CN101434386A - Method for producing fine phosphate by using dilute acid to decompose middle and low grade phosphate ore using - Google Patents
Method for producing fine phosphate by using dilute acid to decompose middle and low grade phosphate ore using Download PDFInfo
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- CN101434386A CN101434386A CNA2007101694306A CN200710169430A CN101434386A CN 101434386 A CN101434386 A CN 101434386A CN A2007101694306 A CNA2007101694306 A CN A2007101694306A CN 200710169430 A CN200710169430 A CN 200710169430A CN 101434386 A CN101434386 A CN 101434386A
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Abstract
The invention relates to a method for producing fine phosphate by using a dilute acid to decompose mid-low grade phosphorite, which pertains to the technical field of phosphate production. The method is applicable to decomposing the mid-low grade phosphorite by a dilute hydrochloric acid or a nitric acid (including a waste acid), the impurities in the phosphorite are effectively removed during the decomposition course of the phosphorite, and most of P2O5 can be converted to pure product, thus remarkably improving the recovery ratio of the P2O5 and reducing the production cost. The invention uses the dilute acid (the hydrochloric acid or the nitric acid) to carry out normal-temperature two-section leaching to the phosphorite, thus effectively removing the main impurities in the phosphorite, directly producing the fine phosphate and effectively improving the recovery ratio of the P2O5. In the production process, pure gypsum is produced and can directly separate water-soluble compound fertilizer out without evaporation concentration after being converted, thus saving energy source grealty and reducing the production cost. The method is applicable to decomposing the mid-low grade phosphorite by all kinds of dilute acid (including waste acid), can effectively remove the impurities, recover the P2O5, lead the impurities and the P2O5 to be converted to pure products completely, and fully realize energy conservation and emission reduction.
Description
Technical field the present invention relates to the method that the sour decomposing medium and low grade of a kind of rare salt of use (nitre) is produced fine phosphate, belongs to the technical field of phosphate production.
The technology of the sour decomposing medium and low grade of the rare salt of the use of indication of the present invention (nitre) and effective separating impurity, refer to and use the sour decomposing medium and low grade direct production of rare salt (nitre) fine phosphate, the major impurity in the phosphorus ore is effectively separated in process of production simultaneously.
Method provided by the invention is applicable to dilute hydrochloric acid or nitric acid (comprising spent acid) decomposing medium and low grade, and the impurity in the phosphorus ore is effectively got rid of in the phosphorus ore decomposition course, most P
2O
5Can transform into pure product, therefore significantly improve P
2O
5The rate of recovery has reduced production cost.
Below explanation is an example with hydrochloric acid.
Here said diluted acid refers to the diluted acid or the spent acid of content in any concentration more than 8%.
Background technology is present, and known fine phosphate production technology is generally used thermal phosphoric acid, because contain various impurity, for example aluminum oxide, ferric oxide, calcium oxide, magnesium oxide or the like in the phosphoric acid by wet process inevitably.These impurity making under the phosphatic operational condition, generate AlPO
4, FePO
4, CaHPO
4, MgHPO
4, MgNH
4PO
4, Ca
3(PO
4)
2, Mg
3(PO
4)
2Or the like throw out, cause a large amount of losses and the severe exacerbation sepn process and the quality product of Vanadium Pentoxide in FLAKES.The phosphorus ore of China generally contains many iron, aluminium, calcium, magnesium or the like impurity, and the situation of this phosphorus pentoxide losing is just more serious.These calcium phosphate precipitations generally have colloidal state character, are difficult to be used, and therefore, use impure many phosphoric acid by wet processes to make fine phosphate, are difficult to receive reasonable economic benefit.
Since a large amount of losses of the Vanadium Pentoxide in FLAKES that these impurity cause, the selected phosphorus ore of having to, and a large amount of mid low grade phosphate rocks can't utilize, and causes the serious waste of resource.
In addition, because the influence of above-mentioned phosphoric acid by wet process impurity when using phosphoric acid by wet process or wet phosphate to produce compound manure, can only obtain the water miscible product of part, this brings the problem of two aspects.On the one hand be that this fertilizer is not suitable for spraying, drip irrigation etc., limited their result of use, be owing to contain a large amount of colloidal precipitate things on the other hand, give concentrate, the course of processing such as drying brings difficulty.Generally can only use slip to concentrate and spray granulating, not only equipment complexity, and increase energy consumption.
