CN104085866A - Production method for improving quality and yield of phosphoric acid - Google Patents
Production method for improving quality and yield of phosphoric acid Download PDFInfo
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- CN104085866A CN104085866A CN201410163783.5A CN201410163783A CN104085866A CN 104085866 A CN104085866 A CN 104085866A CN 201410163783 A CN201410163783 A CN 201410163783A CN 104085866 A CN104085866 A CN 104085866A
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- phosphoric acid
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Abstract
The invention discloses a production method for improving the quality and the yield of phosphoric acid. The method comprises drying and calcining operations, phosphate ores obtained after natural ore drying, calcining and purifying undergo wet phosphoric acid production as a raw material, and the content of impurities in the above obtained byproduct phosphogypsum is low, so the obtained phosphogypsum can be directly used as industrial gypsum. The method for producing phosphoric acid by drying the natural phosphate ore, calcining and carrying out heat treatment overcomes the disadvantages of the prior art. The method enabling the natural phosphate ores to be dried and calcined improves the activity of the reaction of P2O5 in the natural phosphate ores with sulfuric acid, so the reaction is full, the output of phosphoric acid is increased, impurities in sulfuric acid can be reduced, and sulfuric acid can be used in a grading manner; and the byproduct phosphogypsum can be directly used as the industrial gypsum due to a small content of phosphorus, so the problems of large occupied area and low utilization of phosphogypsum are solved.
Description
Technical field
The present invention relates to a kind of method of preparing phosphoric acid, be specifically related to a kind of production method that improves phosphoric acid quality and yield.
Background technology
Phosphoric acid that (sulfuric acid, nitric acid, hydrochloric acid etc.) decomposing phosphate rock makes is referred to as phosphoric acid by wet process, and with the method for sulfuric acid decomposing phosphate rock preparing phosphoric acid be topmost method in Wet-process Phosphoric Acid Production.[main component is to use the natural phosphorus ore of vitriolization
] decompose, generate the calcium sulfate precipitation of phosphoric acid solution and insoluble.Its total chemical equation is as follows:
Reaction is carried out in two steps.The first step is that phosphorus ore and circulation slip (or phosphoric acid of retrieval system) carry out top decomposition reaction, contains phosphoric acid and internal circulating load very large in the slip of circulation, and first phosphorus ore is dissolved in and in excessive phosphoric acid solution, generates mono-calcium phosphate:
(CaSO
42H
2o), calcium sulphate hemihydrate (CaSO
4.
h
2and anhydrous calciumsulphate (CaSO O)
4) three kinds, therefore above-mentioned CaSO
4nH
2n in O can equal 2,1/2 or 0.In correspondingly producing, there is i.e. two water thing methods, half water thing method and the anhydride method of three kinds of basic skills.The HF generating in reaction with phosphorus ore in the SiO that brings into
2generate H
2siF
6.
Again with SiO
2reaction generates SiF
4gas.
SiF
4form exist, after water absorbs, generate fluorine silicic acid aqueous solution and also separate out silica gel precipitation
CO
2。
Existing phosphoric acid by wet process uses natural crystal (or through coal preparation) as raw material, makes phosphoric acid with strong inorganic acid (mainly using sulfuric acid) decomposing phosphate rock, still in this process, and the carbonate in natural crystal, iron, aluminium, sodium, potassium, silicofluorides etc. have also been brought in phosphoric acid in vitriolization process, cause the activity of the Vanadium Pentoxide in FLAKES that strong inorganic acid decomposing phosphate rock makes not high, and Wet-process Phosphoric Acid Production yield is on the low side, and purity is not high, and phosphoric acid by wet process product foreign matter content is high, and impurity existing way is very complicated, is unfavorable for the downstream application of phosphoric acid by wet process, and is that in byproduct phosphogypsum, phosphorus content is high in company with what bring, and contain Calcium Fluoride (Fluorspan), iron, aluminum compound, acid non-soluble substance, the plurality of impurities such as organic matter, the utilization of these impurity effect phosphogypsums, makes phosphogypsum can only be taken as refuse and abandons, and the problem phosphogypsum slag causing like this takies a large amount of soils, and the 2nd, stockyard investment is large, operating charges is high, and the 3rd, waste valuable sulphur resource, the 4th, contaminate environment.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, providing a kind of dries natural Rock Phosphate (72Min BPL), the ground phosphate rock after heat treatment obtaining after calcining and sulfuric acid reaction carry out the method for Wet-process Phosphoric Acid Production, the method is dried natural Rock Phosphate (72Min BPL), calcining is decomposed Rock Phosphate (72Min BPL), be exactly to control the purity in reaction source to reach the object of subsequent control phosphoric acid quality, the method is conducive to wet-process phosphoric acid reaction, improve phosphoric acid output, having simplified phosphoric acid is the pure operation that classification utilizes, phosphorus content and foreign matter content in byproduct phosphogypsum have been reduced simultaneously, making phosphogypsum can directly be used as industrial gypsum uses, solve that Wet-process Phosphoric Acid Production yield was on the low side in the past, phosphoric acid by wet process product foreign matter content is high, and impurity existing way is very complicated, be unfavorable for the problem of the downstream application of phosphoric acid by wet process, and byproduct phosphogypsum can also be directly used in industrial gypsum, solved existing phosphoric acid by wet process byproduct phosphogypsum deposit take up an area large, utilize the low problem that easily causes environmental pollution.
