CN1137488A - Process for preparing magnesium sulfate by using chlorine alkali offscum salt slurry - Google Patents
Process for preparing magnesium sulfate by using chlorine alkali offscum salt slurry Download PDFInfo
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- CN1137488A CN1137488A CN95111658A CN95111658A CN1137488A CN 1137488 A CN1137488 A CN 1137488A CN 95111658 A CN95111658 A CN 95111658A CN 95111658 A CN95111658 A CN 95111658A CN 1137488 A CN1137488 A CN 1137488A
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- salt slurry
- offscum
- sal epsom
- sulfuric acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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Abstract
The present invention discloses a technological process for preparing magnesium sulfate by using waste sludge, and is characterized by that sulfuric acid is added in sludge to produce magnesium sulfate. Its advantage is elimination of three wastes in the course of whole production and change of the wastes into useful substances, free from secondary pollution, so that it is applicable to comprehensive utilization of chlorine alkali industry.
Description
The invention belongs to the comprehensive utilization of chlorine alkali offscum salt slurry, especially utilize composition magnesium hydroxide in the salt slurry to be converted into the industrial method of sal epsom.
Salt slurry in the chlorine industry, its comprehensive utilization is the problem that manufacturer pays close attention to for a long time always, some producers have changed the way of direct discharging and have adopted the press filtration recovered brine, and the salt slurry filter cake is used to banket and the research of aspects such as cement baking, brick and inorganic fiberboard report.Reclaim wherein effective ingredient production chemical product as for salt slurry do chemical treatment, as produce magnesium, Magnesium Carbonate Light 41-45, barium sulfate also because of complex process, production cost is higher relatively, benefit is also undesirable, add the various reasons that ion interference is above-mentioned, make these research projects fail to make one's wish fulfilled, and do not have bibliographical information to produce sal epsom so far.
The purpose of this invention is to provide the method that a kind of technology is simple, non-secondary pollution can fully be converted into the magnesium hydroxide in the salt slurry magnesium sulfate heptahydrate.
The object of the present invention is achieved like this, adds sulfuric acid by chlorine alkali offscum salt slurry and produce sal epsom.
In order to improve the transformation efficiency of salt slurry, controlling suitable condition, to produce sal epsom be necessary, be specially: in reactor, add tap water or tap water and mother liquor, under agitation slowly add salt slurry, add sulfuric acid by proportioning then, salt slurry and sulfuric acid weight and volume proportioning are 1: 2～3.5, control reaction temperature is 50～80 ℃, becomes orange until the reaction solution color by native white, and PH is 3～6, reaction solution proportion is till 1.16～1.25, i.e. reaction is finished; Reactor internal reaction liquid concentrates after filtering, thickening temperature is 100～110 ℃, until the concentrated solution color become by orange light yellow till, measure Bo Midu and be at least 32 ° of B, concentrated solution is through crystallisation by cooling, drying is product, and mother liquor remaining after the crystallization is reused as the salt slurry thinner, thereby reaches non-secondary pollution.
The present invention is owing to adopt chemical process that one of " three wastes " in chlorine industry salt slurry is become available sal epsom, and sal epsom is of many uses, as cotton, the weighting agent of silk and the filler of kapok goods, also be used for the manufacturing of process hides, fire-retardant material, on agricultural, can be converted into fertilizer.And when salt slurry is converted into sal epsom, also can produce the calcium sulfate of slagging tap, as the manufacture of cement additive.Therefore present method has elimination " three wastes " and no longer produces new " three wastes " source of pollution.The transformation efficiency height of present method reaches between 60～80%, and it is fertile as farming that sal epsom can make ammonium sulfate magnesium.
Describe the present invention below in conjunction with embodiment and experimental data.
Embodiment:
The present invention adopts 7 experimental example to illustrate that chlorine alkali offscum salt slurry produces sal epsom, concrete data are shown in subordinate list, its reactant salt slurry and sulfuric acid ratio are with the weight and volume ratio, used vitriolic concentration can be 5～50%, 20% sulfur waste acid is all adopted in this experiment, the sulfuric acid concentration height, then just with few, it is too acutely inapplicable that sulfuric acid concentration is higher than 50% reaction for the sulfuric acid volume.Whether the present invention mainly is a control reaction solution pH value, control reaction and finish, and the present invention adds tap water or tap water and mother liquor in reactor, under agitation add salt slurry then, salt slurry fully is dispersed in wherein, press 7 proportionings on the subordinate list then respectively, slowly add sulfuric acid, slow earlier back is fast, and controlled temperature is 50 ℃ respectively, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, do seven experiments for 80 ℃, on PH that reaction terminating is measured and solution proportion are seen attached list; Filter then, filtrate concentrates, and thickening temperature and time have 7 to see attached list, the Bo Midu of final concentrated solution is all more than or equal to 32 ° of B, final filtrate cooling is obtained the product of seven differentiated yields from crystallization, and these seven products all reach national industrial first grade after measured.By above-mentioned seven experiments as can be known, control reaction solution PH is 3～6, the assaying reaction liquor ratio heavily is 1.16～1.25, thickening temperature is 100～110 ℃, the final fluid wave rice degree that concentrates is 32 ° more than the B, the sal epsom crystallization transformation efficiency of then producing is all very up to 68%～71.5%, and product is national industrial first grade.And PH is 5 o'clock, and then economic benefit is best, i.e. optimum point.The present invention is the crystallization filtrated stock, recycling, thereby secondary pollution does not appear, and eliminate three industrial wastes, reach environmental requirement.
