CN103274378A - Electric calcination furnace and application of electric calcination furnace in preparing industrial-grade phosphoric acid - Google Patents
Electric calcination furnace and application of electric calcination furnace in preparing industrial-grade phosphoric acid Download PDFInfo
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- CN103274378A CN103274378A CN2013102318480A CN201310231848A CN103274378A CN 103274378 A CN103274378 A CN 103274378A CN 2013102318480 A CN2013102318480 A CN 2013102318480A CN 201310231848 A CN201310231848 A CN 201310231848A CN 103274378 A CN103274378 A CN 103274378A
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Abstract
The invention relates to the field of production devices of industrial-grade phosphoric acid, in particular to an electric calcination furnace adopted in the process for producing industrial-grade phosphoric acid by using low-grade phosphate rock. A specific application method of the electric calcination furnace adopted in the process of preparing the industrial-grade phosphoric acid comprises the steps as follows: firstly, the temperature inside the furnace is set to be 100 DEG C, then a rotating tube is started and preheated for one hour, the temperature inside the furnace is heated to 250 DEG C, and the rotating tube is preheated for half an hour again; and materials are uniformly fed, solid materials are directly rolled into a hydrolyzing barrel, gaseous materials enter a fluorine recycling barrel from six gas collecting pipes at the top, pyrophosphoric acid and iron-aluminum oxides are solidified after the materials are calcinated, the spilt gas is hydrogen fluoride, and the temperature is controlled to be 100 DEG C during discharging. The electric calcination furnace is adopted for preparing the industrial-grade phosphoric acid and is low in energy consumption, simple in process, easy to operate, low in cost and capable of effectively saving energy.
Description
Technical field
The present invention relates to PHOSPHORIC ACID TECH.GRADE and produce the equipment field, specifically is a kind of electric formula calcining furnace that adopts in low-grade phosphorus ore manufacture level phosphoric acid process that adopts.
Background technology
In the prior art, the production method of PHOSPHORIC ACID TECH.GRADE has two kinds, and a kind of is thermal phosphoric acid: because the more impurity such as iron, aluminium, calcium, magnesium that contain in the phosphorus ore of China are selected P for use
2O
5The quality percentage composition at the phosphorus ore more than 27%, be heated to about 1350 ℃ with electrical heating method, produce the steam contain P, make again and produce phosphoric acid with air roasting, make phosphoric acid salt again, this method power consumption is high, it is big to pollute, and is the project of progressively eliminating.Another kind is phosphoric acid by wet process: this kind method can produce impurity such as aluminum oxide, ferric oxide, calcium oxide, generates the material of a lot of precipitations like this through regular meeting, such as AlPO
4, FePO
4Etc., these precipitations have colloidal state character usually, are difficult to be used, and select P usually for use
2O
5The quality percentage composition be phosphorus ore more than 28%, in the reaction storage tank, add as the vitriol oil and water, make the phosphoric acid of lower concentration, through concentrating, make fertilizer grade and feed-grade phosphate again, purify again and just can make industrial grade phosphate, the cost method of specific heat is low.China's phosphorus ore is low-grade phosphate ore more than 60%, to serve as at most below 25%, adopt wet method relieving haperacidity, must carry out washing to this part phosphorus ore and could use, and has increased production cost, also causes the waste of a lot of resources.Kiln method manufacture level phosphoric acid technology is not also used in industrial production, also has technology not have merit broken.
Calcining furnace is a kind of for pyroprocessing, makes the energy with Sweet natural gas, oil and electricity, is used for ironmaking, reclaims rare metal, and Catalyst Production is improved environment, produces the equipment of extraordinary chemicals.The calcinatory stove is with direct or indirect thermal source, available in gentle high temperature handle batch material continuously, can guarantee that thermal source and product are isolated in the course of processing.In industrial production, the insulation of calcining furnace is very important, and very big value is arranged.Calcining is general for the treatment of very little material, and to oxidation, burning, blast and heat sensitive material, every kind of calcining furnace is by special needs and unique specifications design, but electricity consumption or Sweet natural gas are made thermal source, the hot-zone is arranged in the stove, independently control region is arranged, water cooler can make product in the preceding cooling of coming out of the stove.Calcining furnace be mainly used in pottery, metallurgy, chemical industry, iron and steel, etc. industry, and electric formula calcining furnace is a kind of Thermal Equipment of utilizing electric energy to calcine naturally.
