CN102126712A - Method for producing phosphoric acid by utilizing middle grade phosphate ore - Google Patents
Method for producing phosphoric acid by utilizing middle grade phosphate ore Download PDFInfo
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Abstract
The invention discloses a method for producing phosphoric acid by utilizing middle grade phosphate ore, comprising the following steps: (1) preparing a double-layer composite structure pellet containing the middle grade phosphate ore, wherein, the water content of the pellet is less than or equal to 0.5wt%; (2) sending the pellet into a rotary kiln from the tail part of the rotary kiln; delivering the carbon monoxide (CO) coal gas, dehydration air or dehydration oxygen-enriched air into the rotary kiln from the head part of the rotary kiln; carrying out heat exchanging on the high-temperature gas generated in burning of the CO coal gas and the pellet in reversed operation in the rotary kiln; heating the pellet to the reaction temperature of 1250-1400 DEG C; carrying out heat exchanging on the tail gas containing P2O5 generated in reaction and the pellet entering into the rotary kiln; cooling to the temperature of 600-650 DEG C, and leading out from the tail part of the rotary kiln; and (3) dedusting the tail gas containing the P2O5 led out from the rotary kiln; and absorbing P2O5 by utilizing recycle acid to prepare the phosphoric acid.
Description
Technical field
The invention belongs to kiln legal system phosphoric acid field, particularly a kind of technology of producing phosphoric acid with middle grade phosphorus mine stone.
Background technology
The technological core of kiln-process phosphoric acid is the reduction that phosphorus combustion reaction heat is used for phosphorus ore, few electricity consumption, need not acid, grade phosphorus mine stone in can directly using, the high silicon ore that is specially adapted to be difficult to ore dressing.It is the kiln-process phosphoric acid technological test of principal reaction equipment with the rotary kiln that the U.S. has just begun to carry out as far back as eighties of last century the '30s, particularly eighties of last century has been finished interim test (US patent No.4389384 in late nineteen seventies to early eighties U.S. Occidental Petroleum Corporation (Occidental Research Corporation), 4351813,7378070).China also begins to have carried out the technical study of kiln-process phosphoric acid in the eighties of last century the eighties middle and later periods, with Designing Institute of Nanjing Chemical Industry Corp. river kind assist be representative tunnel furnace technology (Chinese patent ZL 89100292.8) and with Changsha Mining ﹠ Metallurgy Inst wait gather around and be representative rotary kiln technology (Chinese patent ZL 93111447.0) all last century the nineties finished pilot scale or type approval test.But up to now, the whole world does not also have the kiln-process phosphoric acid process units that a cover can long-period stable operation.
The rotary kiln technology has the realization industrialized prospect, but one of subject matter that hinders this skilled industryization is P in the gas phase
2O
5The metaphosphoric acid that generates with water vapour (water vapour mainly generates up to about 12% mixed gas burning from airborne moisture and hydrogen richness) is separated out (Jiang Shanxiang will being viscous liquid from gas phase below 900 ℃, improve the discussion of kiln-process phosphoric acid reduction ratio, phosphate fertilizer and multiple fertilizer, 2 phases of nineteen ninety-five, P
10～15), causing reaching the easy ring formation of exhaust pipe, obstruction in the rotary kiln, the kiln discharge exhaust temperature can not be lower than 900 ℃, and the system thermal loss is big.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing rotary kiln technology, a kind of method of producing phosphoric acid with middle grade phosphorus mine stone is provided, to solve P in the gas phase
2O
5Generate in the rotary kiln that metaphosphoric acid causes with steam and the problem of exhaust pipe ring formation, obstruction, and improve heat utilization efficiency.
Technical scheme of the present invention: adopt the air or the oxygen-enriched air that have removed moisture to hang down H as oxidant, the employing of combustion adjuvant and phosphorus steam
2Act as a fuel with the CO coal gas of hydrocarbon content, thereby reduce the interior moisture of rotary kiln, avoid or significantly reduce the formation of metaphosphoric acid.In view of P
2O
5Fusion temperature is that 570 ℃, sublimation temperature are 360 ℃, will contain P
2O
5Tail gas and the reverse raw material ball that enters rotary kiln carry out heat exchange, make to contain P
2O
5Exhaust temperature be down to 600～650 ℃ of again kiln discharges, to improve heat utilization efficiency.