For achieving the above object, the present invention by the following technical solutions:
Be raw material by the ground phosphate rock obtaining after natural Rock Phosphate (72Min BPL) drying, calcining, adopt Wet-process Phosphoric Acid Production method sulfuric acid and the reaction of described ground phosphate rock to produce.Because the existence of P and Ca is not limited to Ca in natural Rock Phosphate (72Min BPL)
3(PO
4)
2form, and have the compound that a lot of other materials (as carbonate combines) mix to obtain phosphoric acid by wet process through similarly reacting, ore is carried out to the complex construction that dynamic calcining has decomposed natural crystal in certain degree, obtain comparatively single tricalcium phosphate structure, improved the P in natural crystal
2o
5activity, thus make it can fully react and reduce foreign matter content with sulfuric acid, be beneficial to fully carrying out of later stage wet-process phosphoric acid reaction.
Described drying process is flash drying, adopts screw feeder to be conveyed in moisture eliminator and to pass into hot blast in moisture eliminator containing wet ground phosphate rock, obtains phosphorus ore dry powder through warm air drying, with tornado dust collector collection phosphorus ore dry powder;
Calcination process is dynamic calcining operation, to after the phosphorus ore dry powder preheating obtaining after dry, send in calcining furnace, pass into again high-temperature flue gas, high-temperature flue gas drives the phosphorus ore dry powder obtaining after flash drying and high-temperature flue gas is mixed and is moved upward, and described phosphorus ore dry powder makes the described phosphorus ore dry powder calcining temperature that is rapidly heated obtain the raw materials for production ground phosphate rock of phosphoric acid by wet process through sack cleaner and tornado dust collector combination dedusting after fully calcined through the rapid dispersion effect moment matter heat exchange of the high-temperature flue gas in calcining furnace.
Inlet temperature in described flash drying is 280 DEG C-600 DEG C, 50 DEG C-300 DEG C of the temperature outs of described flash drying.
The calcining temperature of described calcination process is 720 DEG C-1050 DEG C, and described phosphorus ore dry powder is 1-10s at calcining residing time in furnace.In when calcining, how to control the CO in the removal Rock Phosphate (72Min BPL) that calcining process can be effective and reasonable
2, F, organism etc. be key of the present invention.It is exactly to be beneficial to the quality and the yield that improve phosphoric acid that organic matter removal also has a large advantage, organic constitution complexity, after Rock Phosphate (72Min BPL) is by vitriolization, more complex compounds are generated, and the complexity of phosphoric acid by wet process aftertreatment is just the complicacy of impurity, too the impurity of multiple types has had a strong impact on the selection of removal of impurities method of purification, thereby to select the purity of controlling product from source be main thought of the present invention.Calcining process of the present invention is that the variation of these three parameters can have influence on the variation of the constituent content in Rock Phosphate (72Min BPL) in the control of temperature, calcination time, wind speed, and then has influence on the quality of follow-up phosphoric acid.
The speed of described hot blast is 10-15m/s.
The heat of the tail gas that described calcination process produces hot blast, the thermal source of phosphorus ore dry powder preheating and high-temperature flue gas of calcination process as flash drying after the normal temperature air of interchanger absorbs uses.
The purposes that the phosphogypsum that a kind of production method that improves phosphoric acid quality and yield obtains directly uses as industrial gypsum.
