CN103569980A - Production method of solid phosphoric acid - Google Patents
Production method of solid phosphoric acid Download PDFInfo
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- CN103569980A CN103569980A CN201210276488.1A CN201210276488A CN103569980A CN 103569980 A CN103569980 A CN 103569980A CN 201210276488 A CN201210276488 A CN 201210276488A CN 103569980 A CN103569980 A CN 103569980A
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Abstract
The invention belongs to the technical field of phosphoric acid production in inorganic chemical industry, and relates to a brand new production technology of solid phosphoric acid. The technical principle of the production method provided by the invention is as follows: the method comprises the following steps: stirring and mixing phosphoric acid and phosphorus pentoxide; maintaining a certain temperature; continuously adding phosphorus pentoxide and stirring to react; packing as soon as possible in a flowing state when concentration of phosphoric acid reaches 118-128%; naturally cooling at normal temperature and water-cooling; and after cooling to normal temperature, solidifying to generate block solid phosphoric acid. Compared with conventional common phosphoric acid, the packing, transporting and storing costs of the solid phosphoric acid produced by the method are greatly saved, and the safety performance is further greatly enhanced. Compared with crystal phosphoric acid, the solid phosphoric acid provided by the invention is lower in production cost, higher in production efficiency and yield, simpler in technological operation and higher in effective P2O5 content, and has a great practical value.
Description
Technical field
The invention belongs to the phosphoric acid production technical field in inorganic chemistry industry, is a kind of production technology of brand-new solid phosphoric acid.
Background technology
Phosphoric acid is a kind of basic chemical industry raw material of being used widely in all trades and professions, be usually used in the industries such as phosphoric acid salt, foodstuff additive, feed, agricultural chemicals, washing, electronics, medicine, water treatment, smelting, fire retardant, chemical fertilizer, also can be used for pigment, plating, antirust, sequestrant, anti-oxidant synergistic agent, sweetener etc.According to the impure number of phosphoric acid, generally phosphoric acid is divided into fertilizer grade, technical grade, food grade and electronic-grade.
At present, the phosphoric acid that national standard often refers to is containing H
3pO
4concentration is 75% to 85% liquid phosphoric acid, and multiplex dress phosphoric acid net weight is the plastic tank packing of 35kg, 330kg, the standard such as 1 ton.Its packing and transportation cost are high, and client stores inconvenience.Therefore, if change the physical aspect of phosphoric acid, the cost that just can greatly save packing, store and transport with packaged, storage and the transportation phosphoric acid of solid phosphoric acid, and solid phosphoric acid thin up can obtain the phosphoric acid of the various concentration specifications such as 75%, 85%, 95%, 105%, will be subject to people's welcome energetically.Up to now, all solid phosphoric acids of mentioning of pertinent literature report all refer under changing the conditions such as temperature the resulting crystal phosphoric acid of crystallization from saturated phosphoric acid solution.
Crystal phosphoric acid has two kinds, and a kind of is the crystal that contains crystal water, and molecular formula is H
3pO
4.1/2H
2o claims half water phosphoric acid crystal; That molecular formula is H not containing a crystal for crystal water
3pO
4claim phosphoric acid crystal.Half water phosphoric acid crystal is owing to containing crystal water, H in crystal
3pO
4theoretical Mass degree is 91.6%.The fusing point of half water phosphoric acid crystal is 29.32 ℃, and the fusing point of phosphoric acid crystal is 42.35 ℃.
China Patent Publication No. CN 101269804A, discloses " a kind of production method of high-purity phosphoric acid crystal ".Detailed process is with H
3pO
4mass percent is 96～99% for raw material, control temperature of charge in the time of 28～42 ℃, add the crystal seed that accounts for raw material acid quality 1～10%, insulation 0.1～2h, then cools to 26～35 ℃, is incubated after 0.5～2.5h, centrifuging, the crystal washing obtaining, obtain phosphoric acid crystal, then recrystallization is purified.
China Patent Publication No. CN 101531352A, discloses a kind of " by the method for phosphoric oxide to concentrate diluted phosphoric acid to prepare crystal polyphosphoric acid ", has introduced and has used P
2o
5make phosphoric acid enrichment, more cooling in crystallizer, add phosphoric acid crystal seed, stir, make phosphoric acid crystallization, centrifugation obtains crystal phosphoric acid product.
China Patent Publication No. CN 101544360A, discloses " a kind of preparation method of crystal phosphoric acid ", is that 85% phosphoric acid is directly cooling or concentrated rear cooling, adds crystal seed, stir, and slow cooling, growing the grain, centrifugation, can make crystal phosphoric acid.
