CN101367533A - Process for preparing magnesium sulphate heptahydrate in treatment of industrial waste sulphuric acid liquid - Google Patents
Process for preparing magnesium sulphate heptahydrate in treatment of industrial waste sulphuric acid liquid Download PDFInfo
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- CN101367533A CN101367533A CNA2007100260935A CN200710026093A CN101367533A CN 101367533 A CN101367533 A CN 101367533A CN A2007100260935 A CNA2007100260935 A CN A2007100260935A CN 200710026093 A CN200710026093 A CN 200710026093A CN 101367533 A CN101367533 A CN 101367533A
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- magnesium sulfate
- flocculation agent
- sulfate heptahydrate
- magnesia
- solution
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Abstract
The invention provides a method for producing the magnesium sulfate heptahydrate, which is characterized in that the waste sulfuric acid that is generated in the sulfonation alkaline fusion process is adopted as the raw material; the waste sulfuric acid solution is mixed with magnesia, so that the ion exchanging reaction can be adequately performed; after the adequate reaction, flocculating agent is adopted for precipitation, foreign matters removal and the color removal, and then the solution is compressed and filtered by a framework to get the magnesium sulfate clear solution; the magnesium sulfate clear solution is cooled down, crystallized and centrifugally filtered to get the solid magnesium sulfate heptahydrate. The method not only resolves the problems of the vast discharging of the waste sulfuric acid, but also can produce the product of the magnesium sulfate from the waste sulfuric acid solution; moreover, the method has less investment, simple craftwork and high recycling rate, thereby having remarkable social benefit and economic benefit.
Description
Technical field
The invention provides a kind of production method of novel magnesium sulfate heptahydrate.It is characterized in that utilizing the sulfur waste acid that produces in the sulfonation alkali fusion process as the raw material production magnesium sulfate heptahydrate.
Background technology
Present method invention is to produce a large amount of sulfur waste acid in industrial production m-Salicylic acid, 4-xenol sulfonation alkali fusion process, and a large amount of sulfur waste acid is if will bring very big environmental issue without handling.
Summary of the invention
In order to handle these sulfur waste acid, the technical scheme that present method invention is adopted is to utilize magnesia and sulfuric acid fully to carry out the method for ion exchange reaction, make it to generate sal epsom and sal epsom has 7 crystal water in the time of crystalline, so just can sponge the most of water in the sulfur waste acid, adopt flocculation agent to help in addition and coagulate the effect of settling that has obviously improved later waste water, and the COD and the chromaticity index of water also improves significantly after handling.It is neutral that its waste water is, and COD value compliance with environmental protection requirements can directly be discharged, thereby make sulfur waste acid obtain recycling, and solved a large amount of useless vitriolic emission problems, reduced the pollution to environment.
Wherein: the method includes the steps of:
1, the ion exchange reaction step is to add in the sulfur waste acid of 25-30% to contain 85% magnesian magnesia to concentration, makes its generation sal epsom that fully reacts completely, and regulates pH value 7～8.Its chemical reaction is:
MgO+H
2SO
4→MgSO
4+H
2O
MgSO
4+7H
2O→MgSO
4·7H
2O
2, flocculation agent sedimentation, removal of impurities, decolouring step add a certain amount of flocculation agent in the solution that has reacted, so that remove mud and other mechanical impurity in the magnesia, can obviously improve effect of settling later through helping with fixed attention of flocculation agent.And COD and the chromaticity index of handling back water also can improve significantly.
3, press filtration step will be mixed with the solution of flocculation agent, throw plate-and-frame filter press into high-pressure pump, slough flocculation agent, mud and other mechanical impurity.
4, cooling crystallization step filter press is isolated filter residue, obtains sal epsom filtrate, and gained filtrate is separated out crystal through naturally cooling.
5, centrifuging step places whizzer to filter aforesaid liquid can obtain the magnesium sulfate heptahydrate crystal.
6, dry packaging step and the wet magnesium sulfate heptahydrate crystal of centrifuging gained was both dried to obtain the exsiccant magnesium sulfate heptahydrate, can obtain finished product after the packing.
The inventive method has not only solved a large amount of useless vitriolic emission problems, and can make the sal epsom product from waste sulfuric acid, moreover the inventive method less investment technology is simple, the rate of recovery is high, therefore has remarkable social benefit and certain economic benefits.
