CN103011112A - Production method of diammonium phosphate product - Google Patents

Production method of diammonium phosphate product Download PDF

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Publication number
CN103011112A
CN103011112A CN2012105324440A CN201210532444A CN103011112A CN 103011112 A CN103011112 A CN 103011112A CN 2012105324440 A CN2012105324440 A CN 2012105324440A CN 201210532444 A CN201210532444 A CN 201210532444A CN 103011112 A CN103011112 A CN 103011112A
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Prior art keywords
phosphoric acid
diammonium phosphate
ammonia
liquefied ammonia
tubular reactor
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CN2012105324440A
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Chinese (zh)
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杜秀荣
覃庆海
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Wengfu Group Co Ltd
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Wengfu Group Co Ltd
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Priority to CN2012105324440A priority Critical patent/CN103011112A/en
Publication of CN103011112A publication Critical patent/CN103011112A/en
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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a production method of a diammonium phosphate product. Two pipe type reactors are adopted, so that strong phosphoric acid and liquid ammonia are sharply reacted in pipe type reactors and granulated by using reaction pressure to spray slurry in a granulating machine. The process method for producing the diammonium phosphate product has the advantages of short reaction time, stable system material reverting and less system scaling; the produced diammonium phosphate product is high in product water soluble phosphorus, uniform in particle size, and good in particle roundness; and compared with a traditional process method, the novel process method is increased by 10-15% in yield load.

