CN106698377A - Production method of feed-grade tricalcium phosphate - Google Patents
Production method of feed-grade tricalcium phosphate Download PDFInfo
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- CN106698377A CN106698377A CN201510776630.2A CN201510776630A CN106698377A CN 106698377 A CN106698377 A CN 106698377A CN 201510776630 A CN201510776630 A CN 201510776630A CN 106698377 A CN106698377 A CN 106698377A
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Abstract
The invention discloses a production method of feed-grade tricalcium phosphate. The method comprises the following steps: 1, drying of phosphorus rock powder; 2, mixing and ball milling; 3, disc granulation; 4, calcination defluorination; 5, cooling, crushing and sieving; 6, ball-milling of a semi-finished product; 7, screening deironing; and 8, product packaging. The method has the following advantages: 1, the raw material component and the granularity range of the phosphorus rock powder are prescribed; 2, addition of a sodium salt to raw materials facilitates decomposition defluorination of phosphorus rocks; 3, addition of phosphoric acid to the raw materials improves the content of phosphorus in the above product and facilitates granulation and calcination defluorination; 4, addition of steam in the calcining process promotes decomposition defluorination of the phosphorus rocks; 5, the product goes through the area of an electromagnet or a permanent electromagnet to remove iron fillings and other metal impurities, so operation control is simple, and the impurity removal efficiency is high; and 6, calcination tail gas is fully used to produce saturated steam and superheated steam, so energy is saved, and the energy consumption and the production cost are reduced. The method is suitable for producing the feed-grade tricalcium phosphate product.
Description
Technical field
The present invention relates to phosphate, more particularly to calcium phosphate, be furthermore related to tricalcium phosphate.
Background technology
The sintering process technology of feed-level tricalcium phosphate has 5 kinds of silicon process high, low silicon process, low alkaline process, sodium salt phosphoric acid method and phosphoric acid method etc., and these methods all successively realize industrialized production abroad.Silicon process high mainly utilizes various mine tailings, but product P2O5Content is low, and sintering temperature close to fusing point, eliminated at present by easy ring formation in kiln, fluctuation of service；P in low silicon process product2O5Content is higher, but harsher to phosphorus ore requirement, and firing temperature is higher, and industrial production is not used；Low alkaline process is strict unlike low silicon process to ingredient requirement, but firing temperature is with dispensing softening point relatively, operates more difficult control；Current China be used for it is industrial a certain amount of saltcake or NaCl are mainly added with heavy oil as fuel, in raw material, these production Technologies all have that product cost is high, and Oil repellent is high, and product quality is unstable, the aspect shortcoming such as yield is small.
At present, being related to the patent application of feed-level tricalcium phosphate production method has No. 011127910《Feed-level tricalcium phosphate is produced using containing phosphorus waste liquid》, No. ZL021280363《The method of preparing feedstuff grade of defluorination tricalcium phosphate by two times of agglomeration》, No. 20071005756871《The method that feed-level tricalcium phosphate is produced using industrial production of sodium hypophosphite waste residue》, No. 2014105396753《A kind of method for producing feed-level tricalcium phosphate》, these methods can no doubt produce feed-level tricalcium phosphate, but still have that product quality is unstable, the relatively low defect of yield.
The content of the invention
The present invention is intended to provide the relatively low new feed-level tricalcium phosphate production method of a kind of process is simple, easy to operate, product with stable quality, energy consumption, to overcome the defect of prior art.
The feed-level tricalcium phosphate production method that inventor provides mainly includes following operation：
(1) ground phosphate rock drying
Wet ground phosphate rock is sent into dryer, moisture content reaches technological requirement after drying it；
(2)
Mixing and ball milling
The ground phosphate rock dried is mixed with sodium salt in ball mill, the granularity of technological requirement is milled to；
(3) disc granulation
Phosphoric acid is added to be granulated in granulating disc the feed powder after ball milling；
(4) defluorinate is calcined
The material for granulating is calcined in rotary kiln, adds steam promotion rock phosphate in powder to decompose defluorinate in material;Calcining waste heat from tail gas produces saturated vapor or superheated steam as waste heat boiler thermal source；
(5) broken sieving is cooled down
Material after calcining is cooled down in cooler, subsequently into crusher in crushing；Broken material sieving, qualified is semi-finished product；
(6) semi-finished product ball milling
Semi-finished product are sent into ball mill, the particle size range of technological requirement is milled to；
(7) screening, except iron
After semi-finished product ball milling, sieved, oversize returns to disintegrating machine and re-starts the（6）Step semi-finished product ball milling, screenings is then the qualified finished product of granularity；The metal iron tramp of finished product carrying in production process is removed by electromagnet or alnico magnets absorption；
(8) product packaging
The qualified finished product of granularity carries out being packaged to be feed-level tricalcium phosphate product after removing iron.