Description of drawings
Figure is simple process figure of the present invention
Embodiment
Embodiment one:
Following case description summary of the invention of the present invention.The spent acid that this example produces in utilize producing m-Salicylic acid, 4-xenol sulfonation alkali fusion process is such as the technology of raw material production magnesium sulfate heptahydrate: get concentration and be 30% sulfonation alkali fusion sulfur waste acid 1388g and put into the 2000ml round-bottomed flask that has stirring, slowly add and contain 85% magnesian magnesia 200g, stir 30min, conditioned reaction liquid PH makes it become 7, continues to stir it is fully reacted.Question response finishes and adds the poly-silicon aluminium chloride ferrum of 0.1g in the reactor and carry out sedimentation, removal of impurities, decolouring, stirs 15min, and filter and obtain the filter residue cationic polyacrylamide, and the mud of removing through sedimentation, mechanical impurity.Mother liquid obtained naturally cooling is separated out crystal, filters to obtain magnesium sulfate heptahydrate white crystal 1045.5g.
Embodiment two:
Add concentration and be 30% sulfonation alkali fusion sulfur waste acid 120L and 59.8kg in the 200L reactor and contain 85% magnesian magnesia, open and stir, make its reaction 1 hour, conditioned reaction liquid PH makes it become 7, continues to stir it is fully reacted.Treat that fully effect back adding 12g cationic polyacrylamide in the reaction solution carries out sedimentation, removal of impurities, decolouring, to be mixed with the solution of cationic polyacrylamide behind the stirring 30min, throw plate-and-frame filter press into high-pressure pump, the mud of sloughing cationic polyacrylamide and removing through sedimentation, mechanical impurity.Filter press is isolated filter residue 10.47kg, sal epsom filtrate 312.6kg, and gained filtrate is separated out crystal through naturally cooling.The magnesium sulfate heptahydrate crystal that above-mentioned mixed solution is placed whizzer to filter can to obtain wetting both dried and can obtain the exsiccant magnesium sulfate heptahydrate, can obtain finished product after the packing.
Claims (2)
- In the improvement of industrial waste sulfuric acid solution, produce the technology of magnesium sulfate heptahydrate, it is characterized in that:1, utilize the spent acid that produces in the sulfonation alkali fusion process as the raw material production magnesium sulfate heptahydrate.2, handle sulfur waste acid and can adopt the wherein preferred magnesia in magnesia, magnesite, boron magnesium ore deposit.3, according to the method for claim 1, present method invention mainly comprises following steps:The ion exchange reaction step is to add in the sulfur waste acid of 25-30% to contain 85% magnesian magnesia to concentration, makes its generation sal epsom that fully reacts completely, and regulates pH value to 7～8.Flocculation agent sedimentation, removal of impurities, decolouring step add a certain amount of flocculation agent in the solution that has reacted, so that remove mud and other mechanical impurity in the magnesia, can obviously improve effect of settling later through helping with fixed attention of flocculation agent.And COD and the chromaticity index of handling back water also can improve significantly.The press filtration step will be mixed with the solution of flocculation agent, throw plate-and-frame filter press into high-pressure pump, slough flocculation agent, mud and other mechanical impurity.Cooling crystallization step filter press is isolated filter residue, obtains sal epsom filtrate, and gained filtrate is separated out crystal through naturally cooling.The centrifuging step places whizzer to filter aforesaid liquid can obtain the magnesium sulfate heptahydrate crystal.Dry packaging step and the wet magnesium sulfate heptahydrate crystal of centrifuging gained was both dried to obtain the exsiccant magnesium sulfate heptahydrate, can obtain finished product after the packing.
- 4. employing flocculation agent according to claim 3 carries out sedimentation, removal of impurities, decolouring step, and the flocculation agent that is adopted can be polyacrylamide (PAM), polymerize aluminum chloride (PAC), ferric-aluminum chloride, poly-silicon aluminum chloride (PASC), polymeric aluminum sulfate silicate (PASS), poly-silicon iron(ic) chloride (PFSC), ferric sulfate of polymerized silica (PFSS), poly-silicon aluminium chloride ferrum (PAFSC) and polymeric aluminum sulfate silicate iron (PAFSS).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100260935A CN101367533A (en) | 2007-08-16 | 2007-08-16 | Process for preparing magnesium sulphate heptahydrate in treatment of industrial waste sulphuric acid liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100260935A CN101367533A (en) | 2007-08-16 | 2007-08-16 | Process for preparing magnesium sulphate heptahydrate in treatment of industrial waste sulphuric acid liquid |