Description

A kind of production method of diammonium phosphate product
Technical field
The present invention relates to fertilizer, specifically a kind of phosphoric acid by wet process and liquefied ammonia are produced the method for diammonium phosphate product.
Background technology
Traditional Method diammonium phosphate product production method adopts " pre-neutralization+pipe is anti-" technique, adopts this production method to have the shortcomings such as long reaction time, the water-soluble phosphorus of product descend, the product roundness degree is poor.
The contriver adopts the production technique of " two-tube anti-" that be different from Traditional Method, i.e. two methods that diammonium phosphate product is produced in the tubular reactor granulation.
In Chinese patent database, there is no at present diammonium phosphate product production and adopt " two-tube anti-" technique.The contriver provides two tubular reactor granulations to produce the method for diammonium phosphate product through exploring and test.
Summary of the invention
The characteristics such as the object of the invention is to provides a kind of method of producing diammonium phosphate product for the deficiencies in the prior art, and it is short that the method has the reaction times of production, and the water-soluble phosphorus of product is high, and the product roundness degree is good.
The present invention is achieved by the following technical solutions: a kind of method of producing diammonium phosphate product,
The method operates according to the following steps: the strong phosphoric acid of (1) phosphoric acid storage tank is transported to the complex acid groove by transferpump, mixes with washings from washing system, and density is controlled at 1.52~1.56g/cm 3, degree of neutralization is that the N/P mol ratio is 0.4;
(2) carry by the anti-feeding pump of pipe, enter the tubular reactor mixing head by strainer, under meter, switch-valve, vacuum breaker successively and fully mix with the liquefied ammonia that the ammonia tank field transports, the liquefied ammonia pressure of conveying is 1.2MPa;
(3) allow strong phosphoric acid and liquefied ammonia that vigorous reaction occurs in tubular reactor, pressure-controlling is at 3~6kgf/cm 2, temperature is controlled at 130~150 ℃, and degree of neutralization is controlled at 1.55~1.65;
(4) slip is by two mouth sprays coating drum granulating of whitewashing, the tablets press material moisture is controlled at 3%, in tablets press, carry out secondary by the ammonia sparger and mend ammonia, degree of neutralization is controlled at 1.88~1.98, system returns the quality of material of tablets press and the ratio of the product quality of material of taking-up (being called for short the returning charge ratio), be 5~5.5:1, material after the granulation enters drying machine and carries out drying, again through screening, fragmentation, the 2-4mm particle enters finished product packing through cooling bed, and rest materials is returned the tablets press secondary granulation;
(5) moisture and effusion ammonia, dust and the air amount that evaporate in tubular reactor and the tablets press are sent into washing system together, add strong phosphoric acid to washing system and carry out circulation cleaning recovery ammonia and dust, and the part washings is sent into the utilization of complex acid groove.
Strong phosphoric acid described in the aforesaid method is P 2O 5Mass percent is the phosphoric acid of 45-47%.
The liquefied ammonia that is transported to tubular reactor described in the aforesaid method adopts the liquefied ammonia force (forcing) pump to finish the about 500m of fed distance.
By the control of variable valve adjust flux realization to complex acid tank liquor position and density in the aforesaid method.
Strong phosphoric acid and liquefied ammonia are to regulate to realize by the automatic regulating valve execution ratio of phosphoric acid and liquefied ammonia in the degree of neutralization control of tubular reactor reaction in the aforesaid method.
In the aforesaid method, the raw material strong phosphoric acid quality index of described production diammonium phosphate product is:
P 2O 5Mass percent 45-47% density 1.62~1.66g/cm 3
The index of another kind of raw materials ammonia is: NH 3〉=99%.
The diammonium phosphate product that aforesaid method is produced, quality index is: total nutrient 〉=64% H 2O≤2.5%, water-soluble phosphorus/available phosphorus 〉=93% 2-4mm 〉=92%, ultimate compression strength 〉=40N, SGN 〉=300.
Method provided by the invention has following advantage:
The advantages such as it is short (1) to adopt this patent " two-tube anti-" technique to have the products production reaction times, and it is few that system's returning charge is steady, system scabs.
(2) adopt the diammonium phosphate product of this patent production to have the characteristics such as the water-soluble phosphorus height of product, epigranular, roundness of granules are good.
(3) adopt this patent producing and manufacturing technique output duty ratio to adopt the Traditional Method processing method to improve 10-15%.
(4) adopt this patent production temperature of reaction high, many at the tablets press transpiring moisture, the thermal load that drying process needs reduces, even can cancel drying source, belongs to the environmental protection and energy saving project.
(5) simple to operate, reduce labour intensity.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Among the figure: 1-complex acid groove; 2-pipe reaction feeding pump; The 3-strainer; The 4-under meter; The 5-switch-valve; The 6-vacuum breaker; 7-tubular reactor mixing head; The 8-liquid ammonia ball tank; The 9-tubular reactor; The 10-tablets press; The 11-force (forcing) pump; The 12-variable valve; The 13-pressure unit; The 14-stopcock; The 15-ball valve; The 16-thermometer.
Embodiment
Embodiment 1
Certain factory adopts method of the present invention to produce, change the 1200kt/a diammonium phosphate device into " two-tube anti-" technique by " pre-neutralization+pipe anti-" technique of Traditional Method, pre-neutralization reactor in original technique and spray pump, shotcrete pipe have been cancelled, as shown in the figure, increase tubular reactor complex acid groove 1, pipe reaction feeding pump 2 and tubular reactor 9.
The strong phosphoric acid of phosphoric acid storage tank is transported to complex acid groove 1 by transferpump, mixes with washings from washing system, density is controlled at 1.54g/cm 3Degree of neutralization (N/P mol ratio) is 0.4, carry by pipe reaction feeding pump 2, entering tubular reactor mixing head 7 by strainer 3, under meter 4, switch-valve 5, vacuum breaker 6 successively fully mixes with the liquefied ammonia that the ammonia tank field transports, the liquefied ammonia pressure that transports is 1.2MPa, allow strong phosphoric acid and liquefied ammonia in tubular reactor 9 vigorous reaction occur, pressure-controlling is at 4kgf/cm 2, temperature is controlled at 140 ℃, and degree of neutralization is controlled at 1.58.Slip is by two mouth sprays coating drum granulating of whitewashing, and tablets press 10 material moistures are controlled at 3%, carries out secondary by the ammonia sparger and mend ammonia in tablets press 10, and degree of neutralization is controlled at 1.95, and the returning charge ratio is 5~5.5:1.Moisture and effusion ammonia, dust and the air amount of evaporation are sent into washing system together in tubular reactor 9 and the tablets press 10, add strong phosphoric acid to washing system and carry out circulation cleaning recovery ammonia and dust.The part washings is sent into complex acid groove 1, by the control of variable valve 12 adjust fluxes realization to complex acid tank liquor position and density.Material after the granulation enters drying machine and carries out drying, again through screening, fragmentation.The 2-4mm particle enters finished product packing through cooling bed, and rest materials is returned tablets press 10 and carried out secondary granulation.