Method of producing phosphoric acid of the present invention with middle grade phosphorus mine stone, processing step is as follows:
(1) the two-layer composite pellet of grade phosphorus mine during preparation contains, the water content≤0.5wt.% of described pellet;
(2) pellet is sent into rotary kiln from the rotary kiln afterbody, CO coal gas, dehydration air or dehydration oxygen-enriched air are imported rotary kiln from the rotary kiln head, in rotary kiln, high-temperature gas and pellet antikinesis that the CO gas-fired produces carry out heat exchange, pellet is warming up to 1250 ℃～1400 ℃ of reaction temperatures, reacts the P that contains that generates
2O
5Tail gas carries out heat exchange with the pellet that enters rotary kiln, and temperature is down to 600～650 ℃ and is drawn from the rotary kiln afterbody;
(3) will contain P from what rotary kiln was drawn
2O
5Absorb P with recycle acid behind the tails dedusting
2O
5Make phosphoric acid.
The method of the invention, the water content≤0.1vol.% of dehydration air, the oxygen concn of dehydration oxygen-rich air is 22～35vol.%, water content≤0.1vol.%.
The method of the invention, H in the CO coal gas
2Total content≤1vol.% with hydrocarbons.
The method of the invention carries out dehydration air or dehydration oxygen-enriched air to import rotary kiln from the rotary kiln head after the heat exchange preheating with the high temperature hot residue that transfers out from rotary kiln end, with further raising heat utilization efficiency.
The method of the invention, the preparation manipulation of CO coal gas is: will be processed phosphoric acid discharge take off P
2O
5Tail gas carries out defluorinate processing, processed successively, and introducing oxygen concentration in the dehydration process steps of described tail gas is the oxygen-enriched air of 65～99vol.%, will dewater then to react to the mist of water content≤0.1vol.% and coke namely to form CO coal gas.In addition, CO coal gas also can transform continuously by oxygen and carbonic acid gas make (technical scheme of seeing ZL 200610030347.6 patent disclosures), or adopts and make after various coal gas (comprising water-gas, semi-water gas, mixed gas etc.) are removed hydrogen and hydro carbons.
The method of the invention, the internal layer pellet feed of two-layer composite pellet comprises middle grade phosphorus mine, silica and carbonaceous reducing agent, during batching, carbonaceous reducing agent is pressed P in the rock phosphate in powder
2O
5Reduce 1～2 times of metering of required fixed carbon theoretical amount, silica is by middle grade phosphorus mine stone, carbonaceous reducing agent and three kinds of contained SiO of raw material of silica
2With the mol ratio of CaO be 2～5 meterings; The outer wrapping layer raw material of two-layer composite pellet comprises silica and carbonaceous reducing agent, SiO in the silica
2With the mol ratio of fixed carbon in the carbonaceous reducing agent be 0.5～4.The pellet of described two-layer composite can be with reference to the technical scheme preparation of ZL93111447.0 patent disclosure.
In the method for the invention, the dehydration of air and mist can be adopted the conventional methods such as sulfuric acid drying, molecular sieve adsorption; Obtaining of oxygen-enriched air can be adopted conventional air deep-cooling partition method, pressure-variable adsorption partition method.
The present invention has following beneficial effect:
(1) because employing dehydration air or dehydration oxygen-enriched air are the oxidant of combustion adjuvant and phosphorus steam, adopts H
2The CO coal gas low with hydrocarbons content acts as a fuel, thereby the metaphosphoric acid that forms is few or do not have metaphosphoric acid and separate out, efficiently solve rotary kiln and exhaust pipe ring formation and obstruction that metaphosphoric acid causes, be conducive to realize kiln process phosphoric acid process long-period stable operation.
(2) when the CO coal gas that adopts dehydration air and identical calorific value substituted the mixed gas of existing process using, the heat utilization efficiency of tail gas can improve 17%.
