CN106395774A - Gradient technology method for wet process phosphoric acid production - Google Patents
Gradient technology method for wet process phosphoric acid production Download PDFInfo
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- CN106395774A CN106395774A CN201610815891.5A CN201610815891A CN106395774A CN 106395774 A CN106395774 A CN 106395774A CN 201610815891 A CN201610815891 A CN 201610815891A CN 106395774 A CN106395774 A CN 106395774A
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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
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/223—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen only one form of calcium sulfate being formed
- C01B25/225—Dihydrate process
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Abstract
The invention relates to a gradient technology method for wet process phosphoric acid production. Phosphate ore acidolysis digestion includes three stages, wherein the first stage is a quick reaction stage, the second stage is a stable reaction stage, and the third stage is a solid grain growing stage; in the quick reaction stage, hyperphosphate mixed acid solution of which the molar ratio of phosphoric acid to sulfuric acid is 1:0.5-1:1 is added; in the stable reaction stage, high-sulfur mixed acid solution of which the molar ratio of phosphoric acid to sulfuric acid is 0:1-0.5:1 is added; in the grain growing stage, the temperature of a crystallization tank is lowered, calcium sulphate dihydrate crystal in ardealite is accelerated to form particles with a large particle size; residual phosphorus content in the ardealite is smaller than 1.9%. According to the method, ground phosphate rock digestion time is shortened by 50%, the residual phosphorus content in the obtained ardealite can be lowered by 20% or more, and a filtering rate can be improved by 30% or more.
Description
Technical field
The invention belongs to phosphoric acid by wet process extraction relieving haperacidity production technical field is and in particular to improve in a kind of Wet Processes of Phosphoric Acid
The method of ardealite quality.
Technical background
The production method of phosphoric acid mainly has Re Fa and wet method, compared with the thermal phosphoric acid using electric furnace reduction, phosphoric acid by wet process
There is obvious cost advantage and less ambient influnence because energy consumption is low.Phosphoric acid by wet process utilizes inorganic acid to be mainly sulfuric acid decomposition phosphorus
The raw phosphoric acid that ore obtains and the ardealite with calcium sulfate as main component.In process of production, its main method is a step
Method produces phosphoric acid.Although preferably, the acidolysis time is long, and the residual phosphorus content of product is higher for its acidolysis rate, and separates phosphoric acid and phosphorus
The efficiency of gypsum is too low, and ardealite is difficult to the production efficiency of the problems such as filter strong influence phosphoric acid.
Conventional wet phosphoric acid process flow chart.Its sour extracting technology reacts for one-step method, i.e. phosphoric acid, sulfuric acid, phosphorus ore one
Secondary property adds is reacted to reactive tank.The defect of this kind of technique has the following aspects：1. the reaction time is longer, conventional wet
The reaction time of method phosphoric acid extracting technology, production efficiency was relatively low up to eight hours；2. it is easily caused phosphorus ore cladding, reaction effect
The problems such as difference or reaction terminating；3. filtering rate is slower, and energy consumption is higher；4. the problems such as in ardealite, residual phosphorus content is higher.
The method improving phosphoric acid by wet process quality mainly increased phosphorus ore pretreatment process in front end, and its operation is more multiple
Miscellaneous, processing cost is higher.
Content of the invention
Long in order to solve phosphoric acid extraction time, the problem that the residual phosphorus content of ardealite is high and filter effect is poor, improves life
Produce economic benefit, the present invention provides a kind of gradient processes method of Wet-process Phosphoric Acid Production.