The liquefied ammonia that is transported to tubular reactor described in the aforesaid method adopts the liquefied ammonia force (forcing) pump to finish the about 500m of fed distance.
By the control of variable valve adjust flux realization to complex acid tank liquor position and density in the aforesaid method.
Strong phosphoric acid and liquefied ammonia are to regulate to realize by the automatic regulating valve execution ratio of phosphoric acid and liquefied ammonia in the degree of neutralization control of tubular reactor reaction in the aforesaid method.
In the aforesaid method, the raw material strong phosphoric acid quality index of described production diammonium phosphate product is:
P 2O 5Mass percent 46% density 1.65g/cm 3
The index of another kind of raw materials ammonia is: NH 3〉=99%.
The diammonium phosphate product that aforesaid method is produced, quality index is: total nutrient 〉=64% H 2O≤2.5%, water-soluble phosphorus/available phosphorus 〉=93% 2-4mm 〉=92%, ultimate compression strength 〉=40N, SGN 〉=300.
Embodiment 2
The strong phosphoric acid of phosphoric acid storage tank is transported to complex acid groove 1 by transferpump, mixes with washings from washing system, density is controlled at 1.56g/cm 3Degree of neutralization (N/P mol ratio) is 0.4, carry by pipe reaction feeding pump 2, entering tubular reactor mixing head 7 by strainer 3, under meter 4, switch-valve 5, vacuum breaker 6 successively fully mixes with the liquefied ammonia that the ammonia tank field transports, the liquefied ammonia pressure that transports is 1.2MPa, allow strong phosphoric acid and liquefied ammonia in tubular reactor 9 vigorous reaction occur, pressure-controlling is at 6kgf/cm 2, temperature is controlled at 150 ℃, and degree of neutralization is controlled at 1.65.Slip is by two mouth sprays coating drum granulating of whitewashing, and tablets press 10 material moistures are controlled at 3%, carries out secondary by the ammonia sparger and mend ammonia in tablets press 10, and degree of neutralization is controlled at 1.98, and the returning charge ratio is 5~5.5:1.Moisture and effusion ammonia, dust and the air amount of evaporation are sent into washing system together in tubular reactor 9 and the tablets press 10, add strong phosphoric acid to washing system and carry out circulation cleaning recovery ammonia and dust.The part washings is sent into complex acid groove 1, by the control of variable valve 12 adjust fluxes realization to complex acid tank liquor position and density.Material after the granulation enters drying machine and carries out drying, again through screening, fragmentation.The 2-4mm particle enters finished product packing through cooling bed, and rest materials is returned tablets press 10 and carried out secondary granulation.
The liquefied ammonia that is transported to tubular reactor described in the aforesaid method adopts the liquefied ammonia force (forcing) pump to finish the about 500m of fed distance.
By the control of variable valve adjust flux realization to complex acid tank liquor position and density in the aforesaid method.
Strong phosphoric acid and liquefied ammonia are to regulate to realize by the automatic regulating valve execution ratio of phosphoric acid and liquefied ammonia in the degree of neutralization control of tubular reactor reaction in the aforesaid method.
In the aforesaid method, the raw material strong phosphoric acid quality index of described production diammonium phosphate product is:
P 2O 5Mass percent 47% density 1.66g/cm 3
The index of another kind of raw materials ammonia is: NH 3〉=99%.
The diammonium phosphate product that aforesaid method is produced, quality index is: total nutrient 〉=64% H 2O≤2.5%, water-soluble phosphorus/available phosphorus 〉=93% 2-4mm 〉=92%, ultimate compression strength 〉=40N, SGN 〉=300.
Embodiment 3
The strong phosphoric acid of phosphoric acid storage tank is transported to complex acid groove 1 by transferpump, mixes with washings from washing system, density is controlled at 1.52g/cm 3Degree of neutralization (N/P mol ratio) is 0.4, carry by pipe reaction feeding pump 2, entering tubular reactor mixing head 7 by strainer 3, under meter 4, switch-valve 5, vacuum breaker 6 successively fully mixes with the liquefied ammonia that the ammonia tank field transports, the liquefied ammonia pressure that transports is 1.2MPa, allow strong phosphoric acid and liquefied ammonia in tubular reactor 9 vigorous reaction occur, pressure-controlling is at 3kgf/cm 2, temperature is controlled at 130 ℃, and degree of neutralization is controlled at 1.55.Slip is by two mouth sprays coating drum granulating of whitewashing, and tablets press 10 material moistures are controlled at 3%, carries out secondary by the ammonia sparger and mend ammonia in tablets press 10, and degree of neutralization is controlled at 1.88, and the returning charge ratio is 5~5.5:1.Moisture and effusion ammonia, dust and the air amount of evaporation are sent into washing system together in tubular reactor 9 and the tablets press 10, add strong phosphoric acid to washing system and carry out circulation cleaning recovery ammonia and dust.The part washings is sent into complex acid groove 1, by the control of variable valve 12 adjust fluxes realization to complex acid tank liquor position and density.Material after the granulation enters drying machine and carries out drying, again through screening, fragmentation.The 2-4mm particle enters finished product packing through cooling bed, and rest materials is returned tablets press 10 and carried out secondary granulation.
The liquefied ammonia that is transported to tubular reactor described in the aforesaid method adopts the liquefied ammonia force (forcing) pump to finish the about 500m of fed distance.
By the control of variable valve adjust flux realization to complex acid tank liquor position and density in the aforesaid method.
Strong phosphoric acid and liquefied ammonia are to regulate to realize by the automatic regulating valve execution ratio of phosphoric acid and liquefied ammonia in the degree of neutralization control of tubular reactor reaction in the aforesaid method.
In the aforesaid method, the raw material strong phosphoric acid quality index of described production diammonium phosphate product is:
P 2O 5Mass percent 45% density 1.62g/cm 3
The index of another kind of raw materials ammonia is: NH 3〉=99%.
The diammonium phosphate product that aforesaid method is produced, quality index is: total nutrient 〉=64% H 2O≤2.5%, water-soluble phosphorus/available phosphorus 〉=93% 2-4mm 〉=92%, ultimate compression strength 〉=40N, SGN 〉=300.
 