Owing to these reasons, use the technology of Wet-process Phosphoric Acid Production phosphoric acid salt and sulphur based compound fertilizer and equipment to become complicated, product yield is low, and is of poor quality, hindered the development of phosphate industry and chemical fertilizer industry.
The impurity of summary of the invention when overcoming above-mentioned use Wet-process Phosphoric Acid Production phosphoric acid salt disturbs and solves making full use of of mid low grade phosphate rock or the like problem, and the present invention advises a kind of method of using the various fine phosphates of diluted acid decomposing medium and low grade direct production.This method not only can solve smoothly uses mid low grade phosphate rock to produce phosphatic impurity interference problem, can bring up to the rate of recovery of Vanadium Pentoxide in FLAKES more than 95%, and can use the very low phosphorus ore inferior of various low-concentration waste acids and content, make full use of various resources, simplify technology simultaneously, reduce corrosion, simplified apparatus is received reasonable economical and technical benefit.
The another one characteristics are that the use present technique is produced in the phosphatic process, is convenient to realize comprehensive utilization, directly separates out the by-product water soluble fertilizer, has not only reduced production cost, and has saved a large amount of energy, realizes energy-saving and emission-reduction.
The present invention will be further described below in conjunction with accompanying drawing for description of drawings.
Accompanying drawing is produced the schema of fine phosphate for the diluted acid decomposing medium and low grade.
In the accompanying drawings, two sections leaching solution and ground phosphate rock (40-80 order) are according to the 105-110% of theoretical amount of calculation Ratio metering, in one section leaching groove, stirring at normal temperature reaction 1-4 hour. Add flocculant and stir, Precipitation is fully separated leaching liquid and is sent to the neutralization reaction groove.
Then, whole slag slurries are transferred in two sections leaching grooves, added the watery hydrochloric acid of amount of calculation, at normal temperatures Stirring reaction 1-4 hour, to filter through the slag filter, filtrate is returned one section leaching groove.
One section leaching liquid in the neutralization reaction groove uses the milk of lime neutralization.Neutralization reaction can be finished or be divided into two steps a step and finish.
One the step in and the time, use the milk of lime of CaO=80-150g/l, PH=3.5-6.0 once neutralizes, the slip that neutralization is finished all goes to wash the pressure filter filtration, filtrate dechlorination calcium solution is handled workshop section, after filter cake washing dries up, after using corresponding crystalline mother solution pressurized air to stir to size mixing, go the conversion reaction groove to carry out conversion reaction.
Two the step in and the time, at first use the milk of lime of the CaO=80-150g/l PH=1.5-2.0 that neutralizes, the slip that neutralization is finished all removes to wash pressure filter and filters, the filtrate of flushing pressure filter goes the calcium hydrophosphate fodder reactive tank to continue the PH=3.5-6.0 that neutralizes, obtain the calcium hydrophosphate fodder finished product behind the filtration drying, flushing is after cake of filter-press dries up, and uses after corresponding crystalline mother solution pressurized air stirring sizes mixing, and goes the conversion reaction groove to carry out conversion reaction.
Add sal enixum (perhaps vitriolate of tartar and sulfuric acid) in the conversion reaction groove, stirring reaction is to reacting completely control PH=0.5-4.5, temperature of reaction 40-100 ℃.Reaction is finished slip and is filtered to isolate purified gypsum (go the gypsum conversion and separate out compound manure) through the gypsum filter, and filtrate is potassium dihydrogen phosphate.This solution enters the crystallizer tank crystallisation by cooling after purifying through purification system, filters through whizzer then, isolates the potassium primary phosphate finished product.The crystalline mother solution that whizzer filters out returns flushing pressure filter flushing cinder batching again, enters the conversion reaction groove and carries out conversion reaction again.
Embodiment the technical solution adopted for the present invention to solve the technical problems is:
Technical scheme 1: technical scheme 1 solves the problem that impurity is got rid of and reduction hydrochloric acid consumes in the decomposing phosphate rock by chlorhydric acid.Technical scheme is: carry out low temperature, two sections leachings of low-concentration hcl.