In (1st) step of the above method, the composition of the wet ground phosphate rock is calculated as with mass fraction：P2O5Content 15%~50%, CaO 30%~60%, MgO≤5%, SiO2≤20%、Pb≤100×10-6、Cd≤100×10-6、As≤100×10-6、(Al2O3+ Fe2O)≤10.0%, moisture content 1%~50%；Ground phosphate rock Task-size Controlling is≤10mm；The process conditions of the drying are：150-1000 DEG C of drying temperature, drying mode：Following current or adverse current；Ground phosphate rock moisture control is≤5% after drying.
In (2nd) step of the above method, the sodium salt is one or more in soda ash, saltcake, sodium chloride, sodium bicarbonate, and NaO mass fractions are 20%~59% in sodium salt；The ground phosphate rock is 0.68~0.85: 0.05~0.30 with the mass ratio of sodium salt；The granularity of the technological requirement is granularity≤10mm.
In (3rd) step of the above method, P in the phosphoric acid2O5Content is 10%~72%；It is described addition phosphoric acid be with the quality proportioning of sodium salt with ground phosphate rock in terms of 100%：0.05~0.30: 0.68~0.85: 0.05~0.30.
In (4th) step of the above method, calcining heat control is at 800 DEG C~2000 DEG C in the rotary kiln；150 DEG C~600 DEG C of the vapor (steam) temperature, 2~30kg/cm of steam pressure2；The temperature control of the calcining tail gas is at 600 DEG C~1600 DEG C.
In (5th) step of the above method, the temperature control of material is at 50 DEG C~250 DEG C after the cooling；The qualified semi-finished product granularity of the sieving is≤25mm.
In (6th) step of the above method, the Task-size Controlling after the semi-finished product ball milling is in 0.013~5mm.
In (7th) step of the above method, the product grading for obtaining that sieves is controlled in 0.013~5mm；The requirement except iron is content≤0.02% for controlling metal iron tramp.
In (8th) step of the above method, the fluorine mass fraction of the finished product is controlled≤0.18%.
The present invention has advantages below compared with the prior art：1. detailed composition range and particle size range is provided to phosphorus ore powder raw material, it is ensured that production process is controlled, reduces product quality fluctuation, be conducive to product to granulate, be conducive to fully calcined and be difficult to tie wall；2. sodium salt is added in raw material, using the low-melting attribute of alkali carbonate, is conducive to rock phosphate in powder to decompose defluorinate, while reducing calcining heat, save energy, reducing energy consumption；3. phosphoric acid is added in raw material can lift product phosphorus content, and reduce the requirement to head grade；Contained humidity is also beneficial to granulate and promotes to calcine defluorinate in phosphoric acid, and without add again it is any be a granulated into globule, meet feed product quality requirement；4. calcination process adds steam, promotes rock phosphate in powder to decompose defluorinate, and without adding other defluorinating agent, process is simple is easy to control；5. product has the attachment of the metal impurities such as iron filings by ball milling, and in this method production process, product passes through the metal impurities such as the region for being provided with electromagnet or alnico magnets, iron filings will be removed, and operational control is simple, except metal impurities efficiency high, product with stable quality；6. beneficial to calcining waste heat from tail gas as waste heat boiler thermal source, saturated vapor and superheated steam are produced, save energy, reducing energy consumption index reduces production cost.Suitable for production feed-level tricalcium phosphate product.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention.
