CN101602498A - A kind of purification treatment method of wet-process phosphoric acid - Google Patents
A kind of purification treatment method of wet-process phosphoric acid Download PDFInfo
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- CN101602498A CN101602498A CNA2008100585113A CN200810058511A CN101602498A CN 101602498 A CN101602498 A CN 101602498A CN A2008100585113 A CNA2008100585113 A CN A2008100585113A CN 200810058511 A CN200810058511 A CN 200810058511A CN 101602498 A CN101602498 A CN 101602498A
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- phosphoric acid
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- wet process
- soda ash
- reactive tank
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Abstract
The invention discloses a kind of purification treatment method of wet-process phosphoric acid, the steps include: at first secondly phosphoric acid by wet process to be added in the reactive tank by fluorine and the sulfur trioxide content analyzed in the phosphoric acid by wet process; Get the white carbon black and the yellow soda ash of defluorinate consumption by analytical data, meter is got the ground phosphate rock of desulfurization consumption, respectively white carbon black and yellow soda ash and ground phosphate rock is successively dropped into to purify in the reactive tank with solid phase and stirs; The 3rd is to feed saturation steam in reactive tank, the temperature of reaction and the time of control material, has obtained the material that reacts; The 4th with the reaction material with being pumped in the filter press trough, the filtrate after the press filtration is purification of wet process phosphoric acid, is directly used in the production feed-level calcium biphosphate; The 5th places surge tank with filter cake after pressure filtration, adds clear water and is modulated into slip, with being pumped into extraction tank, reclaims residual phosphorus.Dust removal rate height of the present invention, the phosphorus loss is little, and cleaner is easy to get, and is with low cost, and easy handling control, and the phosphoric acid by wet process after the purification can be directly used in the production feed-level calcium biphosphate.
Description
Technical field
The present invention relates to the wet phosphoric acid purifying production technical field, specially refer to the method that a kind of wet phosphoric acid purifying that is used to produce feed-level calcium biphosphate is handled.
Background technology
In the production of phosphoric acid by wet process, especially use the phosphoric acid by wet process of mid low grade phosphate rock stone production, after it is concentrated, can produce a large amount of solidss, reduction along with the gelled acid temperature, can produce the postprecipitation thing again, add that the phosphoric acid material made 50%P to the abrasion of graphite evaporator when organism was carbonized and concentrates when Rock Phosphate (72Min BPL) leaches
2O
5The solids quality content of phosphoric acid by wet process reaches as high as more than 8%, and acid solution is black.These solidss are collectively referred to as sludge.Also contain SO in the phosphoric acid simultaneously
3, harmful element such as F, these harmful elements and sludge all must be gone out it by purifying.But because mineral difference, purifying method are different, the purification acid quality that obtains is also uneven.For guarantee quality product quality and control production cost, just most producer can only will can produce qualified product with the thermal phosphoric acid collocation of some amount behind the wet phosphoric acid purifying.But the thermal phosphoric acid cost is far above phosphoric acid by wet process, and the blend proportion of thermal phosphoric acid is high more, and then cost is high more.The waste residue that simultaneously general wet phosphoric acid purifying process produces is generally directly abandoned owing to contain a large amount of undesired impurities, and phosphorus decreases bigger, and environmental pollution is serious.
Up to now, do not find that by retrieval similar method published on the publication at home and abroad, and public use is crossed or is otherwise known by the public at home.
Summary of the invention
The objective of the invention is to be to provide a kind of method of wet phosphoric acid purifying processing, this method adopts three kinds of cleaner mixing removal of impurities, effectively purify the impurity in the phosphoric acid by wet process, improved the utilization ratio of phosphoric acid by wet process, thereby significantly reduced the production cost of feed-level calcium biphosphate.Simultaneously this technology also have simple and easy to do, the characteristics that the phosphorus wastage rate are low, gained purifying phosphoric acid sulfur-bearing SO
3≤ 1.5%, fluorine-containing F≤0.2%, P
2O
5/ F 〉=230, total phosphorus utilization 〉=98%.
In order to realize purpose of the present invention, the applicant gropes and repetition test research by secular, developed the perfect wet phosphoric acid purifying method of a cover, can all adopt the Wet-process Phosphoric Acid Production calcium hydrogen phosphate fodder, and obtain good effect aborning.
Three kinds of cleaners of the present invention are respectively: ground phosphate rock, white carbon black and yellow soda ash, the wherein P of ground phosphate rock
2O
5〉=32%.
The step of its impurity removal process is:
A, at first analyze the mass percentage content of fluorine in the phosphoric acid by wet process, the mass percentage content of press sulphur trioxide in barium sulfate weighting method (HG/T 2957.4-2004) the analysis phosphoric acid by wet process by Fluoride ion selective electrode method (HG2636-2000).
