CN1096273A - Method for producing phosphoric acid by directly reducing phosphate ore - Google Patents
Method for producing phosphoric acid by directly reducing phosphate ore Download PDFInfo
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- CN1096273A CN1096273A CN 93111447 CN93111447A CN1096273A CN 1096273 A CN1096273 A CN 1096273A CN 93111447 CN93111447 CN 93111447 CN 93111447 A CN93111447 A CN 93111447A CN 1096273 A CN1096273 A CN 1096273A
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- phosphoric acid
- rock phosphate
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Abstract
A process for preparing phosphoric acid by direct reduction of phosphorus ore features that the phosphorus ore, silica, carbonaceous reducing agent and adhesive are used to prepare double-layer composite pellets, and the CaO/SiO ratio of inner pellet is controlled2The mol ratio ensures that the melting point of the pellets is higher than the carbothermic reduction temperature of the phosphorite, the pellets on the outer layer are carbon-containing materials, the carbon in the pellets on the inner layer is protected from being oxidized too early in the flame furnace, and the carbon is used as fuel to provide energy for maintaining the temperature of the flame furnace. The pellet is put into a flame furnace for reduction and oxidation, so that P in the pellet can be reduced2O5The volatility is more than 80 percent, and the product will contain P2O5The kiln gas is hydrated to prepare the phosphoric acid.
Description
The present invention relates to prepare the technology of phosphoric acid.
The method of suitability for industrialized production phosphoric acid mainly contains two kinds in the world at present: (1). sulfuric acid extraction process: promptly utilize Rock Phosphate (72Min BPL) and vitriolic replacement(metathesis)reaction, generate phosphoric acid and calcium sulfate and obtain phosphoric acid.This method needs the phosphorus ore of the low impurity of higher-grade and a large amount of sulfuric acid; (2). electric furnace yellow phosphorus method: promptly produce yellow phosphorus, generate P with air combustion yellow phosphorus then with electric furnace
2O
5, water absorbs and produces phosphoric acid again.This method needs a large amount of electric energy and blocky Rock Phosphate (72Min BPL).
Reduce influence year by year in order to overcome electric energy anxiety, ferro-sulphur ore deficiency and higher-grade Rock Phosphate (72Min BPL) to phosphoric acid production, early eighties U.S. Occidental Research Corporation(ORC) propose to adopt the KPA method promptly to produce the method for phosphoric acid with rotary kiln, (see industrial and Engineering chemistry process Design and Development magazine, 1985, the 24th phase, 688～697 pages), and carried out in the φ 0.84 * interim test of 9.14 meters rotary kiln pilot plants, (US patent No.4,389,384).Its method is with Rock Phosphate (72Min BPL), silica and carbonaceous reducing agent (coke powder or coal dust) fine grinding to 50～85%-325 order, ball is made in swelling with addition of 1% with local methods, behind chain type drying machine drying and preheating, send in the rotary kiln of kiln hood gas-firing, pelletizing reduces in kiln, controlling high solid temperature is 1400～1500 ℃, adjusts pelletizing CaO/SiO
2Mol ratio is 0.26～0.55, make the pelletizing fusing point be higher than the carbothermic reduction temperature of Rock Phosphate (72Min BPL) in the pelletizing, phosphorus comes out with form reduction volatilization from pelletizing of phosphorus steam, and the atmospheric oxygen that is passed in the central space of kiln changes into Vanadium Pentoxide in FLAKES then, and the heat that oxidation is emitted is supplied with reduction conversely again.The kiln gas aquation that will contain Vanadium Pentoxide in FLAKES absorbs and promptly makes phosphoric acid.
