CN108726496A - A kind of defluorination method of high-content sesquichloride phosphoric acid by wet process - Google Patents
A kind of defluorination method of high-content sesquichloride phosphoric acid by wet process Download PDFInfo
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- CN108726496A CN108726496A CN201810877834.9A CN201810877834A CN108726496A CN 108726496 A CN108726496 A CN 108726496A CN 201810877834 A CN201810877834 A CN 201810877834A CN 108726496 A CN108726496 A CN 108726496A
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- phosphoric acid
- defluorinating agent
- sesquichloride
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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
- C01B25/234—Purification; Stabilisation; Concentration
- C01B25/237—Selective elimination of impurities
- C01B25/2372—Anionic impurities, e.g. silica or boron compounds
- C01B25/2375—Fluoride or fluosilicate anion
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the preparing technical fields of phosphoric acid, and in particular to a, the Si powder that defluorinating agent and purity are 90% or more is sufficiently mixed grinding and forms the mixture that grain size is 1 ~ 3um by a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process；B, 30 ~ 60min of time is added in the mixture being gradually added under 800 ~ 100 DEG C, stirring condition in step a；C, after defluorinating agent adds, under conditions of 90 ~ 110 DEG C of temperature, 0.4 ~ 0.5 kilowatt/cube of stirring intensity, continue to react；D, when phosphorus fluorine ratio is more than 310, defluorinate is completed.The present invention has carried out pretreatment early period to defluorinating agent, silicon is added to be sufficiently mixed, defluorinating agent is set to be added in phosphoric acid solution in the way of more disperseing by silicon, avoid the agglomeration of defluorinating agent, defluorinate efficiency is improved, the production cycle is shortened, improves production efficiency, the waste for reducing defluorinating agent improves the economic benefit of enterprise.
Description
Technical field
The invention belongs to the preparing technical fields of phosphoric acid, and in particular to a kind of high-content sesquichloride phosphoric acid by wet process takes off
Fluorine method.
Background technology
In existing phosphoric acid purification technology, common method for purifying phosphoric acid has:Chemical precipitation method, vapor phase method, solvent are heavy
Shallow lake method and solvent extraction.Solvent precipitation and solvent extraction are mainly used to the defluorination method of high-content sesquichloride phosphoric acid
Method.Although can be purified to high-content sesquichloride phosphoric acid by wet process using solvent precipitation or solvent extraction, lead to
It often needs using reaction of high order equipment and is stripped taking equipment, thus equipment is more, investment cost is high.Vapor phase method be by silicate with
Hydrofluoric acid forms ocratation, achievees the purpose that defluorinate.But due in phosphoric acid solution fluohydric acid content it is relatively low, defluorinating agent
It into being difficult to react for the moment in phosphoric acid solution, causes reaction efficiency low, wastes defluorinating agent.Therefore it is higher to be badly in need of a kind of defluorinate efficiency
The defluorination method of ground high-content sesquichloride phosphoric acid by wet process.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process, energy
Enough purifications for effectively realizing phosphoric acid.
A kind of this patent defluorination method of high-content sesquichloride phosphoric acid by wet process newly developed, includes the following steps：
A, the Si powder that defluorinating agent and purity are 90% or more is sufficiently mixed grinding and forms the mixture that grain size is 1 ~ 3um；With silicon
For medium, defluorinating agent is made to play good peptizaiton in phosphoric acid solution so that defluorinating agent is dispersed in phosphoric acid solution well,
Defluorinating agent can be contacted preferably with the hydrofluoric acid in phosphoric acid solution in this way, and then reacted and improved the efficiency of reaction, be reduced
The waste of defluorinating agent improves reaction rate and increases economic efficiency；And silicon can react with the hydrofluoric acid in solution, shape
Impurity is not introduced at gas effusion, and silicon is reacted with hydrofluoric acid can release certain heat, can be effectively promoted defluorinate
Agent is reacted with hydrofluoric acid, further increases defluorinate efficiency.
B, 30 ~ 60min of time is added in the mixture being gradually added under 800 ~ 100 DEG C, stirring condition in step a；Compared with
Under high temperature condition and stirring condition, defluorinating agent can be made to be come into full contact with the hydrofluoric acid in phosphoric acid solution, higher temperature
Defluorinate efficiency can be improved；The addition time of defluorinating agent is in order to ensure defluorinating agent is to be added in phosphoric acid solution in a slowly manner
, it avoiding after being added at one time, defluorinating agent is reunited in phosphoric acid solution so that defluorination reaction only occurs in reunion layer outer surface,
And it is not sufficiently reacted.
C, after defluorinating agent adds, under conditions of 90 ~ 110 DEG C of temperature, 0.4 ~ 0.5 kilowatt/cube of stirring intensity, continue into
Row reaction, detects a phosphorus fluorine ratio per hour；After defluorinating agent is added completely into step b, defluorinating agent is not also completely molten with phosphoric acid
Hydrofluoric acid reaction in liquid, needs the regular hour, therefore continuing to provide certain temperature and stirring condition so that solution is transported
It moves up, defluorinating agent and hydrofluoric acid more fully haptoreaction；A phosphorus fluorine ratio is detected per hour, reacts shape convenient for grasping in time
State, association reaction time determine whether reaction is complete, in order to decide whether to add defluorinating agent；Stirring intensity, because
The difference of stirring blade shape（The other structures being arranged in the angle and stirring blade of stirring blade so that mixing effect is difficult
With description）So that stirring is less accurate with the describing mode of linear velocity and angular speed, therefore with the power of cubic unit blender
It is described for unit of measurement.The present invention carries out under the conditions of 0.4 ~ 0.5 kilowatt/cube, and effect is preferable.
D, when phosphorus fluorine ratio be more than 310, the phosphoric acid defluorination in system is drawn out to defluorinate acid storage tank, when phosphorus fluorine ratio be higher than 300
The standard of food grade phosphoric acid product is just reached, that is, fluorine removal is completed.
Further, the defluorinating agent is white carbon, sodium carbonate and silica or potassium carbonate and silica, provides silicon
Hydrochlorate utilizes vapor phase method fluorine removal.
Further, the weight ratio of the defluorinating agent and silicon is 1：1~5.
Further, the mixture formed in the step a is added in a manner of dusting in step b, makes defluorinating agent one more
The mode of dispersion is added in phosphoric acid solution, avoids reuniting.
Further, the mixture formed in the step a is added in step b after adding water to mix in a manner of sprinkling, makes to take off
Fluorine agent is added in a manner of more disperseing in phosphoric acid solution, improves reaction efficiency.
Further, the weight ratio of the mixture and water that are formed in the step a is 1：50 ~ 100 ratio mixing.
Beneficial effects of the present invention：The present invention has carried out pretreatment early period to defluorinating agent, and silicon is added and is sufficiently mixed, utilizes silicon
So that defluorinating agent is added in phosphoric acid solution in a manner of more disperseing, avoid the agglomeration of defluorinating agent, improves defluorinate effect
Rate shortens the production cycle, improves production efficiency, reduces the waste of defluorinating agent, improves the economic benefit of enterprise.
Specific implementation mode
Embodiment 1
A, by defluorinating agent（White carbon）The Si powder for being 90% with purity is 1 according to weight ratio：1 ratio is sufficiently mixed grinding shape
At the mixture that grain size is 1 ~ 3um；
B, under 800 DEG C, stirring condition by the mixture in step a with spray powder or with water according to weight ratio be 1:50
Ratio mixing after the mode sprayed be gradually added in phosphoric acid solution, time 60min is added；
C, after defluorinating agent adds, under conditions of 90 DEG C of temperature, 0.5 kilowatt/cube of stirring intensity, continue to react；
D, when phosphorus fluorine ratio is more than 310, the phosphoric acid defluorination in system is drawn out to defluorinate acid storage tank, defluorinate is completed.
Embodiment 2
A, by defluorinating agent（Sodium carbonate and silica）The Si powder for being 92% with purity is 1 according to weight ratio：5 ratio is abundant
Mixed grinding forms the mixture that grain size is 1 ~ 3um；
B, under 900 DEG C, stirring condition by the mixture in step a with spray powder or with water according to weight ratio be 1:
The mode sprayed after 100 ratio mixing is gradually added in phosphoric acid solution, and time 60min is added；
C, after defluorinating agent adds, under conditions of 80 DEG C of temperature, 0.4 kilowatt/cube of stirring intensity, continue to react；
D, when phosphorus fluorine ratio is more than 310, defluorinate is completed.
Embodiment 3
A, by defluorinating agent（Sodium carbonate and silica）The Si powder for being 95% with purity is 1 according to weight ratio：3 ratio is abundant
Mixed grinding forms the mixture that grain size is 1 ~ 3um；
B, under 850 DEG C, stirring condition by the mixture in step a with spray powder or with water according to weight ratio be 1:80
Ratio mixing after the mode sprayed be gradually added in phosphoric acid solution, time 50min is added；
C, after defluorinating agent adds, under conditions of 90 DEG C of temperature, 0.45 kilowatt/cube of stirring intensity, continue to react；
D, when phosphorus fluorine ratio is more than 310, defluorinate is completed.
Claims (6)
1. a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process, which is characterized in that pass through following steps：
A, the Si powder that defluorinating agent and purity are 90% or more is sufficiently mixed grinding and forms the mixture that grain size is 1 ~ 3um；
B, gradually add into the phosphoric acid solution for wait for defluorinate under conditions of 800 ~ 100 DEG C, 0.4 ~ 0.5 kilowatt/cube of stirring intensity
Enter the mixture in step a, 30 ~ 60min of time is added；
C, after defluorinating agent adds, under conditions of 90 ~ 110 DEG C of temperature, 0.4 ~ 0.5 kilowatt/cube of stirring intensity, continue anti-
It answers；
D, when phosphorus fluorine ratio is more than 310, defluorinate is completed.
2. a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process as described in claim 1, which is characterized in that described
Defluorinating agent is white carbon, sodium carbonate and silica or potassium carbonate and silica.
3. a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process as claimed in claim 2, which is characterized in that described
The weight ratio of defluorinating agent and silicon is 1：1~5.
4. a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process as claimed in claim 3, which is characterized in that described
The mixture formed in step a is added in a manner of dusting in step b.
5. a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process as claimed in claim 3, which is characterized in that described
The mixture formed in step a is added in step b after adding water to mix in a manner of sprinkling.
6. a kind of defluorination method of high-content sesquichloride phosphoric acid by wet process as claimed in claim 5, which is characterized in that described
The weight ratio of the mixture and water that are formed in step a is 1：50 ~ 100 ratio mixing.
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| CN201810877834.9A CN108726496A (en) | 2018-08-03 | 2018-08-03 | A kind of defluorination method of high-content sesquichloride phosphoric acid by wet process |
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| CN201810877834.9A CN108726496A (en) | 2018-08-03 | 2018-08-03 | A kind of defluorination method of high-content sesquichloride phosphoric acid by wet process |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4330517A (en) * | 1981-03-27 | 1982-05-18 | International Minerals & Chemical Corp. | Defluorination of wet process phosphoric acid |
| CN1207366A (en) * | 1998-08-22 | 1999-02-10 | 杨显庆 | Process for producing calcium hydrogen phosphate by once-through defluorination |
| CN106698372A (en) * | 2015-11-16 | 2017-05-24 | 贵州省化工技术研发中心 | Wet-process phosphoric acid defluorination method |
| CN108147383A (en) * | 2018-01-05 | 2018-06-12 | 贵州川恒化工股份有限公司 | The defluorination method of phosphoric acid by wet process |
-
2018
- 2018-08-03 CN CN201810877834.9A patent/CN108726496A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4330517A (en) * | 1981-03-27 | 1982-05-18 | International Minerals & Chemical Corp. | Defluorination of wet process phosphoric acid |
| CN1207366A (en) * | 1998-08-22 | 1999-02-10 | 杨显庆 | Process for producing calcium hydrogen phosphate by once-through defluorination |
| CN106698372A (en) * | 2015-11-16 | 2017-05-24 | 贵州省化工技术研发中心 | Wet-process phosphoric acid defluorination method |
| CN108147383A (en) * | 2018-01-05 | 2018-06-12 | 贵州川恒化工股份有限公司 | The defluorination method of phosphoric acid by wet process |
Non-Patent Citations (6)
| Title |
|---|
| ABDEL-AAL ET AL.: "Defluorination of wet-process phosphoric acid for production of dicalcium phosphate", 《HUNGARIAN JOURNAL OF INDUSTRIAL CHEMISTRY》 * |
| AHMED ET AL.: "Purification of phosphoric acid by minimizing iron,copper,cadmium and fluoride", 《SEPARATION AND PURIFICATION TECHNOLOGY》 * |
| 何宾宾等: "湿法磷酸生产中减压热空气法脱氟技术开发", 《磷肥与复肥》 * |
| 向江: "硅能与氢氟酸发生化学反应吗?", 《化学教育》 * |
| 蒲江涛等: "浓缩湿法磷酸空气气提脱氟的研究", 《磷肥与复肥》 * |
| 蔡建利等: "活性硅复合脱氟剂的试验研究", 《云南化工》 * |
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