Specific embodiment
It is as follows to the detailed description of the invention below in conjunction with accompanying drawing：
Embodiment
During production, composition is calculated as with mass fraction：P2O5Content 15%~50%, CaO 30%~60%, MgO≤5%, SiO2≤20%、Pb≤100×10-6、Cd≤100×10-6、As≤100×10-6、(Al2O3+ Fe2O)≤10.0%, moisture content about 45%；Ground phosphate rock Task-size Controlling is≤and the wet ground phosphate rock of 10mm lifted by bucket elevator, and dryer is entered through measuring belt metering, and in drying temperature, 900 DEG C carry out adverse current drying；Ground phosphate rock moisture control is≤5% after drying.The sodium salt of ground phosphate rock and soda ash, saltcake, the sodium chloride composition after drying presses ratio requirement, is metered into ball mill mixing and ball milling, and the feed powder obtained after mixing is sent to comminutor, and ground phosphate rock and sodium salt and phosphoric acid are granulated in 0.25: 0.80: 0.25 ratio；The material feeding rotary calciner kiln tail for having granulated carries out preheating and Calcination: Calcination temperature control at 800 DEG C~2000 DEG C；, kiln hood is passed through 500 DEG C of temperature, pressure 20kg/cm2Superheated steam, using counter current contacting formula calcine, temperature be 1000 DEG C tail gas from kiln tail exclude, into waste heat boiler produce saturated vapor or superheated steam.Material discharges from rotary kiln end, counter current contacting formula cooling is carried out into cooler afterwards, 50 DEG C~250 DEG C is cooled to and is obtained feed-level tricalcium phosphate semi-finished product, then semi-finished product are entered to crush and sieve, Task-size Controlling is re-started after crushing and sieved in below 25mm, oversize return disintegrating machine；Again by screening after finished product ball milling, screenings is the qualified finished product of granularity, and product grading is controlled in 0.013~5mm；By electromagnet or alnico magnets, the impurity such as metallic iron finally obtains qualified feed-level tricalcium phosphate product to the qualified finished product of granularity by magnet adsorption, and packaging is dispatched from the factory.
Claims (9)
1. a kind of feed-level tricalcium phosphate production method, it is characterised in that comprise the following steps：
(1) ground phosphate rock drying
Wet ground phosphate rock is sent into dryer, moisture content reaches technological requirement after drying it；
(2) mixing and ball milling
The ground phosphate rock dried is mixed with sodium salt in ball mill, the granularity of technological requirement is milled to；
(3) disc granulation
Phosphoric acid is added to be granulated in granulating disc the feed powder after ball milling；
(4) defluorinate is calcined
The material for granulating is calcined in rotary kiln, adds steam promotion rock phosphate in powder to decompose defluorinate in material;Calcining waste heat from tail gas produces saturated vapor or superheated steam as waste heat boiler thermal source；
(5) broken sieving is cooled down
Material after calcining is cooled down in cooler, subsequently into crusher in crushing；Broken material sieving, qualified is semi-finished product；
(6) semi-finished product ball milling
Semi-finished product are sent into ball mill, the particle size range of technological requirement is milled to；
(7) screening, except iron
After semi-finished product ball milling, sieved, oversize returns to disintegrating machine and re-starts the（6）Step semi-finished product ball milling, screenings is then the qualified finished product of granularity；The metal iron tramp of finished product carrying in production process is removed by electromagnet or alnico magnets absorption；
(8) product packaging
The qualified finished product of granularity carries out being packaged to be feed-level tricalcium phosphate product after removing iron.
2. production method as claimed in claim 1, it is characterised in that in (1st) step, the composition of the wet ground phosphate rock is calculated as with mass fraction：P2O5Content 15%~50%, CaO 30%~60%, MgO≤5%, SiO2≤20%、Pb≤100×10-6、Cd≤100×10-6、As≤100×10-6、(Al2O3+ Fe2O)≤10.0%, moisture content 1%~50%；Ground phosphate rock Task-size Controlling is≤10mm；The process conditions of the drying are：150-1000 DEG C of drying temperature, drying mode：Following current or adverse current；Ground phosphate rock moisture control is≤5% after drying.
3.
Production method as claimed in claim 1, it is characterised in that in (2nd) step, the sodium salt is one or more in soda ash, saltcake, sodium chloride, sodium bicarbonate, and NaO mass fractions are 20%~59% in sodium salt；The ground phosphate rock is 0.68~0.85: 0.05~0.30 with the mass ratio of sodium salt；The granularity of the technological requirement is granularity≤10mm.
