CN106348271A - Production method for preparing ammonium polyphosphate from wet-process phosphoric acid serving as raw material - Google Patents
Production method for preparing ammonium polyphosphate from wet-process phosphoric acid serving as raw material Download PDFInfo
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- CN106348271A CN106348271A CN201610778504.5A CN201610778504A CN106348271A CN 106348271 A CN106348271 A CN 106348271A CN 201610778504 A CN201610778504 A CN 201610778504A CN 106348271 A CN106348271 A CN 106348271A
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- phosphoric acid
- raw material
- wet process
- production method
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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
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
- C01B25/405—Polyphosphates of ammonium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
- C05D9/02—Other inorganic fertilisers containing trace elements
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a production method for preparing ammonium polyphosphate from wet-process phosphoric acid serving as a raw material. The wet-process phosphoric acid serving as the raw material, a nitrogen-containing compound is added, the charge ratio of the wet-process phosphoric acid to a nitrogen source agent is (1.5-3):1, the wet-process phosphoric acid and the nitrogen-containing compound are put into a stirring type reactor, mixed uniformly and heated to 100 to 150 DEG C, and stirring reaction is conducted for 80 to 150 minutes under the conditions that the pressure is 0.1 to 0.3 MPa and constant temperature is maintained, so that an ammonium polyphosphate solution with low polymerization degree can be prepared. The wet-process phosphoric acid serves as the raw material, so that the production cost is obviously reduced, the polymerization degree n of the produced ammonium polyphosphate is less than or equal to 15, and the ammonium polyphosphate has full water solubility and can directly serve as water-soluble fertilizer.
Description
Technical field
The invention belongs to the Quadrafos production technical field in inorganic chemistry industry, it is specifically related to the life of APP
Product method.
Background technology
APP, also known as ammonium polyphosphate or polycondensation ammonium phosphate (abbreviation app), is a kind of Quadrafos containing n.According to
The difference of specifically used demand, can produce oligomeric, in poly- and high poly- 3 kinds different extent of polymerizations product, its degree of polymerization gets over
Highly-water-soluble is less, otherwise then water solublity is bigger.Crystalline and amorphous can be divided into by its structure, crystalline state APP is
Long chain water-insoluble salt.The general molecular formula of APP is (nh4)(n+2)pno(3n+1), when n is 2~20, it is water solublity;When
When n is more than 20, it is slightly solubility.High-purity high polymerization degree water-insoluble long chain APP is used for preparing high-grade fireproof painting
Material, flame retardant plastics.The water miscible product of low polymerization degree can use as fire retardant it can also be used to high-grade plant nutritional solution (liquid
Fertile).
Phosphoric acid used in APP production at present is mainly the preferable thermal phosphoric acid of quality.Phosphoric acid production method master
Wet method to be had and full-boiled process.Phosphorus ore is mainly smelted in electric furnace, distils, condensing the yellow phosphorus burning obtaining, Hou Shui by thermal phosphoric acid
Conjunction, again dearsenization purify and are obtained, and have the advantages that product design height, purity are high, but high energy consumption, high cost.The life of phosphoric acid by wet process
Product mode is phosphoric acid to be obtained with mineral acid with rock phosphate in powder decomposition reaction, and the concentration of phosphoric acid by wet process is low, impurity is many, but cost is relatively low,
Also occur in that some purification of wet process phosphoric acid with the preferable phosphoric acid of the quality of production now.
China at present have research using thermal phosphoric acid, full-boiled process polyphosphoric acid at relatively high temperatures ammonification, dehydration, make solid again
Or liquid APP fertilizer.Phosphoric acid by wet process impurity content is high, is concentrated into the easy fouling of high concentration process, solidification, and polymerization is difficult, and one
As APP is not prepared using Wet-process Phosphoric Acid Production.
But normal wet phosphoric acid method of specific heat phosphoric acid cost will low 20% to 40%, purification of wet process phosphoric acid method of specific heat phosphoric acid cost
Low by 10% about, normal wet phosphoric acid impurities method of specific heat phosphoric acid will be multiplied, if normal wet phosphoric acid can be utilized
Full water-soluble low-polymerization-dammonium ammonium polyphosphate in accordance with prescription is obtained, then production cost can be made to substantially reduce, to Liquid Fertilizer
Material industry is significant.
Content of the invention:
The present invention proposes a kind of production method for raw material APP for phosphoric acid in a wet process, is former using phosphoric acid by wet process
Material, adds nitrogen-containing compound to carry out condensation reaction and prepares APP, polymerization degree n≤15 of the APP produced, tool
There is full water-soluble, can be directly as Water soluble fertilizer.
