CN106698375A - Calcining defluorination method in feed-grade tricalcium phosphate production - Google Patents
Calcining defluorination method in feed-grade tricalcium phosphate production Download PDFInfo
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- CN106698375A CN106698375A CN201510775692.1A CN201510775692A CN106698375A CN 106698375 A CN106698375 A CN 106698375A CN 201510775692 A CN201510775692 A CN 201510775692A CN 106698375 A CN106698375 A CN 106698375A
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- calcining
- materials
- fluorine
- steam
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/328—Defluorination during or after the preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a calcining defluorination method in feed-grade tricalcium phosphate production. According to the method, phosphoric acid is added to dry rock phosphate and sodium salt and the materials undergo granulation in a disk granulating machine; the granulated materials enter a rotary calcining kiln from the tail part; primary air and secondary air are introduced into the kiln head of the rotary calcining kiln so as to support combustion of fuel in the combustion section, and the materials undergo countercurrent calcining in the combustion section of the rotary calcining kiln; a steam pipeline extends into the kiln, steam which accounts for 10-60% of content of the total materials is added according to content of the materials and content of fluorine in the raw materials during calcining, and letting the steam fully react with the materials to take away the fluorine in the form of HF from the materials by tail gas. After the calcining, mass fraction of the fluorine in the materials is less than 0.18%. The method is simple, convenient and stable to operate, and no defluorination agent is added. Cost is low, and content of fluorine in the product can be effectively reduced. In the production, steam can be adjusted according to the content of fluorine in the materials. The method is easy to control, and the content of fluorine in the product is stable. The method is an ideal defluorination technology for the feed-grade tricalcium phosphate production.
Description
Technical field
The present invention relates to phosphate, more particularly to calcium phosphate, be furthermore related to the production method of tricalcium phosphate.
Background technology
It is well known that in feed-level tricalcium phosphate production process, defluorinate is most important operation；Traditional feed-level tricalcium phosphate defluorination process predominantly adds defluorinating agent in the feed, and put into rotary kiln carries out high-temperature calcination defluorinate afterwards.Because calcining heat is higher, temperature is difficult to control during production operation；During system driving and parking, temperature fluctuation is big, and defluorination effect is unstable, easily produces defective work；Meanwhile, defluorinating agent costly, therefore, production cost is high.These factors are to cause feed-level tricalcium phosphate to produce the main cause for not yet forming large-scale production at present.
At present, the Chinese patent application part of defluorination method is few in being related to feed-level tricalcium phosphate to produce, only No. ZL2011100836679《A kind of defluorination method of tricalcium phosphate》With No. ZL021280363《The method of preparing feedstuff grade of defluorination tricalcium phosphate by two times of agglomeration》2.The former is to add adhesive to cause spherolite to send into calcined by rotary kiln to semi-molten state with smart ground phosphate rock, silica, calcium carbonate stone powder, sodium sulphate, Diammonium phosphate (DAP) to carry out defluorinate；The latter is that ground phosphate rock is worn into fine powder, is mixed with defluorinating agent soda ash, agstone, adds thermal phosphoric acid to bond and is made bead, carries out second sintering in rotary kiln afterwards.These methods can no doubt produce feed-level tricalcium phosphate, but still have that product quality is unstable, the defect that production cost is high, yield is relatively low.
The content of the invention
The present invention is intended to provide a kind of defluorinate efficiency high, simple to operate, the calcining defluorination method saved in equipment investment and the feed-level tricalcium phosphate production of operating cost, to overcome the defect of prior art.
Inventor provide feed-level tricalcium phosphate production in calcining defluorination method be：Phosphoric acid is added to be granulated in granulating disc dry ground phosphate rock and sodium salt, the material of granulation enters rotary calciner from afterbody；First air and Secondary Air are passed through in the kiln hood of rotary calciner to help the fuel combustion in burning zone, burning zone adverse current of the material in rotary calciner is calcined；There is jet chimney to stretch into the inside of kiln, during calcining according to Oil repellent in inventory and raw material how much, after adding the steam of total material 10%~60%, steam fully to be reacted with material, substantial amounts of fluorine is taken away with HF gas forms by tail gas in material, and the mass fraction of fluorine is less than 0.18% in material after calcining；
Calcining heat control is at 800 DEG C~2000 DEG C in the rotary calciner；The steam is saturated vapor or superheated steam, and its temperature is 150 DEG C~600 DEG C, and pressure is 2~30kg/cm2。
Fuel in above-mentioned burning zone is the one kind in heavy oil, coal tar, petroleum coke, yellow phosphoric tail gas, coal, natural gas.
Above-mentioned jet chimney is directly 15~100mm, and it is the 1/10~1/4 of barrel lenght to stretch into the length of rotary calcining kiln cylinder body.
