CN101857465B - Production method of low-fluoride granular monoammonium phosphate product - Google Patents
Production method of low-fluoride granular monoammonium phosphate product Download PDFInfo
- Publication number
- CN101857465B CN101857465B CN 201010181855 CN201010181855A CN101857465B CN 101857465 B CN101857465 B CN 101857465B CN 201010181855 CN201010181855 CN 201010181855 CN 201010181855 A CN201010181855 A CN 201010181855A CN 101857465 B CN101857465 B CN 101857465B
- Authority
- CN
- China
- Prior art keywords
- phosphoric acid
- neutralization
- fluorine
- monoammonium phosphate
- massfraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention discloses a production method of a low-fluoride granular monoammonium phosphate product. The method comprises the following steps: (1) acid preparation: taking pretreated phosphoric acid which is produced in the process of purifying wet-process phosphoric acid, and proportionally mixing the pretreated phosphoric acid with the extracted phosphoric acid to ensure the mass fraction of fluorine in the mixed acid to be lower than 0.6%, wherein, the pretreated phosphoric acid contains 52-54% of phosphoric acid and no more than 0.4% of the fluorine in mass percent, and the extracted phosphoric acid contains 48% of phosphoric acid and 1-1.5% of fluorine in mass percent; (2) pre-neutralization and blowing: pre-neutralizing the mixed acid by ammonia in a pre-neutralization slot in which an air blowing device is arranged, and then blowing out part of fluorine-containing gas in slurry by compressed air quantity; and (3) neutralization and granulation: utilizing a tubular reactor to neutralize the pre-neutralized slurry and ammonia once again, controlling the neutralization degree of the slurry to be 0.65, spraying slurry and granulating to obtain the low-fluoride granular monoammonium phosphate product. The method overcomes the technical problem of utilizing the extracted phosphoric acid to produce the low-fluoride granular monoammonium phosphate product; and the good product quality can satisfy the market demand at home and abroad. The method is suitable for manufacturers having both a purified wet-process phosphoric acid device and a phosphoric acid extraction device for producing monoammonium phosphate.
Description
Technical field
The present invention relates to phosphate fertilizer, specifically, relate to monoammonium phosphate product.
Background technology
Traditional granular monoammonium phosphate product with slurry concentrated process or the production of pre-neutralization spray granulating, fluorine content is applied to environment unfavorable up to 1.5%～2.0%.Yet the world market requires quite high to the fluorine content's index, requires in product fluorine content lower than below 1%, if can't reach the requirement of production qualified product with the phosphoric acid of traditional wet-process phosphoric acid concentration production at all; With the granular monoammonium phosphate product that diluted acid enriching slurry method is produced, its fluorine content can be higher, can not get low-fluoride granular monoammonium phosphate product.This has become the technical barrier that monoammonium phosphate product is produced.
In existing patented technology, No. CN1305945 " a kind of feed grade, technical grade and technical grade monoammonium phosphate production method " of Sichuan Lomon Group Co., Ltd's application, with containing calcification and thing such as calcium carbonate etc. and extraction wet-process phosphoric acid reaction, ammonification neutralizes with negatively charged ion F in calcification and thing form precipitated acid
-, SO
4 2-With the Fe in the phos-phate forms precipitated acid
2O
3, Al
2O
3Then carry out solid-liquid separation, supernatant, evaporation concentration, crystallization, oven dry; Obtain feed grade, industrial grade monoammonium phosphate.Its product master content monoammonium phosphate is greater than 98%, and fluorine is lower than 0.16%.But can this technology stably produce low-fluoride granular monoammonium phosphate product, still unknown.
Summary of the invention
The object of the present invention is to provide a kind of production method of low-fluoride granular monoammonium phosphate product, to solve the technical barrier that reduces monoammonium phosphate product fluorine content.
The contriver calculates according to product structure analysis and concrete index, and point out: the fluorine in phosphoric acid mainly is H
2SiF
6Form exist, in ammonia and the time will carry out following balanced reaction:
SiF
2- 6+4OH
-+(n-2)H
2O＝＝＝SiO
2.nH
2O+6F
-
Therefore, as long as in acid, fluorine content is lower than in 0.6%, just can reach the requirement of production low-fluoride granular monoammonium phosphate product.But therefore the phosphoric acid fluorine content that conventional Wet Processes of Phosphoric Acid is produced do not reach the requirement of producing low fluorine product all more than 1%.The contriver is by research, find a scheme that puts the axe in the helve, that is: as long as the fluorine content in the reduction raw material acid just can reach the requirement that reduces the fluorine content in product, then use the producing granular monoammonium phosphate with diammonium phosphate device product, can produce low-fluoride granular monoammonium phosphate product.