The concrete technical scheme of the present invention is as follows：
There are three phases in the rock phosphate in powder acidolysis extraction of Wet-process Phosphoric Acid Production, first stage is the fast reaction stage, the
Two stages are to stablize the stage of reaction, and three phases are the solid growing the grain stage；
Adding phosphoric acid in the fast reaction stage is 1 with the mol ratio of sulfuric acid:0.5～1:1 high phosphorus mixed acid solution；Stable
It is 0 with the mol ratio of sulfuric acid that the stage of reaction adds phosphoric acid:1～0.5:1 high-sulfur mixed acid solution；
Calcium oxide molar ratio in the total addition of sulfuric acid and phosphorus ore is 1:Between 1 (± 5%), the total addition of phosphoric acid and sulphur
Sour addition mol ratio 1:0.5～1:1.3 between；
In the growing the grain stage, reduce crystallization tank temperature, promote calcium sulphate dihydrate Crystallization large-size particles in ardealite；
In ardealite, residual phosphorus content is less than 1.9%.
The technical scheme limiting further is as follows：
Phosphoric acid is added to be 1 with the mol ratio of sulfuric acid in the initial 10min in fast reaction stage:0.5～1:1 high phosphorus mixes
Acid solution.
Phosphoric acid is added to be 0 with the mol ratio of sulfuric acid in the initial 10min stablizing the stage of reaction:1～0.5:1 high phosphorus mixes
Acid solution.
The process conditions in growing the grain stage, crystallization tank temperature is 50～80 DEG C, and rearing crystal time is 1～3 hour.
The principle of the invention and being analyzed as follows：
Research finds, rock phosphate in powder acidolysis extraction has three phases.First stage, when solid product calcium sulphate crystal not
When coating rock phosphate in powder particle completely, its extraction reaction rate is very fast, is the fast reaction stage.Second stage, when calcium sulfate is brilliant
After body coats rock phosphate in powder particle completely, extraction reaction rate slows down and tends towards stability, for stablizing the stage of reaction.Three phases,
When rock phosphate in powder crystal completes, calcium sulphate crystal starts to grow, i.e. the solid growing the grain stage.
Referring to Fig. 1, wherein its fast reaction stage of traditional handicraft is 0～10min, and the fast reaction rank of gradient type technique
Section is 0～30min.Illustrate that gradient processes can effectively extend fast reaction phases-time, shorten whole leaching process and taken
Between, improve the efficiency of phosphoric acid production.
(1) the fast reaction stage is 0～30min in Fig. 1, and the purpose of high phosphorus nitration mixture is to improve reaction efficiency, its master
The reaction equation wanted is：
Ca5F(PO4)3+7H3PO4→5Ca(H2PO4)2+HF↑
The addition of high phosphorus nitration mixture, can strengthen and can effectively reduce in course of reaction, the degree of supersaturation of sulfate radical in solution,
Reduce the impact to reaction efficiency for the cladding on rock phosphate in powder surface for the calcium sulfate.(high phosphorus nitration mixture can promote rock phosphate in powder to make in phosphoric acid
With lower generation initial acid solution reaction, reduce, suitable, the production rate that fast reaction elementary reaction speed can prevent from reducing, significantly
Reduce and generate CaSO due to being swift in response4·2H2O is coated on rock phosphate in powder surface and causes passivation it is ensured that reactivity).
(2) stablize the stage of reaction stage for 90min, add high-sulfur nitration mixture, improve the consumption of sulfuric acid.Purpose is in order that becoming
Slow phosphorus ore reaction rate is improved.Add after high phosphorus nitration mixture synthesis with first time, overall reaction rates tend to be steady.Now
The Leach reaction of P, Ca and CaSO in rock phosphate in powder4·2H2O reaction of formation speed relative equilibrium.Reach the same of high reaction rate
When, reduce the residual phosphorus of P, also effectively promote CaSO4·2H2O stably generates.Its key reaction formula is：
Ca(H2PO4)2+H2SO4+2H2O→CaSO4·2H2O+2H3PO4
Stablize stage of reaction reaction to be made up of two parts, the respectively generation of the generation of one-lime phosphate and calcium sulfate.
