CN104150456A - Method for producing calcium phosphate salt and sodium phosphate salt by using sodium sulfate wastewater - Google Patents
Method for producing calcium phosphate salt and sodium phosphate salt by using sodium sulfate wastewater Download PDFInfo
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- CN104150456A CN104150456A CN201410396598.0A CN201410396598A CN104150456A CN 104150456 A CN104150456 A CN 104150456A CN 201410396598 A CN201410396598 A CN 201410396598A CN 104150456 A CN104150456 A CN 104150456A
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Abstract
The invention relates to a method for producing calcium phosphate salt and sodium phosphate salt by using sodium sulfate wastewater. According to the method, wastewater comprising sodium sulfate is adopted as a raw material; 5-15% excessive phosphoric acid with a mass concentration of 80-90% is added to the raw material sodium sulfate wastewater, such that the solution is acidic, and sodium sulfate is completely acidified; lime cream is added into the material, and a pH value is controlled at 2.6-3.2, such that calcium sulfate precipitate is produced, and sulfate radicals in the solution are removed; filtration is carried out; lime cream is continued to be added into a filtrate, and a pH value is controlled at 6.5-7.0; when a reaction is finished, obtained solid is calcium hydrogen phosphate, and obtained liquid is mainly sodium phosphate salt. The method provided by the invention has the advantages of simple and reasonable process, high operability, and high conversion rate. With the method, wastewater is treated, resource is saved, environment is protected, and resource recycling is realized. As a result of experiments, 80-90% of sodium sulfate can be converted.
Description
Technical field
The present invention relates to a kind of method for production of phosphate salt, particularly a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater.
Background technology
Sodium sulfate, mineral compound, Disodium sulfate decahydrate has another name called saltcake, and white, odorless, the crystallization that has bitter taste or powder, have water absorbability.Profile is colourless, transparent, large crystallization or the little crystallization of graininess.Be mainly used in water glass processed, glass, enamel, paper pulp, refrigeration mixture, washing composition, siccative, dye-dilution agent, analytical chemistry reagent, pharmaceuticals etc.Sodium sulfate is extensively present in nature and chemical spent material.In silicon-dioxide production process, can produce the waste water that contains in a large number sodium sulfate, in prior art, can not utilize well this waste water, cause certain wasting of resources.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, and a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater is provided, and the method is reasonable in design, easy to operate, and cost is low, has effectively utilized waste resource.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, is characterized in: the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 80-90% to the mass concentration that adds excessive 5-15% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 2.6 ~ 3.2, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 6.5 ~ 7.0, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.
The raw material of the inventive method can be the waste water that contains sodium sulfate producing in the waste water that contains sodium sulfate producing in technique, particularly silicon-dioxide production process.
In method and technology scheme of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater of the present invention, further preferred technical scheme or technical characterictic are: be excessive 8-12% to the phosphoric acid adding in raw material sulphuric acid sodium waste water, and most preferably 10%; The mass concentration of phosphoric acid is 84-86%, most preferably 85%.
In method and technology scheme of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater of the present invention, further preferred technical scheme or technical characterictic are: while adding milk of lime first, control pH value 2.8 ~ 3.0, most preferably pH value 2.9; While continuing to add milk of lime, control pH value 6.6 ~ 6.8, most preferably pH value 6.7.
Technical solution of the present invention is to adopt in metabisulfite solution, to add a kind of weak acid and milk of lime to react, and under acidic conditions, driving a reaction carries out.The present invention utilizes calcium hydroxide and phosphoric acid, displaces the sodium ion in sodium sulfate wastewater under sour environment, and produces calcium phosphate salt and sodium phosphate salt.Its reaction equation is as follows:
2?Na2SO4?+?3?Ca（OH)2?+?2H3PO4?=?2CaSO4?+?CaHPO4?+?Na2HPO4
The present invention adopts at sodium sulfate and calcium hydroxide and phosphatase reaction and makes calcium phosphate salt and sodium phosphate salt, and because sodium sulfate and calcium hydroxide are all alkaline matters, under general condition, this reaction is difficult to carry out.By add suitable phosphoric acid in solution, solution is transformed into sour environment, molecular balance is moved to left, wherein sulfate radical and calcium ion more easily generate calcium sulfate precipitation.
Compared with prior art, technique advantages of simple of the present invention, workable, transformation efficiency is high.It has been processed waste water and has saved resource, has not only protected environment also to realize the recycling of resource.Through experimental verification, the present invention can transform 80 ~ 90% sodium sulfate.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 80% to the mass concentration that adds excessive 5% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 2.6, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 6.5, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.
Embodiment 2, a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 90% to the mass concentration that adds excessive 15% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 3.2, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 7.0, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.
Embodiment 3, a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 85% to the mass concentration that adds excessive 10% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 2.9, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 6.7, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.This programme can be realized the sodium sulfate that transforms 90%.
Embodiment 4, a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 84% to the mass concentration that adds excessive 8% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 2.8, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 6.6, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.