In one section reaction, leaching temperature of reaction: normal temperature.
The phosphoric acid that contains a small amount of excessive hydrochloric acid-calcium chloride mixing solutions and the reaction of fresh ground phosphate rock of using two sections leachings to obtain, because temperature of reaction is low, solution acidic weak (mainly being phosphoric acid), therefore, times oxide compound is not gone up substantially and can be reacted, what mainly take place is the partial acidification reaction of carbonate and the reaction between the phosphoric acid and the tricalcium phosphate of calcium magnesium, as:
CaCO
3+2H
3PO
4＝Ca(H
2PO
4)
2+CO
2+H
2O
MgCO
3+2H
3PO
4＝Mg(H
2PO
4)
2+CO
2+H
2O
Ca
3(PO
4)
2+2H
3PO
4＝Ca(H
2PO
4)
2+2CaHPO
4
In the scope of the terminal point PH=0.1-3.5 of reaction.
Reaction times: 0.5-6 hour.
The result of these reactions is:
The lime carbonate and the magnesiumcarbonate overwhelming majority are decomposed and enter solution, and the tricalcium phosphate overwhelming majority in the phosphorus ore transforms into secondary calcium phosphate, and consumption mainly is phosphoric acid and a spot of hydrochloric acid excessive in second-stage reaction.Phosphoric acid in the solution changes into for monocalcium phosphate and continues to stay in the solution.A overwhelming majority times oxide compound continues to stay in the phosphorus ore residue.
After reaction is finished, add flocculation agent (0.1-0.5% polyacrylamide solution), postprecipitation stirs.
So far, one section reaction finishes.
Clear liquid removes the neutralization reaction groove, uses the neutralization of milk of lime or lime carbonate.
Neutral terminal point PH=2.5-6.0.
After neutralization is finished, use special flushing discharging pressure filter to filter, filtrate discharge or recovery calcium chloride.After filter cake washing dries up, crystalline mother solution after the Crystallization Separation finished product phosphoric acid salt that input recycles in flushing discharging pressure filter (for example, if production potassium primary phosphate, just import Crystallization Separation finished product potassium primary phosphate crystalline mother solution afterwards), use pressurized air stirs, all being modulated to uniform slurry, delivering to the conversion reaction groove and carry out conversion reaction attached to the filter cake on the filter plate.
The neutral principal reaction is:
Ca(H
2PO
4)
2+Ca(OH)
2＝2CaHPO
4+2H
2O
Magnesium is stayed in the solution, with P
2O
5Success separates.
Second-stage reaction carries out in such a way:
The phosphorus ore slag slurry of having got rid of clear liquid in one section reaction behind the flocculation sediment, 100-110% according to the reaction theory calculated amount adds hydrochloric acid, mixed concentration of hydrochloric acid 5-15%, continued stirring reaction 1-3 hour, after reacting completely, deliver to filter and filter to get rid of slag, filtrate is second-stage reaction solution, turns back to one section reaction and adds fresh ground phosphate rock again and react.
Temperature of reaction: normal temperature.
In second-stage reaction, because concentration of hydrochloric acid is low, temperature of reaction is low, and times oxide compound decomposition amount seldom continues to remain among the slag.
Technical scheme 2: technical scheme 2 solves the problem of directly using the various fine phosphates of producing above of intermediate (more purified secondary calcium phosphate, it also is a product) production.Technical scheme is: use the more purified secondary calcium phosphate reaction that has identical cationic bisul-phate and prepare above with the phosphoric acid salt that needs to produce, make dihydrogen phosphate, separate pure gypsum.
For example, during the production SODIUM PHOSPHATE, MONOBASIC, use sodium pyrosulfate.
When producing potassium primary phosphate, use sal enixum.
When producing primary ammonium phosphate, use monoammonium sulfate.
Direct and phosphatase reaction is made monocalcium phosphate.
Certainly, also can adopt double decomposition to produce other phosphoric acid salt, as potassium primary phosphate through the pilot process of SODIUM PHOSPHATE, MONOBASIC or primary ammonium phosphate.