When stablizing the stage of reaction, unreacted rock phosphate in powder is coated by calcium sulfate, now increases the concentration of sulfuric acid, promotes reaction interface
Further to the internal propulsion of reaction, its reaction mechanism is as follows：1. the H in phosphorus sulphur nitration mixture+By the liquid film layer outside phosphorus ore particle
Diffuse to the outer surface of particle；2.H+Unreacted phosphorus ore particle table is diffused to by solid product layer by mineral powder granular outer surface
Face；3.H+React with phosphorus ore；4. product passes through the transmission of solid product layer exterior surface.
(3), after being reacted into the growing the grain stage, produced by above two sections of gradient types, effectively make CaSO4·2H2The growing the grain of O
Environment is changed.Excessive P, SO is remained in traditional handicraft4 2-Make CaSO4·2H2O generating rate is too fast, and crystal grain trends towards
Little, flattening develops.And solution low P, SO of the process conditions after changing4 2-Crystallization processes parameter after content and adjustment can
To ensure CaSO4·2H2The preferable crystallization condition of O.
It is different to the cladding degree of rock phosphate in powder in differential responses stage sulfuric acid calcium, initially that response characteristic is primarily referred to as rock phosphate in powder
Stage of reaction reaction speed is the fastest, easily causes particles coat.Nitration mixture and phosphorus ore are adopted gradient type technique by the present invention, extend just
Begin the reaction time, improve the reaction rate stablizing the stage of reaction, the growing environment of control growing the grain stage crystal and condition can be obvious
Reduce cladding degree, make Reaction-diffusion terms speed and kinetics reach balance, reaction is continued, constantly carries out, and is specifically shown in
Fig. 2.
In sum, in the present invention, phosphorus sulphur nitration mixture ratio and joining day determine according to phosphorus ore response characteristic, its main mesh
Be to promote reaction starting stage reaction efficiency, suitably reduce fast reaction stage speed, when extending the fast reaction stage and continuing
Between.Sulfuric acid and the reaction completely of ore, improve solution and collect Ca2+And SO4 2-Concentration, the more conducively growth of calcium sulfate.Prevent sulphur
Sour coated mineral particle, hindered acid extracts process, improves reaction efficiency.Stablize the stage of reaction and control sulfate radical degree of supersaturation, promote
Make the formation of required phosphogypsum crystal pattern, improve the rate of filtration.
The present invention reduces ground phosphate rock extraction time 50%, and in gained ardealite, residual phosphorus content can reduce by more than 20%, filters
Speed can improve more than 30%.
Brief description
Fig. 1 is the gradient processes comparison diagram with the present invention for the phosphorus ore acid hydrolysis traditional handicraft of prior art.
Fig. 2 is rock phosphate in powder acidolysis modification of surface morphology figure.
In Fig. 2, a～c is that fast reaction stage surface topography, c～f stablize stage of reaction surface topography, f～g reaction terminating
Stage surface topography.
Specific embodiment
Below in conjunction with the accompanying drawings, by embodiment, the present invention is further described.
Embodiment 1
Hubei phosphate ore A chemical composition is as follows：P2O5Content 31.26%, CaO content 46.24% (Wt%).
The gradient processes concrete operation step of Wet-process Phosphoric Acid Production is as follows：
There are three phases in rock phosphate in powder acidolysis extraction, first stage is the fast reaction stage, and second stage is stable
The stage of reaction, three phases are the solid growing the grain stage.
1. adjustment formula
According to the response characteristic of phosphorus ore A, preferably go out the ratio (mol ratio) of the phosphorus ore of required addition and sulfuric acid twice, specifically
As follows：
| For the first time | Second | |
| H3PO4：H2SO4 | 1:0.7 | 0.2:1 |
2. the fast reaction stage
By 40g phosphorus ore, (phosphatase 11 9.41g, sulfuric acid 13.59g, phosphoric acid is 1 with the mol ratio of sulfuric acid with 33g high phosphorus nitration mixture:
0.7) start to react in disposable addition reactive tank, reaction temperature is 80 DEG C, reaction time 30min, and stir speed (S.S.) is 100r/
min.
