CN103979498A - Method for efficiently recovering iodine in phosphoric acid production process - Google Patents
Method for efficiently recovering iodine in phosphoric acid production process Download PDFInfo
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- CN103979498A CN103979498A CN201410251963.9A CN201410251963A CN103979498A CN 103979498 A CN103979498 A CN 103979498A CN 201410251963 A CN201410251963 A CN 201410251963A CN 103979498 A CN103979498 A CN 103979498A
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Abstract
The invention discloses a method for efficiently recovering iodine in a phosphoric acid production process, which comprises the steps of slurrying, reaction and after-treatment. The method specifically comprises the following steps: preparing the raw material phosphorite into phosphorite slurry; adding sulfuric acid into the phosphorite slurry while introducing ozone for stirring to react for 1-3 hours to obtain a fluid a; adding an organic solvent into the fluid a to perform extraction separation, adding an eluting agent into part of the organic solvent for elution, and adding sodium nitrate into the eluate to precipitate a black substance which is the target substance. The iodine is recovered in the phosphoric acid production process by using the ozone as the oxidizer, so that the phosphorite reaction is more thorough, and the iodine conversion rate is enhanced. The method can promote the sustainable development of phosphorus chemical industry, enhances the economic benefit of the whole phosphorus chemical industry, and can remit the actual state of lack of iodine in China.
Description
Technical field
The invention belongs to chemical technology field, further belong to resource engineering chemistry comprehensive utilization field, 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.Iodine is extremely important elements to the life of animal and plant, and the iodide in seawater are the metabolic conditions of most of marine organisms.Iodine is again the basic raw material of manufacturing inorganic and organic iodide simultaneously, is also the requisite raw material of manufacturing various Operands, sterilizing agent and agricultural chemicals.The compound 2/3rds of iodine and iodine is for the production of various sanitass, sterilizing agent and medicine, and Silver iodide are materials of 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 imports.
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 liquids every year, as direct discharge, not only can cause the wasting of resources, also can environment be produced and be polluted.Carry out the research of iodine changing rejected material to useful resource, can make full use of limited iodine resource, 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 in phosphoric acid by wet process contains a large amount of iodine, and ton phosphoric acid amount of iodine exceedes 0.02%, if propose, can meet domestic needs.In phosphorous chemical industry is produced, reclaim iodine, concerning sulphur dioxide of phosphor chemical industry, not only there is important economic implications, and be one of important means of participating in market competition, increase phosphorus ore added value.So must take rationally effectively recovery measure to iodine.In recent years, numerous scholars and engineering technical personnel are to a large amount of concerns in addition of the recycling of iodine.But the recovery quality of the rate of recovery of iodine and iodine is always lower.
The method that reclaims at present iodine is a lot, but these methods also exist some problems, is all to carry out adding of iodine product, waste residue or the waste liquid from producing, and the rate of recovery of iodine is lower, iodine product second-rate, class is lower, in application, has also been subject to some restrictions.Therefore, developing a kind of method that can simultaneously carry out iodine recovery in the production process of phosphoric acid is 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 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: will in fluid a, add organic solvent to carry out extracting and separating, organic solvent part adds eluent wash-out, adds Sodium Nitrite in elutriant again, separates out atrament and obtains target compound.
The present invention carries out the recovery of iodine in production process of phosphoric acid simultaneously, utilizes gas ozone as oxygenant, makes Rock Phosphate (72Min BPL) react more thoroughly and improve 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.
Brief description of the drawings
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but never in any form the present invention is limited, and any conversion or the replacement done based on training centre of the present invention, 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: will in fluid a, add organic solvent to carry out extracting and separating, organic solvent part adds eluent wash-out, adds Sodium Nitrite in elutriant again, separates out atrament and obtains target compound.
Phosphate ore pulp solid-to-liquid ratio described in A step is 2.5 ~ 3:1.
Sulphuric acid described in B step is 0.6 ~ 0.8 times of phosphate ore pulp volume ratio.
Described sulfuric acid concentration is more than 98%.
Ozone intake described in B step and phosphate ore pulp volume ratio are 0.03 ~ 0.08:1.
The rotating speed stirring described in B step is 30 ~ 40rps/min.
Organic solvent described in C step 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 C step 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 that simultaneously reclaims iodine and the raising iodine rate of recovery and iodine recovery quality in production process of phosphoric acid, in the process of Rock Phosphate (72Min BPL) and acid-respons generation phosphoric acid, pass into oxidation by ozone gas agent, can make Rock Phosphate (72Min BPL) and the acid of reacting in the situation that passing into ozone, react more abundant on the one hand, make on the other hand phosphoric acid just contact fully with the ozone in solution in the process generating at the beginning, iodine wherein can occur fully to react with ozone, more easily separate out, obviously improve thereby realize recovery iodine and the iodine rate of recovery and 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): 1 phosphate ore pulp.
