CN108059139A - The technique that a kind of sulfuric acid hydrochloric acid combines phosphoric acid co-producing sulfuric acid calcium processed - Google Patents
The technique that a kind of sulfuric acid hydrochloric acid combines phosphoric acid co-producing sulfuric acid calcium processed Download PDFInfo
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- CN108059139A CN108059139A CN201711423205.0A CN201711423205A CN108059139A CN 108059139 A CN108059139 A CN 108059139A CN 201711423205 A CN201711423205 A CN 201711423205A CN 108059139 A CN108059139 A CN 108059139A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
A kind of method that sulfuric acid hydrochloric acid combines phosphoric acid co-producing sulfuric acid calcium pyroborate processed includes following process：Phosphorus ore, dilute hydrochloric acid are mixed into acidolysis in proportion, gained reaction slurry is filtered, and remaining acid non-soluble substance adds in sulfuric acid in filtrate, obtains calcium sulfate crystal whiskers as Solid state fermentation after Washing of Filter Cake；Filtrate containing calcium sulfate crystal whiskers is filtered, the calcium sulfate crystal whiskers of high-purity are obtained after Washing of Filter Cake, filtrate is phosphoric acid and the mixed acid of hydrochloric acid, phosphate rock-sulfuric acid is returned using mixed acid as sour regurgitation, makes to start to take out after phosphoric acid concentration reaches a certain level in mixed acid, the HCl and water steamed obtains dilute hydrochloric acid after cooling absorbs, dilute hydrochloric acid returns to phosphate rock-sulfuric acid, phosphoric acid after concentration is through sedimentation, and the solid slag of discharge returns to phosphate rock-sulfuric acid, and supernatant liquor is finished product concentrated phosphoric acid.It is an advantage of the invention that by phosphorus ore acid hydrolysis and obtaining two links of calcium sulfate precipitation and efficiently separating, the calcium sulfate crystal whiskers of high-quality are obtained, accomplish no coupling product ardealite in phosphoric acid production.
Description
Technical field
The invention belongs to chemical technology fields, are related to the side that a kind of sulfuric acid hydrochloric acid combines phosphoric acid co-producing sulfuric acid calcium pyroborate processed
Method is specially a kind of decomposing phosphate rock by chlorhydric acid and combines the method for sulfuric acid phosphoric acid by-product high-quality calcium sulfate crystal whiskers.
Background technology
Phosphorus is the primary raw material of Global Agriculture production and the raw material of fine chemistry industry production.The process of Phosphate Rock acid
In can generate substantial amounts of ardealite, phosphoric acid by wet process per ton（P2O5）According to the calcium oxide content number of phosphorus ore, about in 4-5 tons of phosphorus stones
Cream, the whole world produce phosphoric acid by wet process about 40,000,000 tons every year, generate 200,000,000 tons of ardealite.The ardealite poor quality, comprehensive profit
With very difficult.Huge ardealite, which is stacked, occupies substantial amounts of soil, due also to ardealite is through rainwater long period of soaking, it is therein can
The problem of dissolubility phosphorus, fluorine etc. are transferred using water body as medium to environment, cause the pollution of soil, water system, air, ardealite has become
The problem of industry common concern and containing industry development.
The content of the invention
The purpose of the present invention is in view of the above problems, providing a kind of sulfuric acid hydrochloric acid combines phosphoric acid co-producing sulfuric acid calcium pyroborate processed
Method by phosphorus ore acid hydrolysis and obtains two links of calcium sulfate precipitation and efficiently separates, the impurity in phosphorus ore and calcium sulfate are effectively divided
From obtaining the calcium sulfate crystal whiskers of high-quality, accomplish no coupling product ardealite in phosphoric acid production.