This factory uses the inventive method, and the product that obtains obviously improves on Yield and quality.
Adopt Traditional Method process yields, quality table:
Date manufactured Order of classes or grades at school Color Quantity t Total nutrient % Total nitrogen % Available phosphorus % P water/P has % Moisture % 2-4% 2.5- 3.5% The pH value SGN Grade
2012-9-18 Night Yellow 1726 64.8 17.5 47.3 90 1.9 93 52 8.06 263 Premium grads
2012-9-18 In vain Yellow 1883 64.4 17.6 46.8 91 2.4 95 53 8.15 276 Premium grads
2012-9-19 Night Yellow 1768 64.8 17.4 47.4 91 2.3 91 55 8.02 268 Premium grads
2012-9-19 In vain Yellow 1589 64.9 17.5 47.4 91 2.3 94 55 8.02 274 Premium grads
2012-9-20 Night Yellow 1802 64.5 17.4 47.1 91 2.1 92 56 8.02 263 Premium grads
2012-9-20 In vain Yellow 1763 64.8 17.4 47.4 91 2.1 90 50 7.91 255 Premium grads
Adopt " two-tube anti-" rear process yields, quality table:
Date manufactured Order of classes or grades at school Color Quantity t Total nutrient % Total nitrogen % Available phosphorus % P water/P has % Moisture % 2-4% 2.5- 3.5% The pH value SGN Grade
2012-11-13 Night Yellow 1864 64.8 17.8 47.0 95 1.9 98 82 8.06 308 Premium grads
2012-11-13 In vain Yellow 1956 64.4 17.6 46.8 96 1.2 96 78 8.13 303 Premium grads
2012-11-14 Night Yellow 1962 64.3 17.7 46.6 95 1.8 97 78 8.26 307 Premium grads
2012-11-14 In vain Yellow 2089 64.1 17.6 46.5 96 1.6 98 79 8.21 313 Premium grads
2012-11-15 Night Yellow 1946 64.6 17.7 46.9 97 1.1 98 71 8.1 295 Premium grads
2012-11-15 In vain Yellow 2056 64.3 17.6 46.7 96 1.2 97 76 8.17 310 Premium grads

