CN1067644A - The production method of nitrophosphate fertilizer - Google Patents
The production method of nitrophosphate fertilizer Download PDFInfo
- Publication number
- CN1067644A CN1067644A CN 91106447 CN91106447A CN1067644A CN 1067644 A CN1067644 A CN 1067644A CN 91106447 CN91106447 CN 91106447 CN 91106447 A CN91106447 A CN 91106447A CN 1067644 A CN1067644 A CN 1067644A
- Authority
- CN
- China
- Prior art keywords
- nitric acid
- nitrocalcite
- weight
- phosphate
- nitrophosphate fertilizer
- 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.)
- Pending
Links
- 239000003337 fertilizer Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 34
- 239000002367 phosphate rock Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 50
- 239000011575 calcium Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims description 13
- 239000001506 calcium phosphate Substances 0.000 claims description 13
- 229910000150 monocalcium phosphate Inorganic materials 0.000 claims description 13
- 235000019691 monocalcium phosphate Nutrition 0.000 claims description 13
- 239000012452 mother liquor Substances 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001640 fractional crystallisation Methods 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000005649 metathesis reaction Methods 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000007738 vacuum evaporation Methods 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims 5
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims 4
- 239000006012 monoammonium phosphate Substances 0.000 claims 4
- 239000000203 mixture Substances 0.000 claims 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 12
- 239000006227 byproduct Substances 0.000 description 7
- 239000004254 Ammonium phosphate Substances 0.000 description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 3
- 235000019289 ammonium phosphates Nutrition 0.000 description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 2
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical class [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
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- Fertilizers (AREA)
Abstract
The present invention is the production method of nitrophosphate fertilizer.
The present invention is that raw material, cold method are produced nitrophosphate fertilizer with Rock Phosphate (72Min BPL), nitric acid.
Description
Known is raw material with Rock Phosphate (72Min BPL), nitric acid, and cold method is produced the method for nitrophosphate fertilizer, has only with denseer nitric acid, lower freezing temp, could produce the product of higher water-soluble rate.
The objective of the invention is to rarer nitric acid, higher freezing temp, cold method is produced the nitrophosphate fertilizer product of full water-soluble.
The working of an invention method is as follows:
1, preparation circulate soln:
In the water of 1000 parts of weight under 25～55 ℃ temperature, add monocalcium phosphate, nitrocalcite, make respectively to be saturated, the nitric acid that adds a certain amount of 98% weight concentration in solution, the HNO that contains in the concentrated nitric acid
3Total moles and solution in the P that contains
2O
5The ratio of total moles be: 1: 0.4～0.6.Add certain density rare nitric acid A then.The HNO that contains in rare nitric acid
3The ratio of weight and water weight is same as and adds the HNO that contains in the solution behind the concentrated nitric acid
3The ratio of weight and water weight, rare nitric acid water content of adding is: 50～300 portions of weight/1000 portion weight preparation circulate soln waters.The solution that adds behind rare nitric acid is the circulate soln that will prepare.
2, produce the nitrocalcite byproduct with circulate soln
The circulate soln of producing 1 preparation is refrigerated to-5～25 ℃, separates out Ca(NO
3)
24H
2The O crystallization, freezing 2-8 hour Ca(NO to the solution
3)
2Separate out fully, fractional crystallization gets nitrocalcite byproduct B, separates mother solution C and is used for following production.
3, produce the nitrophosphate fertilizer intermediate with the nitric acid decomposing phosphate rock:
Be that 35～60% nitric acid decomposes a certain amount of Rock Phosphate (72Min BPL) with concentration under 40～55 ℃ temperature, make the P in the Rock Phosphate (72Min BPL)
2O
5Be converted into Ca(H fully
2PO
4)
2, HNO in the solution after decomposition is finished
3Weight content be 0.2%～3%.Keep the product of 20～60 ℃ of above-mentioned nitric acid decomposing phosphate rocks of vacuum-evaporation, free-water (crystal water non-chemically) content is 2～10%(weight to the product).This product after evaporation is finished contains Ca(H
2PO
4)
2H
2O and Ca(NO
3)
24H
2O is for being used to produce the intermediate D of nitrophosphate fertilizer.