(3) (oxygen concentration is 22～35vol.%) and the CO coal gas of identical calorific value when substituting the mixed gas that has process using now when adopting oxygen-enriched air, can reduce significantly CO gas using quantity (reducing by 8～63%) and go out kiln exhaust gas amount (reducing by 6～44%), thereby reduce the P of unit
2O
5The coal consumption of product about 26～34%; Simultaneously, equipment input expense and the operating cost of gas generator system, exhaust treatment system (comprising relieving haperacidity and defluorinate process) etc. have also significantly been reduced.
Description of drawings
Fig. 1 is a kind of process flow sheet of producing the method for phosphoric acid with middle grade phosphorus mine stone of the present invention.
Embodiment
Below by embodiment the method with middle grade phosphorus mine stone production phosphoric acid of the present invention is described further.Among the following embodiment, rotary kiln is of a size of Φ 200 * 2000mm.
Embodiment 1
In the present embodiment, the method for producing phosphoric acid is as follows:
(1) pellet of preparation two-layer composite.The raw material of internal layer pelletizing comprises middle grade phosphorus mine stone flour, coal dust and Cab-O-sil, and the chemical composition of middle grade phosphorus mine stone flour (being percetage by weight) is: P
2O
520.6%, CaO 25.8%, SiO
246.9%; The chemical composition of coal dust (being percetage by weight) is: fixed carbon 77.9%, ash content 17.4% (SiO wherein
284.3%, Fe
2O
38.3%, CaO 2.0%); SiO in the Cab-O-sil
2Content be 95.3% (percetage by weight).During batching, coal dust is pressed P in the rock phosphate in powder
2O
5Reduce 1.5 times of meterings of required fixed carbon theoretical amount, Cab-O-sil is by middle grade phosphorus mine stone flour, coal dust and three kinds of contained SiO of raw material of Cab-O-sil
2/ CaO=3 (mol ratio) metering.The mixed powder of above-mentioned three kinds of raw materials is milled to 80% mistake, 160 mesh sieves, adopt ordinary method (making ball method, cylinder pelletizing method) to make ball as disk, the water of clay of adding mixed powder weight 1.5% when making ball (also can use the bentonite or the silicates of a great deal of) and mixed powder weight 10% is as binding agent, and the pelletizing particle diameter is 10mm.Cross the Cab-O-sil of 200 mesh sieves and fine coal as outer wrapping layer raw material take granularity 80%, during batching, press SiO in the Cab-O-sil
2With the mol ratio of fixed carbon in the coal dust be 1.5 stoichiometric silicon stone flour and coal dusts, the internal layer pelletizing is carried out secondary makes ball, wrap outer wrapping layer raw material, the THICKNESS CONTROL of outer wrapping layer is at 2mm.Place baking oven under 150 ℃, to carry out drying pellet, reduce to 0.35wt.% with its water content time of drying and exceed.
(2) pellet is sent into rotary kiln continuously from the rotary kiln afterbody, it sends into speed is 220kg/h, and CO coal gas is imported rotary kiln continuously from the rotary kiln head, and its input speed is 53Nm
3/ h imports rotary kiln continuously from the rotary kiln head after the air preheat to 550 ℃ of will dewatering, and its input speed is 156Nm
3/ h, in rotary kiln, high-temperature gas and pellet antikinesis that the CO gas-fired produces carry out heat exchange, and pellet is warming up to 1300 ℃～1350 ℃ of reaction temperatures in the main reaction section, and pellet is at least 40min in the main reaction section time of staying, reacts the P that contains that generates
2O
5Tail gas carries out heat exchange with the pellet that enters rotary kiln, and temperature is down to 1000 ℃ and is drawn oxygen concentration≤1vol.% in the tail gas from the rotary kiln afterbody; The percentage by volume of described each component of CO coal gas is: CO 45%, CO
215%, N
239.5%, H
2With hydrocarbons content sum be 0.5.%, calorific value is 5685kJ/Nm
3Described dehydration air moisture content is 0.05vol.%, the dehydration preheating of air is to carry out heat exchange by will dewater air and the high temperature hot residue that transfers out from rotary kiln end to realize, concrete operations are to make the high temperature hot residue that transfers out from rotary kiln end enter cooler, are down to temperature behind the air heat-exchange of dehydration≤discharge after 100 ℃.