Producing the technical subject matter that runs into of phosphoric acid with rotary kiln is: (1). owing to contain a large amount of CO in the rotary kiln kiln gas
2With H
2Following reaction, will take place with the carbon allocated in the pelletizing skin in O steam after temperature is greater than 800 ℃:
To making carbon i.e. a large amount of oxidations of quilt before pelletizing is heated to reduction temperature (greater than 1250 ℃) of allocating in the pelletizing skin.Because the loss of the outer carbon of pelletizing makes that the Vanadium Pentoxide in FLAKES in the outer Rock Phosphate (72Min BPL) of pelletizing can not be reduced.In addition, losing under the carbon situation P in pelletizing and kiln gas
2O
5When contacting, will generate phosphoric acid salt again, make the outer white shell of the rich phosphorus of one deck that generates of pelletizing, to the P that makes technology
2O
5Yield reduces greatly.(2). process using carbon-burdened pellet scheme, for fear of the oxidation of carbon, the pelletizing consolidation temperature can not be higher than the oxidizing temperature of carbon.KPA process using bentonite is made binding agent, and pellet strength is difficult to guarantee.Pelletizing is easily efflorescence in rotary kiln, and the part Rock Phosphate (72Min BPL) is separated with silica, carbonaceous reducing agent, has both influenced the reduction of Rock Phosphate (72Min BPL), produces ring formation at rotary kiln preheating section again, destroys the normal operation of technology, and acid causes difficulty to the kiln gas receipts to increase the dust amount of blowing out simultaneously.(3). rotary kiln needs with gas or liquid fuel heat supply, and price is more expensive, has increased the production cost of phosphoric acid.For preventing the outer carbon of pelletizing premature oxidation problem in rotary kiln, ORC company once proposed: feed rare gas element by the kiln body by the bed of material, form a transition isolation strip between the rotary kiln bed of material and oxidation zone, stop oxidation (the US patent No.4 of kiln gas to pelletizing carbon, 351,813); In going into the stove pelletizing, sneak into free burnt grain,, stop the oxidation of kiln gas carbon in the pelletizing between the bed of material and oxidation zone, to form a free burnt grain sealing coat; Add pelletizing with phosphoric acid or Sodium Tetraborate silica flux, make pelletizing form a sealing ply, stop the oxidation (US patent No.4,397,826) of kiln gas carbon in the pelletizing at 700～1100 temperature lower surfaces.
The objective of the invention is to: adopt and a kind ofly directly reduce the technology that Rock Phosphate (72Min BPL) produces phosphoric acid with the two-layer compound pelletizing, the pellet strength that overcomes the existence of kiln-process phosphoric acid technology is poor, carbon is in the problem of preheating in rotary kiln band premature oxidation in the pelletizing, make pelletizing not efflorescence in kiln, the Vanadium Pentoxide in FLAKES yield is greater than 80% in the pelletizing, replace or partly replace gas or liquid fuel simultaneously with solid fuel, to reduce the phosphoric acid production cost.
Technical solution of the present invention is: with Rock Phosphate (72Min BPL) with allocate material into and make pelletizing, in flame furnace, P in the pelletizing
2O
5Be reduced into phosphorous vapor and volatilization, the atmospheric oxidation that phosphorous vapor is introduced in the stove above the bed of material generates P
2O
5Gas is absorbed in the aquation device and changes into phosphoric acid.Special character of the present invention is: pelletizing adopts two-layer composite.Its internal layer is through grinding, making ball behind the mixing and form with Rock Phosphate (72Min BPL), silica (or lime or Wingdale), carbonaceous reducing agent, its skin is to wrap one deck carbon content again greater than 20% solid fuel on this pelletizing, add binding agent during pelletizing ectonexine batching, pelletizing adopts drying and consolidating.
This pelletizing internal layer CaO/SiO
2The mol ratio can be less than 0.6 or greater than 6.5, and carbonaceous reducing agent is 1～3 times of reduction Rock Phosphate (72Min BPL) theoretical amount, and the outer solid fuel dosage of pelletizing can be 5%～25% of internal layer pelletizing weight; The binding agent that the pelletizing ectonexine adds can be one of following seven kinds or combination therebetween, i.e. pitch, Sodium salts humic acids, ammonium humate, water glass, cellulose lye, syrup, sulfonated lignin.Addition is the 0.2～15%(butt that is added weight of material).This pelletizing can adopt drying and consolidating, and consolidation temperature is 80～600 ℃, and consolidation time is 3～120 minutes.