The technical solution adopted in the present invention is：A kind of sulfuric acid hydrochloric acid combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed,
It is characterized in that：The described method includes following processes：
（1）Phosphorus ore, dilute hydrochloric acid are mixed into acidolysis, and controlling reaction temperature, reaction time in proportion, make the abundant acidolysis of phosphorus ore；
（2）By step 1）Gained reaction slurry is filtered I, and gained filtrate enters the reaction of next step, is left after Washing of Filter Cake I
Acid non-soluble substance as Solid state fermentation；
（3）To step 2）Sulfuric acid is added in gained filtrate, suitable reaction condition is controlled, obtains calcium sulfate crystal whiskers；
（4）By step 3）The filtrate containing calcium sulfate crystal whiskers of gained is filtered II, and high-purity is obtained after Washing of Filter Cake II
Calcium sulfate crystal whiskers, filtrate is phosphoric acid and the mixed acid of hydrochloric acid, into filtrate receiver；
（5）Start to take out after phosphoric acid concentration reaches a certain level in mixed acid in filtrate receiver；
（6）By step 5）The mixed acid of middle taking-up is concentrated, and the HCl and water steamed obtains dilute hydrochloric acid after cooling absorbs, dilute
Hydrochloric acid return to step 1）Middle phosphate rock-sulfuric acid；Mixed acid concentrated after phosphoric acid through sedimentation, supernatant liquor is finished product concentrated phosphoric acid.
Preferably, the step 1）It is middle that phosphorus ore, dilute hydrochloric acid are mixed and added into Xun Huan acid solution mixing in proportion；
Step 5）The middle mixed acid using in filtrate receiver is as Xun Huan acid solution return to step 1）Middle phosphate rock-sulfuric acid；
Step 6）It is middle mixed acid is concentrated after phosphoric acid through sedimentation, the liquid of the solid slag of discharge after asing is as cycling
Acid solution return to step 1）Middle phosphate rock-sulfuric acid.
Preferably, step（1）Described in phosphorus ore input amount for return acidolysis slot sour regurgitation and dilute hydrochloric acid in HCl gross masses
1.0 ~ 2.0 times.
Preferably, step（1）Liquid-solid ratio control is 5 ~ 20 in middle acidolysis slot:1, reaction temperature is room temperature, the reaction time >=
60 minutes.
Preferably, step（3）Middle sulfuric acid dosage is Ca in filtrate2+0.95-1.1 times of content.
Preferably, step（3）The liquid-solid ratio of middle crystallization reaction is controlled 5 ~ 20:1, reaction temperature is room temperature, the reaction time
For >=30 minutes.
Preferably, step（5）Phosphoric acid concentration control is 18 ~ 28% in middle filtrate receiver mixed acid.
Preferably, step（6）Phosphoric acid concentration control 45 ~ 55% after middle concentration.
The invention has the advantages that：
1st, phosphorus ore acid hydrolysis and calcium sulfate generation are carried out at the same time in traditional phosphoric acid by wet process, by-product calcium sulfate poor quality.This method energy
It is enough by phosphorus ore acid hydrolysis and to obtain two links of calcium sulfate precipitation and efficiently separate, the impurity in phosphorus ore and calcium sulfate are efficiently separated,
The calcium sulfate crystal whiskers of high-quality are obtained, accomplish no coupling product ardealite in phosphoric acid production, effectively solve by-product phosphorus in phosphoric acid production
Environmental issue and safety problem caused by gypsum is stored up.
2nd, this method reaction condition is mild, good product quality, consumes low, system closed cycle, comprehensive utilization of resources.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
It is further illustrated the present invention with reference to case study on implementation and attached drawing, but case study on implementation will not be formed to the present invention's
Limitation.