(3) kiln discharge contains P
2O
5Tail gas enters the absorption tower by an exhaust temperature adjustable pipe and absorbs P with recycle acid after dedusting
2O
5Phosphoric acid processed contains P by changing exhaust temperature adjustable pipe length, the outer keeping warm mode of adjustable pipe and add the measure such as cooling, regulating
2O
5The tower temperature that enters that tail gas enters the absorption tower is 900 ± 20,800 ± 20,700 ± 20,600 ± 20, enters under the tower temperature stable operation 3 hours at given each tail gas, measures to contain P
2O
5Tail gas enters in the corresponding kiln discharge high temperature of the tower temperature hot residue to remain P in difference
2O
5Content and receipts acid system gained phosphoric acid amount and acid concentration, percent reduction and the P of calculating phosphorus ore
2O
5Yield, it the results are shown in Table 1.
Table 1 adopts dehydration air and CO coal gas result of the test
Comparative Examples 1
This Comparative Examples is a simultaneous test, adopts the air (water content 1.6wt.%) that do not dewater to make ignition dope, and (percent by volume of each component is mixed gas: CO 32%, CO
24%, H
2Reach hydrocarbons 13%, N
250%, H
2O 1%, and calorific value is 5505kJ/Nm
3) make fuel, pellet and other operations and condition are with embodiment 1.Mensuration contains P
2O
5Tail gas enters in the corresponding kiln discharge high temperature hot residue of absorption tower with different temperatures and remains P
2O
5Content, receipts acid system gained phosphoric acid amount and acid concentration, percent reduction and the P of calculating phosphorus ore
2O
5Yield, it the results are shown in Table 2.
Table 2 adopts do not dewater air and mixed gas result of the test
Contrast table 1 and table 2 can be found out, adopt when dewatering air and CO gas-fired heat supply the percent reduction of phosphorus ore and P
2O
5Yield is very approaching, and adopts when not dewatering air and mixed gas the percent reduction of phosphorus ore and P
2O
5It is bigger that yield differs, and this difference enters the absorption tower temperature with phosphorous tail gas and reduces fast increase.Observe in test, adopting when not dewatering air and mixed gas test has thick material to separate out in the exhaust temperature adjustable pipe, and exhaust temperature is more low, and to separate out thick material more many, are metaphosphoric acid through the chemical analysis main component.And adopt dehydration air and the test of CO coal gas, even reducing to, exhaust temperature also almost can't see above-mentioned thick material in 600 ℃ of exhaust temperature adjustable pipes.
Above-mentioned result of the test shows that the kiln discharge exhaust temperature must remain on more than 900 ℃ in existing kiln-process phosphoric acid production technology, otherwise metaphosphoric acid will be separated out in a large number, and this not only reduces P
2O
5Yield causes kiln afterbody and exhaust pipe knot kiln circle, obstruction, and tail gas has also been taken away the heat of system about 41% with this understanding; But if adopt air and the CO gas-fired heat supply that removes water, the kiln discharge exhaust temperature can be reduced to 600 ℃, P
2O
5Yield is unaffected, also can not produce metaphosphoric acid kiln circle at kiln afterbody and exhaust pipe, and tail gas has only been taken away the heat of system about 24% with this understanding, thereby has reduced significantly energy consumption.