Above-described bisul-phate can be corresponding bisulphate product salt, or use sulfuric acid and corresponding vitriol to react, the bisul-phate that obtains after the separating hydrogen chloride perhaps, directly uses sulfuric acid (perhaps other acid) and corresponding vitriol to react.
The reaction equation of above process is:
CaHPO
4+H
3PO
4＝Ca(H
2PO
4)
2
CaHPO
4+NaHSO
4＝NaH
2PO
4+CaSO
4
CaHPO
4+NH
4HSO
4＝NH
4H
2PO
4+CaSO
4
CaHPO
4+KHSO
4＝KH
2PO
4+CaSO
4
More than Fan Ying operational condition is:
Temperature: 30-100 ℃
PH＝0-5
The ingredients concentration of reaction: P
2O
5=100-400g/l.
Operation is to use round-robin to produce phosphatic crystalline mother solution input flushing discharging pressure filter, under pressurized air stirs, all CaHPO
4Filter cake washes from the screen plate upper punch, and modulation becomes uniform slurry, is transported to the conversion reaction groove, adds bisul-phate (perhaps vitriol+sulfuric acid or other acid) and carries out stirring reaction.
After-filtration is finished in reaction, promptly obtains more purified phosphate solution and pure gypsum.
Following processing just purifies and the Crystallization Separation problem, and is identical with general production method.
Technical scheme 3: the gypsum quantity that produces in technical scheme 2 has only general use sulfuric acid decomposing phosphate rock to produce 40% of phosphoric acid salt generation gypsum quantity, and content can reach more than 95%, can directly sell, perhaps be used for the production building and ornament materials as product.For outlet that further solves gypsum tailings and the added value that increases production, we have advised following technical proposals 3, and promptly gypsum transforms directly circulation and separates out the technical scheme of water-soluble potassium nitrogenous fertilizer.
Production process is:
Containing near ammonium chloride and the vitriolate of tartar concentration of reaching capacity that circulate, and added gypsum in the saturated circulating mother liquor of bicarbonate of ammonia, making itself and bicarbonate of ammonia (ammonification or not ammonification) reaction:
CaSO
4+NH
4HCO
3+NH
3＝(NH
4)
2SO
4+CaCO
3
CaSO
4+2NH
4HCO
3＝(NH
4)
2SO
4+CaCO
3+CO
2+H
2O
Filter to isolate purified lime carbonate, filtrate adds Repone K and bicarbonate of ammonia, filters and obtains the potassium-nitrogen fertilizer that main component is vitriolate of tartar and ammonium chloride, and filtering Recycling Mother Solution is proceeded the gypsum conversion reaction to the gypsum conversion tank.
Because the smaller solubleness of vitriolate of tartar and form double salt, common-ion effcet or the like factor, this process can be without evaporation concentration and directly circulation carry out, therefore in a large number save energy with reduce production costs.
The implement scale of above process is 100 tons of every days.
The invention has the beneficial effects as follows:
(1) use many mid low grade phosphate rock and the watery hydrochloric acid of impurity, employing two-step method decomposing phosphate rock can Reduce salt acid consumption about 30%, the impurity in the effective separation phosphorus ore directly makes pure phosphoric acid simultaneously Product salt (for example potassium dihydrogen phosphate), product quality can reach the same level of product that thermal phosphoric acid is produced, Since effective separation impurity, can realize the phosphorus yield more than 95%.
(2) in the situation of using watery hydrochloric acid, nitric acid etc. decomposing phosphate rock, owing to leach the P that2O
5Separate P in this process with mother liquor through coprecipitation mode2O
5Obtain simultaneously enrichment, therefore can use 5% with The diluted acid of upper concentration (comprising spent acid) and process meticulous phosphoric acid with the lower mid low grade phosphate rock of content Product salt can be realized the most sufficient resource utilization and maximum economic benefit.
(3) well-known, using any inorganic acid and phosphorus ore to react the purification of the phosphoric acid by wet process that makes and concentrate is very difficult thing, not only a P2O
5Loss is serious, and equipment corrosion is serious. The present invention avoids The process of phosphoric acid by wet process, directly produce various phosphate, process is simple, equipment corrosion no longer becomes Problem.