3. stablize the stage of reaction
In initial 2min, in reactive tank throw in 23.30g high-sulfur nitration mixture (phosphoric acid 3.88g, sulfuric acid 19.42g, phosphoric acid with
The mol ratio of sulfuric acid is 0.2:1) to reaction system, continue reaction 88min.
4. the growing the grain stage
React and stablize the stage of reaction to entrance during 100min, adjust reactive tank temperature to 50 DEG C, growing the grain 2h.
5. separate slip
After reaction terminates, in slip to filtration system, carry out filtration separation.
Contrast traditional handicraft result is as follows
| Traditional handicraft | Gradient processes | |
| Reaction time | 8 hours | 4 hours |
| Residual phosphorus rate | 2.64% | 1.85% |
| Filtering rate | 0.013cm/s | 0.021cm/s |
Contrast not improved process, after improvement, the method reaction time foreshortens to 4 hours, it is residual for the ardealite being produced
Phosphorus content declines 30%, and filtering rate improves 62%.
Embodiment 2
Hubei phosphate ore B chemical composition is as follows：P2O5Content 30.18%, CaO content 44.51% (Wt%).
The gradient processes concrete operation step of Wet-process Phosphoric Acid Production is as follows：
There are three phases in rock phosphate in powder acidolysis extraction, first stage is the fast reaction stage, and second stage is stable
The stage of reaction, three phases are the solid growing the grain stage.
1. adjustment formula
According to the response characteristic of phosphorus ore B, preferably go out the ratio (mol ratio) of the phosphorus ore of required addition and sulfuric acid twice, specifically
As follows：
| For the first time | Second | |
| H3PO4：H2SO4 | 1:0.6 | 0.3:1 |
2. the fast reaction stage
By 40g phosphorus ore and 31.91g high phosphorus nitration mixture, (phosphatase 11 9.94g, sulfuric acid 11.17g, phosphoric acid with the mol ratio of sulfuric acid is
1:0.6) start to react in disposable addition reactive tank, reaction temperature is 80 DEG C, and stir speed (S.S.) is 100r/min.
3. stablize the stage of reaction
In initial 2min, in reactive tank throw in 25.92g high-sulfur nitration mixture (phosphoric acid 5.98g, sulfuric acid 19.94g, phosphoric acid with
The mol ratio of sulfuric acid is 0.3:1) to reaction system, continue reaction 88min.
4. the growing the grain stage
React and stablize the stage of reaction to entrance during 100min, adjust reactive tank temperature to 50 DEG C, growing the grain 2h.
5. separate slip
After reaction terminates, in slip to filtration system, carry out filtration separation.
Contrast traditional handicraft result is as follows
| Traditional handicraft | Gradient processes | |
| Reaction time | 8 hours | 4 hours |
| Residual phosphorus rate | 2.13% | 1.89% |
| Filtering rate | 0.013cm/s | 0.025cm/s |
Contrast Conventional processing methods, after improvement, the method reaction time foreshortens to 4 hours, and its residual phosphorus of the ardealite being produced contains
Amount decline 11%, filtering rate improves 92%.
Embodiment 3
Hubei phosphate ore C chemical composition is as follows：P2O5Content 30.02%, CaO content 43.90% (Wt%).
The gradient processes concrete operation step of Wet-process Phosphoric Acid Production is as follows：
There are three phases in rock phosphate in powder acidolysis extraction, first stage is the fast reaction stage, and second stage is stable
The stage of reaction, three phases are the solid growing the grain stage.