The reason of technique scheme is: with Rock Phosphate (72Min BPL), silica (or lime), carbonaceous reducing agent is through grinding, once making ball after the batching, mixing.Add binding agent during the system ball to guarantee pellet strength.Control pelletizing CaO/SiO
2Mol is than less than 0.6 or greater than 6.5, makes the pelletizing fusing point be higher than the carbothermic reduction temperature of Rock Phosphate (72Min BPL) in the pelletizing, to avoid pelletizing soft heat in flame furnace.This pelletizing is carried out secondary system ball, promptly on this pelletizing, wrap up in one deck solid fuel again.In solid fuel, can add simultaneously and contain SiO
2, Al
2O
3, CaO etc. material, make its carbothermic reduction temperature to adjust solid-fuelled ash fusion point greater than Rock Phosphate (72Min BPL) in the pelletizing.Add binding agent during the system ball, so that outer solid fuel can be well attached on the internal layer pelletizing.This two-layer compound pelletizing drying is sent in the flame furnace after fixed, pelletizing is heated to above the carbothermic reduction temperature of Rock Phosphate (72Min BPL) in the pelletizing, the P in the internal layer pelletizing
2O
5Will be according to reaction formula (1), (2)
(work as CaO/SiO
2The mol ratio was less than 0.6 o'clock) (1)
(work as CaO/SiO
2The mol ratio is greater than 6.5) (2)
Become phosphorous vapor by carbon reduction, following oxidizing reaction takes place at flame furnace central space and the extraneous oxygen-containing gas that feeds in phosphorous vapor that reaction produces and CO:
The heat that oxidizing reaction is emitted satisfies the required heat of phosphorus ore heat absorption reduction reaction also has a surplus, and can make full use of this part heat and be used for reduction in flame furnace.The pelletizing skin is one deck carbon solid fuel.In flame furnace, when pelletizing is exposed to charge level, following reaction will take place with furnace gas in pelletizing top layer material:
Because can providing, the pelletizing skin enough satisfies reaction (5), (6), and therefore the carbon amount that (7) are required, has protected the reduction and carbonization in the internal layer pelletizing not oxidized, guarantees to react (1) or (2) and can carry out fully.In addition, because the pelletizing skin has carbon to have P in kiln gas
2O
5When contacting,, promptly be reduced into P again according to (7) formula with pelletizing
4↑, this has just prevented P in the kiln gas that the phosphoric acid salt back suction causes
2O
5P in the pelletizing is guaranteed in loss
2O
5Yield is greater than 80%.
By reaction formula (5), (6), (7) as can be known, carbon gasification in the solid fuel can be become geseous fuel CO to enter the oxidation zone fuel of flame furnace by these reactions, keep the temperature required energy of pelletizing reduction reaction to replenish, thereby the cancellation or the reduction of trying one's best need other more expensive gas or the liquid fuel of price that adds to flame furnace in order to keep the pelletizing reduction temperature, the production cost of phosphoric acid is reduced.
Example
Raw materials used chemical ingredients: Rock Phosphate (72Min BPL) contains P
2O
525%, silica contains SiO
298%, coke powder contains fixed carbon 75%, and three kinds of raw materials are pressed CaO/SiO
2The mol ratio is 0.4, and mixed carbon comtent is P in the Rock Phosphate (72Min BPL)
2O
51.5 times of batchings of theory of reduction amount add water system ball, pelletizing moisture content 12%, pelletizing particle diameter 10～16mm after mix grinding to granularity reaches-200 orders＞80% remix, 2% Sodium salts humic acids binding agent.Above-mentioned pelletizing is carried out secondary make ball, wrap one deck-200 order greater than 80% coke powder.Coke powder weight is 10% of pelletizing weight.With the pelletizing of above-mentioned chemical ingredients and physical specification at 100 ℃ of following drying and consolidatings, send in the φ 0.8 * 10 meters radial ventilation rotary kiln, the pelletizing reduction temperature is 1300 ℃ in the control kiln, and material stopped in kiln 1.5 hours, the evaporation rate of phosphorus is greater than 80%, with the P that contains that produces in the pelletizing
2O
5The kiln gas body carries out aquation and absorbs, and makes concentration for containing H
3PO
485% phosphoric acid.
The advantage that the present invention has and the effect of generation are: (1) pellet strength height, the finished ball intensity index can reach: dropping strength is greater than 20 times/meter, ultimate compression strength is greater than 25Kg/ ball, and abrasion resistance index (0.5mm) less than 1.3%, thereby guarantees that pelletizing is in not efflorescence of rotary kiln.(2) by adjusting the CaO/SiO of internal layer pelletizing
2Mol ratio and outer solid-fuelled ash fusion point make pelletizing soft heat point be higher than the carbothermic reduction temperature of Rock Phosphate (72Min BPL) in the pelletizing, guarantee pelletizing not soft heat in flame furnace.(3) carbonaceous reducing agent on the one hand phosphorus supply ore reduction in the internal layer pelletizing used of the outer field solid fuel of pelletizing shields, and makes it not by the O in the kiln gas
2, CO
2And H
2The O vapor-phase oxidation guarantees that the carbothermic reduction of Vanadium Pentoxide in FLAKES in the internal layer pelletizing can be carried out smoothly, and the Vanadium Pentoxide in FLAKES yield can utilize the O in the kiln gas again on the other hand greater than 80% in the pelletizing
2, CO
2, H
2O steam and P
2O
5With the gasification reaction that the outer solid fuel of pelletizing takes place, generate CO and offer flame furnace as the energy of keeping the pelletizing reduction temperature.(4) infeed oxygen-containing gas by the flame furnace airduct, CO that in bed of material upper area and pelletizing, produces and phosphorous vapor generation oxidizing reaction, the supply heat is given the bed of material, satisfy the needs of reduction reaction, thereby remove or reduce gas or the liquid fuel that infeeds flame furnace by the outside as far as possible, reduced the phosphoric acid production cost of technology.