(4) by-product gypsum is containing near ammonium chloride and the potassium sulfate concentration of reaching capacity that circulate, and By in the saturated circulating mother liquor of carbonic hydroammonium with the carbonic hydroammonium reaction, separate out calcium carbonate, mother liquor and potassium chloride are anti-Should, in the presence of carbonic hydroammonium, directly separate out water-soluble potassium nitrogenous fertilizer, not only solved the gypsum problem of outlet, And directly separate out multiple fertile finished product without evaporation and concentration, a large amount of energy savings have reduced production cost.
(5) if making salt (nitre) acid, the waste liquid circulation of using sulfuric acid and neutralization to filter is used for decomposing phosphate rock, Then all calcium becomes the high-quality calcium carbonate that building material industry needs in a large number, the not headachy phosphorus of regeneration Gypsum is conducive to environmental protection, has solved simultaneously diluted acid source and transportation problem.
Total effect of all these usefulness can produce very high economic benefit and social benefit.
Claims (3)
1, a kind of method of using diluted acid decomposing medium and low grade direct production fine phosphate, it is characterized in that: use diluted acid to be divided into two sections decomposing phosphate rocks at normal temperatures, at first use the reaction of two sections leaching liquids and phosphorus ore, isolating solution removes the purified secondary calcium phosphate of neutralization preparation, use diluted acid to continue to decompose then through the phosphorus ore after one section leaching, remaining P
2O
5All leaching is come out, and leaching solution turns back to again that one section leaching is gone and the reaction of fresh breeze, and so circulation is carried out, and can save decomposition about 30% with acid, and effectively despumation.One section temperature of reaction is 0 to+50 ℃, and the pH value of reaction mass is controlled within the scope of 0.5-1.5,0.5-6 hour stirring reaction time.The second-stage reaction temperature is 0 to+50 ℃, and the pH value of reaction mass is controlled within the scope of 0.1-0.5,0.5-6 hour stirring reaction time, dilute acid concentration 〉=8%.P
2O
5Water-soluble transformation efficiency can reach more than 95%.
2, method according to claim 1, it is characterized in that: one section reaction leaching liquid uses the lime carbonate neutralization that circulation produces in milk of lime (CaO=80-150g/l) or this process, make purified secondary calcium phosphate, this secondary calcium phosphate directly transforms with sal enixum (sodium pyrosulfate, monoammonium sulfate or the like) reaction and makes the biphosphate product salt that needs.
The neutral reaction conditions is: can neutralize in a step (product all goes conversion to produce phosphoric acid salt) perhaps is divided into two steps neutralization (the first step neutralized product removes conversion production phosphoric acid salt, and the second step neutralized product is a calcium hydrophosphate fodder).
One step neutralization: normal temperature, terminal point PH=3.5-6.0.
Two steps neutralization: the first step: normal temperature, terminal point PH=1.5-2.0.
Second step: normal temperature, terminal point PH=3.5-6.0.
Conversion reaction conditions is: temperature: 0-100 ℃, and terminal point PH=0.5-4.0.Proportion scale is CaO: hydrosulfate=1:1 (mol ratio).
3, method according to claim 1, it is characterized in that: transform the gypsum circulate soln reaction saturated that generates with being chlorinated ammonium, vitriolate of tartar and bicarbonate of ammonia, in this circulate soln, introduce ammonium sulfate, separate lime carbonate simultaneously, this has been introduced the solution of ammonium sulfate and Repone K and bicarbonate of ammonia reaction and has directly separated out Water Soluble Compound fertilizer then, and the mother liquor of generation returns to initial composition and recycles once more.
The condition that gypsum transforms is: every cubic metre of circulate soln is handled 200-500 kilogram gypsum, temperature of reaction 20-80 ℃, terminal point PH=7.0-9.0.