1. adjustment formula
According to the response characteristic of phosphorus ore C, preferably go out the ratio (mol ratio) of the phosphorus ore of required addition and sulfuric acid twice, specifically
As follows：
| For the first time | Second | |
| H3PO4：H2SO4 | 1:0.6 | 0.3:1 |
2. the fast reaction stage
By 40g phosphorus ore and 31.33g high phosphorus nitration mixture, (phosphatase 11 9.58g, sulfuric acid 11.75g, phosphoric acid with the mol ratio of sulfuric acid is
1:0.6) start to react in disposable addition reactive tank, reaction temperature is 80 DEG C, and stir speed (S.S.) is 100r/min.
3. stablize the stage of reaction
In initial 1min, in reactive tank throw in 25.45g high-sulfur nitration mixture (phosphoric acid 5.87g, sulfuric acid 19.58g, phosphoric acid with
The mol ratio of sulfuric acid is 0.3:1) to reaction system, continue reaction 89min.
4. the growing the grain stage
React and stablize the stage of reaction to entrance during 100min, adjust reactive tank temperature to 50 DEG C, growing the grain 2h.
5. separate slip
After reaction terminates, in slip to filtration system, carry out filtration separation.
Contrast traditional handicraft result is as follows
| Traditional handicraft | Gradient processes | |
| Reaction time | 8 hours | 4 hours |
| Residual phosphorus rate | 2.19% | 1.86% |
| Filtering rate | 0.016cm/s | 0.027cm/s |
Contrast Conventional processing methods, after improvement, the method reaction time foreshortens to 4 hours, and its residual phosphorus of the ardealite being produced contains
Amount decline 15%, filtering rate improves 69%.
Embodiment 4
Shanxi phosphorus ore D chemical composition is as follows：P2O5Content 28.01%, CaO content 42.79% (Wt%).
The gradient processes concrete operation step of Wet-process Phosphoric Acid Production is as follows：
There are three phases in rock phosphate in powder acidolysis extraction, first stage is the fast reaction stage, and second stage is stable
The stage of reaction, three phases are the solid growing the grain stage.
1. adjustment formula
According to the response characteristic of phosphorus ore A, preferably go out the ratio of the phosphorus ore of required addition and sulfuric acid twice, specific as follows：
| For the first time | Second | |
| H3PO4：H2SO4 | 1:0.4 | 0.3:1 |
2. the fast reaction stage
By 40g phosphorus ore, (phosphoric acid 21.82g, sulfuric acid 8.73g, phosphoric acid is 1 with the mol ratio of sulfuric acid with 30.55g high phosphorus nitration mixture:
0.4) disposably it is incorporated in reactive tank and starts to react, reaction temperature is 80 DEG C, stir speed (S.S.) is 100r/min.
3. stablize the stage of reaction
In initial reaction 10min, in reactive tank throw in 28.37g high-sulfur nitration mixture (phosphoric acid 6.55g, sulfuric acid 21.82g,
Phosphoric acid is 0.3 with the mol ratio of sulfuric acid:1) to reaction system, 80min is reacted in continuation.
4. the growing the grain stage
React and stablize the stage of reaction to entrance during 100min, adjust reactive tank temperature to 60 DEG C, growing the grain 2h.
5. separate slip
After reaction terminates, in slip to filtration system, carry out filtration separation.
Contrast Conventional processing methods, result is as follows
| Traditional handicraft | Gradient processes | |
| Reaction time | 8 hours | 4 hours |
| Residual phosphorus rate | 3.15% | 1.48% |
| Filtering rate | 0.008cm/s | 0.020cm/s |
Contrast Conventional processing methods, after improvement, the method reaction time foreshortens to 4 hours, and its residual phosphorus of the ardealite being produced contains
Amount decline 53%, filtering rate improves 150%.