Compared with prior art, the invention has the beneficial effects as follows:
(1) the present invention first will carry out Wet-process Phosphoric Acid Production with the inorganic acid reaction such as sulfuric acid after natural Rock Phosphate (72Min BPL) drying, calcination processing again, starts to purify Rock Phosphate (72Min BPL), increase P with heat treating process from source
2o
5active, but not take after reaction, phosphoric acid to be purified, in ground phosphate rock in after calcining, the clearance of F is more than 50%, the clearance of arsenic is more than 80%, reduce the foreign matter content in raw material, and then reduced the foreign matter content of phosphoric acid by wet process product, simplified impurity existing way simultaneously, be conducive to the further purifying treatment of phosphoric acid by wet process or classification utilization, improved yield and the utilization ratio of different stage phosphoric acid;
(2) the present invention improves P
2o
5activity make Rock Phosphate (72Min BPL) and sulfuric acid reaction abundant, reduced the phosphorus content in byproduct phosphogypsum, phosphogypsum is directly used as industrial gypsum;
The present invention is dry, calcining, and production technique is consecutive production technique, constant product quality, the production environment of stopping property, particularly tail gas is repeated circulation and puts into flash drying, dynamic calcining technique, can also save energy, and exhaust emissions has reached national requirements for environmental protection, to environmental protection close friend.
Embodiment
According to concrete embodiment, the present invention is further elaborated below.
But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment.
embodiment 1
With P
2o
5content is 21.54%, natural Rock Phosphate (72Min BPL) is as raw ore, first dries at 420 DEG C-480 DEG C or 480-550 DEG C, obtains P 950-1050 DEG C of calcination processing again after raw ore is pulverized
2o
5content is 22.25% ground phosphate rock, then carries out Wet-process Phosphoric Acid Production with sulfuric acid reaction and obtain product phosphoric acid and byproduct phosphogypsum.
Above-described embodiment all can be first by drying again after natural crystal flotation, calcination processing, and then carry out Wet-process Phosphoric Acid Production.
embodiment 2
Similar with embodiment 1, difference is:
With P
2o
521.54% Rock Phosphate (72Min BPL) is as raw ore, raw ore is carried out after efflorescence pre-treatment, obtain containing wet ground phosphate rock, to send in moisture eliminator containing wet ground phosphate rock with screw feeder, utilize heat that calcining produces tail gas after the normal temperature air of interchanger absorbs as drying source---hot blast uses, hot blast will containing wet ground phosphate rock flash drying obtain phosphorus ore dry powder in inlet temperature as 500-550 DEG C taking the speed of 10m/s, now dryer export place temperature out is 100 DEG C of 50≤T <, phosphorus ore dry powder is collected completely and carried out after preheating with cyclonic separator, put into calcining furnace, drying source high-temperature flue gas when calcining in phosphorus ore dry powder and calcining furnace mixes, be and revolve fluidization and move upward, phosphorus ore dry powder has been increased the specific surface area of whole phosphorus ore dry powder significantly by high-temperature flue gas rapid dispersion, therefore phosphorus ore dry powder and high-temperature flue gas energy moment are carried out matter heat exchange, calcining temperature is that after 800 DEG C of calcining 1-10s of 720≤T <, cooled phosphorus ore dry powder obtains ground phosphate rock through sack cleaner and tornado dust collector combination dedusting again, and gather up calcining tail gas, the heat of the tail gas simultaneously calcining being produced drying source---drying source of hot blast and calcination process---high temperature flue gas drying as flash drying operation after the cold fluid of interchanger absorbs uses, preheating thermal source provides after interchanger is processed by calcining tail gas.Using screw feeder feeding, is by containing wetting, ground phosphate rock is screw type to add in moisture eliminator, allows and spreads out and fully contact with hot blast containing wet ground phosphate rock, increases heat transfer surface area, is conducive to like this improve drying efficiency, reduces and consumes energy.
The P of the ground phosphate rock obtaining
2o
5content is 22.30%, adopts phosphoric acid by wet process to make phosphoric acid and byproduct phosphogypsum using ground phosphate rock as raw materials for production.
The tail gas producing with calcining uses as preheating thermal source after interchanger is processed, and need not expend like this electric power again and improve thermal source, thereby save power consumption.And the setting of preheating is in order to reach faster calcining temperature in calcination process process, calcine the thorough time thereby can more save phosphorus ore dry powder.
embodiment 3
Similar with embodiment 1 step, be specially:
With P
2o
5content be 21.54% natural Rock Phosphate (72Min BPL) as raw ore, carry out flash drying and dynamic calcining, wherein the hot blast wind speed of flash drying is 12m/s, moisture eliminator inlet temperature is 280-350 DEG C, dryer export temperature is 150 DEG C of 100≤T <; Dynamic calcining temperature is 850-900 DEG C, calcination time 8s.
