 | 中国科学院青海盐湖研究所 | Process for recovering magnesium sulfate monohydrate from boron extraction mother liquor |
| CN104947154A (en) * | 2015-07-08 | 2015-09-30 | 长沙矿冶研究院有限责任公司 | Method for demagging anolyte of electrolytic manganese |
| CN105040038A (en) * | 2015-07-08 | 2015-11-11 | 长沙矿冶研究院有限责任公司 | Method for carrying out demagging on electrolytic manganese anolyte with ammonium sulfate |
| CN105040038B (en) * | 2015-07-08 | 2017-07-07 | 长沙矿冶研究院有限责任公司 | The method for carrying out demagging to electrolytic manganese anolyte using ammonium sulfate |
| CN109133127A (en) * | 2017-06-17 | 2019-01-04 | 新疆丰泰化工科技有限公司 | A kind for the treatment of process of ammonia process of desulfurization waste liquid |
| CN108164046A (en) * | 2018-01-17 | 2018-06-15 | 郑州轻工业学院 | A kind of method that high-concentration ammonia nitrogenous wastewater and recycling are handled with desulfurization wastewater |
| CN110921691A (en) * | 2019-12-05 | 2020-03-27 | 安徽皖东树脂科技有限公司 | Treatment process of mother liquor pigment in magnesium sulfate production |
| CN110921691B (en) * | 2019-12-05 | 2022-04-22 | 安徽皖东树脂科技有限公司 | Treatment process of mother liquor pigment in magnesium sulfate production |
| CN116081660A (en) * | 2023-02-22 | 2023-05-09 | 西南科技大学 | Preparation method of hydrated ammonium sulfate salt |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1251968C (en) | 2006-04-19 |
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