4, use nitrophosphate fertilizer intermediate D and circulate soln C productions, biphosphate calcium product:
Add in the separation mother solution C after producing 2 production nitrocalcite and produce the 3 nitrophosphate fertilizer intermediate D that produce.Keep 25～55 ℃ temperature stirring and dissolving 1～4 hour, make the Ca(NO in the intermediate
3)
24H
2O is dissolved in the solution fully, Ca(H
2PO
4)
2H
2O stays solid phase.The Ca(NO that contains in the intermediate that adds
3)
2Weight equals to produce the Ca(NO that contains among the 2 isolating nitrocalcite B
3)
20.8～1.2 times of weight after solvency action finishes, under 25～55 ℃ of temperature, separates solid formation, Ca(H
2PO
4)
2H
2O product, this product are the calcareous nitrophosphate fertilizer product F that will produce.From separation of C a(H
2PO
4)
2H
2Draw 5～35% of total amount in the mother liquor behind the O and add the nitric acid that production 3 is used for decomposing phosphate rock, add in drawing the remaining separation mother liquor in back and produce the nitric acid of 1 preparation circulate soln with rare nitric acid A same concentrations, the nitric acid of adding contains separation mother liquor that water inventory equals to draw and contains 0.8～1.2 times of water inventory.This separation mother liquor that adds behind the nitric acid is the circulate soln that is used to produce nitric acid fertilizer of producing 1 preparation.
More than produce and finished a circulation, 2,3,4 the continuous cyclic production nitrocalcite of method byproduct B and monocalcium phosphate product F are just pressed in later production with circulate soln.
In order to make not calcareous compound nitrophosphate fertilizer, with following method monocalcium phosphate all is converted into the final nitrophosphate fertilizer product of ammonium phosphate, and by-product nitrocalcite:
In containing 20～55 ℃ the aqueous solution of saturated ammonium phosphate, ammonium chloride, add a certain amount of nitrocalcite and water, be refrigerated to 0～25 ℃, crystallization goes out Ca(NO
3)
24H
2O, fractional crystallization get the nitrocalcite byproduct, separate and to add ammonium nitrate after mother liquid evaporation falls portion water under 20～55 ℃ temperature, the monocalcium phosphate replacement(metathesis)reaction gets the ammonium phosphate crystallization, and fractional crystallization gets final nitrophosphate fertilizer product.Separate to be refrigerated to 0～25 ℃ of crystallization after mother liquor adds a certain amount of water, produce the nitrocalcite byproduct, the separation mother liquor of having produced behind the nitrocalcite is reused for and ammonium nitrate, monocalcium phosphate effect production ammonium phosphate and by-product nitrocalcite.
Claims (6)
1, the production method of nitrophosphate fertilizer, it is characterized in that: at first be mixed with and contain monocalcium phosphate nitrocalcite, the circulate soln of nitric acid and freeze cycle solution are produced nitrocalcite, separate behind the nitrocalcite the separation mother liquor with make the biphosphate calcium product with the nitrophosphate fertilizer intermediate solvency action that contains monocalcium phosphate nitrocalcite that makes with phosphorus ore in the nitric acid.Separation mother liquor behind the system monocalcium phosphate becomes circulate soln after adjusting composition with nitric acid, is reused for and produces freezing nitrocalcite and monocalcium phosphate.In order to make not calcareous nitrophosphate fertilizer, the biphosphate calcium product and the ammonium nitrate metathesis of producing made monoammonium phosphate.
2, according to the production method of the described nitrophosphate fertilizer of claim 1, it is characterized in that:
The circulate soln that is used to produce nitrophosphate fertilizer is made into following method:
In the water of 1000 parts of weight under 25 ℃ of-55 ℃ of temperature, add monocalcium phosphate, nitrocalcite makes and respectively is saturated.The nitric acid that adds a certain amount of 98% concentration, the HNO that contains in the concentrated nitric acid
3Mole number and solution in the P that contains
2O
5The ratio of mole number be: 1: 0.4-0.6.Add certain density rare nitric acid then, the HNO that contains in rare nitric acid
3The HNO that contains in the solution behind the ratio of weight and water weight and the adding concentrated nitric acid
3Weight is identical with the ratio of water weight.The rare nitric acid water content that adds is: 50-300 part weight/1000 portions of weight preparation circulate soln waters.