China Patent Publication No. CN 101525128A, " a kind of production method of solid orthophosphoric acid " disclosed, by phosphoric acid evaporation concentration at 130～262 ℃, after under temperature is 60～130 ℃ and the condition that stirs, add hydrogen peroxide, reaction finishes, and product is down to after 10～28 ℃, the ortho-phosphoric acid crystal seed that adds raw material phosphoric acid quality 0.5%～1%, obtains solid orthophosphoric acid.
Russ P RU2209178 has also reported crystallization process.They make raw material with thermal phosphoric acid, first phosphoric acid are heated to 35～55 ℃, and being concentrated to density is 1.685g/cm
3above, be then cooled to 4～9 ℃, add crystal seed, crystallization 7～8h, and then be further cooled to 0～7 ℃, and continue growing the grain 50～70min, then centrifugation obtains crystal phosphoric acid.
Above solid phosphoric acid production method be all under changing the conditions such as temperature from saturated phosphoric acid solution crystallization produce crystal phosphoric acid, there is crystallisation process complex process, have in process of production the generation of a large amount of filtrate, the problem such as gained crystal phosphoric acid yield is very low.
Summary of the invention
The object of the invention is to overcome the shortcoming of aforesaid method and provide that a kind of technique is simple, easily industrialization, production cost is low, production efficiency is high, produce that yield is high, product is convenient to packing and the production method of the solid phosphoric acid of transportation.
Solid phosphoric acid of the present invention refers to from phosphoric acid form and is piece bulk solid phosphoric acid, different from crystallization phosphoric acid.
The main technique principle of a kind of brand-new solid phosphoric acid production method of the present invention is as follows:
Phosphoric acid and Vanadium Pentoxide in FLAKES are uniformly mixed, keep certain temperature, constantly add Vanadium Pentoxide in FLAKES stirring reaction, when the concentration of phosphoric acid reaches 118%～128%, packing, is cooled to normal temperature after coagulation to become piece bulk solid phosphoric acid at once.
The production method of above-mentioned a kind of brand-new solid phosphoric acid, wherein phosphoric acid is that the phosphoric acid by wet process of thermal phosphoric acid or purification, concentrate is raw material, concentration can be 75%～115%, wherein with the polyphosphoric acid of 95%～105% concentration for well.Polyphosphoric acid can be to produce with thermal phosphoric acid technique, and under cooling technology mode, yellow phosphorus and airborne oxygen combustion generate P
2o
5, the dilute phosphoric acid spray-absorption P for mode that adopts circulation to absorb
2o
5, dilute phosphoric acid concentration is brought up to more than 95%～105%; Polyphosphoric acid can be also to take Wet Phosphoric Acid Market to produce as raw material carries out concentrate polymerization.
The production method of above-mentioned a kind of brand-new solid phosphoric acid, wherein adds Vanadium Pentoxide in FLAKES and is uniformly mixed reaction mass temperature in process and remains on 80～150 ℃; The time that is uniformly mixed is at 1～10 hour, according to the differential responses times such as acid amount, mixing effect of once throwing can difference, when the concentration of phosphoric acid is 118%～128% time, can produce a desired effect after testing; The phosphoric acid of heat need to be under flow state packing as early as possible, can normal temperature naturally cooling, also can water-cooled, be cooled to normal temperature after coagulation to become piece bulk solid phosphoric acid; The phosphoric acid of heat in time after packing, while adopting water cooling mode, often need can drop to normal temperature, solidify out into piece bulk solid phosphoric acid after 1～10 hour.
The invention provides a kind of and diverse bulk solid phosphoric acid production technology of crystal phosphoric acid.The starting material that adopt are mainly polyphosphoric acid and Vanadium Pentoxide in FLAKES, and the major equipment of using is the stirred reactor of jacketed water-chilling plant.
Can, from comparing with the common phosphoric acid of tradition and with crystal phosphoric acid two aspects, illustrate that the advantage of the piece bulk solid phosphoric acid that the present invention produces is as follows:
First aspect, the advantage that the piece bulk solid phosphoric acid that the present invention produces is compared with the common phosphoric acid of tradition:
1, maximum advantage is that the packing cost of piece bulk solid phosphoric acid can save greatly.