Claims (5)
1, a kind of direct reduction Rock Phosphate (72Min BPL) is produced the method for phosphoric acid, its process be with Rock Phosphate (72Min BPL) with allocate material into and make pelletizing, in flame furnace, P in the pelletizing
2O
5Be reduced into phosphorous vapor and volatilization, the atmospheric oxidation that phosphorous vapor is introduced in the stove above the bed of material generates P
2O
5Gas, P in the aquation device
2O
5Be absorbed into phosphoric acid.It is characterized in that: pelletizing is made two-layer composite, that is: internal layer be with Rock Phosphate (72Min BPL), silica (or lime or Wingdale), carbonaceous reducing agent through grinding, make pelletizing after the batching, mixing and form, skin is to wrap up in one deck carbon content again (can add and contain SiO greater than 20% solid fuel on this pelletizing
2, Al
2O
3, material such as CaO solid fuel), add binding agent during pelletizing ectonexine batching, pelletizing adopts drying and consolidating.
2, according to the method for the described production phosphoric acid of claim 1, it is characterized in that: pelletizing internal layer CaO/SiO
2Mol than＜0.6 or＞6.5, the dosage of carbonaceous reducing agent is managed 1～3 times of senior amount for the reduction Rock Phosphate (72Min BPL).
3, according to the method for the described production phosphoric acid of claim 1, it is characterized in that: the outer solid fuel dosage of pelletizing is 5%～25% of an internal layer pelletizing weight.
4, according to the method for the described production phosphoric acid of claim 1, it is characterized in that: the binding agent that the pelletizing ectonexine adds can be one of following seven kinds or combination therebetween, be pitch, Sodium salts humic acids, ammonium humate, water glass, cellulose lye, syrup, sulfonated lignin, addition is the 0.2～15%(butt that is added weight of material).
5, according to the method for the described production phosphoric acid of claim 1, it is characterized in that: pelletizing drying and consolidating temperature is 80～600 ℃, consolidation time 3～120 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93111447A CN1040199C (en) | 1993-06-11 | 1993-06-11 | Method for producing phosphoric acid by directly reducing phosphate ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93111447A CN1040199C (en) | 1993-06-11 | 1993-06-11 | Method for producing phosphoric acid by directly reducing phosphate ore |
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| Publication Number | Publication Date |
|---|---|
| CN1096273A true CN1096273A (en) | 1994-12-14 |
| CN1040199C CN1040199C (en) | 1998-10-14 |
Family
ID=4989230
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93111447A Expired - Lifetime CN1040199C (en) | 1993-06-11 | 1993-06-11 | Method for producing phosphoric acid by directly reducing phosphate ore |
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| CN100342041C (en) * | 2006-01-10 | 2007-10-10 | 许贵宾 | Method for making fluxed iron ore powder composite pellet |
| WO2008043222A1 (en) * | 2006-09-30 | 2008-04-17 | Hubei Sanxin Phosphoric Acid Co. Ltd | Method for directly producing phosphoric acid and several silicate or aluminate byproducts from phosphate ore raw materials |
| CN100390091C (en) * | 2006-04-14 | 2008-05-28 | 湖北三新磷酸有限公司 | Method for preparing phosphoric acid and byproduct building brick by using phosphatic ore tailings after phosphate ore dressing |
| WO2009152643A1 (en) * | 2008-06-19 | 2009-12-23 | 鞍钢股份有限公司 | An additive used in secondary refining process, the producing method and the application thereof |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4351813A (en) * | 1981-05-20 | 1982-09-28 | Occidental Research Corporation | Process for producing phosphorus pentoxide or phosphorus or phosphoric acid |
| CN1003367B (en) * | 1985-06-14 | 1989-02-22 | 广西磷酸盐化工厂 | Prodn. of phosphoric acid by combustion of lean phosporus mud in rotary kiln |
| CN1023862C (en) * | 1989-01-14 | 1994-02-23 | 化学工业部化肥工业研究所 | Preparation of phosphorus by frunace |
| CN1026403C (en) * | 1990-03-22 | 1994-11-02 | 冶金工业部长沙矿冶研究院 | Method for producing phosphoric acid by special-shaped rotary kiln |
-
1993
- 1993-06-11 CN CN93111447A patent/CN1040199C/en not_active Expired - Lifetime
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| WO2009152643A1 (en) * | 2008-06-19 | 2009-12-23 | 鞍钢股份有限公司 | An additive used in secondary refining process, the producing method and the application thereof |
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