Summary of the invention
The present invention just is being based on above technical problem, provides a kind of rational in infrastructure, the electric formula calcining furnace that can adopt low-grade phosphorus ore to use in the manufacture phosphoric acid process.
Technical scheme of the present invention is:
Select low-grade phosphate ore direct production industrial phosphoric acid for use, in quality percentage composition, P
5O
2It is low-grade phosphate ore that content is lower than 21% phosphorus ore, and its production technique is: low-grade phosphate ore is through pulverize-being blended into change-electric formula calcining furnace calcining-hydrolysis-filtration-purification-concentrate-PHOSPHORIC ACID TECH.GRADE.In this technology, electric formula calcining furnace is key equipment.
Electricity formula calcining furnace, comprise intake zone, preheat the district, heating zone, flat-temperature zone and cooling area, intake zone is connected with opening for feed by the screw feeder pipe, the burner hearth of electricity formula calcining furnace is cylinder-like structure, the burner hearth of electricity formula calcining furnace is disposed across on the service platform, lower end one side at the burner hearth of electric formula calcining furnace arranges electric heating tube uniformly, intake zone is connected with the import of burner hearth, branch is in the burner hearth of electric formula calcining furnace successively to preheat district, heating zone, flat-temperature zone and cooling area, and the outlet of the other end of burner hearth is connected with hydrolytic tank.This electricity formula calcining furnace comprises that also hydrogen fluoride regains receiving apparatus, and hydrogen fluoride is collected arm and is connected with cooling area, flat-temperature zone, heating zone and preheating zone in the burner hearth respectively, gathers then to be the hydrogen fluoride collection tube, and the hydrogen fluoride collection tube is connected with the hydrogen fluoride retrieving arrangement.
Intake zone is connected by rotatable boiler tube with burner hearth, at the rotatable boiler tube of intake zone the hydrogen fluoride collection tube is set.Boiler tube and in-out end adopt high aluminum wool maze-type structure, and each section of high aluminum wool maze-type structure be sealing relatively, and the reduction of heat amount flows and runs off.The hydrogen fluoride collection tube adopts hydrofluoric acid resistant and sulfuric acid and resistant to elevated temperatures material, avoids being corroded breaking with non-refractory.The service platform lower end all adopts Steel Prop to do supporting structure, and such steel construction is more firm.The obliquity 0.5-2 degree of the body of heater of electricity formula calcining furnace.
Electric formula calcining furnace is applied to prepare in the field of PHOSPHORIC ACID TECH.GRADE, in the preparation PHOSPHORIC ACID TECH.GRADE, at first with Rock Phosphate (72Min BPL) after just breaking, pulverize again, the Rock Phosphate (72Min BPL) powder after the pulverizing is crossed 120 mesh sieves, wherein the quality percentage composition of fluorine is about 2.1%; With mixing of materials one-tenthization: Rock Phosphate (72Min BPL) powder and sulfuric acid are entered mixing agitator in proportion stir, mix the back material and be transported to into one-tenth in the change field, both mix and stir in the acidolysis mixing agitator uniformly, in this calcining furnace, calcine then, its calcining step is: the grog after at first will one-tenth is transported to calcining furnace, the temperature of setting in the stove is 100 ℃ earlier, start tube then, in the rotating speed control 1.2-1.5rpm scope of tube, tube was carried out preheating 1 hour, preheating is in order to make the tube preheating even, inequality keeps from heat, influence the work-ing life of calcining furnace, again the temperature in the stove is risen to 250 ℃, with tube preheating half an hour again, press the even charging of 400kg/h again, reach discharging (time of calcining) control at 1.5h-2.5h from charging, the solid-state hydrolysis bucket that directly changes over to, gaseous state enters the fluorine recycling bin by 6 the gas collection tubes in top, the tetra-sodium that the calcining back generates, iron-aluminium oxide solidifies, overflowing gas is hydrogen fluoride, need add water and reclaim, and so just removes fluorine substantially; Reclaim the generation silicofluoric acid through the gaseous substance after the calcining after recovery adds water, solid matter enters the circular hydrolytic tank that has added water and catalyzer, stirs to generate phosphoric acid, and the concentration of phosphoric acid control of generation is about 15%; Material after the hydrolysis is filtered, isolate liquid state and solid-state, liquid dilute phosphoric acid enters reactor to carry out concentrating the first time, and the temperature that