The present invention compared with the prior art, has obvious beneficial effect in defluorinate：Steam is added in calcining, 30 DEG C~80 DEG C of calcining heat reduction can be made；High-temperature steam reacts with the fluorine in ground phosphate rock, generates HF gases, drains with tail gas, and significantly, the fluorine-containing mass fraction of product is less than 0.18% to defluorination effect, less than Oil repellent index in feed-level tricalcium phosphate national standard.
The inventive method is simple, convenient, stabilization, and without adding any defluorinating agent, low cost can effectively reduce product fluorinated volume；Steam can be adjusted according to the Oil repellent of calcining product in production, steam is easily controllable, product Oil repellent index stabilization meets the requirement of industrialized production, is a kind of preferable feed-level tricalcium phosphate defluorination process technology.
Brief description of the drawings
Fig. 1 is calcining defluorination process schematic flow sheet in feed-level tricalcium phosphate of the invention production.
In figure, 1 is calcining kiln, and 2 is jet chimney, and 3 is gas pipeline, and 4 is Secondary Air pipeline, and 5 is First air pipeline, and 6 is material inlet, and 7 is offgas outlet.
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 of granulation enters rotary calciner from afterbody；First air and Secondary Air are passed through in the kiln hood of rotary calciner to help the fuel combustion in burning zone, fuel is yellow phosphoric tail gas, and calcining heat is controlled at 1200 DEG C ± 100 DEG C；Burning zone adverse current of the material in rotary calciner is calcined；It is directly the jet chimney of 80mm that the inside of kiln has, and it is the 1/5 of barrel lenght that the pipeline stretches into the length of rotary calciner, during calcining according to Oil repellent in inventory and raw material how much, add the superheated steam of total material 50%, its temperature is 500 DEG C, pressure 20kg/cm2.Steam fully reacts with material, and fluorine is taken away with HF gas forms by tail gas in material, and the mass fraction of fluorine is less than 0.18% in material after calcining.
Claims (3)
1. the one kind in feed-level tricalcium phosphate production calcines defluorination method, it is characterised in that：Phosphoric acid is added to be granulated in granulating disc dry ground phosphate rock and sodium salt, the material of granulation enters rotary calciner from afterbody；First air and Secondary Air are passed through in the kiln hood of rotary calciner to help the fuel combustion in burning zone, burning zone adverse current of the material in rotary calciner is calcined；There is jet chimney the inside of kiln, during calcining according to Oil repellent in inventory and raw material how much, after adding the steam of total material 10%~60%, steam fully to be reacted with material, substantial amounts of fluorine is taken away with HF gas forms by tail gas in material, and the mass fraction of fluorine is less than 0.18% in material after calcining；
Calcining heat control is at 800 DEG C~2000 DEG C in the rotary calciner；The steam is saturated vapor or superheated steam, and its temperature is 150 DEG C~600 DEG C, and pressure is 2~30kg/cm2。
2.
Calcining defluorination method as claimed in claim 1, it is characterised in that the fuel in the burning zone is the one kind in heavy oil, coal tar, petroleum coke, yellow phosphoric tail gas, coal, natural gas.
3. as claimed in claim 1 to calcine defluorination method, it is characterised in that a diameter of 15~100mm of the jet chimney, the length that the pipeline stretches into rotary calciner is the 1/10~1/4 of barrel lenght.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510775692.1A CN106698375A (en) | 2015-11-15 | 2015-11-15 | Calcining defluorination method in feed-grade tricalcium phosphate production |
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| CN201510775692.1A CN106698375A (en) | 2015-11-15 | 2015-11-15 | Calcining defluorination method in feed-grade tricalcium phosphate production |
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| CN201510775692.1A Pending CN106698375A (en) | 2015-11-15 | 2015-11-15 | Calcining defluorination method in feed-grade tricalcium phosphate production |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN113061202A (en) * | 2021-04-21 | 2021-07-02 | 武汉科林化工集团有限公司 | Defluorination method of high-fluorine-content petroleum resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323737A (en) * | 2000-05-16 | 2001-11-28 | 单光渝 | Process of preparing defluorinated phosphate and purifying fluoric tail gas |
| 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 |
-
2015
- 2015-11-15 CN CN201510775692.1A patent/CN106698375A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323737A (en) * | 2000-05-16 | 2001-11-28 | 单光渝 | Process of preparing defluorinated phosphate and purifying fluoric tail gas |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN113061202A (en) * | 2021-04-21 | 2021-07-02 | 武汉科林化工集团有限公司 | Defluorination method of high-fluorine-content petroleum resin |
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Application publication date: 20170524 |
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