The P of the ground phosphate rock obtaining
2o
5content is 22.45%, using ground phosphate rock as raw materials for production and sulfuric acid reaction adopt wet phosphoric acid make phosphoric acid and byproduct phosphogypsum.
embodiment 4
Similar with embodiment 3, difference is, the processing condition that embodiment 4 adopts and embodiment 3 are slightly different:
With P
2o
5content is that 21.54% natural Rock Phosphate (72Min BPL) is as raw ore, by after raw ore washing, carry out flash drying and dynamic calcining, wherein the hot blast wind speed of flash drying is 13m/s, moisture eliminator inlet temperature is 500-550 DEG C, and dryer export temperature is 200 DEG C of 150≤T <; Dynamic calcining temperature is 900-950 DEG C, and calcination time is 7s.
The P of the ground phosphate rock obtaining
2o
5content is 22.50%, adopts phosphoric acid by wet process to make phosphoric acid and byproduct phosphogypsum using ground phosphate rock as raw materials for production.
embodiment 5
Similar with embodiment 4, difference is: the processing condition that embodiment 4 adopts and embodiment 5 are slightly different, are specially:
With P
2o
5content be 21.54% natural Rock Phosphate (72Min BPL) as raw ore, by after raw ore washing, carry out flash drying and dynamic calcining, wherein the hot blast wind speed of flash drying is 15m/s, moisture eliminator inlet temperature is 550-600 DEG C, dryer export temperature is 200≤T≤300 DEG C; Dynamic calcining temperature is 1000-1050 DEG C, and calcination time is 4-6s.
The P of the ground phosphate rock obtaining
2o
5content is 22.58%, adopts phosphoric acid by wet process to make phosphoric acid and byproduct phosphogypsum using ground phosphate rock as raw materials for production.
Produced as shown in the table in the phosphorus ore obtaining when phosphoric acid by above-described embodiment:
Table 1 the present invention and existing production technique comparison
The byproduct phosphogypsum comparison of table 2 the present invention and existing production technique
As can be seen from Table 1, through drying, calcine the Rock Phosphate (72Min BPL) P obtaining after thermal treatment
2o
5yield obviously than drying not, calcine the Rock Phosphate (72Min BPL) P that thermal treatment obtains
2o
5yield high, the clearance that organic impurity content is not more than 0.5%, F reaches more than 50%, the phosphoric acid yield making is up to more than 95%.After calcining, make that foreign matter content in the raw material of phosphoric acid by wet process reduces, existing way is simplified, be conducive to further purification and the classification utilization of phosphoric acid by wet process.
As can be seen from Table 2, the liquid content of phosphogypsum of the present invention, water-soluble phosphorus are dry and molten phosphorus content is lower again, thereby can directly be used as industrial gypsum and use.
To sum up, the present invention adopts the thermal treatment way of oven dry, calcining, on the one hand, overcome the deficiency that existing wet method phosphoric acid manufacture process directly uses former natural crystal, after oven dry of the present invention, calcining, in former natural crystal, be unfavorable for that the existence form of the P element of Wet-process Phosphoric Acid Production has become the existence form that is beneficial to Wet-process Phosphoric Acid Production, as organophosphorus etc., increase the reactive behavior of P element in ore, thereby in Wet-process Phosphoric Acid Production process, more P element comes in the middle of participating in reaction, has therefore improved on the whole phosphoric acid output; Overcome on the other hand in existing Wet-process Phosphoric Acid Production the heat utilization efficiency because of heat treatment mode not high, raw material needs the heat of fully calcined needs excessive, and energy expenditure is excessive, and the high cost causing cannot be applied to the deficiency of scale operation.
And when improving phosphoric acid output, what bring is that the liquid content, water-soluble phosphorus of by product phosphogypsum is dry and molten phosphorus content is few again, can directly use as industrial gypsum, stockyard investment, the running cost that can reduce in a large number the land seizure area of phosphogypsum and cause with this, can improve the utilization ratio of sulphur resource, and reduce environmental pollution simultaneously.
Claims (7)
1. a production method that improves phosphoric acid quality and yield, is characterized in that:
Be raw material by the ground phosphate rock obtaining after natural Rock Phosphate (72Min BPL) drying, calcining, adopt Wet-process Phosphoric Acid Production method sulfuric acid and the reaction of described ground phosphate rock to produce.