Claims (7)

1. the production technique of a diammonium phosphate is characterized in that its operation is as follows:
(1) strong phosphoric acid with phosphoric acid storage tank is transported to complex acid groove (1) by transferpump, mixes with washings from washing system, and density is controlled at 1.52~1.56g/cm 3, degree of neutralization is that the N/P mol ratio is 0.4;
(2) by the strong phosphoric acid in pipe reaction feeding pump (2) the conveying complex acid groove (1), enter tubular reactor mixing head (7) by strainer (3), under meter (4), switch-valve (5), vacuum breaker (6) successively and fully mix with the liquefied ammonia that the ammonia tank field transports, the liquefied ammonia pressure of conveying is 1.2MPa;
(3) allow strong phosphoric acid and liquefied ammonia that vigorous reaction occurs in tubular reactor (9), pressure-controlling is at 3~6kgf/cm 2, temperature is controlled at 130~150 ℃, and degree of neutralization is controlled at 1.55~1.65;
(4) after the reaction slip by two mouth sprays coating drum granulating of whitewashing, the mass percent of the material moisture in the tablets press (10) is controlled at 3%, in tablets press (10), carry out secondary by the ammonia sparger and mend ammonia, degree of neutralization is controlled at 1.88~1.98, the quality of material that system returns tablets press is 5~5.5:1 with the ratio of the product quality of material of taking-up, material after the granulation enters drying machine and carries out drying, again through screening, fragmentation, the 2-4mm particle enters finished product packing through cooling bed, and rest materials is returned tablets press (10) secondary granulation;
(5) moisture and effusion ammonia, dust and the air amount of evaporation are sent into washing system together in tubular reactor (9) and the tablets press (10); add strong phosphoric acid to washing system and carry out circulation cleaning recovery ammonia and dust, the part washings is sent in the complex acid groove (1) utilized.
2. the production technique of diammonium phosphate according to claim 1 is characterized in that strong phosphoric acid is P 2O 5Mass percent is the phosphoric acid of 45-47%.
3. the production technique of diammonium phosphate according to claim 1 is characterized in that the liquefied ammonia that is transported to tubular reactor (9) adopts liquefied ammonia force (forcing) pump (11) to finish fed distance 500m.
4. the production technique of diammonium phosphate according to claim 1 is characterized in that by the control of variable valve (12) adjust flux realization to complex acid groove (1) liquid level and density.
5. the production technique of diammonium phosphate according to claim 1 is characterized in that the degree of neutralization control that described strong phosphoric acid and liquefied ammonia react is to regulate to realize by variable valve (12) the execution ratio of phosphoric acid and liquefied ammonia in tubular reactor (9).
6. the production technique of diammonium phosphate according to claim 1 is characterized in that the raw material strong phosphoric acid quality index of described production diammonium phosphate product is: P 2O 5Mass percent 45-47%, density 1.52~1.56g/cm 3, the index of raw materials ammonia is: NH 3〉=99%.
7. the production technique of diammonium phosphate according to claim 1 is characterized in that the diammonium phosphate product quality index of aforesaid method production is: total nutrient 〉=64% H 2O≤2.5%, water-soluble phosphorus/available phosphorus 〉=93% 2-4mm 〉=92%, ultimate compression strength 〉=40N, SGN 〉=300.
CN2012105324440A 2012-12-12 2012-12-12 Production method of diammonium phosphate product Pending CN103011112A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103274852A (en) * 2013-06-17 2013-09-04 中国农业科学院农业资源与农业区划研究所 Algae synergistic ammonium phosphate fertilizer and preparation method thereof
CN103303887A (en) * 2013-05-28 2013-09-18 瓮福(集团)有限责任公司 Method for producing high-nutrient monoammonium phosphate by dual-tube reverse process
CN104860283A (en) * 2015-04-17 2015-08-26 湖北六国化工股份有限公司 Granulator comprising double tubular reactors and application thereof in diammonium phosphate production
CN105236374A (en) * 2015-09-16 2016-01-13 贵州开磷集团股份有限公司 Preparation method for granular diammonium phosphate
CN106008115A (en) * 2016-08-08 2016-10-12 山西广宇通科技股份有限公司 Preparation method of humic acid-containing diammonium phosphate
CN106831053A (en) * 2017-02-10 2017-06-13 云南三环中化化肥有限公司 A kind of production method of graininess, function intensified type phosphorus containing magnesium ammonium
CN108046934A (en) * 2018-01-22 2018-05-18 北京三聚绿能科技有限公司 A kind of charcoal base Diammonium phosphate (DAP) and its preparation process
CN108484246A (en) * 2018-05-29 2018-09-04 云南祥丰金麦化工有限公司 A kind of prilling process producing chemical fertilizer
CN112457090A (en) * 2020-11-06 2021-03-09 云南磷化集团海口磷业有限公司 Contain sulphur phosphorus fertilizer apparatus for producing and contain sulphur ammonium phosphate apparatus for producing