Embodiment 5, a kind of method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 86% to the mass concentration that adds excessive 12% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 3.0, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 6.8, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.
In method described in embodiment 1-5, raw material is the waste water that contains sodium sulfate to produce in silicon-dioxide production process.
Claims (6)
1. a method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater, is characterized in that: the method is taking the waste water that contains sodium sulfate as raw material; The phosphoric acid that is first 80-90% to the mass concentration that adds excessive 5-15% in raw material sulphuric acid sodium waste water, makes solution be acid, makes the complete acidifying of sodium sulfate; Then add wherein milk of lime, control pH value 2.6 ~ 3.2, generate calcium sulfate precipitation, and remove the sulfate radical in solution; Filter, in filtrate, continue to add milk of lime, control pH value 6.5 ~ 7.0, after reaction finishes, obtaining solid is secondary calcium phosphate, and liquid is mainly sodium phosphate salt.
2. method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater according to claim 1, is characterized in that: the method is taking the waste water that contains sodium sulfate that produces in silicon-dioxide production process as raw material.
3. method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater according to claim 1, is characterized in that: be excessive 8-12% to the phosphoric acid adding in raw material sulphuric acid sodium waste water, the mass concentration of phosphoric acid is 84-86%.
4. method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater according to claim 1, is characterized in that: be excessive 10% to the phosphoric acid adding in raw material sulphuric acid sodium waste water, the mass concentration of phosphoric acid is 85%.
5. method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater according to claim 1, is characterized in that: while adding milk of lime first, control pH value 2.8 ~ 3.0; While continuing to add milk of lime, control pH value 6.6 ~ 6.8.
6. method of producing calcium phosphate salt and sodium phosphate salt with sodium sulfate wastewater according to claim 1, is characterized in that: while adding milk of lime first, control pH value 2.9; While continuing to add milk of lime, control pH value 6.7.
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| CN201410396598.0A CN104150456B (en) | 2014-08-13 | 2014-08-13 | The method producing synthos and sodium ascorbyl phosphate with sodium sulfate wastewater |
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| CN201410396598.0A CN104150456B (en) | 2014-08-13 | 2014-08-13 | The method producing synthos and sodium ascorbyl phosphate with sodium sulfate wastewater |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241851A (en) * | 2016-07-26 | 2016-12-21 | 四川高绿平环境科技有限公司 | A kind of processing method of useless phosphoric acid,diluted |
| CN117902610A (en) * | 2024-01-19 | 2024-04-19 | 天津大学 | Method for recycling sodium sulfate high-salt wastewater |
| CN117902610B (en) * | 2024-01-19 | 2024-07-05 | 天津大学 | Method for recycling sodium sulfate high-salt wastewater |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87103218A (en) * | 1987-04-26 | 1988-11-23 | 杜良才 | Novel method with saltcake production SODIUMNITRATE |
| CN1285312A (en) * | 1999-08-22 | 2001-02-28 | 李怀然 | novel process for preparing fodder grade calcium hydrophosphate and by-product calcium carbonate and ammonium chloride by hydrochloric acid method |
| CN103880209A (en) * | 2014-03-12 | 2014-06-25 | 广东宇星阻燃新材有限公司 | Processing method of sodium sulfate wastewater |
-
2014
- 2014-08-13 CN CN201410396598.0A patent/CN104150456B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87103218A (en) * | 1987-04-26 | 1988-11-23 | 杜良才 | Novel method with saltcake production SODIUMNITRATE |
| CN1285312A (en) * | 1999-08-22 | 2001-02-28 | 李怀然 | novel process for preparing fodder grade calcium hydrophosphate and by-product calcium carbonate and ammonium chloride by hydrochloric acid method |
| CN103880209A (en) * | 2014-03-12 | 2014-06-25 | 广东宇星阻燃新材有限公司 | Processing method of sodium sulfate wastewater |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241851A (en) * | 2016-07-26 | 2016-12-21 | 四川高绿平环境科技有限公司 | A kind of processing method of useless phosphoric acid,diluted |
| CN106241851B (en) * | 2016-07-26 | 2018-01-05 | 四川高绿平环境科技有限公司 | A kind of processing method of useless phosphoric acid,diluted |
| CN117902610A (en) * | 2024-01-19 | 2024-04-19 | 天津大学 | Method for recycling sodium sulfate high-salt wastewater |
| CN117902610B (en) * | 2024-01-19 | 2024-07-05 | 天津大学 | Method for recycling sodium sulfate high-salt wastewater |
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Effective date of registration: 20191112 Address after: No.66, Huanghe Road, Donghai Economic Development Zone, Lianyungang City, Jiangsu Province Patentee after: Jiangsu Debang Doling Health Technology Co., Ltd. Address before: 222000 No. 180, new sea road, Haizhou District, Jiangsu, Lianyungang Patentee before: Lianyungang Debang Fine Chemical Co., Ltd. |