The purpose of the present invention is achieved through the following technical solutions:
A kind of phosphoric acid in a wet process is the production method of raw material APP, and phosphoric acid is raw material in a wet process, according to rate of charge
Add nitrogen-containing compound for 1.5~3:1, put into mix homogeneously in stirring reactor, be heated to 100~150 DEG C, in pressure
Constant temperature stirring reaction 80~150min is kept, you can prepared low-polymerization-dammonium ammonium polyphosphate solution under 0.1~0.3mpa.
Further preferred as technical scheme, described nitrogen-containing compound is liquefied ammonia, ammonia, ammonium hydrogen carbonate, carbamide, three
At least one in poly cyanamid or dicyandiamide.
Further preferred as technical scheme, the mutual proportioning between described nitrogen-containing compound is 1:1~2.
Further preferred as technical scheme, described reacting by heating temperature is 110~120 DEG C.
Further preferred as technical scheme, described pressure is 0.2~0.3mpa.
Further preferred as technical scheme, the described stirring reaction time is 100~120min.
Further preferred as technical scheme, described mixing speed is 50~200r/min.
Further preferred as technical scheme, the present invention can adopt 30~50% phosphoric acid by wet process;May also be employed
Purity reaches more than 95% purification of wet process phosphoric acid.
Compared with prior art, the synthetic method of the present invention is advantageous in that:
1. phosphoric acid to produce APP solution for raw materials for production to the present invention in a wet process, compared to existing thermal phosphoric acid,
Polyphosphoric acid produces APP technique and can save 30%~50% on cost.
2. the impurity in phosphoric acid by wet process phosphoric acid condensation become APP solution after be chelated and molten be integrated, and these
Impurity is mainly fluorine, magnesium, ferrum, aluminum, silicon, sulfate radical etc., and these elements mostly are the middle trace element beneficial to plant growing, can be straight
It is connected into the nutrition for Water soluble fertilizer, to plant growing, there is facilitation.And it is believed that wet in traditional APP production method
The easy fouling of impurity in method phosphoric acid, solidification, it is unfavorable for that APP produces, therefore these impurity are cleared by FEOL early,
Therefore long the production cycle, production cost increases.
3. polymerization degree n≤15 of the APP solution that the present invention produces, can be dissolved in water entirely, be rich in plant growing simultaneously
Required middle trace element, can be used for agricultural production directly as Water soluble fertilizer.
Specific embodiment
With reference to embodiment, the present invention will be further described, but the scope of protection of present invention is not limited to
The scope of embodiment statement.
Embodiment 1
A kind of phosphoric acid in a wet process is the production method of raw material APP, with 30~40% phosphoric acid by wet process as raw material,
Add ammonium hydrogen carbonate according to rate of charge for 2:1, mix homogeneously in common input stirring reactor, it is heated to 120 DEG C, in pressure
Constant temperature stirring reaction 90min is kept, control rotating speed is 100r/min, you can prepared low-polymerization-dammonium ammonium polyphosphate is molten under 0.3mpa
Liquid, its polymerization degree n≤15, containing the middle trace element needed for the plants such as magnesium, ferrum, silicon.
Embodiment 2
A kind of phosphoric acid in a wet process is the production method of raw material APP, with 40~50% phosphoric acid by wet process as raw material,
Add tripolycyanamide according to rate of charge for 3:1, mix homogeneously in common input stirring reactor, it is heated to 120 DEG C, in pressure
Constant temperature stirring reaction 150min is kept, control rotating speed is 200r/min, you can prepared low-polymerization-dammonium ammonium polyphosphate is molten under 0.2mpa
Liquid, its polymerization degree n≤10, containing the middle trace element needed for the plants such as magnesium, ferrum, silicon.
Embodiment 3
A kind of phosphoric acid in a wet process is the production method of raw material APP, with 95% purification of wet process phosphoric acid as raw material,
Add dicyandiamide according to rate of charge for 1.5:1, mix homogeneously in common input stirring reactor, it is heated to 100 DEG C, in pressure
Constant temperature stirring reaction 80min is kept, control rotating speed is 50r/min, you can prepared low-polymerization-dammonium ammonium polyphosphate solution under 0.1mpa,
Its polymerization degree n≤10, containing the middle trace element needed for the plants such as magnesium, ferrum, silicon.
Embodiment 4
A kind of phosphoric acid in a wet process is the production method of raw material APP, with 40~50% phosphoric acid by wet process as raw material,
Add carbamide according to rate of charge for 2:1, mix homogeneously in common input stirring reactor, it is heated to 120 DEG C, in pressure
Constant temperature stirring reaction 100min is kept, control rotating speed is 100r/min, you can prepared low-polymerization-dammonium ammonium polyphosphate is molten under 0.2mpa
Liquid, its polymerization degree n≤10, containing the middle trace element needed for the plants such as magnesium, ferrum, silicon.