The production method of the low-fluoride granular monoammonium phosphate product that the contriver provides comprises following main points:
(1) complex acid: take the phosphoric acid quality mark of producing in the purification of wet process phosphoric acid process and be 52%～54%, the pre-treatment phosphoric acid of fluorine massfraction≤0.4%, be 48% with common phosphoric acid quality mark, the fluorine massfraction is that 1%～1.5% phosphoric acid extraction is mixed in proportion, and makes the fluorine-containing massfraction of mixing acid lower than 0.6%;
(2) pre-neutralization, air blowing: mixing acid first carries out pre-neutralization with ammonia in the pre-neutralization groove, establish the Air blowing device in groove, blows out part fluoro-gas in the pre-neutralization slip with air supply;
(3) neutralization, granulation: with tubular reactor, pre-neutralization slip and ammonia are neutralized again, controlling the slip degree of neutralization is 0.65, according to the common process spray granulating, produces low-fluoride granular monoammonium phosphate product.
The add-on of the pre-treatment phosphoric acid of producing in above-mentioned purification of wet process phosphoric acid process is calculated as follows:
X×1.5％+Y×0.3％≤0.6％(X+Y)
In formula: X is the amount for the common phosphoric acid extraction that mixes,
Y is the add-on for the pre-treatment phosphoric acid that mixes;
The 1.5%th, the massfraction that common phosphoric acid extraction is fluorine-containing,
The 0.3%th, the massfraction that pre-treatment phosphoric acid is fluorine-containing,
The 0.6%th, the fluorine-containing massfraction of phosphoric acid after default the mixing;
Draw: the X/0.3% of Y≤(1.5%-0.6%)
Just can calculate needed pre-treatment acid amount by the raw material acid amount of sending, just can reach dispensing acid amount.
Above-mentioned pressurized air is by 20m
3The speed of/h is injected in reactor.
The contriver points out, after mixing, the massfraction of phosphoric acid is lower than pre-treatment phosphoric acid, and higher than common phosphoric acid extraction, therefore, its degree of neutralization should suitably reduce, and could satisfy the technique needs.
The contriver also points out, along with the carrying out of neutralization reaction, can increase free F
-, after blowing air blows out, contain F gas and overflow from reaction slurry, just can reduce its fluorine content.Certainly, the fluorine of discharge need to be processed, with protection of the environment.Due to fluorine usually with hydrogen fluoride HF and silicon tetrafluoride SiF
4Discharge, the method for used water carrying out washing treatment: by washing tail gas, two fluorine-containing materials all are adsorbed, and form very rare silicofluoric acid and then return the system recoveries utilization.
The contriver points out again, produces the technology of granular monoammonium phosphate with the features of DAP production device, has been documented among No. 200910263800.1, Chinese patent application part, its characteristics are to adopt tubular reactor to neutralize with strong phosphoric acid and ammonia, control degree of neutralization, then spray granulating, obtain granulated product.
The inventive method has overcome this technical barrier of granulated product that utilizes the low fluorine of original phosphoric acid extraction production, and superior product quality can satisfy the needs in market at home and abroad.Present method is applicable to the producer that existing purification of wet process phosphoric acid device has again the phosphoric acid extraction device, produces monoammonium phosphate.
Description of drawings
Accompanying drawing is the pre-neutralization groove schematic diagram that is provided with the Air blowing device.
In figure: 1 is the pre-neutralization groove, and 2 is spray pump, and 3 is acid tube, and 4 is the Air blowing device; 5 is vapour ammonia pipe, and 6 is ammonia stripping system induced exhaust.
Embodiment
Diammonium phosphate subsidiary factory of urn good fortune phosphate fertilizer plant produces the embodiment of the monoammonium phosphate granulated product of low fluorine:
At first complex acid: make pre-treatment acid through defluorinate, desulfurization from purifying phosphoric acid factory, its phosphoric acid quality mark is 52%～54%, the fluorine massfraction is 0.3%; And the common phosphoric acid by wet process that diammonium phosphate subsidiary factory produces, i.e. the fluorine-containing massfraction of extraction acid is 1.5% left and right.