The condition of separating out compound manure is: temperature 10-40 ℃, dissolving bicarbonate of ammonia quantity is 150-350g/l, and dissolving Repone K quantity is the 80-150% according to the theoretical amount of sulfate radical quantity calculating in the solution.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050642A (en) * | 2009-11-05 | 2011-05-11 | 徐杰 | Method for producing qualified calcium superphosphate fertilizer with low-grade phosphate ore |
| CN102923681A (en) * | 2012-09-26 | 2013-02-13 | 武汉新协达精细化工研发有限公司 | Method for directly preparing industrial monopotassium phosphate through low-grade phosphate ores by hydrochloric acid process |
| CN104724686A (en) * | 2015-03-13 | 2015-06-24 | 成都乐氏化工工程有限公司 | Method for preparing yellow phosphorus and co-producing potassium phosphate from potassium-containing phosphorus ore |
| JP2017505280A (en) * | 2013-12-02 | 2017-02-16 | エコフォス・エス・アー | Phosphate source for agriculture and food industry |
| CN108473309A (en) * | 2016-03-03 | 2018-08-31 | 矿产化工公司和欧洲化学公司联合股份公司 | solid phosphate and preparation method thereof |
| CN109231179A (en) * | 2018-11-28 | 2019-01-18 | 杨新艳 | A kind of potassium dihydrogen phosphate preparation method |
| CN109476484A (en) * | 2016-06-23 | 2019-03-15 | 普拉昂技术公司 | The method for preparing calcium sulfate |
| CN109835935A (en) * | 2017-11-27 | 2019-06-04 | 川恒生态科技有限公司 | Utilize the method for hydrochloric acid and Phosphate Rock acid calcium salt and high purity plaster |
| CN111187100A (en) * | 2020-01-07 | 2020-05-22 | 贵州芭田生态工程有限公司 | Beneficiation method for separating calcium and magnesium in medium-low-grade phosphorite, urea ammonium nitrate calcium magnesium fertilizer and ammonium sulfate magnesium fertilizer |
-
2007
- 2007-11-12 CN CNA2007101694306A patent/CN101434386A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050642A (en) * | 2009-11-05 | 2011-05-11 | 徐杰 | Method for producing qualified calcium superphosphate fertilizer with low-grade phosphate ore |
| CN102050642B (en) * | 2009-11-05 | 2013-07-17 | 徐杰 | Method for producing qualified calcium superphosphate fertilizer with low-grade phosphate ore |
| CN102923681A (en) * | 2012-09-26 | 2013-02-13 | 武汉新协达精细化工研发有限公司 | Method for directly preparing industrial monopotassium phosphate through low-grade phosphate ores by hydrochloric acid process |
| CN102923681B (en) * | 2012-09-26 | 2014-12-24 | 武汉新协达精细化工研发有限公司 | Method for directly preparing industrial monopotassium phosphate through low-grade phosphate ores by hydrochloric acid process |
| JP2017505280A (en) * | 2013-12-02 | 2017-02-16 | エコフォス・エス・アー | Phosphate source for agriculture and food industry |
| CN104724686A (en) * | 2015-03-13 | 2015-06-24 | 成都乐氏化工工程有限公司 | Method for preparing yellow phosphorus and co-producing potassium phosphate from potassium-containing phosphorus ore |
| CN108473309A (en) * | 2016-03-03 | 2018-08-31 | 矿产化工公司和欧洲化学公司联合股份公司 | solid phosphate and preparation method thereof |
| CN109476484A (en) * | 2016-06-23 | 2019-03-15 | 普拉昂技术公司 | The method for preparing calcium sulfate |
| CN109476484B (en) * | 2016-06-23 | 2022-07-15 | 普拉昂技术公司 | Method for preparing calcium sulfate |
| CN109835935A (en) * | 2017-11-27 | 2019-06-04 | 川恒生态科技有限公司 | Utilize the method for hydrochloric acid and Phosphate Rock acid calcium salt and high purity plaster |
| CN109231179A (en) * | 2018-11-28 | 2019-01-18 | 杨新艳 | A kind of potassium dihydrogen phosphate preparation method |
| CN111187100A (en) * | 2020-01-07 | 2020-05-22 | 贵州芭田生态工程有限公司 | Beneficiation method for separating calcium and magnesium in medium-low-grade phosphorite, urea ammonium nitrate calcium magnesium fertilizer and ammonium sulfate magnesium fertilizer |
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Open date: 20090520 |