CN104725098A - Method for producing all-water-soluble calcium ammonium magnesium nitrate by steel strip granulation - Google Patents
Method for producing all-water-soluble calcium ammonium magnesium nitrate by steel strip granulation Download PDFInfo
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- CN104725098A CN104725098A CN201510123149.3A CN201510123149A CN104725098A CN 104725098 A CN104725098 A CN 104725098A CN 201510123149 A CN201510123149 A CN 201510123149A CN 104725098 A CN104725098 A CN 104725098A
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- Prior art keywords
- calcium
- nitrate
- magnesium
- concentrated solution
- ammonium nitrate
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 36
- 239000010959 steel Substances 0.000 title claims abstract description 36
- RBIDTZUOKZFXOO-UHFFFAOYSA-O [N+](=O)([O-])[O-].[NH4+].[Mg].[Ca] Chemical compound [N+](=O)([O-])[O-].[NH4+].[Mg].[Ca] RBIDTZUOKZFXOO-UHFFFAOYSA-O 0.000 title claims abstract description 18
- 238000005469 granulation Methods 0.000 title claims abstract description 15
- 230000003179 granulation Effects 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 87
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 81
- NGLMYMJASOJOJY-UHFFFAOYSA-O azanium;calcium;nitrate Chemical compound [NH4+].[Ca].[O-][N+]([O-])=O NGLMYMJASOJOJY-UHFFFAOYSA-O 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 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 abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims description 37
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 36
- 239000000706 filtrate Substances 0.000 claims description 36
- 229910017604 nitric acid Inorganic materials 0.000 claims description 36
- 239000011573 trace mineral Substances 0.000 claims description 34
- 235000013619 trace mineral Nutrition 0.000 claims description 34
- 239000000292 calcium oxide Substances 0.000 claims description 31
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 31
- 239000000395 magnesium oxide Substances 0.000 claims description 31
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 31
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 30
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 30
- 239000012141 concentrate Substances 0.000 claims description 28
- 238000001704 evaporation Methods 0.000 claims description 27
- 230000008020 evaporation Effects 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 27
- 239000006200 vaporizer Substances 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 19
- 238000006386 neutralization reaction Methods 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- 238000009834 vaporization Methods 0.000 claims description 18
- 230000008016 vaporization Effects 0.000 claims description 18
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 17
- 229910052749 magnesium Inorganic materials 0.000 claims description 17
- 239000011777 magnesium Substances 0.000 claims description 17
- 230000001105 regulatory effect Effects 0.000 claims description 17
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- JVXHQHGWBAHSSF-UHFFFAOYSA-L 2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate;hydron;iron(2+) Chemical compound [H+].[H+].[Fe+2].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O JVXHQHGWBAHSSF-UHFFFAOYSA-L 0.000 claims description 9
- 244000025254 Cannabis sativa Species 0.000 claims description 9
- -1 EDTA-manganese Chemical compound 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 9
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 9
- 239000011609 ammonium molybdate Substances 0.000 claims description 9
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 9
- 229940010552 ammonium molybdate Drugs 0.000 claims description 9
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- YTSDVWYUJXKXCC-UHFFFAOYSA-L zinc;2-[2-[carboxylatomethyl(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound [Zn+2].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O YTSDVWYUJXKXCC-UHFFFAOYSA-L 0.000 claims description 9
- 239000003337 fertilizer Substances 0.000 abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052791 calcium Inorganic materials 0.000 abstract description 9
- 239000011575 calcium Substances 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 235000015097 nutrients Nutrition 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- RPASNPADOARUAP-UHFFFAOYSA-N calcium magnesium tetranitrate Chemical compound [Mg++].[Ca++].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O RPASNPADOARUAP-UHFFFAOYSA-N 0.000 abstract 2
- 230000007774 longterm Effects 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 102000004190 Enzymes Human genes 0.000 description 5
- 108090000790 Enzymes Proteins 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- AOFSUBOXJFKGAZ-UHFFFAOYSA-O azanium nitric acid nitrate Chemical compound [NH4+].O[N+]([O-])=O.[O-][N+]([O-])=O AOFSUBOXJFKGAZ-UHFFFAOYSA-O 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 1
- DIOLOCSXUMYFJN-UHFFFAOYSA-N calcium;azane Chemical compound N.[Ca+2] DIOLOCSXUMYFJN-UHFFFAOYSA-N 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C1/00—Ammonium nitrate fertilisers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to a chemical fertilizer production technique, particularly a method for producing all-water-soluble calcium ammonium magnesium nitrate by steel strip granulation. The method solves the technical problems that the existing single magnesium nitrate or calcium nitrate is not convenient for long-term storage and the existing calcium magnesium nitrate fertilizer is simple physical mixing. By adjusting the production technique, the method thoroughly solves the problems of high caking tendency, nonuniform content, unstable quality and the like in the product. The method detects the optimum proportion for synthesizing calcium magnesium nitrate from calcium nitrate, magnesium nitrate and ammonium nitrate. According to the method, calcium ammonium nitrate is firstly synthesized from the calcium nitrate and ammonium nitrate in a specific proportion, and the addition amount of the magnesium nitrate is further determined on such basis; and the calcium ammonium magnesium nitrate fertilizer obtained by the method has the advantages of no caking phenomenon, uniform content, stable quality, multiple nutrient varieties, higher calcium absorptivity and the like. The calcium ammonium magnesium nitrate produced by the method is hemispherical flakes. The product can form a clear transparent solution after being dissolved in water. The method solves the problems of high caking tendency, nonuniform content, unstable quality and the like in the product.
