CN105036852B - Utilize the method for industrial grade monoammonium phosphate mother liquor production a great number of elements water-soluble fertilizer - Google Patents
Utilize the method for industrial grade monoammonium phosphate mother liquor production a great number of elements water-soluble fertilizer Download PDFInfo
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Abstract
Utilize the method for industrial grade monoammonium phosphate mother liquor production a great number of elements water-soluble fertilizer, urea liquid or ammonium nitrate solution, potash fertilizer, microelement and chelating agent will be added in industrial grade monoammonium phosphate mother liquor, through chelating, filtering, concentration, dry obtained a great number of elements water-soluble fertilizer.Whole process three-waste free discharge of the invention, realizes cascade utilization and the comprehensive utilization of resource, reduces production cost, economic benefit is improved, and a great number of elements water-soluble fertilizer produced is compared with physics mixture method, it is with high purity, appearance is good, at low cost, is especially advantageous for marketing and agricultural application.
Description
Technical field
The invention belongs to technical field of fertilizers, and in particular to water-soluble using industrial grade monoammonium phosphate mother liquor production a great number of elements
The method of fertilizer.
Background technique
Water-soluble fertilizer refers to polyelement composite fertilizer that can be completely soluble, after water dissolves or dilutes, can be used for filling
Irrigate the solid or liquid fertilizer of the purposes such as fertilising, foliage dressing.Since water-soluble fertilizer can completely dissolve in water, more hold
Easily be absorbed by crops, it is instant, without residue, absorptivity is high, quick, application facilitates etc. is the remarkable advantage of water-soluble fertilizer, and
By being applied to the industrialized agricultures such as spray, trickle irrigation, water-fertilizer integral may be implemented.The Ministry of Agriculture's " water-fertilizer integral printed and distributed in 2013
Technological guidance's opinion " it points out, the gross area, which is promoted, to the Integration of Water into Fertilizer in 2015 reaches 80,000,000 mu or more.
At present the country water-soluble fertilizer production method be mainly physics mixture method, i.e., by industrial grade monoammonium phosphate, potassium sulfate,
The raw materials such as potassium dihydrogen phosphate carry out simple physics mixture.Using method production water-soluble fertilizer, there are two problems: first is that, because of raw material
At high cost to cause water-soluble fertilizer price high, peasant, which holds, to dare not accept, and significantly limits the promotion and application of water-soluble fertilizer；Second is that
Easily there is the problems such as deliquescence, agglomeration, flatulence, excessive impurity in the water-soluble fertilizer of method production.Compared with physics mixture method, chemistry is closed
The water-soluble fertilizer appearance produced at method is good, and quality, existing related patents are reported.103011122 B of Chinese patent CN
A kind of method of Wet-process Phosphoric Acid Production water-soluble phosphoric acid potassium ammonium is disclosed, this method through desulfurization, takes off using phosphoric acid by wet process as raw material
Fluorine, ammonia neutralize to obtain monoammonium phosphate solution, and monoammonium phosphate clear liquid and potassium chloride carry out metathesis reaction, and crystallization obtains potassium phosphate
Chloro water-soluble fertilizer is made after being evaporated, being dried in ammonium, mother liquor.102633551 B of Chinese patent CN, which is disclosed, a kind of uses agricultural fertilizer
The method of material production a great number of elements water-soluble fertilizer, method includes the following steps: 1, potassium dihydrogen phosphate or agricultural potassium sulfate matched
Saturated solution is made, clear liquid is obtained by filtration, urea then is added into saturation clear liquid, crystalline substance is made after crystallisation by cooling, centrifugal filtration
Body potassium dihydrogen phosphate or potassium sulfate；2, agricultural monoammonium phosphate is dissolved with the mother liquor from potassium dihydrogen phosphate or potassium sulfate, ammonia is added
Monoammonium phosphate clear liquid is obtained by filtration in water reaction；3, by monoammonium phosphate clear liquid, crystal phosphoric acid potassium dihydrogen or potassium sulfate, urea, nitric acid
Water-soluble fertilizer reaction kettle is added in potassium and microelement, carries out being spray-dried obtained a great number of elements Water soluble fertilizer after isothermal reaction half an hour
Material.