concentrates is controlled to be 90 ℃, and concentration of phosphoric acid is controlled 35%, enters in the storage tank after filtering again; Phosphoric acid in the storage tank is injected in the reactor, add a spot of barium sulfate, caustic soda and carbon black, remove and wherein contain a spot of calcium, iron, aluminium, arsenic and discolor, put into storage tank after filtering then; Phosphoric acid in the storage tank is injected reactor, heat then to 110 ℃, control pH value and time, to carry out simultaneously concentrating the second time, the concentration that obtains the product industrial phosphoric acid after concentrating is 63%, 360 tons of symbiosis output 63% PHOSPHORIC ACID TECH.GRADE.To PHOSPHORIC ACID TECH.GRADE finished product sampling analysis, the result all satisfies the PHOSPHORIC ACID TECH.GRADE standard in the national test of trust Sichuan University.
Having adopted rotating speed is the boiler tube of 1-3rpm, tilting furnace degree 0.5-2 degree, and the obliquity of body of heater can guarantee the regulation and control of charging preferably, and temperature control mode is PID control, and drive manner is that speed control by frequency variation is rotated, and being convenient to the velocity of flow of material in boiler tube can regulate.
Electricity formula calcining furnace is except pedestal is Q234, other are the 316L stainless material, the helical feed mode is adopted in charging, boiler tube and in-out end adopt high aluminum wool maze-type structure, temperature control system Japanese fuji temperature controller (thermopair is that signal detection, silicon controlled toggle are that controlling elements, silicon controlled rectifier are for carrying out controlling elements), constant temperature is controlled to be the degenerative closed loop Controlling System of temperature automatically: first set temperature value, feed back the pyroelectric signal of coming by thermopair, the temp controlled meter master chip compares processing, calculates to adjust work output by PID.Transmission rig adopts Mitsubishi's frequency transformer, and the silicon controlled rectifier triggering system is Siemens's technology.
Positively effect of the present invention is embodied in:
Adopt electric formula calcining furnace prepare that PHOSPHORIC ACID TECH.GRADE power consumption is low, technology is simple, easy to operate, cost is low.
If adopt hot legal system to be equipped with PHOSPHORIC ACID TECH.GRADE, need at least material is heated to 1350
0C needs 13000 degree/ton, and this law only need be heated to 290
0C needs 200 degree/ton, and direct generation PHOSPHORIC ACID TECH.GRADE after this calcining, the hydrolysis is cleaned into lowly, and phosphogypsum is anhydrous calciumsulphate, can directly utilize, and effectively saved the energy.
Description of drawings
Fig. 1 is the structural representation of the electric formula calcining furnace that adopts among the present invention.
Wherein, 1---opening for feed, 2---feed zone, 3---screw feeder pipe, 4---tube, 5---preheating zone, 6---heating zone, 7---flat-temperature zone, 8---cooling area, 9---electric heating tube, 10---discharge port, 11---hydrogen fluoride collection tube
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1:
A kind of electric formula calcining furnace that applies in preparation technology's level phosphoric acid, this calcining furnace comprises intake zone, preheat the district, the heating zone, flat-temperature zone and cooling area, intake zone is connected with opening for feed by the screw feeder pipe, the burner hearth of electricity formula calcining furnace is cylinder-like structure, the burner hearth of electricity formula calcining furnace is disposed across on the service platform, lower end one side at the burner hearth of electric formula calcining furnace arranges electric heating tube uniformly, intake zone is connected with the import of burner hearth, preheat the district, the heating zone, flat-temperature zone and cooling area are distributed in the burner hearth of electric formula calcining furnace successively, and the outlet of the other end of burner hearth is connected with hydrolytic tank.This electricity formula calcining furnace comprises that also hydrogen fluoride regains receiving apparatus, and hydrogen fluoride is collected arm and is connected with cooling area, flat-temperature zone, heating zone and preheating zone in the burner hearth respectively, gathers then to be the hydrogen fluoride collection tube, and the hydrogen fluoride collection tube is connected with the hydrogen fluoride retrieving arrangement.Intake zone is connected by rotatable boiler tube with burner hearth, at the rotatable boiler tube of intake zone the hydrogen fluoride collection tube is set.Boiler tube and in-out end adopt high aluminum wool maze-type structure.The hydrogen fluoride collection tube adopts hydrofluoric acid resistant and sulfuric acid and resistant to elevated temperatures material.