Description
Technical field
The present invention relates to chemical fertilizer production process, be specially a kind of method that full water-soluble calcium ammonium nitrate magnesium is produced in steel band granulation.
Background technology
Because single magnesium nitrate or nitrocalcite crystal (or particle) surface exist a large amount of dissociating water molecules, this just causes product in packed and transported, easily occur the plate that lumps, be unfavorable for long-distance transport and lengthy warehousing, direct impact sell and cause peasant household use inconvenience, and market existing nitrocalcite fertiliser containing magnesium is simple physical mixed, causes content detection wild effect to happen occasionally.Correlative study simultaneously shows, single calcium Crop utilization ratio is very low, this is because the absorption of calcium needs the participation of multiple enzyme, and enzyme can not get activating the absorption that just can not promote calcium, but magnesium can play the effect of activating enzymes, therefore the absorption of magnesium to calcium plays a part, and art is good for strength.Existing ca and mg fertilizer is simple physical mixed due to what adopt, causes the activation of magnesium to enzyme not obvious.Therefore if produce a kind of surface without free-water can promote the chemical fertilizer products of enzyme activation effect, greatly will improve the absorption to calcium of crop and be convenient to transport for long-distance.
Summary of the invention
The present invention is that solution magnesium nitrate single at present or nitrocalcite are unfavorable for lengthy warehousing, and existing nitrocalcite fertiliser containing magnesium is the technical problem of simple physical mixed, provides a kind of steel band granulation to produce the method for full water-soluble calcium ammonium nitrate magnesium.
The present invention realizes by the following technical solutions: the method for full water-soluble calcium ammonium nitrate magnesium is produced in a kind of steel band granulation, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 70 ~ 80 DEG C of stirring reaction 1.5 ~ 2h, reaction solution pH to 6.5 ~ 7.5 are regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380 ~ 1.510g/cm
3;
(2), quantitatively ammonium nitrate solid is added to the ca nitrate soln after concentrated, ammonium nitrate solid content is calculated by quality ratio and is accounted for 3 ~ 8.5% of nitrocalcite quality (namely previous step reacts the quality of generated nitrocalcite in theory), carry out double evaporation-cooling after stirring to concentrate, concentrate to proportion is 1.440 ~ 1.640g/cm
3, vaporization temperature is 150 ~ 180 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 70 ~ 80 DEG C of stirring reaction 1.5 ~ 2h, reaction solution pH to 6.5 ~ 7.5 are regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380 ~ 1.430g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:2.8 ~ 3.5, evaporation concentration, and concentrate to proportion is 1.150 ~ 1.540g/cm
3, vaporization temperature is 150 ~ 180 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product through steel band tablets press.
1, the present invention is by adjusting production technique, thoroughly solves the problems such as product easily lumps (surface does not exist dissociating water molecule), content is uneven, quality is unstable.
2, present invention process emphasis is the optimum proportion having searched out nitrocalcite, magnesium nitrate and ammonium nitrate nitric acid synthesis calcium magnesium, first by nitrocalcite and ammonium nitrate nitric acid synthesis ammonium calcium in specific proportions, determine the addition of magnesium nitrate on this basis further, the calcium ammonium nitrate fertiliser containing magnesium obtained like this solves product not caking phenomenon, content is even, steady quality, and nutrient wide variety, calcium absorptivity improves.