B, phosphoric acid by wet process metering back is added reactive tank.Get the white carbon black and the yellow soda ash of 1.2 times of the theoretical consumptions of defluorinate by analytical data, meter is got the ground phosphate rock of 1.2 times of the theoretical consumptions of desulfurization simultaneously.Under agitation condition, respectively three kinds of cleaners (ground phosphate rock and white carbon black and yellow soda ash) are successively dropped in the purification reactive tank with solid phase form.
C, feed saturation steam in reactive tank, the temperature of reaction of control material is 65～70 ℃, in 110～130 minutes reaction times, has obtained a kind of good material that reacts.
D, will react good material with being pumped into plate-and-frame filter press, the filtrate after the press filtration is qualified purification of wet process phosphoric acid, can be directly used in the production feed-level calcium biphosphate.
E, filter cake after pressure filtration is placed surge tank, add clear water and be modulated into that to contain liquid be 40～60% slip, with being pumped into extraction tank, abundant recovery residual phosphorus wherein.
Described three kinds of cleaners are white carbon black, yellow soda ash, ground phosphate rock.
Described white carbon black is meant: the active silica that satisfies HG/T 3061-1999 standard.
Described yellow soda ash is meant: industrial soda ash, total alkali content 〉=98.8% (mass percent).
Described ground phosphate rock is meant: with containing P
2O
5Fineness 200～325 purpose powders that 〉=32% (mass percent) phosphorus ore is worn into.
Wet phosphoric acid purifying method of the present invention compared with prior art has following enthusiasm effect:
1, adopts cleaner of the present invention and purification process thereof, the phosphoric acid quality height after the purification, wherein sulfur-bearing SO
3≤ 1.5%, fluorine-containing F≤0.2%, P
2O
5/ F 〉=230, total phosphorus utilization 〉=98%.
2, cleaner raw material of the present invention is easy to get, and with low cost, method is simple, the dust removal rate height.
3, the cleaner ground phosphate rock of the present invention's employing has two effects, and the one, in order to remove a small amount of sulfuric acid in the phosphoric acid, very important effect simultaneously is to play filtrating aid function.The phosphoric acid sludge adds the Sodium Silicofluoride that generates after the defluorinate, and is because crystallization is tiny, very difficult when filtering.Play filtrating aid function therein by excessive ground phosphate rock, solved this technical barrier, easy handling control, the phosphoric acid by wet process after the purification can be directly used in the production feed-level calcium biphosphate.
Description of drawings
Fig. 1 is the method flow diagram that a kind of wet phosphoric acid purifying is handled.
1 reactive tank
2 press filtration troughs
3 surge tanks
4 pumps
5 extraction tanks
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but be not limitation of the present invention, all any this areas of doing according to the disclosure of invention be equal to replacement, all belong to protection scope of the present invention.
A, be 1.3% (F) by Fluoride ion selective electrode method with by the mass percentage content of fluorine in the barium sulfate gravimetric determination phosphoric acid; The mass percentage content of sulphur trioxide is: 3.2% (SO
3).
B, in reactive tank 1, add 75 tons of phosphoric acid by wet processes.Under agitation condition, add 615 kilograms of yellow soda ash that satisfy the active silica of HG/T 3061-1999 standard, 1080 kilograms of total alkali content 〉=98.8% and 3500 kilograms respectively and contain P
2O
5Fineness 200 that 〉=32% phosphorus ore is worn into or 230 or 250 or 270 or 300 or 325 purpose powder ground phosphate rock.
C, feed saturation steam in reactive tank 1, material is heated to 65 or 67 or 69 or 70 ℃, constant temperature stirred 110 or 115 or 125 or 130 minutes, had just obtained a kind of good material that reacts.
D, the material that will react good are sent in the filter press trough 2 with pump 4, and the filtrate after the press filtration is qualified purification of wet process phosphoric acid, wherein contains SO
3≤ 1.5%, fluorine-containing F≤0.2%, P
2O
5The monocalcium phosphate production plant is delivered to pump 4 in/F 〉=230.
E, place surge tank 3 to add clear water filter cake after pressure filtration to be modulated into that to contain liquid be 40 or 45 or 55 or 60% slip, with being pumped into extraction tank 5, recovery residual phosphorus wherein.
A, be 1.3% (F) by Fluoride ion selective electrode method with by the mass percentage content of fluorine in the barium sulfate gravimetric determination phosphoric acid; The mass percentage content of sulphur trioxide is: 3.2% (SO
3).
B, in reactive tank 1, add 75 tons of phosphoric acid by wet processes.Under agitation condition, add 615 kilograms of yellow soda ash that satisfy the active silica of HG/T 3061-1999 standard, 1080 kilograms of total alkali content 〉=98.8% and 3500 kilograms respectively and contain P
2O
5Fineness 200 that 〉=32% phosphorus ore is worn into or 235 or 245 or 260 or 313 or 323 purpose powder ground phosphate rock.