If common phosphoric acid by wet process is proportion is 1.6, massfraction is 48%, send the acid amount to be 40m
3/ h; The proportion of pre-treatment acid is 1.65, massfraction is 52%, and pre-treatment acid is Y; In phosphoric acid extraction, the massfraction of fluorine is by 1.5%, and in pre-treatment acid, fluorine content is by 0.3%, according to the required pre-treatment acid of following calculating:
X×1.5％+Y×0.3％≤0.6％(X+Y)
The X/0.3% of Y≤(1.5%-0.6%)
Be calculated as follows:
In phosphoric acid extraction, fluorine content is: X * 1.5%=40 * 1.6 * 1.5%=0.96
Y≤(1.5%-0.6%) * 0.96/0.3%
Y≤2.24
Get by maximum value, just pre-treatment acid amount is: 2.24/1.65=1.3575m
3/ h.
Then, blow: mixing acid first carries out pre-neutralization with ammonia in the pre-neutralization groove, the Air blowing device in groove is pressed 20m
3The speed of/h blows out part fluoro-gas in the pre-neutralization slip with air supply;
Neutralization, granulation again: with tubular reactor, pre-neutralization slip and ammonia are neutralized again, controlling the slip degree of neutralization is 0.65, according to the common process spray granulating, produces low-fluoride granular monoammonium phosphate product.
Claims (2)
1. the production method of low-fluoride granular monoammonium phosphate product, its feature comprises:
(1) complex acid: take the phosphoric acid massfraction 52%～54% of producing in the purification of wet process phosphoric acid process, the pre-treatment phosphoric acid solution of fluorine-containing massfraction≤0.4%, mix with common phosphoric acid massfraction 48%, the phosphoric acid extraction of fluorine-containing massfraction 1%～1.5%, make the fluorine-containing massfraction of mixed phosphate solution lower than 0.6%;
The add-on of described pre-treatment phosphoric acid is calculated as follows:
X×1.5％+Y×0.3％≤0.6％(X+Y)
In formula: X is the amount for the common phosphoric acid extraction that mixes,
Y is the add-on for the pre-treatment phosphoric acid that mixes,
The 1.5%th, the massfraction that common phosphoric acid extraction is fluorine-containing,
The 0.3%th, the massfraction that pre-treatment phosphoric acid is fluorine-containing,
The 0.6%th, the fluorine-containing massfraction of phosphoric acid after default the mixing;
Draw: the X/0.3% of Y≤(1.5%-0.6%);
Amount by the common phosphoric acid extraction of sending into calculates needed pre-treatment phosphoric acid amount;
(2) pre-neutralization, air blowing: mixing acid first carries out pre-neutralization with ammonia in the pre-neutralization groove, establish the Air blowing device in groove, blows out part fluoro-gas in the pre-neutralization slip with pressurized air;
(3) neutralization, granulation: with tubular reactor, pre-neutralization slip and ammonia are neutralized again, controlling the slip degree of neutralization is 0.65, according to the common process spray granulating, produces low-fluoride granular monoammonium phosphate product.
2. according to production method claimed in claim 1, it is characterized in that described pressurized air is by 20m
3The speed of/h is injected in reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010181855 CN101857465B (en) | 2010-05-25 | 2010-05-25 | Production method of low-fluoride granular monoammonium phosphate product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010181855 CN101857465B (en) | 2010-05-25 | 2010-05-25 | Production method of low-fluoride granular monoammonium phosphate product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101857465A CN101857465A (en) | 2010-10-13 |
| CN101857465B true CN101857465B (en) | 2013-05-22 |
Family
ID=42943659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010181855 Active CN101857465B (en) | 2010-05-25 | 2010-05-25 | Production method of low-fluoride granular monoammonium phosphate product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101857465B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445121B (en) * | 2014-11-21 | 2017-02-08 | 贵州开磷集团股份有限公司 | Mono-ammonium phosphate produced by using wet process phosphoric acid and production method of mono-ammonium phosphate |
| CN108751152B (en) * | 2018-05-30 | 2022-03-18 | 湖北三宁化工股份有限公司 | Method for improving pH value of industrial monoammonium phosphate produced by wet-process phosphoric acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1520059A1 (en) * | 1986-08-19 | 1989-11-07 | В.И.Левераш, ВоМоРонкин и В.И.Жебелев | Method of producing feed diammonium phosphate |
| CN1154350A (en) * | 1996-01-08 | 1997-07-16 | 肥城市磷铵厂 | Art for phosphoric ore secondary decomposition by using extracted phosphoric acid |
| CN101538027A (en) * | 2008-03-20 | 2009-09-23 | 江西贵溪化肥有限责任公司 | Production process for granular monoammonium phosphate |
-
2010