Embodiment 2
(1) pellet of preparation two-layer composite, raw material and proportioning thereof and operation are with embodiment 1;
(2) pellet is sent into rotary kiln continuously from the rotary kiln afterbody, it sends into speed is 220kg/h, CO coal gas is imported rotary kiln continuously from the rotary kiln head, its input speed changes with oxygen concn in the oxygen-rich air, to dewater and import rotary kiln continuously from the rotary kiln head after oxygen-rich air is preheated to 550 ℃, its input speed changes with CO coal gas input speed, can calculate according to feeding the equal required theoretical oxygen amount excessive 10% of perfect combustion of CO coal gas and Rock Phosphate (72Min BPL) reduzate (phosphorus and CO).In rotary kiln, high-temperature gas and pellet antikinesis that the CO gas-fired produces carry out heat exchange, and pellet is warming up to 1300 ℃～1350 ℃ of reaction temperatures in the main reaction section, and pellet is at least 40min in the main reaction section time of staying, react the P that contains that generates
2O
5Tail gas carries out heat exchange with the pellet that enters rotary kiln, and temperature is down to 1000 ℃ and is drawn from the rotary kiln afterbody, goes out oxygen concentration≤1vol.% in the kiln exhaust gas; The percentage by volume of described each component of CO coal gas is: CO 45%, CO
215%, N
239.5%, H
2With hydrocarbons content sum be 0.5.%, calorific value is 5685kJ/Nm
3Described dehydration oxygen-enriched air water content is 0.05vol.%, oxygen concentration is respectively 22vol.%, 27vol.%, 30vol.%, 35vol.% (stable operation is 3 hours under each described oxygen-rich concentration), the preheating of dehydration oxygen-enriched air is to carry out heat exchange by will dewater oxygen-enriched air and the high temperature hot residue that transfers out from rotary kiln end to realize, concrete operations are to make the high temperature hot residue that transfers out from rotary kiln end enter cooler, are down to temperature after the oxygen-enriched air heat exchange of dehydration≤discharge after 100 ℃;
(3) kiln discharge contains P
2O
5Tail gas enters the absorption tower and makes phosphoric acid after the exhaust temperature adjustable pipe is cooled to 600 ℃.Stable operation is 3 hours under each given oxygen-rich concentration, measures in the corresponding kiln discharge high temperature hot residue and remains P
2O
5Content, receipts acid system gained phosphoric acid amount and acid concentration and kiln discharge contain P
2O
5Exhaust flow, percent reduction and the P of calculating phosphorus ore
2O
5Yield, it the results are shown in Table 3.
(4) will be processed phosphoric acid discharge take off P
2O
5Tail gas carries out successively defluorinate and processes (adopting the lime neutralisation), processed (sulfuric acid drying), introducing oxygen concentration in dehydration process steps is the oxygen-enriched air of 80vol.%, will dewater then to react to the mist of water content≤0.1vol.% and coke namely to form CO coal gas.
The test-results of table 3 different oxygen-enriched air oxygen concentration
| Dehydration oxygen-enriched air oxygen concentration | 22vol.% | 27vol.% | 30vol.% | 35vol.% |
| The percent reduction of phosphorus ore | 89% | 89% | 87% | 86% |
| P 2O 5Yield | 88% | 88% | 86% | 85% |
| CO coal gas amount | 0.92 | 0.63 | 0.52 | 0.37 |
| Kiln discharge contains P 2O 5Exhaust flow | 0.94 | 0.74 | 0.66 | 0.56 |
Annotate: CO coal gas amount and contain P in the table
2O
5Exhaust flow is all processed the equal number pellet as benchmark take the unit interval, the CO gas consumption amount when adopting dehydration air (oxygen concentration 21vol.%) as combustion adjuvant and go out the kiln exhaust gas amount and relatively get as a unit.
Claims (9)
1. method of producing phosphoric acid with middle grade phosphorus mine stone is characterized in that processing step is as follows:
(1) the two-layer composite pellet of grade phosphorus mine during preparation contains, the water content≤0.5wt.% of described pellet;
(2) pellet is sent into rotary kiln from the rotary kiln afterbody, CO coal gas, dehydration air or dehydration oxygen-enriched air are imported rotary kiln from the rotary kiln head, in rotary kiln, high-temperature gas and pellet antikinesis that the CO gas-fired produces carry out heat exchange, pellet is warming up to 1250 ℃～1400 ℃ of reaction temperatures, reacts the P that contains that generates
2O
5Tail gas carries out heat exchange with the pellet that enters rotary kiln, and temperature is down to 600 ℃～650 ℃ and is drawn from the rotary kiln afterbody;
(3) will contain P from what rotary kiln was drawn
2O
5Absorb P with recycle acid behind the tails dedusting
2O
5Make phosphoric acid.
2. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 1 is characterized in that the water content≤0.1vol.% of described dehydration air, and the oxygen concn of described dehydration oxygen-rich air is 22～35vol.%, water content≤0.1vol.%.
3. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 1 and 2 is characterized in that in the described CO coal gas H
2Total content≤1vol.% with hydrocarbons.
4. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 1 and 2 is characterized in that dehydration air or dehydration oxygen-enriched air are carried out importing rotary kiln from the rotary kiln head after the heat exchange preheating with the high temperature hot residue that transfers out from rotary kiln end.
5. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 3 is characterized in that dehydration air or dehydration oxygen-enriched air are carried out importing rotary kiln from the rotary kiln head after the heat exchange preheating with the high temperature hot residue that transfers out from rotary kiln end.
6. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 1 and 2 is characterized in that the preparation method of described CO coal gas is: will phosphoric acid discharge processed take off P
2O
5Tail gas carries out defluorinate processing, processed successively, and introducing oxygen concentration in the dehydration process steps of described tail gas is the oxygen-enriched air of 65～99vol.%, will dewater then to react to the mist of water content≤0.1vol.% and coke namely to form CO coal gas.
7. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 3 is characterized in that the preparation method of described CO coal gas is: will phosphoric acid discharge processed take off P
2O
5Tail gas carries out defluorinate processing, processed successively, and introducing oxygen concentration in the dehydration process steps of described tail gas is the oxygen-enriched air of 65～99vol.%, will dewater then to react to the mist of water content≤0.1vol.% and coke namely to form CO coal gas.
8. method of producing phosphoric acid with middle grade phosphorus mine stone according to claim 4 is characterized in that the preparation method of described CO coal gas is: will phosphoric acid discharge processed take off P
2O
5Tail gas carries out defluorinate processing, processed successively, and introducing oxygen concentration in the dehydration process steps of described tail gas is the oxygen-enriched air of 65～99vol.%, will dewater then to react to the mist of water content≤0.1vol.% and coke namely to form CO coal gas.
9. the method for producing phosphoric acid with middle grade phosphorus mine stone of stating according to claim 5 is characterized in that the preparation method of described CO coal gas is: will phosphoric acid discharge processed take off P
2O
5Tail gas carries out defluorinate processing, processed successively, and introducing oxygen concentration in the dehydration process steps of described tail gas is the oxygen-enriched air of 65～99vol.%, will dewater then to react to the mist of water content≤0.1vol.% and coke namely to form CO coal gas.
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| CN109916186A (en) * | 2019-01-04 | 2019-06-21 | 贵州芭田生态工程有限公司 | A kind of recovery method for calcining phosphorus ore thermal energy |
| CN114477115A (en) * | 2022-03-18 | 2022-05-13 | 西安吉利电子新材料股份有限公司 | Method for directly producing electronic grade phosphoric acid solution from phosphorite |
| CN115159481A (en) * | 2021-12-03 | 2022-10-11 | 四川大学 | Preparation method of kiln-process phosphoric acid reaction material ball for preventing phosphorus pentoxide from being sucked back |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014194571A1 (en) * | 2013-06-04 | 2014-12-11 | 四川玖长科技有限公司 | Raw material pre-treatment process and raw material pre-treatment process system suitable for kiln process for production of phosphoric acid |
| CN104211034A (en) * | 2013-06-04 | 2014-12-17 | 四川玖长科技有限公司 | Raw material pretreatment method and raw material pretreatment process system suitable for kiln method phosphoric acid technology |
| RU2637909C2 (en) * | 2013-06-04 | 2017-12-07 | Сычуань Ко Чанг Технолоджи Ко., Лтд | Initial material preparing process and technological process developed for burning in furnace when receiving phosphoric acid |
| US10744512B2 (en) | 2013-06-04 | 2020-08-18 | Sichuan Ko Chang Technology Co., Ltd. | Raw material pre-treatment method and raw material pre-treatment process system suitable for kiln phosphoric acid process |
| CN109916186A (en) * | 2019-01-04 | 2019-06-21 | 贵州芭田生态工程有限公司 | A kind of recovery method for calcining phosphorus ore thermal energy |
| CN115159481A (en) * | 2021-12-03 | 2022-10-11 | 四川大学 | Preparation method of kiln-process phosphoric acid reaction material ball for preventing phosphorus pentoxide from being sucked back |
| CN114477115A (en) * | 2022-03-18 | 2022-05-13 | 西安吉利电子新材料股份有限公司 | Method for directly producing electronic grade phosphoric acid solution from phosphorite |
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