The present invention utilizes the method for chlorine alkali offscum salt slurry system sal epsom, be useful for sediment---the salt slurry that produces before sea salt, lake salt, the rock salt refined brine, its composition contains magnesium oxide more than 15～50%, just produce value, turn waste into wealth thereby reach comprehensive utilization, no longer reappear the remarkable society and the economic benefits of " three wastes ".Now tabulate relevant testing data as follows.
Subordinate list: salt slurry is produced the sal epsom testing data
| Numbering | Salt slurry and sulfuric acid ratio | Temperature of reaction | PH value | Solution proportion | Thickening temperature and time | Transformation efficiency | Detect unit and result |
| Examination-1 | ?0.5Kg∶1.3L | ????50℃ | ??3 | ????1.16 | ?100℃?1.5h | ???68％ | Get through the Fujian Province Agriculture InstituteSoil and Fertilizer Institute and to mix sample determination Mg% 9.64 MgSO as a result 4％?47.38 ?MgSO 4·7H 2O％97.0 |
| Examination-2 examinations-3 | ?0.5Kg∶1.3L ?0.5Kg∶1.3L | ????55℃ ????????60℃ | ??3.5 ??4 | ????1.18 ????1.19 | ?100℃?1.2h ?105℃?1h | ???69％ ???69％ | |
| Examination-4 examinations-5 | ?0.5Kg∶1.4L ?1Kg∶2.4L | ????65℃ ????????70℃ | ??4.5 ??5 | ????1.22 ????1.23 | ?110℃?0.8h ?105℃?1h | ???70.5％ ???70.6％ | |
| Examination-6 examinations-7 | ?1Kg∶2.4L ?1Kg∶2.4L | ????75℃ ????????80℃ | ??5.5 ??6 | ????1.23 ????1.24 | ?105℃?0.7h ?110℃?0.5h | ???70.9％ ???71.5％ |
Mud is raw material.
Its sulfur waste acid is by very, and the salt slurry major ingredient is as follows: (with the salt qualitative changeization)
Magnesium oxide 43.61% calcium oxide 10.07%
Aluminum oxide 3.24% silicon oxide 7.90%
Other impurity surplus
Claims (3)
1, a kind of technology of utilizing chlorine alkali offscum salt slurry to produce sal epsom is characterized in that the salt slurry adding sulfuric acid of chlor-alkali waste residue is produced sal epsom.
2, the technology of utilizing chlorine alkali offscum salt slurry to produce sal epsom according to claim 1, it is characterized in that salt slurry is with tap water or tap water and mother liquor dilution, slowly add the sulfuric acid that concentration is 5-50%, its temperature of reaction is 50～80 ℃, until reaction solution PH is 3-6, proportion is 1.16～1.25, and reaction is finished; Filter then, filter residue is as cement additire, and filtrate concentrates under 100～110 ℃ of temperature, until become by orange light yellow till, measure Bo Midu and be at least 32 ° of B, crystallisation by cooling then, drying is product, and the mother liquor after the crystallization recycles as the salt slurry thinner.
3, the technology of utilizing chlorine alkali offscum salt slurry to produce sal epsom according to claim 1 and 2, it is characterized in that salt slurry adds sulfuric acid reaction after, its reaction solution optimum control PH is 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95111658A CN1137488A (en) | 1995-06-08 | 1995-06-08 | Process for preparing magnesium sulfate by using chlorine alkali offscum salt slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95111658A CN1137488A (en) | 1995-06-08 | 1995-06-08 | Process for preparing magnesium sulfate by using chlorine alkali offscum salt slurry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1137488A true CN1137488A (en) | 1996-12-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN95111658A Pending CN1137488A (en) | 1995-06-08 | 1995-06-08 | Process for preparing magnesium sulfate by using chlorine alkali offscum salt slurry |
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| CN (1) | CN1137488A (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823738A (en) * | 2010-04-30 | 2010-09-08 | 汪晋强 | Method for co-production of fine calcium carbonate and sodium silicate, in preparation of light magnesium carbonate by chlor-alkali brine sludge |
| CN101823736A (en) * | 2010-04-30 | 2010-09-08 | 汪晋强 | Method for co-production of calcium carbonate and sodium silicate in preparation of light magnesium carbonate by chlor-alkali brine sludge |
| CN101830493A (en) * | 2010-04-30 | 2010-09-15 | 汪晋强 | Method for processing waste salt slurry of calcined soda with sodium carbonate and sodium sulfate |