The technique of country's preparing industrial grade monoammonium phosphate from wet-process phosphoric acid is usual at present are as follows: phosphoric acid by wet process is through desulfurization, defluorinate, ammonia
Purer monoammonium phosphate solution is obtained after neutralizing removal of impurities, filtering, monoammonium phosphate solution is concentrated again, crystallisation by cooling, was centrifuged
Filter, dry obtained industrial grade monoammonium phosphate.It is general to the processing of mother liquor that there are two types of methods: first is that, return system and phosphorus after desulfurization
Desulfurization again after acid-mixed conjunction or return system are mixed with phosphoric acid, but the desulfurizing agents such as barium carbonate, phosphate ore pulp need to be additionally introduced, increase
Production cost, and excessive calcium ion can be introduced when using phosphate ore pulp, it calcium monohydrogen phosphate is produced in ammonifying process, causes product
Water-insoluble is exceeded.It is used to produce agricultural monoammonium phosphate second is that directly sending mother liquor to phosphate fertilizer plant, due in the mother liquor after purification
Impurity it is seldom, send to the agricultural monoammonium phosphate of production and undoubtedly cause artificial, the waste of resource and the energy.Patent
A kind of method with Wet-process Phosphoric Acid Production monoammonium phosphate coproduction N-P binary compound fertilizer is disclosed in 201210329385.
Summary of the invention
The purpose of the present invention is recycling to industrial grade monoammonium phosphate mother liquor, a kind of utilization PHOSPHORIC ACID TECH.GRADE one is provided
The method that ammonium mother liquor produces a great number of elements water-soluble fertilizer, the effectively save cost of energy, improves benefit.
In order to solve the above technical problems, the technical scheme adopted by the invention is that: it is raw using industrial grade monoammonium phosphate mother liquor
The method for producing a great number of elements water-soluble fertilizer, specific steps are as follows:
1) according to a great number of elements water-soluble fertilizer of required preparation and according to the regulation of NY1107-2010 standard, to technical grade
Urea liquid, potash fertilizer, middle microelement and chelating agent are added in monoammonium phosphate mother liquor；It then passes to ammonia or ammonium hydroxide is added and adjust
The pH value of solution is reacted to 4.5~5.0, is controlled 70~90 DEG C of reaction temperature, is stirred simultaneously, and 30~60min is reacted
It filters while hot afterwards；
2) filtrate obtained by step 1) is concentrated, until being spray-dried, being obtained when water content mass fraction is 25~35%
To a great number of elements water-soluble fertilizer.
Further, the temperature of the urea liquid in step 1) is 90~105 DEG C, mass concentration is 68~75%.
Urea liquid in step 1) is substituted using ammonium nitrate solution, and temperature is 110~125 DEG C, mass concentration
It is 85~90%.Specific substitution amount matches determination according to needed for fertilizer, can not use urea liquid using ammonium nitrate solution.
The urea liquid or ammonium nitrate solution can be directly from urea plant or ammonium nitrate production device, sufficiently
Utilize its heat, energy saving.
Potash fertilizer described in step 1) is agricultural potassium chloride, agricultural potassium sulfate, Agricultural Potassium Nitrate and agricultural potassium dihydrogen phosphate
One or more of combination.
Middle microelement described in step 1) is calcium nitrate, magnesium sulfate, sodium metasilicate, ferrous sulfate, manganese sulfate, sulfuric acid
The combination of one or more of copper, zinc sulfate, ammonium molybdate, boric acid etc..
Chelating agent described in step 1) is ammonium polyphosphate, ethylenediamine tetra-acetic acid, citric acid, amino acid, humic acid, few shell
The combination of one or more of sugar, glucose saccharic acid etc..
Microelement and when chelating agent in addition in step 1), chelating agent additive amount and the middle microelement in solution are total
The molar ratio of content is 1~3 ﹕ 1.
Filter residue after filtering in step 1) is rinsed with water, the filter residue after flushing and the water containing effective phosphorus composition send to
It is recycled in the process units of agricultural monoammonium phosphate.