The invention solves the high problem of packing cost of liquid phosphoric acid, the conventional dress of 85% phosphoric acid phosphoric acid net weight is the plastic tank packing of 35kg, 330kg, the standard such as 1 ton.Press 35kg plastic tank packing and calculate, 85% phosphoric acid per ton needs 28.57 of pail packs, and each presses 21 yuan of calculating of Vehicles Collected from Market valency, and packing cost per ton needs 600 yuan; Press 1000kg plastic tank packing and calculate, 85% phosphoric acid per ton needs 1 of pail pack, and each presses 900 yuan of calculating of Vehicles Collected from Market valency, and packing cost per ton needs 900 yuan; And make after 125% bulk solid phosphoric acid, pack 85% phosphoric acid per ton and be only equivalent to pack 0.68 ton of 125% bulk solid phosphoric acid, if pack with 27.2,25kg bag, in Vehicles Collected from Market valency, be about 1.4 yuan/, need 38.08 yuan, if with double casing, need altogether 76.16 yuan of packing costs, pack 85% phosphoric acid per ton and can save packing cost more than 520 yuan, save packing cost more than 86%, there is the very strong market competitiveness.
2, transportation cost can be saved greatly.
From transportation cost, also can greatly save, for example, sea-freight price to that port of savart, harbour, East Coast Savannah of the U.S. is 4500 dollars/27 tons, the ocean freight that 85% phosphoric acid per ton needs is 166.67 dollars, being equivalent to transport bulk solid phosphoric acid only needs 18.36 tons, and required ocean freight is 3060 dollars, and the ocean freight that is equivalent to transport 85% phosphoric acid needs per ton is only 113.33 dollars, it is 53.34 dollars that 85% phosphoric acid per ton can be saved ocean freight, transports cost-saved 32.00%.
3, can save storage cost, the safety performance that stores, transports also strengthens greatly.
Store 85% phosphoric acid per ton, be equivalent to store bulk solid phosphoric acid and only need 0.68 ton, storage capacity can reduce 32%, and storage cost can be saved naturally.
Liquid phosphoric acid rocks easy to leak; Solid phosphoric acid be solid-state, be difficult for rocking, stable, store, the safety performance of transportation strengthens greatly.Solid phosphoric acid does not need special container to store, easy to use, and solid phosphoric acid can, with water arbitrarily than dissolving each other, can meet the demand of client to the various concentration of phosphoric acid.
Second aspect, the advantage that the piece bulk solid phosphoric acid that the present invention produces is compared with crystal phosphoric acid:
1, solid phosphoric acid yield improves greatly.Provided by the present invention bulk solid phosphoric acid production technology, input polyphosphoric acid and phosphorus pentoxide raw material can all be converted into piece bulk solid phosphoric acid product; And crystal phosphoric acid has the generation of a large amount of filtrate in process of production, gained crystal phosphoric acid yield is lower.
2, effective P of unit mass product
2o
5content is higher than crystal phosphoric acid.In phosphoric acid crystal, half water phosphoric acid crystal is owing to containing crystal water, H in crystal
3pO
4theoretical Mass degree is 91.6%, effectively P
2o
5content is 66.4%; H in anhydrous phosphoric acid crystal
3pO
4content is 100%, effectively P
2o
5content is 72.4%.And H in the piece bulk solid phosphoric acid that the present invention produces
3pO
4theoretical Mass degree can reach 125%, effectively P
2o
5content can reach 90.6%, the phosphoric acid of unit mass product, effective P
2o
5content will exceed 25% than positive crystal phosphoric acid, than half water phosphoric acid crystal, will exceed 27.4%.
3, technique more simply, more easy to operate, only need stirring reaction, greatly reduced processing step and difficulty, reduced productive labor intensity, improved working condition; Crystal phosphoric acid produce be under concentrating, heat, add the conditions such as crystal seed, cooling from saturated phosphoric acid solution crystallization produce crystal phosphoric acid, crystallisation process complex process.
Accompanying drawing explanation
Fig. 1 is the production technological process of a kind of brand-new solid phosphoric acid production method of the present invention.
Embodiment
Below by embodiment, the present invention is specifically described.Be necessary to be pointed out that at this following examples are only for further illustrating that the present invention is carried out; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the invention described above content.Raw material phosphor acid concentration used can be 75% to 115%.
Embodiment 1
In the cooling stirred reactor of jacketed, first add 115% concentration polyphosphoric acid 1800kg, in the situation that constantly stirring, add Vanadium Pentoxide in FLAKES 1260kg, after 3 hours, it is 124.8% that sampling records product phosphorus acid content, stop stirring, open valve discharging, phosphoric acid can comparatively fast flow out, flow is little, with bag, pack, sack is harmless at once, and outside is cooling with cold water.Install sealing, be placed in water, the temperature of the outer water coolant of sack rises very slow, after 3 hours, takes out placement, and phosphoric acid has no longer had mobility, while arriving 30 ℃ of room temperatures, has been generated as piece bulk solid phosphoric acid completely.