The service platform lower end all adopts Steel Prop to do supporting structure.The obliquity 0.5-2 degree of the body of heater of electricity formula calcining furnace.
The technology of preparation PHOSPHORIC ACID TECH.GRADE is:
In on October 18th, 1 2011 on July 9th, 2011, we utilize the old mercury of Jinkouhe District mountain, Leshan, Sichuan Province phosphorus ore to contain P for 1260 tons
2O
521.5% phosphorus ore manufacture phosphoric acid, at first with Rock Phosphate (72Min BPL) after just broken, pulverize again, the Rock Phosphate (72Min BPL) powder after the pulverizing is crossed 120 mesh sieves, wherein the quality percentage composition of F is about 2.1%;
(2) being mixed into: be that 98% sulfuric acid enters mixing agitator in proportion and stirs with Rock Phosphate (72Min BPL) powder and concentration, mix the back material and be transported to into one-tenth 3h in the change field, mass ratio=the 1:0.5 of ground phosphate rock and sulfuric acid, both mix and stir in the acidolysis mixing agitator uniformly, one-tenthization is for further acidolysis, just the calcium phosphate of Sheng Chenging and phosphoric acid are more stable like this;
(3) calcining: the grog after will one-tenth is transported to calcining furnace and calcines, set 100 ℃ earlier, start tube, in the tube rotating speed control 1.2-1.5rpm scope, tube was carried out preheating 1 hour, again temperature is risen to 250 ℃, tube is preheating half an hour again, presses the even charging of 400kg/h again, reach discharging (time of calcining) control about 2h from charging, the solid-state hydrolysis bucket that directly changes over to, gaseous state enters the fluorine recycling bin by 6 the gas collection tubes in top, the tetra-sodium that the calcining back generates, iron-aluminium oxide solidifies, overflowing gas is hydrogen fluoride,, need add water and reclaim, so just remove fluorine substantially;
(4) hydrolysis: reclaim the generation silicofluoric acid through the gaseous substance after the calcining after recovery adds water, solid matter enters the circular hydrolytic tank that has added water, stirs and generates phosphoric acid, and the concentration of phosphoric acid control of generation is 15%;
(5) filter: the material after the hydrolysis is filtered, isolate liquid state and solid-state, liquid dilute phosphoric acid enters reactor to carry out concentrating the first time, and the temperature that concentrates is controlled to be 90 ℃, and concentration of phosphoric acid is controlled 35%, enters in the storage tank after filtering again;
(6) purify: the phosphoric acid in the storage tank is injected in the reactor, add a spot of barium sulfate, caustic soda and carbon black, remove and wherein contain a spot of calcium, iron, aluminium, arsenic and discolor, put into storage tank after filtering then;
(7) concentrate for the second time: the phosphoric acid in the storage tank is injected reactor, heat then to 110 ℃, control pH value and time, to carry out simultaneously concentrating the second time, the concentration that obtains the product industrial phosphoric acid after concentrating is 63%, 360 tons of symbiosis output 63% PHOSPHORIC ACID TECH.GRADE.To PHOSPHORIC ACID TECH.GRADE finished product sampling analysis, the result all satisfies the PHOSPHORIC ACID TECH.GRADE standard in the national test of trust Sichuan University.