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| CN101367533A true CN101367533A (en) | 2009-02-18 |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219722A (en) * | 2011-07-27 | 2011-10-19 | 上海哈勃化学技术有限公司 | Production technology of high purity peroxyacetic acid |
| CN102320636A (en) * | 2011-08-31 | 2012-01-18 | 四川宜宾县天源离子交换树脂厂 | Magnesium sulfate heptahydrate production method utilizing waste sulfuric acid from production of cation exchange resin |
| CN102320635A (en) * | 2011-06-16 | 2012-01-18 | 青岛奥盖克化工有限公司 | Comprehensive utilization method of waste sulfuric acid of sulfonated products |
| CN102476818A (en) * | 2010-11-26 | 2012-05-30 | 江油市雄晖化工厂 | Method for comprehensively utilizing waste acid and waste alkali for producing high-purity magnesium sulfate |
| CN101698491B (en) * | 2009-08-17 | 2012-10-17 | 陈玉芳 | Magnesium sulfate and manufacturing method thereof |
| CN103254417A (en) * | 2013-05-27 | 2013-08-21 | 南京先声合成材料有限公司溧水分公司 | Polyether filter residue effective component extraction method |
| CN103641568A (en) * | 2013-12-11 | 2014-03-19 | 青岛奥盖克化工股份有限公司 | Comprehensive treatment method for waste sulfuric acid of sulfonated products |
| CN104310447A (en) * | 2014-09-28 | 2015-01-28 | 易科力（天津）环保科技发展有限公司 | Green recovery treatment method of 1,4-dihydroxy anthraquinone waste sulfuric acid |
| CN107473436A (en) * | 2017-08-08 | 2017-12-15 | 江苏建亚环保科技股份有限公司 | The method of coloured Waste Sulfuric Acid production magnesium sulfate in being produced using ion exchange resin |
| CN108101078A (en) * | 2018-01-31 | 2018-06-01 | 四川思达能环保科技有限公司 | A kind of process system and method with boron magnesium mud production epsom salt |
| CN109809447A (en) * | 2019-03-27 | 2019-05-28 | 宋纯 | The recovery method of Waste Sulfuric Acid |
| 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 |
| CN110963510A (en) * | 2020-01-13 | 2020-04-07 | 山东齐创石化工程有限公司 | Recovery processing device and process for waste sulfuric acid |
| CN112758966A (en) * | 2020-12-30 | 2021-05-07 | 莱州市中大贵合化工有限公司 | Production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment |
-
2007
- 2007-08-16 CN CNA2007100260935A patent/CN101367533A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698491B (en) * | 2009-08-17 | 2012-10-17 | 陈玉芳 | Magnesium sulfate and manufacturing method thereof |
| CN102476818A (en) * | 2010-11-26 | 2012-05-30 | 江油市雄晖化工厂 | Method for comprehensively utilizing waste acid and waste alkali for producing high-purity magnesium sulfate |
| CN102320635A (en) * | 2011-06-16 | 2012-01-18 | 青岛奥盖克化工有限公司 | Comprehensive utilization method of waste sulfuric acid of sulfonated products |
| CN102219722A (en) * | 2011-07-27 | 2011-10-19 | 上海哈勃化学技术有限公司 | Production technology of high purity peroxyacetic acid |
| CN102320636A (en) * | 2011-08-31 | 2012-01-18 | 四川宜宾县天源离子交换树脂厂 | Magnesium sulfate heptahydrate production method utilizing waste sulfuric acid from production of cation exchange resin |
| CN103254417A (en) * | 2013-05-27 | 2013-08-21 | 南京先声合成材料有限公司溧水分公司 | Polyether filter residue effective component extraction method |
| CN103641568B (en) * | 2013-12-11 | 2015-04-15 | 青岛奥盖克化工股份有限公司 | Comprehensive treatment method for waste sulfuric acid of sulfonated products |
| CN103641568A (en) * | 2013-12-11 | 2014-03-19 | 青岛奥盖克化工股份有限公司 | Comprehensive treatment method for waste sulfuric acid of sulfonated products |
| CN104310447A (en) * | 2014-09-28 | 2015-01-28 | 易科力（天津）环保科技发展有限公司 | Green recovery treatment method of 1,4-dihydroxy anthraquinone waste sulfuric acid |
| CN107473436A (en) * | 2017-08-08 | 2017-12-15 | 江苏建亚环保科技股份有限公司 | The method of coloured Waste Sulfuric Acid production magnesium sulfate in being produced using ion exchange resin |
| CN108101078A (en) * | 2018-01-31 | 2018-06-01 | 四川思达能环保科技有限公司 | A kind of process system and method with boron magnesium mud production epsom salt |
| CN108101078B (en) * | 2018-01-31 | 2023-07-25 | 四川思达能环保科技有限公司 | Process system and method for producing magnesium sulfate heptahydrate by using boron-magnesium mud |
| CN109809447A (en) * | 2019-03-27 | 2019-05-28 | 宋纯 | The recovery method of Waste Sulfuric Acid |
| 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 |
| CN110963510A (en) * | 2020-01-13 | 2020-04-07 | 山东齐创石化工程有限公司 | Recovery processing device and process for waste sulfuric acid |
| CN112758966A (en) * | 2020-12-30 | 2021-05-07 | 莱州市中大贵合化工有限公司 | Production process of magnesium sulfate heptahydrate and magnesium sulfate heptahydrate production equipment |
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Open date: 20090218 |