| CN102040250A (en) * | 2010-11-17 | 2011-05-04 | 辽宁工程技术大学 | Method for comprehensively utilizing chlor-alkali salt sludge |
| CN101624204B (en) * | 2009-01-12 | 2011-05-18 | 王嘉兴 | Four-great circulation method formed by waste gypsum mud and chlor-alkali industry |
| 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 |
| CN104402024A (en) * | 2014-10-24 | 2015-03-11 | 陕西华陆化工环保有限公司 | Method using salty mud to prepare lightweight magnesium oxide |
| CN107082653A (en) * | 2017-05-16 | 2017-08-22 | 四川金象赛瑞化工股份有限公司 | A kind of utilization calcium and magnesium mud is the method that raw material prepares moderate-element Liquid Fertilizer |
| CN108793208A (en) * | 2018-07-17 | 2018-11-13 | 莘县华祥盐化有限公司 | A kind of technique of salt slurry and spent acid comprehensive utilization production magnesium sulfate |
| CN111115666A (en) * | 2020-01-09 | 2020-05-08 | 西安交通大学 | Reduction treatment process for salt mud in chlor-alkali industry |
| CN111204780A (en) * | 2020-01-09 | 2020-05-29 | 西安交通大学 | Resource utilization process of salt mud in chlor-alkali industry |
| CN112429896A (en) * | 2020-10-29 | 2021-03-02 | 河南佰利联新材料有限公司 | Treatment method of salt mud produced in chlor-alkali production |
| CN114538486A (en) * | 2022-02-22 | 2022-05-27 | 西安交通大学 | Magnesium recovery method and system based on chlor-alkali salt mud |
| CN115286024A (en) * | 2022-08-30 | 2022-11-04 | 上海言征分离技术有限公司 | Resource recycling method and system for salt mud produced by chlor-alkali |
| CN115353132A (en) * | 2022-09-23 | 2022-11-18 | 西安交通大学 | Preparation method and system of magnesium sulfate heptahydrate based on chlor-alkali salt slurry |
-
1995
- 1995-06-08 CN CN95111658A patent/CN1137488A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624204B (en) * | 2009-01-12 | 2011-05-18 | 王嘉兴 | Four-great circulation method formed by waste gypsum mud and chlor-alkali industry |
| CN101823738A (en) * | 2010-04-30 | 2010-09-08 | 汪晋强 | Method for co-production of fine calcium carbonate and sodium silicate, in preparation of light magnesium carbonate by chlor-alkali brine sludge |
| CN101823736A (en) * | 2010-04-30 | 2010-09-08 | 汪晋强 | Method for co-production of calcium carbonate and sodium silicate in preparation of light magnesium carbonate by chlor-alkali brine sludge |
| CN101830493A (en) * | 2010-04-30 | 2010-09-15 | 汪晋强 | Method for processing waste salt slurry of calcined soda with sodium carbonate and sodium sulfate |
| CN102040250A (en) * | 2010-11-17 | 2011-05-04 | 辽宁工程技术大学 | Method for comprehensively utilizing chlor-alkali salt sludge |
| CN102040250B (en) * | 2010-11-17 | 2012-03-28 | 辽宁工程技术大学 | Method for comprehensively utilizing chlor-alkali salt sludge |
| 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 |
| CN104402024A (en) * | 2014-10-24 | 2015-03-11 | 陕西华陆化工环保有限公司 | Method using salty mud to prepare lightweight magnesium oxide |
| CN107082653A (en) * | 2017-05-16 | 2017-08-22 | 四川金象赛瑞化工股份有限公司 | A kind of utilization calcium and magnesium mud is the method that raw material prepares moderate-element Liquid Fertilizer |
| CN108793208A (en) * | 2018-07-17 | 2018-11-13 | 莘县华祥盐化有限公司 | A kind of technique of salt slurry and spent acid comprehensive utilization production magnesium sulfate |
| CN111115666A (en) * | 2020-01-09 | 2020-05-08 | 西安交通大学 | Reduction treatment process for salt mud in chlor-alkali industry |
| CN111204780A (en) * | 2020-01-09 | 2020-05-29 | 西安交通大学 | Resource utilization process of salt mud in chlor-alkali industry |
| CN111204780B (en) * | 2020-01-09 | 2021-04-27 | 西安交通大学 | Resource utilization process of salt mud in chlor-alkali industry |
| CN112429896A (en) * | 2020-10-29 | 2021-03-02 | 河南佰利联新材料有限公司 | Treatment method of salt mud produced in chlor-alkali production |
| CN114538486A (en) * | 2022-02-22 | 2022-05-27 | 西安交通大学 | Magnesium recovery method and system based on chlor-alkali salt mud |
| CN115286024A (en) * | 2022-08-30 | 2022-11-04 | 上海言征分离技术有限公司 | Resource recycling method and system for salt mud produced by chlor-alkali |
| CN115286024B (en) * | 2022-08-30 | 2023-10-27 | 上海言征分离技术有限公司 | Resource recycling method and system for producing salt mud by chlor-alkali |
| CN115353132A (en) * | 2022-09-23 | 2022-11-18 | 西安交通大学 | Preparation method and system of magnesium sulfate heptahydrate based on chlor-alkali salt slurry |
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