When stirring in step 1), 400~800r/min of speed of agitator is controlled.
The present invention primarily to prevent the fixation of soil centering microelement, improves crop using the purpose of chelating technology
The utilization rate of middle microelement.By controlling suitable chelating condition such as temperature, pH and stirring rate etc. to be met the requirements
A great number of elements water-soluble fertilizer.
Mother liquor is concentrated and is spray-dried in method provided by the invention, other raw materials are added before this, it can
To utilize the intermediate product such as urea liquid or ammonium nitrate solution in other workshops.
Method provided by the invention using industrial grade monoammonium phosphate mother liquor production a great number of elements water-soluble fertilizer, has following
The utility model has the advantages that
1, using industrial grade monoammonium phosphate mother liquor as raw material, a great number of elements water-soluble fertilizer of high added value is produced, rather than handle
Purer mother liquor is sent to agricultural monoammonium phosphate device for producing low value-added agricultural monoammonium phosphate, realizes the ladder of resource
Grade utilizes, and is also fully utilized by the heat of urea liquid or ammonium nitrate solution, reduces steam consumption；
2, this method is by microelement in microelement in addition in the solution and chelating agent synthesis chelating, rather than adds
Add microelement in commercially available high price chelating, not only improves the utilization rate of middle microelement, but also reduce production cost；
3, agricultural fertilizer raw material can be used to produce a great number of elements water-soluble fertilizer in this method, and in dissolution, chelating,
Chemical reaction between raw material can carry out completely, avoid often occur in physics mixture method due to the chemical reaction between raw material and
The problems such as caused product agglomeration, flatulence.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, but the scope of protection of present invention is not limited to implement
The range of example statement.
Industrial grade monoammonium phosphate mother liquor involved in following embodiment is to prepare PHOSPHORIC ACID TECH.GRADE one using phosphoric acid by wet process
It is obtained when ammonium, specific steps are as follows:
It 1) is 20~28%P by mass concentration2O5Phosphoric acid,diluted carry out concentrating and impurity removing, added after being concentrated into 46~48%
Sedimentation agent sedimentation removal of impurities, the phosphoric acid after removal of impurities are diluted to 20~28% with process water again；
2) the dilution phosphoric acid that step 1) obtains is pumped to ammoniation reactor, logical ammonia is once neutralized, and degree of neutralization is controlled
1.01~1.04,105~115 DEG C of reaction temperature, a neutralize slip is pumped after filtering to secondary neutralization chamber；
3) diluted acid is added in Xiang Erci neutralization chamber and completes secondary neutralization, control secondary neutralize slip pH value 4.4~4.6, two
Secondary neutralize slip is pumped after filtering to two effect concentration evaporators；
4) pump is to crystallization tank crystallisation by cooling after slurry double effect concentration to relative density 1.34~1.38, and magma was through being centrifuged
Filter, obtained crystal obtain industrial grade monoammonium phosphate after vibra fluidized bed drying, and centrifuge mother liquor is the raw material in the application
Industrial grade monoammonium phosphate mother liquor.
Sedimentation agent used is polyacrylamide or similar additive with the same function, and additive amount is with volume basis
1~5 ‰.Added diluted acid is that the concentration after being diluted in step 1) with process water is 20~28% phosphoric acid,diluteds.
Using the phosphoric acid by wet process of low-grade phosphate ore production as raw material, pretreatment phosphorus is obtained using concentrating and impurity removing and sedimentation removal of impurities
Acid, at low cost and process flow is simple compared with adding compound impurity removing technology, can be in phosphorus compound fertilizer enterprise large-scale promotion；And
Using concentration and settlement pretreatment, secondary neutralization and secondary concentration, process flow is simple, and technic index control is reliable, stablizes, side
Just, product quality is high, and output capacity is high.
Resulting industrial grade monoammonium phosphate mother liquor is the ammonium sulfate and monoammonium phosphate solution of water content 60%~65%, butt nitrogen
Phosphorus potassium nutrition content is 13.5-53.5-0.