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, phosphate ore pulp and sulfuric acid are added in reactor in 1:0.6 ~ 0.8 ratio, start agitator, control agitator speed is 30 ~ 40rps/min, when stirring, pass into ozone, the reaction times is 1 ~ 3 hour, and liquid is variable color slowly, now prove that Rock Phosphate (72Min BPL) and acid react completely, obtain fluid a;
Described acid is more than 98% strength sulfuric acid.Ozone continues supply by ozonizer.
3, the fluid a obtaining in step 2 is added to benzene in proportion, the liquid of variable color can be suspended in liquid level;
4, add V-Brite B to carry out backwash by being suspended in step 3 in the variable color liquid of liquid level;
5, by adding Sodium Nitrite in the liquid of backwash in step 4, separate out atrament, this atrament is product iodine;
6, filter, clean, packaging, obtains product iodine.Have metalluster, become particulate state, foreign matter content is very low, elemental iodine quality better significantly, and test by analysis, the rate of recovery of iodine has increased by 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, in phosphoric acid, contained iodine all transfers to becomes elemental iodine, simultaneously because ozone is a kind of gas at normal temperatures, thereby the passing into of ozone, make Rock Phosphate (72Min BPL) more abundant with contacting of sulfuric acid, 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, can make the elemental iodine generating all dissolve, and not remain in generated phosphoric acid;
(3) reclaiming the chemical reagent low price using 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 that reclaims iodine in follow-up waste liquid or waste residue, reduced the pollution of environment, increased 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, when stirring, pass into the ozone that is continued supply by ozonizer, after question response 2h, liquid is variable color slowly, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment add in proportion benzene, the liquid of variable color can be suspended in liquid level, then in the variable color liquid that is suspended in liquid level, add V-Brite B to carry out backwash, finally the liquid of backwash is added to 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, when stirring, pass into the ozone that is continued supply by ozonizer, after question response 2.5h, liquid is variable color slowly, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment add in proportion benzene, the liquid of variable color can be suspended in liquid level, then in the variable color liquid that is suspended in liquid level, add V-Brite B to carry out backwash, finally the liquid of backwash is added to 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, when stirring, pass into the ozone that is continued supply by ozonizer, after question response 2.5h, liquid is variable color slowly, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment add in proportion benzene, the liquid of variable color can be suspended in liquid level, then in the variable color liquid that is suspended in liquid level, add V-Brite B to carry out backwash, finally the liquid of backwash is added to 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, when stirring, pass into the ozone that is continued supply by ozonizer, after question response 2.5h, liquid is variable color slowly, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment add in proportion benzene, the liquid of variable color can be suspended in liquid level, then in the variable color liquid that is suspended in liquid level, add V-Brite B to carry out backwash, finally the liquid of backwash is added to 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, when stirring, pass into the ozone that is continued supply by ozonizer, after question response 2.5h, liquid is variable color slowly, now prove that Rock Phosphate (72Min BPL) and acid react completely, at this moment add in proportion benzene, the liquid of variable color can be suspended in liquid level, then in the variable color liquid that is suspended in liquid level, add V-Brite B to carry out backwash, finally the liquid of backwash is added to 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 (10)
1. a 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: will in fluid a, add organic solvent to carry out extracting and separating, organic solvent part adds eluent wash-out, adds Sodium Nitrite in elutriant again, separates out atrament and obtains target compound.
2. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the phosphate ore pulp solid-to-liquid ratio described in A step 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 sulphuric acid described in B step is 0.6 ~ 0.8 times of phosphate ore pulp volume ratio.
4. according to the method for high efficiente callback iodine in the process of phosphoric acid production described in claim 1 or 3, it is characterized in that described sulfuric acid concentration 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 ozone intake and the phosphate ore pulp volume ratio described in B step is 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 stirring described in B step is 30 ~ 40rps/min.
7. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, it is characterized in that organic solvent described in C step be benzene,, one in toluene, dimethylbenzene or phenol.
8. according to the method for high efficiente callback iodine in production process of phosphoric acid described in claim 1 or 7, it is characterized in that described organic solvent add-on and the volume ratio of fluid a are 0.2 ~ 0.4:1.
9. the method for high efficiente callback iodine in production process of phosphoric acid according to claim 1, is characterized in that the eluent described in C step is the one in V-Brite B, Sodium Pyrosulfite or sodium methyl mercaptide solution.
10. according to the method for high efficiente callback iodine in production process of phosphoric acid described in claim 1 or 9, it is characterized in that the concentration of described eluent is 70% ~ 90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN115212779A (en) * | 2022-07-05 | 2022-10-21 | 江苏铁锚玻璃股份有限公司 | Iodine removing method for bipolar color-changing particles |
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| 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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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004021801A1 (en) * | 2002-09-06 | 2004-03-18 | Joe Orton | Animal supplement lick blocks |
| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN115212779A (en) * | 2022-07-05 | 2022-10-21 | 江苏铁锚玻璃股份有限公司 | Iodine removing method for bipolar color-changing particles |
| 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 |
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