2. a kind of production method that improves phosphoric acid quality and yield according to claim 1, it is characterized in that: described drying process is flash drying, adopt screw feeder to be conveyed in moisture eliminator and to pass into hot blast in moisture eliminator containing wet ground phosphate rock, obtain phosphorus ore dry powder through warm air drying, with tornado dust collector collection phosphorus ore dry powder;
Calcination process is dynamic calcining operation, to after the phosphorus ore dry powder preheating obtaining after dry, send in calcining furnace, pass into again high-temperature flue gas, high-temperature flue gas drives the phosphorus ore dry powder obtaining after flash drying is moved upward together, and described phosphorus ore dry powder makes the described phosphorus ore dry powder calcining temperature that is rapidly heated obtain the raw materials for production ground phosphate rock of phosphoric acid by wet process through sack cleaner and tornado dust collector combination dedusting after fully calcined through the rapid dispersion effect moment matter heat exchange of the high-temperature flue gas in calcining furnace.
3. a kind of production method that improves phosphoric acid quality and yield according to claim 2, is characterized in that: the speed of described hot blast is 10-15m/s.
4. a kind of production method that improves phosphoric acid quality and yield according to claim 2, is characterized in that: the heat of the tail gas that described calcination process produces hot blast, the thermal source of phosphorus ore dry powder preheating and high-temperature flue gas of calcination process as flash drying after the normal temperature air of interchanger absorbs uses.
5. according to a kind of production method that improves phosphoric acid quality and yield described in claim 2-4 any one, it is characterized in that: the inlet temperature in described flash drying is 280 DEG C-600 DEG C 50 DEG C-300 DEG C of the temperature outs of described flash drying.
6. according to a kind of production method that improves phosphoric acid quality and yield described in claim 1-4 any one, it is characterized in that: the calcining temperature of described calcination process is 720 DEG C-1050 DEG C, described phosphorus ore dry powder is 1-10s at calcining residing time in furnace.
7. according to a kind of production method that improves phosphoric acid quality and yield described in claim 1-4 any one, it is characterized in that: the phosphogypsum obtaining directly uses as industrial gypsum.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107099154A (en) * | 2017-04-21 | 2017-08-29 | 北京路优材料技术有限公司 | A kind of production method of kir powder |
| CN108118142A (en) * | 2017-12-29 | 2018-06-05 | 营口益嘉镁业科技有限公司 | A kind of suspension flash decomposes and homogenizing processing technique |
| CN112341291A (en) * | 2020-11-03 | 2021-02-09 | 中国科学院过程工程研究所 | Device and method for preparing calcium-silicon-potassium phosphate fertilizer and hydrochloric acid by utilizing phosphorite |
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| GB2069987A (en) * | 1980-02-15 | 1981-09-03 | Albright & Wilson | Heat treating phosphate rock |
| US4501724A (en) * | 1984-02-01 | 1985-02-26 | Goers Associates Inc. | Method for the wet process manufacture of phosphoric acid |
| AU4348585A (en) * | 1984-06-13 | 1985-12-19 | Negev Phosphates Ltd. | Thermal treatment of phosphate rock |
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2014
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| GB2069987A (en) * | 1980-02-15 | 1981-09-03 | Albright & Wilson | Heat treating phosphate rock |
| US4501724A (en) * | 1984-02-01 | 1985-02-26 | Goers Associates Inc. | Method for the wet process manufacture of phosphoric acid |
| AU4348585A (en) * | 1984-06-13 | 1985-12-19 | Negev Phosphates Ltd. | Thermal treatment of phosphate rock |
| CN103466573A (en) * | 2013-09-13 | 2013-12-25 | 成都乐氏化工工程有限公司 | Energy-saving method for preparing yellow phosphorus from low-quality phosphate ore |
Non-Patent Citations (1)
| Title |
|---|
| A.A. GUFFEY: "Processing calcined phosphate rock", 《CHEMICAL ENGINEERING PROGRESS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107099154A (en) * | 2017-04-21 | 2017-08-29 | 北京路优材料技术有限公司 | A kind of production method of kir powder |
| CN107099154B (en) * | 2017-04-21 | 2019-07-05 | 北京路优材料技术有限公司 | A kind of production method of rock asphalt powder |
| CN108118142A (en) * | 2017-12-29 | 2018-06-05 | 营口益嘉镁业科技有限公司 | A kind of suspension flash decomposes and homogenizing processing technique |
| CN112341291A (en) * | 2020-11-03 | 2021-02-09 | 中国科学院过程工程研究所 | Device and method for preparing calcium-silicon-potassium phosphate fertilizer and hydrochloric acid by utilizing phosphorite |
| CN112341291B (en) * | 2020-11-03 | 2022-03-11 | 中国科学院过程工程研究所 | Device and method for preparing calcium-silicon-potassium phosphate fertilizer and hydrochloric acid by utilizing phosphorite |
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