Embodiment 1:
1) the industrial grade monoammonium phosphate mother liquor 1071.4kg of water content 65% is taken, the urea liquid of water content 30% is then added
214.3kg, potassium nitrate 380.0kg, cupric sulfate pentahydrate 3.0kg, ferrous sulfate heptahydrate 10.0kg, three water manganese sulfate 7.0kg, seven water
Zinc sulfate 3.0kg, ammonium molybdate tetrahydrate 1.0kg, epsom salt 20.0kg, EDTA52.0kg then pass to ammonia or ammonia are added
The pH value that water adjusts solution is reacted to 4.5~5.0, is controlled 70~90 DEG C of reaction temperature, is stirred simultaneously, is reacted
It is filtered while hot after 30min；
2) filtrate obtained by step 1) is concentrated, until being spray-dried, being obtained when water content mass fraction is 25%
1000.0kg a great number of elements water-soluble fertilizer, wherein containing 17.0%N, 20.0%P2O5、17.0%K2O、0.075%Cu、0.2%Fe、0.2%
Mn、0.07%Zn、0.05%Mo。
Embodiment 2:
1) the industrial grade monoammonium phosphate mother liquor 1400kg of water content 60% is taken, the ammonium nitrate solution of water content 10% is then added
177.8kg, potassium sulfate 185.0kg, cupric sulfate pentahydrate 3.0kg, ferrous sulfate heptahydrate 10.0kg, three water manganese sulfate 7.0kg, seven water
Zinc sulfate 3.0kg, ammonium molybdate tetrahydrate 1.0kg, epsom salt 20.0kg, EDTA52.0kg then pass to ammonia or ammonia are added
The pH value that water adjusts solution is reacted to 4.5~5.0, is controlled 70~90 DEG C of reaction temperature, is stirred simultaneously, is reacted
It is filtered while hot after 60min；
2) filtrate obtained by step 1) is concentrated, until being spray-dried, being obtained when water content mass fraction is 25%
1000.0kg a great number of elements water-soluble fertilizer, wherein containing 13.2%N, 30.0%P2O5、9.3%K2O、0.075%Cu、0.2%Fe、0.2%
Mn、0.07%Zn、0.05%Mo。
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. utilizing the method for industrial grade monoammonium phosphate mother liquor production a great number of elements water-soluble fertilizer, which is characterized in that specific steps are as follows:
1) according to a great number of elements water-soluble fertilizer of required preparation and according to the regulation of NY1107-2010 standard, to PHOSPHORIC ACID TECH.GRADE
Addition temperature is 90~105 DEG C in monoammonium mother liquor, the urea liquid that mass concentration is 68~75% or temperature are 110~125
DEG C, mass concentration be 85~90% ammonium nitrate solution and potash fertilizer, middle microelement and chelating agent；It then passes to ammonia or adds
Enter ammonium hydroxide and adjust the pH value of solution and reacted to 4.5~5.0, controls 70~90 DEG C of reaction temperature, be stirred simultaneously, instead
It is filtered while hot after answering 30~60min；Urea liquid or ammonium nitrate solution used directly from urea plant or
Ammonium nitrate production device；
2) filtrate obtained by step 1) is concentrated, until being spray-dried when water content mass fraction is 25~35%, is obtained big
Secondary element water-soluble fertilizer；
The industrial grade monoammonium phosphate mother liquor obtains when preparing industrial grade monoammonium phosphate using phosphoric acid by wet process, specific steps
Are as follows:
It 1) is 20~28%P by mass concentration2O5Phosphoric acid,diluted carry out concentrating and impurity removing, sedimentation is added after being concentrated into 46~48%
Agent sedimentation removal of impurities, the phosphoric acid after removal of impurities are diluted to 20~28% with process water again；
2) the dilution phosphoric acid that step 1) obtains being pumped to ammoniation reactor, logical ammonia is once neutralized, control degree of neutralization 1.01~
1.04,105~115 DEG C of reaction temperature, a neutralize slip is pumped after filtering to secondary neutralization chamber；
3) diluted acid is added in Xiang Erci neutralization chamber and completes secondary neutralization, control secondary neutralize slip pH value 4.4~4.6, it is secondary in
It is pumped after filtering with slurry to two effect concentration evaporators；
4) to crystallization tank crystallisation by cooling, magma obtains pump through centrifugal filtration after slurry double effect concentration to relative density 1.34~1.38
To crystal industrial grade monoammonium phosphate is obtained after vibra fluidized bed drying, centrifuge mother liquor is industrial grade monoammonium phosphate mother liquor.