3, the production method according to the described nitrophosphate fertilizer of claim 1 is characterized in that:
Circulate soln with preparation is produced nitrocalcite:
The circulate soln that is made into is refrigerated to-5～25 ℃, and under this temperature, separates the nitrocalcite crystallization of separating out.
4, according to the production method of the described nitrophosphate fertilizer of claim 1, it is characterized in that:
Produce the nitrophosphate fertilizer intermediate with the nitric acid decomposing phosphate rock:
With concentration is that the nitric acid decomposing phosphate rock stone of 35-60% makes P wherein
2O
3Transfer Ca(H fully to
2PO
4)
2HNO in the solution after decomposition is finished
3Weight content be: 0.2-3% keeps the product of 20-60 ℃ of vacuum-evaporation nitric acid decomposing phosphate rock, to the weight content of free moisture content wherein be 2-10%.
5, according to the production method of the described nitrophosphate fertilizer of claim 1, it is characterized in that:
Produce monocalcium phosphate and adjust the circulate soln composition with nitrophosphate fertilizer intermediate and circulate soln:
Add the intermediate that the nitric acid decomposing phosphate rock gets in the separation mother liquor after producing nitrocalcite, keep 25-55 ℃ temperature, stirring and dissolving to the nitrocalcite in the intermediate all is dissolved in the solution.The Ca(NO that contains in the intermediate
3)
2Weight equals the Ca(NO that an operation is produced
3)
2The 0.3-1.2 of weight doubly.After dissolving finishes, under 25-55 ℃ temperature, separate solid formation.Separate mother liquor and draw decomposing phosphate rock in the 5-35% adding nitric acid.Add rare nitric acid that the preparation circulate soln is used in remaining separation mother liquor, the nitric acid of adding contains water inventory and equals to draw 0.8-1.2 times that mother liquor contains water inventory.
6, according to the described production method of claim 1, it is characterized in that:
With monocalcium phosphate, ammonium nitrate system monoammonium phosphate:
In the 20-55 that contains saturated monoammonium phosphate, ammonium chloride ℃ the aqueous solution, add nitrocalcite and water, be refrigerated to 0-25 ℃ of fractional crystallization and get nitrocalcite, separate and add monocalcium phosphate after mother liquid evaporation falls portion water under 20-55 ℃ temperature, the ammonium nitrate metathesis gets the monoammonium phosphate crystallization.Mother liquor behind the fractional crystallization adds water-cooled again and freezes and be used to produce nitrocalcite and monoammonium phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106447 CN1067644A (en) | 1991-06-07 | 1991-06-07 | The production method of nitrophosphate fertilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106447 CN1067644A (en) | 1991-06-07 | 1991-06-07 | The production method of nitrophosphate fertilizer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1067644A true CN1067644A (en) | 1993-01-06 |
Family
ID=4907864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91106447 Pending CN1067644A (en) | 1991-06-07 | 1991-06-07 | The production method of nitrophosphate fertilizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1067644A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328224C (en) * | 2000-03-10 | 2007-07-25 | 四川大学 | Process for preparing compound phosphorus nitrate fertilizer by spray, freeze, crystallization and decorbonizing and decalcifying hydrazidine |
| CN101486595B (en) * | 2009-02-25 | 2011-03-30 | 天脊煤化工集团股份有限公司 | A process for producing high-concentration nitrophosphate fertilizer |
| CN109399688A (en) * | 2018-10-17 | 2019-03-01 | 贵州芭田生态工程有限公司 | The method of phosphate fertilizer mother liquor low temperature decalcification and decalcification filtrate and phosphate fertilizer preparation method |
-
1991
- 1991-06-07 CN CN 91106447 patent/CN1067644A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328224C (en) * | 2000-03-10 | 2007-07-25 | 四川大学 | Process for preparing compound phosphorus nitrate fertilizer by spray, freeze, crystallization and decorbonizing and decalcifying hydrazidine |
| CN101486595B (en) * | 2009-02-25 | 2011-03-30 | 天脊煤化工集团股份有限公司 | A process for producing high-concentration nitrophosphate fertilizer |
| CN109399688A (en) * | 2018-10-17 | 2019-03-01 | 贵州芭田生态工程有限公司 | The method of phosphate fertilizer mother liquor low temperature decalcification and decalcification filtrate and phosphate fertilizer preparation method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |