CN103979498B - A kind of method of high efficiente callback iodine in production process of phosphoric acid - Google Patents
A kind of method of high efficiente callback iodine in production process of phosphoric acid Download PDFInfo
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- CN103979498B CN103979498B CN201410251963.9A CN201410251963A CN103979498B CN 103979498 B CN103979498 B CN 103979498B CN 201410251963 A CN201410251963 A CN 201410251963A CN 103979498 B CN103979498 B CN 103979498B
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Abstract
The invention discloses the method for high efficiente callback iodine in a kind of production process of phosphoric acid, comprise slurrying, reaction, post-processing step, specifically comprise: raw material phosphor ore is equipped to phosphate ore pulp; In phosphate ore pulp, add sulfuric acid, pass into ozone stirring reaction 1 ~ 3h simultaneously and obtain fluid a; Carry out extracting and separating by adding organic solvent in fluid a, organic solvent portion adds eluent, adds Sodium Nitrite again in elutriant, separates out atrament and obtains target compound.The present invention carries out the recovery of iodine in production process of phosphoric acid simultaneously, utilizes ozone as oxygenant, Rock Phosphate (72Min BPL) is reacted more thoroughly and improves the transformation efficiency of iodine.The present invention not only can promote the Sustainable development of sulphur dioxide of phosphor chemical industry, adds the economic benefit of whole sulphur dioxide of phosphor chemical industry, also can alleviate the present situation of domestic iodine shortage simultaneously.
Description
Technical field
The invention belongs to chemical technology field, belong to resource engineering chemistry field of comprehensive utilization further, be specifically related to the method for high efficiente callback iodine in a kind of production process of phosphoric acid.
Background technology
Iodine is distributed widely in occurring in nature, but it is a kind of dispersed elements, very limited at occurring in nature content, and average grade is low, due to technology and economically, is difficult to scale exploitation.The life of iodine to animal and plant is extremely important element, and the iodide in seawater are the metabolic conditions of most of marine organisms.Iodine is again manufacture basic raw material that is inorganic and organic iodide simultaneously, is also the requisite raw material manufacturing various Operand, sterilizing agent and agricultural chemicals.The compound 2/3rds of iodine and iodine is for the production of various sanitas, sterilizing agent and medicine, and Silver iodide are the materials manufacturing luminous agent.The use range of iodine is wide, and consumption is large, but our country is poor because of preparation condition, and the high a large amount of required iodine of production cost relies on import.
The iodine of China is produced and can not be met the need of market far away, and phosphorus ore manufacturing enterprise, oil production company and pesticide producing producer all can produce a large amount of waste liquid every year, as direct discharge, not only can cause the wasting of resources, also can produce environment and pollute.Carry out the research of iodine changing rejected material to useful resource, limited iodine resource can be made full use of, alleviate the deficient present situation of current day by day serious iodine, also reduce environmental pollution simultaneously, there is certain Significance for Environment and economic implications.
Our country produces containing a large amount of iodine in phosphoric acid by wet process, and ton phosphoric acid amount of iodine, more than 0.02%, if propose, can meet domestic needs.In phosphorous chemical industry produced, reclaim iodine, concerning sulphur dioxide of phosphor chemical industry, not only there is important economic implications, and be participate in market competition, one of the important means increasing phosphorus ore added value.So rationally effective recovery measure must be taked to iodine.In recent years, numerous scholar and engineering technical personnel's concern all in addition a large amount of to the recycling of iodine.But the rate of recovery of iodine is always lower with the recovery quality of iodine.
The method of current recovery iodine is a lot, but these methods also exist some problems, is all to carry out adding of iodine from the product produced, waste residue or waste liquid, and the rate of recovery of iodine is lower, iodine product second-rate, class is lower, and application also receives some restrictions.Therefore, develop a kind of method simultaneously can carrying out iodine recovery in the production process of phosphoric acid to be very important.
Summary of the invention
The object of the present invention is to provide the method for high efficiente callback iodine in a kind of production process of phosphoric acid.
The object of the present invention is achieved like this, comprises slurrying, reaction, post-processing step, specifically comprise:
A, slurrying: raw material phosphor ore is equipped to phosphate ore pulp;
B, reaction: in phosphate ore pulp, add sulfuric acid, pass into ozone stirring reaction 1 ~ 3h simultaneously and obtain fluid a;
C, aftertreatment: carry out extracting and separating by adding organic solvent in fluid a, organic solvent portion adds eluent, adds Sodium Nitrite again in elutriant, separate out atrament and obtain target compound.
The present invention carries out the recovery of iodine in production process of phosphoric acid simultaneously, utilizes gas ozone as oxygenant, Rock Phosphate (72Min BPL) is reacted more thoroughly and improves the transformation efficiency of iodine.The present invention not only can promote the Sustainable development of sulphur dioxide of phosphor chemical industry, increases the benefit of whole sulphur dioxide of phosphor chemical industry, also can alleviate the present situation of domestic iodine shortage simultaneously.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The method of high efficiente callback iodine in production process of phosphoric acid of the present invention, comprises slurrying, reaction, post-processing step, specifically comprises:
A, slurrying: raw material phosphor ore is equipped to phosphate ore pulp;
B, reaction: in phosphate ore pulp, add sulfuric acid, pass into ozone stirring reaction 1 ~ 3h simultaneously and obtain fluid a;
C, aftertreatment: carry out extracting and separating by adding organic solvent in fluid a, organic solvent portion adds eluent, adds Sodium Nitrite again in elutriant, separate out atrament and obtain target compound.
Phosphate ore pulp solid-to-liquid ratio described in step A is 2.5 ~ 3:1.
Sulphuric acid described in step B is 0.6 ~ 0.8 times of phosphate ore pulp volume ratio.
Described sulfuric acid concentration is more than 98%.
Ozone intake described in step B and phosphate ore pulp volume ratio are 0.03 ~ 0.08:1.
The rotating speed stirred described in step B is 30 ~ 40rps/min.
Organic solvent described in step C is the one in benzene,toluene,xylene or phenol.
Described organic solvent add-on and the volume ratio of fluid a are 0.2 ~ 0.4:1.
Eluent described in step C is the one in V-Brite B, Sodium Pyrosulfite or sodium methyl mercaptide solution.
The concentration of described eluent is 70% ~ 90%.
The add-on of described Sodium Nitrite and the ratio of elutriant are 5 ~ 10mg:1 liter.
The object of this invention is to provide a kind of method reclaiming iodine simultaneously and improve that the iodine rate of recovery and iodine reclaim quality in production process of phosphoric acid, generate in the process of phosphoric acid at Rock Phosphate (72Min BPL) and acid-respons and pass into oxidation by ozone gas agent, the acid of Rock Phosphate (72Min BPL) and reaction can be made when passing into ozone to react more abundant on the one hand, on the other hand phosphoric acid is just contacted in the process generated at the beginning fully with the ozone in solution, abundant reaction can be there is in iodine wherein and ozone, more easily separate out, thus iodine is reclaimed in realization and the iodine rate of recovery significantly improves with recovery quality.
The present invention completes according to the following steps:
1, raw material phosphor ore is equipped to liquid-solid ratio for (2.5 ~ 3): the phosphate ore pulp of 1.
The main chemical compositions mass percent of wherein said raw material phosphor ore is: Vanadium Pentoxide in FLAKES 9.0 ~ 30.2%, silicon-dioxide 3.39 ~ 43.02%, calcium oxide 24.64 ~ 46.33%, magnesium oxide 1.33 ~ 10.28%, ferric oxide 0.79 ~ 4.26%, aluminium sesquioxide 0.29 ~ 3.21%, carbonic acid gas 3.64 ~ 23.03%, fluorine 1.36 ~ 2.63%, total amount is 100%;
2, add in reactor by phosphate ore pulp and sulfuric acid in 1:0.6 ~ 0.8 ratio, start agitator, control agitator speed is 30 ~ 40rps/min, pass into ozone while stirring, the reaction times is 1 ~ 3 hour, and liquid can slowly variable color, now prove that Rock Phosphate (72Min BPL) and acid react completely, obtain fluid a;
Described acid is the strength sulfuric acid of more than 98%.Ozone continues supply by ozonizer.
3, the fluid a obtained in step 2 is added benzene in proportion, then the liquid of variable color can be suspended in liquid level;
4, backwash is carried out by adding V-Brite B in the variable color liquid being suspended in liquid level in step 3;
5, add Sodium Nitrite by the liquid of backwash in step 4, separate out atrament, this atrament is product iodine;
6, filter, cleaning, packaging, obtains product iodine.Have metalluster, become particulate state, foreign matter content is very low, and elemental iodine quality better, tests by analysis significantly, and the rate of recovery of iodine adds 15 ~ 20% compared with the rate of recovery of other method, and does not affect produced phosphoric acid quality.
Major advantage of the present invention has:
(1) utilize ozone as oxygenant, due to the strong oxidizing property of ozone, iodine contained in phosphoric acid all transfers to becomes elemental iodine, simultaneously because ozone is a kind of gas at normal temperatures, thus the passing into of ozone, makes the contact of Rock Phosphate (72Min BPL) and sulfuric acid more abundant, react also more thorough, the transformation efficiency of iodine is also higher, can obtain the rate of recovery of higher iodine, and iodine quality is good;
(2) utilize iodine to be easy to the characteristic of dissolving in the organic solvents such as benzene, the elemental iodine of generation can be made all to dissolve, and do not remain in generated phosphoric acid;
(3) reclaiming the chemical reagent low price used in the process of iodine, can reduce costs;
(4) in the process of phosphoric acid processed, reclaimed the iodine in phosphorus ore simultaneously, solve the problem reclaiming iodine in follow-up waste liquid or waste residue, decrease the pollution of environment, add the income of sulphur dioxide of phosphor chemical industry, and alleviate the deficient present situation of current day by day serious iodine, there is practical significance.
Embodiment 1
The main chemical compositions mass percent of raw material phosphor ore is: Vanadium Pentoxide in FLAKES 28.35%, silicon-dioxide 8.32%, calcium oxide 45.65%, magnesium oxide 5.67%, ferric oxide 3.56%, aluminium sesquioxide 1.95%, carbonic acid gas 4.74%, fluorine 1.76%, total amount is 100%; Raw material phosphor ore is equipped to the phosphate ore pulp that liquid-solid ratio is 2.8:1.The vitriol oil of phosphate ore pulp and 98% is added in reactor in 1:0.65 ratio, start agitator, control agitator speed is 35rps/min, the ozone being continued supply by ozonizer is passed into while stirring, after question response 2h, liquid can slowly variable color, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment benzene is added in proportion, then the liquid of variable color can be suspended in liquid level, then in the variable color liquid being suspended in liquid level, add V-Brite B and carry out backwash, finally the liquid of backwash is added Sodium Nitrite, separate out atrament, this atrament is product iodine, there is obvious metalluster, particulate state, impurity is low, quality better, test by analysis, the rate of recovery of iodine is 98.2%.
Embodiment 2
The main chemical compositions mass percent of raw material phosphor ore is: Vanadium Pentoxide in FLAKES 29.13%, silicon-dioxide 4.62%, calcium oxide 47.21%, magnesium oxide 4.14%, ferric oxide 4.02%, aluminium sesquioxide 2.59%, carbonic acid gas 4.74%, fluorine 1.92%, total amount is 100%; Raw material phosphor ore is equipped to the phosphate ore pulp that liquid-solid ratio is 2.9:1.The vitriol oil of phosphate ore pulp and 98% is added in reactor in 1:0.75 ratio, start agitator, control agitator speed is 40rps/min, the ozone being continued supply by ozonizer is passed into while stirring, after question response 2.5h, liquid can slowly variable color, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment benzene is added in proportion, then the liquid of variable color can be suspended in liquid level, then in the variable color liquid being suspended in liquid level, add V-Brite B and carry out backwash, finally the liquid of backwash is added Sodium Nitrite, separate out atrament, this atrament is product iodine, there is obvious metalluster, particulate state, impurity is low, quality better, test by analysis, the rate of recovery of iodine is 98.9%.
Embodiment 3
The main chemical compositions mass percent of raw material phosphor ore is: Vanadium Pentoxide in FLAKES 43.02%, silicon-dioxide 9.2%, calcium oxide 24.64%, magnesium oxide 10.28%, ferric oxide 4.26%, aluminium sesquioxide 3.21%, carbonic acid gas 3.64%, fluorine 1.75%, total amount is 100%; Raw material phosphor ore is equipped to the phosphate ore pulp that liquid-solid ratio is 2.5:1.The vitriol oil of phosphate ore pulp and 98% is added in reactor in 1:0.75 ratio, start agitator, control agitator speed is 30rps/min, the ozone being continued supply by ozonizer is passed into while stirring, after question response 2.5h, liquid can slowly variable color, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment benzene is added in proportion, then the liquid of variable color can be suspended in liquid level, then in the variable color liquid being suspended in liquid level, add V-Brite B and carry out backwash, finally the liquid of backwash is added Sodium Nitrite, separate out atrament, this atrament is product iodine, there is obvious metalluster, particulate state, impurity is low, quality better, test by analysis, the rate of recovery of iodine is 99.2%.
Embodiment 4
The main chemical compositions mass percent of raw material phosphor ore is: Vanadium Pentoxide in FLAKES 30.2%, silicon-dioxide 3.39%, calcium oxide 37.84%, magnesium oxide 1.33%, ferric oxide 0.79%, aluminium sesquioxide 0.79%, carbonic acid gas 23.03%, fluorine 2.63%, total amount is 100%; Raw material phosphor ore is equipped to the phosphate ore pulp that liquid-solid ratio is 3:1.The vitriol oil of phosphate ore pulp and 98% is added in reactor in 1:0.75 ratio, start agitator, control agitator speed is 35rps/min, the ozone being continued supply by ozonizer is passed into while stirring, after question response 2.5h, liquid can slowly variable color, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment benzene is added in proportion, then the liquid of variable color can be suspended in liquid level, then in the variable color liquid being suspended in liquid level, add V-Brite B and carry out backwash, finally the liquid of backwash is added Sodium Nitrite, separate out atrament, this atrament is product iodine, there is obvious metalluster, particulate state, impurity is low, quality better, test by analysis, the rate of recovery of iodine is 98.8%.
Embodiment 5
The main chemical compositions mass percent of raw material phosphor ore is: Vanadium Pentoxide in FLAKES 28.35%, silicon-dioxide 8.32%, calcium oxide 45.65%, magnesium oxide 5.67%, ferric oxide 3.56%, aluminium sesquioxide 1.95%, carbonic acid gas 4.74%, fluorine 1.76%, total amount is 100%; Raw material phosphor ore is equipped to the phosphate ore pulp that liquid-solid ratio is 2.9:1.The vitriol oil of phosphate ore pulp and 98% is added in reactor in 1:0.75 ratio, start agitator, control agitator speed is 40rps/min, the ozone being continued supply by ozonizer is passed into while stirring, after question response 2.5h, liquid can slowly variable color, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment benzene is added in proportion, then the liquid of variable color can be suspended in liquid level, then in the variable color liquid being suspended in liquid level, add V-Brite B and carry out backwash, finally the liquid of backwash is added Sodium Nitrite, separate out atrament, this atrament is product iodine, there is obvious metalluster, particulate state, impurity is low, quality better, test by analysis, the rate of recovery of iodine is 98.6%.
Claims (9)
1. the method for high efficiente callback iodine in production process of phosphoric acid, is characterized in that comprising slurrying, reaction, post-processing step, specifically comprises:
A, slurrying: raw material phosphor ore is equipped to phosphate ore pulp;
B, reaction: in phosphate ore pulp, add sulfuric acid, pass into ozone stirring reaction 1 ~ 3h simultaneously and obtain fluid a;
C, aftertreatment: carry out extracting and separating by adding organic solvent in fluid a, organic solvent portion adds eluent, adds Sodium Nitrite again in elutriant, separate out atrament and obtain target compound; Described organic solvent is the one in benzene,toluene,xylene or phenol.
2. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the solid-to-liquid ratio of phosphate ore pulp described in step A is 2.5 ~ 3:1.
3. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the add-on of sulfuric acid described in step B is 0.6 ~ 0.8 times of phosphate ore pulp volume ratio.
4. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1 or 3, is characterized in that the concentration of sulfuric acid described in step B is more than 98%.
5. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the intake of ozone described in step B and phosphate ore pulp volume ratio are 0.03 ~ 0.08:1.
6. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the rotating speed stirred described in step B is 30 ~ 40rps/min.
7. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the add-on of organic solvent described in step C and the volume ratio of fluid a are 0.2 ~ 0.4:1.
8. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that eluent described in step C is the one in V-Brite B, Sodium Pyrosulfite or sodium methyl mercaptide solution.
9. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1 or 8, is characterized in that the concentration of eluent described in step C is 70% ~ 90%.
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| CN106430105A (en) * | 2016-10-10 | 2017-02-22 | 云南民族大学 | Method for recycling iodine from acetic acid factory iodine-containing waste liquor |
| CN115212779B (en) * | 2022-07-05 | 2023-05-26 | 江苏铁锚玻璃股份有限公司 | Iodine removal method for bipolar color-changing particles |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683239A (en) * | 2004-04-16 | 2005-10-19 | 四川承源化工有限公司 | Method for producing phosphoric acid with low and medium grade phosphorous mine ore |
| CN1699148A (en) * | 2004-05-21 | 2005-11-23 | 李兴才 | Process for producing industrial phosphoric acid using phosphorus ore as raw material |
| CN101638220A (en) * | 2009-09-03 | 2010-02-03 | 瓮福（集团）有限责任公司 | Method for extracting iodine from iodine-containing phosphorus ore |
| CN103332664A (en) * | 2013-06-22 | 2013-10-02 | 瓮福（集团）有限责任公司 | Hemi-hydrate process wet process phosphoric acid production process |
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| WO2004021801A1 (en) * | 2002-09-06 | 2004-03-18 | Joe Orton | Animal supplement lick blocks |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683239A (en) * | 2004-04-16 | 2005-10-19 | 四川承源化工有限公司 | Method for producing phosphoric acid with low and medium grade phosphorous mine ore |
| CN1699148A (en) * | 2004-05-21 | 2005-11-23 | 李兴才 | Process for producing industrial phosphoric acid using phosphorus ore as raw material |
| CN101638220A (en) * | 2009-09-03 | 2010-02-03 | 瓮福（集团）有限责任公司 | Method for extracting iodine from iodine-containing phosphorus ore |
| CN103332664A (en) * | 2013-06-22 | 2013-10-02 | 瓮福（集团）有限责任公司 | Hemi-hydrate process wet process phosphoric acid production process |
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