2. according to the method described in claim 1, it is characterized by: potash fertilizer described in step 1) is agricultural potassium chloride, agricultural
The combination of one or more of potassium sulfate, Agricultural Potassium Nitrate and agricultural potassium dihydrogen phosphate.
3. according to the method described in claim 1, it is characterized by: middle microelement described in step 1) is calcium nitrate, sulphur
The combination of one or more of sour magnesium, sodium metasilicate, ferrous sulfate, manganese sulfate, copper sulphate, zinc sulfate, ammonium molybdate, boric acid.
4. according to the method described in claim 1, it is characterized by: chelating agent described in step 1) is ammonium polyphosphate, second two
The combination of one or more of amine tetraacethyl, citric acid, amino acid, humic acid, few chitose, glucose saccharic acid.
5. according to the method described in claim 1, it is characterized by: microelement and when chelating agent in addition in step 1),
The molar ratio of middle microelement total content in chelating agent additive amount and solution is 1~3 ﹕ 1.
6. according to the method described in claim 1, it is characterized by: when being stirred in step 1), control speed of agitator 400~
800r/min。
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| CN106916003A (en) * | 2015-12-28 | 2017-07-04 | 江苏绿方园生物科技有限公司 | Amount type Macroelement water-soluble suspension liquid fertilizer and preparation method in organic-inorganic |
| CN107285813A (en) * | 2016-04-11 | 2017-10-24 | 湖北南轻法麦克斯作物营养有限公司 | A kind of method that use rock phosphate in powder produces Water soluble fertilizer |
| CN106335888B (en) * | 2016-08-23 | 2018-12-21 | 湖北中孚化工集团有限公司 | Utilize the method and device of industrial monoammonium crystalline mother solution synthesis ammonium polyphosphate |
| CN106977282A (en) * | 2017-04-06 | 2017-07-25 | 安徽康坶国际化肥股份有限公司 | A kind of insect pest a great number of elements water-soluble fertilizer |
| CN109020695A (en) * | 2018-08-30 | 2018-12-18 | 安徽六国化工股份有限公司 | A kind of N P and K TE compound fertilizer preparation process |
| CN109384208A (en) * | 2018-12-20 | 2019-02-26 | 湖北六国化工股份有限公司 | A kind of the step application method and system of phosphor ammonium slurry |
| CN109574735A (en) * | 2018-12-20 | 2019-04-05 | 四川大学 | The processing and MAP coproduction of phosphorus ammonium mother liquor are containing the technique of middle microelement APP |
| CN111592386A (en) * | 2020-06-10 | 2020-08-28 | 河南中之州植保有限公司 | Preparation method of chelated rare earth |
| CN112938923B (en) * | 2020-12-28 | 2023-07-07 | 瓮福（集团）有限责任公司 | Preparation method of nutrient-controllable ammonium polyphosphate |
| CN115231971A (en) * | 2021-04-23 | 2022-10-25 | 嘉施利（荆州）化肥有限公司 | Preparation process of agricultural zinc-containing fully water-soluble monoammonium phosphate |
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| CN102863267A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Method for producing monoammonium phosphate and coproducing N-P binary compound fertilizer by using wet-process phosphoric acid |
| CN104446968A (en) * | 2014-11-27 | 2015-03-25 | 湖北三宁化工股份有限公司 | Water-soluble high-concentration organic-inorganic compound fertilizer for trickle and sprinkling irrigation and preparation method thereof |
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| CN102863267A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Method for producing monoammonium phosphate and coproducing N-P binary compound fertilizer by using wet-process phosphoric acid |
| CN104446968A (en) * | 2014-11-27 | 2015-03-25 | 湖北三宁化工股份有限公司 | Water-soluble high-concentration organic-inorganic compound fertilizer for trickle and sprinkling irrigation and preparation method thereof |
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