Embodiment 2
In the cooling stirred reactor of jacketed, first add 95% concentration polyphosphoric acid 1000kg, in the situation that constantly stirring, add Vanadium Pentoxide in FLAKES 2000kg, after 4 hours, it is 123.1% that sampling records product phosphorus acid content, stops stirring, open valve discharging, phosphoric acid can comparatively fast flow out, and packs with bag at once, and outside is with cold water is not cooling.Install sealing, naturally place, second day is observed, and has been generated as piece bulk solid phosphoric acid completely.
Embodiment 3
In the cooling stirred reactor of jacketed, first add 105% concentration polyphosphoric acid 1000kg, in the situation that constantly stirring, add Vanadium Pentoxide in FLAKES 1000kg, after 3 hours, it is 121% that sampling records product phosphorus acid content, stop stirring, open valve discharging, phosphoric acid can comparatively fast flow out, and flow is little, with bag, pack, outside is cooling with cold water at once.Install sealing, be placed in water, after 2 hours, take out placement, phosphoric acid has no longer had mobility, while arriving 28 ℃ of room temperatures, has been generated as piece bulk solid phosphoric acid completely.
Claims (3)
1. the production method of a solid phosphoric acid, it is characterized in that, main technique principle is that phosphoric acid and Vanadium Pentoxide in FLAKES are uniformly mixed, keep certain temperature, constantly add Vanadium Pentoxide in FLAKES, when the concentration of phosphoric acid reaches 118%～128%, packing, is cooled to normal temperature after coagulation to generate piece bulk solid phosphoric acid at once.
2. the production method of solid phosphoric acid according to claim 1, is characterized in that, raw material phosphoric acid is the phosphoric acid by wet process that adopts thermal phosphoric acid or purification, concentrate, and concentration can be 75%～115%, wherein with the polyphosphoric acid of 95%～105% concentration for well.
3. the production method of solid phosphoric acid according to claim 1, is characterized in that, adds Vanadium Pentoxide in FLAKES and is uniformly mixed reaction mass temperature in process and remains between 80～150 ℃; When the concentration of phosphoric acid is 118%～128% time, can produce a desired effect after testing.The phosphoric acid of heat need to be under flow state packing as early as possible, can normal temperature naturally cooling, also can water-cooled, be cooled to can solidify out into piece bulk solid phosphoric acid after normal temperature.
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| CN201210276488.1A CN103569980A (en) | 2012-08-06 | 2012-08-06 | Production method of solid phosphoric acid |
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|---|---|---|---|
| CN201210276488.1A CN103569980A (en) | 2012-08-06 | 2012-08-06 | Production method of solid phosphoric acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113716537A (en) * | 2021-08-31 | 2021-11-30 | 云南云天化股份有限公司 | Preparation method of powdery solid phosphoric acid |
| CN113896693A (en) * | 2021-09-08 | 2022-01-07 | 云南云天化股份有限公司 | Preparation method of polyphosphoric acid piperazine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525128A (en) * | 2009-04-08 | 2009-09-09 | 瓮福（集团）有限责任公司 | Production method of solid orthophosphoric acid |
| CN101531352A (en) * | 2009-04-22 | 2009-09-16 | 瓮福（集团）有限责任公司 | Method for using phosphoric oxide to concentrate diluted phosphoric acid to prepare crystal polyphosphoric acid |
| CN101531354A (en) * | 2009-04-22 | 2009-09-16 | 瓮福（集团）有限责任公司 | Method for using phosphoric oxide to concentrate diluted phosphoric acid to prepare polyphosphoric acid |
-
2012
- 2012-08-06 CN CN201210276488.1A patent/CN103569980A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525128A (en) * | 2009-04-08 | 2009-09-09 | 瓮福（集团）有限责任公司 | Production method of solid orthophosphoric acid |
| CN101531352A (en) * | 2009-04-22 | 2009-09-16 | 瓮福（集团）有限责任公司 | Method for using phosphoric oxide to concentrate diluted phosphoric acid to prepare crystal polyphosphoric acid |
| CN101531354A (en) * | 2009-04-22 | 2009-09-16 | 瓮福（集团）有限责任公司 | Method for using phosphoric oxide to concentrate diluted phosphoric acid to prepare polyphosphoric acid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113716537A (en) * | 2021-08-31 | 2021-11-30 | 云南云天化股份有限公司 | Preparation method of powdery solid phosphoric acid |
| CN113896693A (en) * | 2021-09-08 | 2022-01-07 | 云南云天化股份有限公司 | Preparation method of polyphosphoric acid piperazine |
| CN113896693B (en) * | 2021-09-08 | 2024-01-02 | 云南云天化股份有限公司 | Preparation method of piperazine polyphosphate |
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Application publication date: 20140212 |