3, the calcium ammonium nitrate magnesium that the present invention produces is semisphere sheet (diameter 1 ~ 50mm), and product is water-soluble is limpid clear solution, solves the easy agglomeration problems of product, the problems such as content is uneven, quality is unstable, the problems such as calcium absorptivity is low.
4, in the method for the invention, the control of the reaction conditions (temperature, time) of calcium oxide and dust technology, magnesium oxide and dust technology, reacted pH value and concentrated after gravity all can produce wholesome effect to follow-up technique, and can promote that the finished product have the limpid transparent and characteristic of prevented from caking.
Magnesium nitrate, nitrocalcite and a small amount of ammonium nitrate are synthesized by chemical process according to special formulation by the present invention in specific proportions, also with the addition of the trace elements such as boron, iron, copper, manganese, zinc, molybdenum especially, obtain a kind of semisphere sheet calcium ammonium nitrate magnesium medium trace element fertile, not only solve product easily to lump nutrient Single-issue, and the magnesium of specified proportion well can promote the absorption of calcium in product, than use single calcareous fertilisers or fertiliser containing magnesium effect more obvious.
Accompanying drawing explanation
Fig. 1 equipment therefor structural representation of the present invention.
1-first dilute acid bath, 2-calcium oxide groove, 3-first reactor; 4-first plate and frame(type)filter press, 5-nitrocalcite vaporizer, 6-first steam boiler; 7-ammonium nitrate liquid bath, 8-second dilute acid bath, 9-magnesium oxide groove; 10-second reactor; 11-second plate and frame(type)filter press, 12-magnesium nitrate vaporizer, 13-second steam boiler; 14-cooling reactor, 15-steel band tablets press.
Embodiment
The method of full water-soluble calcium ammonium nitrate magnesium is produced in a kind of steel band granulation, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration adds reactor and carries out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 70 ~ 80 DEG C (70 DEG C, 72 DEG C, 74 DEG C, 76 DEG C, 78 DEG C, 80 DEG C) stirring reaction 1.5 ~ 2h(1.5 h, 1.6 h, 1.7 h, 1.8 h, 1.9 h, 2.0 h), reaction solution pH to 6.5 ~ 7.5(6.5 is regulated afterwards with calcium oxide, 6.7, 6.9, 7.1, 7.3, 7.5), the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380 ~ 1.510g/cm
3(1.380 g/cm
3, 1.410 g/cm
3, 1.440 g/cm
3, 1.480 g/cm
3, 1.510 g/cm
3),
(2), quantitatively ammonium nitrate solid is added to the ca nitrate soln after concentrated, ammonium nitrate solid content calculates the 3 ~ 8.5%(3%, 4%, 5%, 6%, 7%, 8.5% accounting for nitrocalcite quality by quality ratio), carry out double evaporation-cooling after stirring to concentrate, concentrate to proportion is 1.440 ~ 1.640g/cm
3(1.440 g/cm
3, 1.480 g/cm
3, 1.520 g/cm
3, 1.560 g/cm
3, 1.600g/cm
3, 1.640g/cm
3), vaporization temperature is 150 ~ 180 DEG C (150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C), generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3), the dilute nitric acid solution being 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 70 ~ 80 DEG C (70 DEG C, 72 DEG C, 74 DEG C, 76 DEG C, 78 DEG C, 80 DEG C) stirring reaction 1.5 ~ 2h(1.5h, 1.6h, 1.7h, 1.8h, 1.9h, 2.0h), reaction solution pH to 6.5 ~ 7.5(6.5 is regulated afterwards with magnesium oxide, 6.7, 6.9, 7.1, 7.3, 7.5), the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380 ~ 1.430g/cm
3(1.380 g/cm
3, 1.390 g/cm
3, 1.400 g/cm
3, 1.410 g/cm
3, 1.420 g/cm
3, 1.430 g/cm
3), for subsequent use,
(4), the magnesium nitrate concentrated solution that step (3) obtains is pumped in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:2.8 ~ 3.5(1:2.8,1:3.0,1:3.2,1:3.4,1:3.5), evaporation concentration, concentrate to proportion is 1.150 ~ 1.540g/cm
3(1.150 g/cm
3, 1.230 g/cm
3, 1.310 g/cm
3, 1.390 g/cm
3, 1.470 g/cm
3, 1.540 g/cm
3), vaporization temperature is 150 ~ 180 DEG C (150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C);
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
The method of full water-soluble calcium ammonium nitrate magnesium is produced in embodiment 1 one kinds of steel band granulations, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 70 DEG C of stirring reaction 1.5h, reaction solution pH to 6.5 is regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.440 g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 7% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.640g/cm
3, vaporization temperature is 150 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 70 DEG C of stirring reaction 1.5h, reaction solution pH to 6.5 is regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.390 g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:3.2, evaporation concentration, and concentrate to proportion is 1.150g/cm
3, vaporization temperature is 160 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