Claims (10)
1. the application of electric formula calcining furnace in the preparation PHOSPHORIC ACID TECH.GRADE is characterized in that: adopted electric formula calcining furnace in the technology of preparation PHOSPHORIC ACID TECH.GRADE;
Its concrete application method is: the temperature of at first setting in the stove is 100 ℃, start tube then, tube was carried out preheating 1 hour, again the temperature in the stove is risen to 250 ℃, with tube preheating half an hour again, evenly charging again, the solid-state hydrolysis bucket that directly changes over to, gaseous state enters the fluorine recycling bin by 6 the gas collection tubes in top, and tetra-sodium, iron-aluminium oxide that the calcining back generates solidify, overflowing gas is hydrogen fluoride, and the temperature control during discharging is at 100 ℃.
2. electric formula calcining furnace according to claim 1 is characterized in that in the application of preparation in the PHOSPHORIC ACID TECH.GRADE: describedly tube is carried out preheating, the rotating speed of tube control 1.2-1.5rpm during its preheating.
3. the application of electric formula calcining furnace according to claim 1 in the preparation PHOSPHORIC ACID TECH.GRADE, it is characterized in that: the speed of described charging is the speed charging of 400kg/h.
4. the application of electric formula calcining furnace according to claim 1 in the preparation PHOSPHORIC ACID TECH.GRADE is characterized in that: reach the time control of discharging at 1.5h-2.5h from charging.
5. electric formula calcining furnace, it is characterized in that: this calcining furnace comprises intake zone, preheats the district, heating zone, flat-temperature zone and cooling area, the burner hearth of electricity formula calcining furnace is cylinder-like structure, intake zone is connected with opening for feed by the screw feeder pipe, the burner hearth of electricity formula calcining furnace is disposed across on the service platform, lower end one side at the burner hearth of electric formula calcining furnace arranges electric heating tube uniformly, intake zone is connected with the import of burner hearth, preheat in the burner hearth that district, heating zone, flat-temperature zone and cooling area be distributed in electric formula calcining furnace successively, the outlet of the other end of burner hearth is connected with hydrolytic tank.
6. electric formula calcining furnace according to claim 5, it is characterized in that: this electricity formula calcining furnace also comprises hydrogen fluoride withdrawal receiving apparatus, hydrogen fluoride is collected arm and is connected with cooling area, flat-temperature zone, heating zone and preheating zone in the burner hearth respectively, gather then and be the hydrogen fluoride collection tube, the hydrogen fluoride collection tube is connected with the hydrogen fluoride retrieving arrangement.
7. according to the described electric formula calcining furnace of claim claim 5, it is characterized in that: described intake zone is connected by rotatable boiler tube with burner hearth, at the rotatable boiler tube of intake zone the hydrogen fluoride collection tube is set; Boiler tube and in-out end adopt high aluminum wool maze-type structure.
8. electric formula calcining furnace according to claim 5 is characterized in that: described hydrogen fluoride collection tube employing hydrofluoric acid resistant and sulfuric acid and resistant to elevated temperatures material.
9. electric formula calcining furnace according to claim 5, it is characterized in that: described service platform lower end all adopts Steel Prop to do supporting structure.
10. electric formula calcining furnace according to claim 5 is characterized in that: the obliquity 0.5-2 degree of the body of heater of described electric formula calcining furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108106432A (en) * | 2017-12-22 | 2018-06-01 | 合肥费舍罗热工装备有限公司 | A kind of ceramics shaping degreasing pre-burning stove |
| CN108459498A (en) * | 2018-02-02 | 2018-08-28 | 中国工程物理研究院化工材料研究所 | The wide temperature range high accuracy temperature control system of high-temperature high-pressure reaction kettle and control method |
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| CN1344226A (en) * | 1999-03-24 | 2002-04-10 | 凯米拉化学有限公司 | Process for prodn. of phosphoric acid by crystallisation of phosphoric acid hemihydrate |
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| CN108106432A (en) * | 2017-12-22 | 2018-06-01 | 合肥费舍罗热工装备有限公司 | A kind of ceramics shaping degreasing pre-burning stove |
| CN108459498A (en) * | 2018-02-02 | 2018-08-28 | 中国工程物理研究院化工材料研究所 | The wide temperature range high accuracy temperature control system of high-temperature high-pressure reaction kettle and control method |
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