Claims (4)
1. the gradient processes method of Wet-process Phosphoric Acid Production, there are three phases in rock phosphate in powder acidolysis extraction, first stage is quick
The stage of reaction, second stage is to stablize the stage of reaction, and three phases are the solid growing the grain stage；It is characterized in that：
Adding phosphoric acid in the fast reaction stage is 1 with the mol ratio of sulfuric acid:0.5～1:1 high phosphorus mixed acid solution；In stable reaction
It is 0 with the mol ratio of sulfuric acid that stage adds phosphoric acid:1～0.5:1 high-sulfur mixed acid solution；
Calcium oxide molar ratio in the total addition of sulfuric acid and phosphorus ore is 1:Between 1 (± 5%), the total addition of phosphoric acid is added with sulfuric acid
Enter amount mol ratio 1:0.5~1:1.3 between；
In the growing the grain stage, reduce crystallization tank temperature, promote calcium sulphate dihydrate Crystallization large-size particles in ardealite；
In ardealite, residual phosphorus content is less than 1.9%.
2. Wet-process Phosphoric Acid Production according to claim 1 gradient processes method it is characterised in that：In the fast reaction stage
Initial 10min in add the mol ratio of phosphoric acid and sulfuric acid to be 1:0.5～1:1 high phosphorus mixed acid solution.
3. Wet-process Phosphoric Acid Production according to claim 1 gradient processes method it is characterised in that：Stablizing the stage of reaction
Initial 10min in add the mol ratio of phosphoric acid and sulfuric acid to be 0:1～0.5:1 high phosphorus mixed acid solution.
4. Wet-process Phosphoric Acid Production according to claim 1 gradient processes method it is characterised in that：The technique in growing the grain stage
Condition, crystallization tank temperature is 50～80 DEG C, and rearing crystal time is 1～3 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408347A (en) * | 2020-12-07 | 2021-02-26 | 安徽六国化工股份有限公司 | Method for preparing large-size calcium sulfate dihydrate through crystallization in wet-process phosphoric acid leaching process |
| CN112758903A (en) * | 2021-01-27 | 2021-05-07 | 金正大生态工程集团股份有限公司 | Medium-low grade phosphorite pretreatment method |
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| CN1239705A (en) * | 1998-06-18 | 1999-12-29 | 威远县磷钙饲料厂 | Wet phosphoric acid producing process |
| CN102390821A (en) * | 2011-08-08 | 2012-03-28 | 云南云天化国际化工股份有限公司 | Method for producing dihydrate wet-process phosphoric acid |
| CN103435021A (en) * | 2013-08-19 | 2013-12-11 | 瓮福（集团）有限责任公司 | Wet process phosphoric acid production device and method |
| CN104495770A (en) * | 2014-12-24 | 2015-04-08 | 金正大诺泰尔化学有限公司 | Method for purifying wet process phosphoric acid by crystallization in extraction process |
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2016
- 2016-09-09 CN CN201610815891.5A patent/CN106395774B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239705A (en) * | 1998-06-18 | 1999-12-29 | 威远县磷钙饲料厂 | Wet phosphoric acid producing process |
| CN102390821A (en) * | 2011-08-08 | 2012-03-28 | 云南云天化国际化工股份有限公司 | Method for producing dihydrate wet-process phosphoric acid |
| CN103435021A (en) * | 2013-08-19 | 2013-12-11 | 瓮福（集团）有限责任公司 | Wet process phosphoric acid production device and method |
| CN104495770A (en) * | 2014-12-24 | 2015-04-08 | 金正大诺泰尔化学有限公司 | Method for purifying wet process phosphoric acid by crystallization in extraction process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408347A (en) * | 2020-12-07 | 2021-02-26 | 安徽六国化工股份有限公司 | Method for preparing large-size calcium sulfate dihydrate through crystallization in wet-process phosphoric acid leaching process |
| CN112758903A (en) * | 2021-01-27 | 2021-05-07 | 金正大生态工程集团股份有限公司 | Medium-low grade phosphorite pretreatment method |
| CN112758903B (en) * | 2021-01-27 | 2023-01-31 | 金正大生态工程集团股份有限公司 | Medium-low grade phosphorite pretreatment method |
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