4.
Production method as claimed in claim 1, it is characterised in that in (3rd) step, P in the phosphoric acid2O5Content is 10%~72%；It is described addition phosphoric acid be with the quality proportioning of sodium salt with ground phosphate rock in terms of 100%：0.05~0.30: 0.68~0.85: 0.05~0.30.
5.
Production method as claimed in claim 1, it is characterised in that in (4th) step, calcining heat control is at 800 DEG C~2000 DEG C in the rotary kiln；150 DEG C~600 DEG C of the vapor (steam) temperature, 2~30kg/cm of steam pressure2；The temperature control of the calcining tail gas is at 600 DEG C~1600 DEG C.
6.
Production method as claimed in claim 1, it is characterised in that in (5th) step, the temperature control of material is at 50 DEG C~250 DEG C after the cooling；The qualified semi-finished product granularity of the sieving is below 25mm.
7.
Production method as claimed in claim 1, it is characterised in that in (6th) step, the Task-size Controlling after the semi-finished product ball milling is in 0.013~5mm.
8.
Production method as claimed in claim 1, it is characterised in that in (7th) step, the product grading for obtaining that sieves is controlled in 0.013~5mm；The requirement except iron is content≤0.02% for controlling metal iron tramp.
9.
Production method as claimed in claim 1, it is characterised in that in (8th) step, the fluorine mass fraction of the finished product is controlled≤0.18%.
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| CN201510776630.2A CN106698377A (en) | 2015-11-15 | 2015-11-15 | Production method of feed-grade tricalcium phosphate |
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| CN201510776630.2A CN106698377A (en) | 2015-11-15 | 2015-11-15 | Production method of feed-grade tricalcium phosphate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522186A (en) * | 2017-09-30 | 2017-12-29 | 上海彩凤环保科技股份有限公司 | A kind of production method of feed-level tricalcium phosphate |
| CN111377423A (en) * | 2020-05-12 | 2020-07-07 | 瓮福（集团）有限责任公司 | Method for producing feed-grade tricalcium phosphate by using low-calorific-value tail gas |
| CN114181560A (en) * | 2021-11-04 | 2022-03-15 | 江阴市星宇化工有限公司 | Special high-activity tricalcium phosphate for enhancing whiteness and brightness of fluorescent coating and production process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458062A (en) * | 2003-01-29 | 2003-11-26 | 贵州开磷集团磷业有限责任公司 | Process for producing defluorinated tricatlcium phosphate |
| CN101318642A (en) * | 2008-07-04 | 2008-12-10 | 湖北三新磷钙有限公司 | Process for preparing tricalcium defluorophosphoric acid |
| CN103071572A (en) * | 2013-01-25 | 2013-05-01 | 连云港市德邦精细化工有限公司 | Preparation method of superfine tricalcium phosphate |
-
2015
- 2015-11-15 CN CN201510776630.2A patent/CN106698377A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458062A (en) * | 2003-01-29 | 2003-11-26 | 贵州开磷集团磷业有限责任公司 | Process for producing defluorinated tricatlcium phosphate |
| CN101318642A (en) * | 2008-07-04 | 2008-12-10 | 湖北三新磷钙有限公司 | Process for preparing tricalcium defluorophosphoric acid |
| CN103071572A (en) * | 2013-01-25 | 2013-05-01 | 连云港市德邦精细化工有限公司 | Preparation method of superfine tricalcium phosphate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522186A (en) * | 2017-09-30 | 2017-12-29 | 上海彩凤环保科技股份有限公司 | A kind of production method of feed-level tricalcium phosphate |
| CN111377423A (en) * | 2020-05-12 | 2020-07-07 | 瓮福（集团）有限责任公司 | Method for producing feed-grade tricalcium phosphate by using low-calorific-value tail gas |
| CN114181560A (en) * | 2021-11-04 | 2022-03-15 | 江阴市星宇化工有限公司 | Special high-activity tricalcium phosphate for enhancing whiteness and brightness of fluorescent coating and production process thereof |
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Application publication date: 20170524 |
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