C, feed saturation steam in reactive tank 1, material is heated to 66 or 68 ℃, constant temperature stirred 113 or 117 or 120 or 128 minutes, had just obtained a kind of good material that reacts.
D, the material that will react good are sent in the filter press trough 2 with pump 4, and the filtrate after the press filtration is qualified purification of wet process phosphoric acid, wherein contains SO
3≤ 1.5%, fluorine-containing F≤0.2%, P
2O
5The monocalcium phosphate production plant is delivered to pump 4 in/F 〉=230.
E, place surge tank 3 to add clear water filter cake after pressure filtration to be modulated into that to contain liquid be 40 or 50 or 58% slip, with being pumped into extraction tank 5, recovery residual phosphorus wherein.
Claims (2)
1, a kind of purification treatment method of wet-process phosphoric acid, its step is as follows:
A, analyze the mass percentage content of fluorine and sulphur trioxide in the phosphoric acid by wet process by Fluoride ion selective electrode method and barium sulfate weighting method;
B, phosphoric acid by wet process metering back is added reactive tank (1); Get the white carbon black and the yellow soda ash of 1.2 times of defluorinate consumptions by analytical data, meter is got the ground phosphate rock of 1.2 times of desulfurization consumptions simultaneously, under agitation condition, white carbon black and yellow soda ash and ground phosphate rock is successively dropped into solid phase purify in the reactive tank respectively;
C, feed saturation steam in reactive tank (1), the temperature of reaction of control material is 65～70 ℃, in 110～130 minutes reaction times, has obtained a kind of material of reaction;
D, with the reaction material send in the filter press trough (2) with pump (4), the filtrate after the press filtration is purification of wet process phosphoric acid, is directly used in the production feed-level calcium biphosphate;
E, filter cake after pressure filtration is placed surge tank (3), add clear water and be modulated into that to contain liquid be 40～60% slip, send into extraction tank (5) with pump (4), recovery residual phosphorus wherein.
2, a kind of purification treatment method of wet-process phosphoric acid according to claim 1 is characterized in that:
Described white carbon black is an active silica;
Described yellow soda ash is the industrial soda ash of total alkali content 〉=98.8%;
Described ground phosphate rock is to use P
20
5〉=32% phosphorus ore is worn into 200～325 purpose powders.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100585113A CN101602498A (en) | 2008-06-10 | 2008-06-10 | A kind of purification treatment method of wet-process phosphoric acid |
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|---|---|---|---|
| CNA2008100585113A CN101602498A (en) | 2008-06-10 | 2008-06-10 | A kind of purification treatment method of wet-process phosphoric acid |
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ID=41468416
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431981A (en) * | 2011-09-01 | 2012-05-02 | 贵州开磷（集团）有限责任公司 | Method for reducing SO3 concentration in diluted phosphoric acid |
| CN104108692A (en) * | 2014-07-31 | 2014-10-22 | 四川龙蟒钛业股份有限公司 | Wet-process phosphoric acid desulphurization method |
| CN104555962A (en) * | 2015-01-05 | 2015-04-29 | 云南铜业胜威化工有限公司 | Method for increasing defluorination rate of high-impurity concentrated phosphoric acid |
| CN104828799A (en) * | 2014-02-12 | 2015-08-12 | 贵州川恒化工有限责任公司 | Process of producing feed-grade calcium dihydrogen phosphate through phosphoric acid circulation impurity removal method |
| CN105800763A (en) * | 2016-05-23 | 2016-07-27 | 瓮福（集团）有限责任公司 | Low-concentration phosphorus-containing waste water treatment method |
| CN112174104A (en) * | 2020-11-10 | 2021-01-05 | 云南磷化集团有限公司 | High-temperature stripping defluorination method and device for wet-process phosphoric acid |
-
2008
- 2008-06-10 CN CNA2008100585113A patent/CN101602498A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431981A (en) * | 2011-09-01 | 2012-05-02 | 贵州开磷（集团）有限责任公司 | Method for reducing SO3 concentration in diluted phosphoric acid |
| CN104828799A (en) * | 2014-02-12 | 2015-08-12 | 贵州川恒化工有限责任公司 | Process of producing feed-grade calcium dihydrogen phosphate through phosphoric acid circulation impurity removal method |
| CN104108692A (en) * | 2014-07-31 | 2014-10-22 | 四川龙蟒钛业股份有限公司 | Wet-process phosphoric acid desulphurization method |
| CN104555962A (en) * | 2015-01-05 | 2015-04-29 | 云南铜业胜威化工有限公司 | Method for increasing defluorination rate of high-impurity concentrated phosphoric acid |
| CN105800763A (en) * | 2016-05-23 | 2016-07-27 | 瓮福（集团）有限责任公司 | Low-concentration phosphorus-containing waste water treatment method |
| CN112174104A (en) * | 2020-11-10 | 2021-01-05 | 云南磷化集团有限公司 | High-temperature stripping defluorination method and device for wet-process phosphoric acid |
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Open date: 20091216 |