- 2010-05-25 CN CN 201010181855 patent/CN101857465B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1520059A1 (en) * | 1986-08-19 | 1989-11-07 | В.И.Левераш, ВоМоРонкин и В.И.Жебелев | Method of producing feed diammonium phosphate |
| CN1154350A (en) * | 1996-01-08 | 1997-07-16 | 肥城市磷铵厂 | Art for phosphoric ore secondary decomposition by using extracted phosphoric acid |
| CN101538027A (en) * | 2008-03-20 | 2009-09-23 | 江西贵溪化肥有限责任公司 | Production process for granular monoammonium phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101857465A (en) | 2010-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104829271B (en) | A kind of method that utilization phosphorus mine tailing prepares ammonium phosphate calcium and magnesium and ammonium nitrate calcium and magnesium | |
| CN103613083B (en) | A kind of phosphoric acid by wet process and high-purity phosphoric acid are in conjunction with the method for manufacture level monoammonium phosphate | |
| CN103113139B (en) | Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge | |
| CN102126738B (en) | Method for producing nitrophosphate fertilizer and co-producing gypsum through decomposing phosphorite with nitric acid | |
| CN101891504A (en) | Method for producing granular monoammonium phosphate with raffinate | |
| CN104860287B (en) | A kind of method for preparing ammonium magnesium phosphate and ammonium nitrate magnesium using phosphorus mine tailing | |
| CN102502551A (en) | Method for recycling phosphorus and fluorine in defluorination residues | |
| CN105600763B (en) | A kind of method that fluoride salt method of purification produces industrial monoammonium phosphate | |
| CN102126742B (en) | Method for producing chloride-based compound fertilizer and co-producing gypsum through decomposing phosphorite with hydrochloric acid | |
| CN104326475A (en) | Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black | |
| CN102126737A (en) | Method for producing nitrate-and-sulfur-based compound fertilizer and co-producing gypsum by utilizing potassium hydrogen sulfate | |
| CN103043684A (en) | Method for producing ammonium hydrogen fluoride by recovering fluorine in wet process phosphoric acid tail gas | |
| CN105314599A (en) | Method for producing anhydrous hydrogen fluoride and white carbon black through fluosilicic acid | |
| CN104843712A (en) | Industrial fluosilicic acid purification and white carbon black co-production method | |
| CN103553722A (en) | Method for preparing super phosphate by use of ardealite slag site sewage | |
| CN107879321B (en) | Method for demagging phosphate rock and co-producing sodium fluosilicate and magnesium sulfate | |
| CN102602904B (en) | Method for producing monoammonium phosphate from raffinate acid | |
| CN101857465B (en) | Production method of low-fluoride granular monoammonium phosphate product | |
| CN104445121A (en) | Mono-ammonium phosphate produced by using wet process phosphoric acid and production method of mono-ammonium phosphate | |
| CN106241834B (en) | Sodium bifluoride technology is prepared using phosphorous chemical industry fluosilicic acid as byproduct | |
| CN101786741A (en) | Method for defluorinating acid waste water with high fluorine | |
| CN105347321B (en) | The method that phosphorus ammonium is produced using low-grade low concentration raffinate | |
| CN103663499A (en) | Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production | |
| CN103539130A (en) | Technological method for preparing white carbon black from potassium feldspar | |
| CN108455647B (en) | Method for producing calcium fluoride and by-products of white carbon black and ammonium sulfate by phosphoric acid by-product phosphogypsum and fluosilicic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: He Haoming Inventor after: Liu Xianbo Inventor after: Zhang Hongying Inventor after: Xu Chun Inventor after: Xiao Sheng Inventor after: Dai Guangyuan Inventor after: Deng Yongda Inventor after: Li Wei Inventor before: Liu Xianbo Inventor before: Zhang Hongying Inventor before: Xu Chun Inventor before: Xiao Sheng Inventor before: Dai Guangyuan Inventor before: Deng Yongda Inventor before: Li Wei |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: LIU XIANBO ZHANG HONGYING XU CHUN XIAO SHENG DAI GUANGYUAN DENG YONGDA LI WEI TO: HE HAOMING LIU XIANBO ZHANG HONGYING XU CHUN XIAO SHENG DAI GUANGYUAN DENG YONGDA LI WEI |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder |
Address after: 550500 Guizhou Province, Qiannan Buyei and Miao Autonomous Prefecture Fuquan Racecourse town Yingbin Road No. 1 Wengfu group Patentee after: WENGFU GROUP Co.,Ltd. Address before: 23, 550002 floor, urn Fuk international, No. 57, South City Road, Guizhou, Guiyang Patentee before: WENGFU GROUP Co.,Ltd. |
|
| CP02 | Change in the address of a patent holder |