Implement 1：A kind of sulfuric acid hydrochloric acid combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, it is characterised in that：The method
Including following process：
（1）Phosphorus ore, dilute hydrochloric acid are mixed into acidolysis in proportion, phosphorus ore input amount be into 1.8 times of the HCl gross masses of acidolysis slot,
Slurry liquid-solid ratio control 10 in acidolysis slot:1, and 40 DEG C of controlling reaction temperature, 60 minutes reaction time make the abundant acidolysis of phosphorus ore；
（2）By step 1）Gained reaction slurry is filtered I, and gained filtrate enters the reaction of next step, is left after Washing of Filter Cake I
Acid non-soluble substance as Solid state fermentation；
（3）To step 2）Sulfuric acid is added in gained filtrate, sulfuric acid dosage is Ca in filtrate2+1.0 times of content, crystal of calcium sulfate
Liquid-solid ratio control is 10 in the process:1, and 50 DEG C of controlling reaction temperature, in 30 minutes reaction time, obtain calcium sulfate crystal whiskers；
（4）By step 3）The filtrate containing calcium sulfate crystal whiskers of gained is filtered II, and high-purity is obtained after Washing of Filter Cake II
Calcium sulfate crystal whiskers, filtrate is phosphoric acid and the mixed acid of hydrochloric acid, and enters filtrate receiver；
（5）Mixed acid enters filtrate receiver and returns to acidolysis slot phosphate rock-sulfuric acid as Xun Huan acid solution, so cycles, makes phosphorus in mixed acid
Acid concentration reaches 24%（With P2O5Meter）Start to take out, and maintain the stabilization of whole system phosphoric acid concentration；
（6）By step 5）The mixed acid of middle taking-up is concentrated, and is concentrated into phosphoric acid concentration and is reached 50%（With P2O5Meter）, steam
HCl and water obtain dilute hydrochloric acid, dilute hydrochloric acid return to step 1 after cooling absorbs）Middle phosphate rock-sulfuric acid；Mixed acid concentrated after phosphorus
Acid returns to phosphate rock-sulfuric acid in acidolysis slot through sedimentation, the liquid of the solid slag of discharge as Xun Huan acid solution, and supernatant liquor is finished product
Concentrated phosphoric acid, concentration 50%（With P2O5Meter）.
Analysis：Concentrated phosphoric acid, P2O5Concentration 50.6%, Cl-Concentration 0.2%；
Calcium sulfate crystal whiskers, purity 98.3%.
Implement 2：.
A kind of sulfuric acid hydrochloric acid combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, it is characterised in that：The described method includes such as
Lower process：
（1）Phosphorus ore, dilute hydrochloric acid are mixed into acidolysis in proportion, phosphorus ore input amount is the acid into 1 times of the HCl gross masses of acidolysis slot
Solve slurry liquid-solid ratio control 20 in slot:1, and 30 DEG C of controlling reaction temperature, 90 minutes reaction time make the abundant acidolysis of phosphorus ore；
（2）By step 1）Gained reaction slurry is filtered I, and gained filtrate enters the reaction of next step, is left after Washing of Filter Cake I
Acid non-soluble substance as Solid state fermentation；
（3）To step 2）Sulfuric acid is added in gained filtrate, sulfuric acid dosage is Ca in filtrate2+1.0 times of content, crystal of calcium sulfate
Liquid-solid ratio control is 20 in the process:1, and 40 DEG C of controlling reaction temperature, in 60 minutes reaction time, obtain calcium sulfate crystal whiskers；
（4）By step 3）The filtrate containing calcium sulfate crystal whiskers of gained is filtered II, and high-purity is obtained after Washing of Filter Cake II
Calcium sulfate crystal whiskers, filtrate is phosphoric acid and the mixed acid of hydrochloric acid, and enters filtrate receiver；
（5）Mixed acid enters filtrate receiver and returns to acidolysis slot phosphate rock-sulfuric acid as Xun Huan acid solution, so cycles, makes phosphorus in mixed acid
Acid concentration reaches 20%（With P2O5Meter）Start to take out, and maintain the stabilization of whole system phosphoric acid concentration；
（6）By step 5）The mixed acid of middle taking-up is concentrated, and is concentrated into phosphoric acid concentration and is reached 45%（With P2O5Meter）, steam
HCl and water obtain dilute hydrochloric acid, dilute hydrochloric acid return to step 1 after cooling absorbs）Middle phosphate rock-sulfuric acid；Mixed acid concentrated after phosphorus
Acid returns to phosphate rock-sulfuric acid in acidolysis slot through sedimentation, the liquid of the solid slag of discharge as Xun Huan acid solution, and supernatant liquor is finished product
Concentrated phosphoric acid, concentration 45%（With P2O5Meter）.
Analysis：Concentrated phosphoric acid, P2O5Concentration 45.9%, Cl-Concentration 0.4%；
Calcium sulfate crystal whiskers, purity 99.1%.
Implement 3：
A kind of sulfuric acid hydrochloric acid combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, it is characterised in that：The described method includes following mistakes
Journey：
（1）Phosphorus ore, dilute hydrochloric acid are mixed into acidolysis in proportion, phosphorus ore input amount is the acid into 1 times of the HCl gross masses of acidolysis slot
Solve slurry liquid-solid ratio control 5 in slot:1, and 50 DEG C of controlling reaction temperature, 90 minutes reaction time make the abundant acidolysis of phosphorus ore；
（2）By step 1）Gained reaction slurry is filtered I, and gained filtrate enters the reaction of next step, is left after Washing of Filter Cake I
Acid non-soluble substance as Solid state fermentation；
（3）To step 2）Sulfuric acid is added in gained filtrate, sulfuric acid dosage is Ca in filtrate2+1.0 times of content, crystal of calcium sulfate
Liquid-solid ratio control is 5 in the process:1, and 40 DEG C of controlling reaction temperature, in 45 minutes reaction time, obtain calcium sulfate crystal whiskers；
（4）By step 3）The filtrate containing calcium sulfate crystal whiskers of gained is filtered II, and high-purity is obtained after Washing of Filter Cake II
Calcium sulfate crystal whiskers, filtrate is phosphoric acid and the mixed acid of hydrochloric acid, and enters filtrate receiver；
（5）Mixed acid enters filtrate receiver and returns to acidolysis slot phosphate rock-sulfuric acid as Xun Huan acid solution, so cycles, makes phosphorus in mixed acid
Acid concentration reaches 26%（With P2O5Meter）Start to take out, and maintain the stabilization of whole system phosphoric acid concentration；
（6）By step 5）The mixed acid of middle taking-up is concentrated, and is concentrated into phosphoric acid concentration and is reached 55%（With P2O5Meter）, steam
HCl and water obtain dilute hydrochloric acid, dilute hydrochloric acid return to step 1 after cooling absorbs）Middle phosphate rock-sulfuric acid；Mixed acid concentrated after phosphorus
Acid returns to phosphate rock-sulfuric acid in acidolysis slot through sedimentation, the liquid of the solid slag of discharge as Xun Huan acid solution, and supernatant liquor is finished product
Concentrated phosphoric acid, concentration 55%（With P2O5Meter）.
Analysis：Concentrated phosphoric acid, P2O5Concentration 55.3%, Cl-Concentration 0.1%；
Calcium sulfate crystal whiskers, purity 96.8%.
Claims (8)
1. a kind of sulfuric acid hydrochloric acid combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, it is characterised in that：The described method includes as follows
Process：
（1）Phosphorus ore, dilute hydrochloric acid are mixed into acidolysis, and controlling reaction temperature, reaction time in proportion, make the abundant acidolysis of phosphorus ore；
（2）By step 1）Gained reaction slurry is filtered I, and gained filtrate enters the reaction of next step, is left after Washing of Filter Cake I
Acid non-soluble substance as Solid state fermentation；
（3）To step 2）Sulfuric acid is added in gained filtrate, suitable reaction condition is controlled, obtains calcium sulfate crystal whiskers；
（4）By step 3）The filtrate containing calcium sulfate crystal whiskers of gained is filtered II, and high-purity is obtained after Washing of Filter Cake II
Calcium sulfate crystal whiskers, filtrate is phosphoric acid and the mixed acid of hydrochloric acid, into filtrate receiver；
（5）Start to take out after phosphoric acid concentration reaches a certain level in mixed acid in filtrate receiver；
（6）By step 5）The mixed acid of middle taking-up is concentrated, and the HCl and water steamed obtains dilute hydrochloric acid after cooling absorbs, dilute
Hydrochloric acid return to step 1）Middle phosphate rock-sulfuric acid；Mixed acid concentrated after phosphoric acid through sedimentation, supernatant liquor is finished product concentrated phosphoric acid.
2. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：The step 1）It is middle that phosphorus ore, dilute hydrochloric acid are mixed and added into Xun Huan acid solution mixing in proportion；
Step 5）The middle mixed acid using in filtrate receiver is as Xun Huan acid solution return to step 1）Middle phosphate rock-sulfuric acid；
Step 6）It is middle mixed acid is concentrated after phosphoric acid through sedimentation, the liquid of the solid slag of discharge after asing is as cycling
Acid solution return to step 1）Middle phosphate rock-sulfuric acid.
3. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：Step（1）Described in phosphorus ore input amount to return in the sour regurgitation and dilute hydrochloric acid of acidolysis slot 1.0 ~ 2.0 times of HCl gross masses.
4. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：Step（1）Liquid-solid ratio control is 5 ~ 20 in middle acidolysis slot:1, reaction temperature is room temperature, reaction time >=60 minute.
5. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：Step（3）Middle sulfuric acid dosage is Ca in filtrate2+0.95-1.1 times of content.
6. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：Step（3）The liquid-solid ratio of middle crystallization reaction is controlled 5 ~ 20:1, reaction temperature is room temperature, and the reaction time is >=30 minutes.
7. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：Step（5）Phosphoric acid concentration control is 18 ~ 28% in middle filtrate receiver mixed acid.
8. a kind of sulfuric acid hydrochloric acid according to claim 1 combines the method for phosphoric acid co-producing sulfuric acid calcium pyroborate processed, feature exists
In：Step（6）Phosphoric acid concentration control 45 ~ 55% after middle concentration.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115092900A (en) * | 2022-06-28 | 2022-09-23 | 新希望化工投资有限公司 | Process for producing potassium dihydrogen phosphate and calcium sulfate whiskers by adopting phosphorite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736404A (en) * | 2010-01-22 | 2010-06-16 | 四川大学 | Co-production method of calcium sulfate whisker and phosphoric acid |
| CN103436950A (en) * | 2013-09-16 | 2013-12-11 | 山东金正大生态工程股份有限公司 | Method for co-producing calcium sulphate crystal whiskers and ammonium dihydrogen phosphate fertilizer by decomposing phosphorite by adopting hydrochloric acid |
| CN104249997A (en) * | 2014-05-23 | 2014-12-31 | 湖北沃裕新材料科技有限公司 | Ammonium phosphate production method |
-
2017
- 2017-12-25 CN CN201711423205.0A patent/CN108059139A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736404A (en) * | 2010-01-22 | 2010-06-16 | 四川大学 | Co-production method of calcium sulfate whisker and phosphoric acid |
| CN103436950A (en) * | 2013-09-16 | 2013-12-11 | 山东金正大生态工程股份有限公司 | Method for co-producing calcium sulphate crystal whiskers and ammonium dihydrogen phosphate fertilizer by decomposing phosphorite by adopting hydrochloric acid |
| CN104249997A (en) * | 2014-05-23 | 2014-12-31 | 湖北沃裕新材料科技有限公司 | Ammonium phosphate production method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115092900A (en) * | 2022-06-28 | 2022-09-23 | 新希望化工投资有限公司 | Process for producing potassium dihydrogen phosphate and calcium sulfate whiskers by adopting phosphorite |
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Application publication date: 20180522 |