Embodiment 5
A kind of phosphoric acid in a wet process is the production method of raw material APP, is thrown with 40~50% phosphoric acid by wet process for raw material
Enter in stirring reactor, be passed through ammonia;The volume mass ratio of intake and phosphoric acid by wet process controlling ammonia for 3:1, is heated to
110 DEG C, keep constant temperature stirring reaction 120min under pressure 0.2mpa, control rotating speed is 150r/min, you can prepared oligomerization
Degree APP solution, its polymerization degree n≤10, containing the middle trace element needed for the plants such as magnesium, ferrum, silicon.
Embodiment 6
A kind of phosphoric acid in a wet process is the production method of raw material APP, with 40~50% phosphoric acid by wet process as raw material,
Add the mixture of ammonium hydrogen carbonate and carbamide, ammonium hydrogen carbonate and urea quality ratio for 2:1 according to rate of charge for 1:1, common put into
Mix homogeneously in stirring reactor, is heated to 150 DEG C, keeps constant temperature stirring reaction 100min under pressure 0.2mpa, controls
Rotating speed is 100r/min, you can prepared low-polymerization-dammonium ammonium polyphosphate solution, its polymerization degree n≤15, containing plants such as magnesium, ferrum, silicon
Required middle trace element.
Embodiment 7
A kind of phosphoric acid in a wet process is the production method of raw material APP, with 40~50% phosphoric acid by wet process as raw material,
The mixture of ammonium hydrogen carbonate and dicyandiamide, ammonium hydrogen carbonate and dicyandiamide mass ratio is added to be 1:2 for 1.5:1 according to rate of charge, altogether
With putting into mix homogeneously in stirring reactor, it is heated to 120 DEG C, keep constant temperature stirring reaction under pressure 0.2mpa
120min, control rotating speed be 100r/min, you can prepared low-polymerization-dammonium ammonium polyphosphate solution, its polymerization degree n≤15, containing magnesium,
Middle trace element needed for the plants such as ferrum, silicon.
Low-polymerization-dammonium ammonium polyphosphate solution prepared by the present invention as Water soluble fertilizer and traditional nitrogen phosphorus fertilizer, all according to 20g
Every plant of peach tree is applied fertilizer (base manure), adds every plant of 40g of fertilising after 50 days;Compare after 90 days, apply low polymerization degree of the present invention
The peach tree of APP solution exceeds 5~10% in plant height than common fertilizer, and branch and leaf are more in great numbers, and growing way is more good.
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not to the present invention
Embodiment restriction.For those of ordinary skill in the art, can also be made it on the basis of the above description
The change of his multi-form or variation.There is no need to be exhaustive to all of embodiment.All essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included in the protection model of the claims in the present invention
Within enclosing.
Claims (9)
1. a kind of phosphoric acid in a wet process for raw material APP production method it is characterised in that: in a wet process phosphoric acid be raw material, press
It is that 1.5~3:1 adds nitrogen-containing compound according to rate of charge, put into mix homogeneously in stirring reactor, be heated to 100~150 DEG C,
Keep constant temperature stirring reaction 80~150min under pressure 0.1~0.3mpa, you can prepared low-polymerization-dammonium ammonium polyphosphate solution.
2. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
Nitrogen-containing compound be liquefied ammonia, ammonia, ammonium hydrogen carbonate, carbamide, at least one in tripolycyanamide or dicyandiamide.
3. phosphoric acid in a wet process according to claim 2 for raw material APP production method it is characterised in that: described
Mutual proportioning between nitrogen-containing compound is 1:1~2.
4. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
Heating-up temperature is 110~120 DEG C.
5. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
Pressure is 0.2~0.3mpa.
6. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
The stirring reaction time is 100~120min.
7. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
Mixing speed is 50~200r/min.
8. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
Phosphoric acid by wet process concentration be 30~50%.
9. phosphoric acid in a wet process according to claim 1 for raw material APP production method it is characterised in that: described
Phosphoric acid by wet process adopt purification of wet process phosphoric acid, purity reaches more than 95%.