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1076680A (en) * 1992-07-17 1993-09-29 莱西市磷肥厂 Enriching slurry process for production of diammonium phosphate
CN101549861A (en) * 2009-04-24 2009-10-07 瓮福(集团)有限责任公司 A diammonium phosphate exhaust washing method
CN101723340B (en) * 2009-12-29 2011-07-27 中国海洋石油总公司 Preparation method of diammonium phosphate
CN102689883A (en) * 2012-06-19 2012-09-26 瓮福(集团)有限责任公司 Method for producing diammonium phosphate from recycled phosphorus-containing filter residues

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1076680A (en) * 1992-07-17 1993-09-29 莱西市磷肥厂 Enriching slurry process for production of diammonium phosphate
CN101549861A (en) * 2009-04-24 2009-10-07 瓮福(集团)有限责任公司 A diammonium phosphate exhaust washing method
CN101723340B (en) * 2009-12-29 2011-07-27 中国海洋石油总公司 Preparation method of diammonium phosphate
CN102689883A (en) * 2012-06-19 2012-09-26 瓮福(集团)有限责任公司 Method for producing diammonium phosphate from recycled phosphorus-containing filter residues

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103303887A (en) * 2013-05-28 2013-09-18 瓮福(集团)有限责任公司 Method for producing high-nutrient monoammonium phosphate by dual-tube reverse process
CN103274852A (en) * 2013-06-17 2013-09-04 中国农业科学院农业资源与农业区划研究所 Algae synergistic ammonium phosphate fertilizer and preparation method thereof
CN104860283A (en) * 2015-04-17 2015-08-26 湖北六国化工股份有限公司 Granulator comprising double tubular reactors and application thereof in diammonium phosphate production
CN105236374A (en) * 2015-09-16 2016-01-13 贵州开磷集团股份有限公司 Preparation method for granular diammonium phosphate
CN105236374B (en) * 2015-09-16 2018-03-13 贵州开磷集团股份有限公司 A kind of preparation method of granular diammonium phosphate
CN106008115A (en) * 2016-08-08 2016-10-12 山西广宇通科技股份有限公司 Preparation method of humic acid-containing diammonium phosphate
CN106831053A (en) * 2017-02-10 2017-06-13 云南三环中化化肥有限公司 A kind of production method of graininess, function intensified type phosphorus containing magnesium ammonium
CN108046934A (en) * 2018-01-22 2018-05-18 北京三聚绿能科技有限公司 A kind of charcoal base Diammonium phosphate (DAP) and its preparation process
CN108484246A (en) * 2018-05-29 2018-09-04 云南祥丰金麦化工有限公司 A kind of prilling process producing chemical fertilizer
CN112457090A (en) * 2020-11-06 2021-03-09 云南磷化集团海口磷业有限公司 Contain sulphur phosphorus fertilizer apparatus for producing and contain sulphur ammonium phosphate apparatus for producing

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Application publication date: 20130403