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107324305A (en) * | 2017-06-30 | 2017-11-07 | 云南芳麟科技有限公司 | A kind of production method of inorganic ammonium salt, the inorganic ammonium salt and application |
CN107502091A (en) * | 2017-08-31 | 2017-12-22 | 苏州仲勉装饰有限公司 | A kind of preparation method of washable interior wall coating |
CN108675275A (en) * | 2018-05-28 | 2018-10-19 | 湖北工业大学 | A method of utilizing the agricultural ammonium polyphosphate of Wet-process Phosphoric Acid Production |
CN109395686A (en) * | 2018-10-16 | 2019-03-01 | 武汉工程大学 | A kind of equipment and its application method for phosphoric acid by wet process preparation low-polymerization-dammonium ammonium polyphosphate |
CN109704818A (en) * | 2017-10-25 | 2019-05-03 | 四川大学 | DAP compound fertilizer and preparation method thereof |
CN110357670A (en) * | 2019-07-04 | 2019-10-22 | 湖北祥云(集团)化工股份有限公司 | A method of compound fertilizer containing ammonium polyphosphate is prepared using industrial monoammonium phosphate slag |
CN111689805A (en) * | 2020-06-23 | 2020-09-22 | 四川大学 | Production method of compound fertilizer |
CN112341251A (en) * | 2020-11-10 | 2021-02-09 | 云南云天化股份有限公司 | Method for preparing ammonium phosphate containing polymeric phosphorus by using wet-process phosphoric acid |
CN112624849A (en) * | 2020-12-28 | 2021-04-09 | 瓮福(集团)有限责任公司 | Preparation method of high-solubility nitrogen-phosphorus water-soluble fertilizer |
CN114773129A (en) * | 2022-04-25 | 2022-07-22 | 什邡市长丰化工有限公司 | Hard water resistant water-soluble fertilizer and application thereof |
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CN104528682A (en) * | 2014-12-18 | 2015-04-22 | 防城港博森化工有限公司 | Method for preparing full water-soluble ammonium polyphosphate water solution by using wet process phosphoric acid |
CN105858633A (en) * | 2016-06-22 | 2016-08-17 | 云南云天化以化磷业研究技术有限公司 | Production method for preparing water-soluble ammonium polyphosphate by using wet-process purified phosphoric acid |
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Patent Citations (2)
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CN104528682A (en) * | 2014-12-18 | 2015-04-22 | 防城港博森化工有限公司 | Method for preparing full water-soluble ammonium polyphosphate water solution by using wet process phosphoric acid |
CN105858633A (en) * | 2016-06-22 | 2016-08-17 | 云南云天化以化磷业研究技术有限公司 | Production method for preparing water-soluble ammonium polyphosphate by using wet-process purified phosphoric acid |
Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107324305A (en) * | 2017-06-30 | 2017-11-07 | 云南芳麟科技有限公司 | A kind of production method of inorganic ammonium salt, the inorganic ammonium salt and application |
CN107502091A (en) * | 2017-08-31 | 2017-12-22 | 苏州仲勉装饰有限公司 | A kind of preparation method of washable interior wall coating |
CN109704818A (en) * | 2017-10-25 | 2019-05-03 | 四川大学 | DAP compound fertilizer and preparation method thereof |
CN109704818B (en) * | 2017-10-25 | 2020-06-30 | 四川大学 | DAP compound fertilizer and preparation method thereof |
CN108675275B (en) * | 2018-05-28 | 2019-11-08 | 湖北工业大学 | A method of utilizing the agricultural ammonium polyphosphate of Wet-process Phosphoric Acid Production |
CN108675275A (en) * | 2018-05-28 | 2018-10-19 | 湖北工业大学 | A method of utilizing the agricultural ammonium polyphosphate of Wet-process Phosphoric Acid Production |
CN109395686A (en) * | 2018-10-16 | 2019-03-01 | 武汉工程大学 | A kind of equipment and its application method for phosphoric acid by wet process preparation low-polymerization-dammonium ammonium polyphosphate |
CN110357670A (en) * | 2019-07-04 | 2019-10-22 | 湖北祥云(集团)化工股份有限公司 | A method of compound fertilizer containing ammonium polyphosphate is prepared using industrial monoammonium phosphate slag |
CN111689805A (en) * | 2020-06-23 | 2020-09-22 | 四川大学 | Production method of compound fertilizer |
CN112341251A (en) * | 2020-11-10 | 2021-02-09 | 云南云天化股份有限公司 | Method for preparing ammonium phosphate containing polymeric phosphorus by using wet-process phosphoric acid |
CN112624849A (en) * | 2020-12-28 | 2021-04-09 | 瓮福(集团)有限责任公司 | Preparation method of high-solubility nitrogen-phosphorus water-soluble fertilizer |
WO2022142861A1 (en) * | 2020-12-28 | 2022-07-07 | 瓮福(集团)有限责任公司 | Method for preparing high-solubility nitrogen-phosphorus water-soluble fertilizer |
CN114773129A (en) * | 2022-04-25 | 2022-07-22 | 什邡市长丰化工有限公司 | Hard water resistant water-soluble fertilizer and application thereof |
CN114773129B (en) * | 2022-04-25 | 2023-08-11 | 什邡市长丰化工有限公司 | Hard water resistant water-soluble fertilizer and application thereof |
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