The method of full water-soluble calcium ammonium nitrate magnesium is produced in embodiment 2 one kinds of steel band granulations, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 74 DEG C of stirring reaction 1.7 h, reaction solution pH to 6.7 is regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.440 g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 6% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.600g/cm
3, vaporization temperature is 170 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 78 DEG C of stirring reaction 1.7h, reaction solution pH to 6.7 is regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:3.2, evaporation concentration, and concentrate to proportion is 1.150g/cm
3, vaporization temperature is 170 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
The method of full water-soluble calcium ammonium nitrate magnesium is produced in embodiment 3 one kinds of steel band granulations, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 76 DEG C of stirring reaction 1.9 h, reaction solution pH to 6.9 is regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.510g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 4% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.480 g/cm
3, vaporization temperature is 180 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 80 DEG C of stirring reaction 2h, reaction solution pH to 6.9 is regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.410 g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:3.5, evaporation concentration, and concentrate to proportion is 1.390 g/cm
3, vaporization temperature is 180 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
The method of full water-soluble calcium ammonium nitrate magnesium is produced in embodiment 4 one kinds of steel band granulations, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 80 DEG C of stirring reaction 2h, reaction solution pH to 7.1 is regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 5% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.440g/cm
3, vaporization temperature is 160 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 74 DEG C of stirring reaction 1.6h, reaction solution pH to 7.1 is regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.400 g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:3.0, evaporation concentration, and concentrate to proportion is 1.230 g/cm
3, vaporization temperature is 150 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
The method of full water-soluble calcium ammonium nitrate magnesium is produced in embodiment 5 one kinds of steel band granulations, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 72 DEG C of stirring reaction 1.6 h, reaction solution pH to 7.3 is regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.410 g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 3% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.560 g/cm
3, vaporization temperature is 150 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 72 DEG C of stirring reaction 1.8h, reaction solution pH to 7.3 is regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.420 g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:2.8, evaporation concentration, and concentrate to proportion is 1.470 g/cm
3, vaporization temperature is 150 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
The method of full water-soluble calcium ammonium nitrate magnesium is produced in embodiment 6 one kinds of steel band granulations, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 78 DEG C of stirring reaction 1.8 h, reaction solution pH to 7.5 is regulated afterwards with calcium oxide, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 8.5% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.520 g/cm
3, vaporization temperature is 180 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 76 DEG C of stirring reaction 1.9h, reaction solution pH to 7.5 is regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.430g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:3.5, evaporation concentration, and concentrate to proportion is 1.540 g/cm
3, vaporization temperature is 180 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor 14; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product (diameter 1 ~ 50mm) through steel band tablets press 15.Mix with arbitrary proportion between each trace element, often kind of trace element can need to consider to add according to concrete;
(6), pack, warehouse-in.
Fig. 1 is device schematic diagram when producing this product.Fill dust technology in first dilute acid bath 1, fill calcium oxide in calcium oxide groove 2, the two is connected with the first reactor 3 by pipeline, and the bottom discharge mouth of the first reactor 3 is connected with the first plate and frame(type)filter press 4, for filtration of calcium nitrate neutralizer by pipeline; Also dust technology is filled in second dilute acid bath 8, magnesium oxide is filled in magnesium oxide groove 9, the two is connected with the second reactor 10 by pipeline, and the bottom discharge mouth of the second reactor 10 is connected with the second plate and frame(type)filter press 11 by pipeline, for filtering magnesium nitrate neutralizer; Magnesium nitrate vaporizer 12 realizes the concentrated of magnesium nitrate, ammonium nitrate liquid bath 7 adds ammonium nitrate solution in nitrocalcite vaporizer 5, the synthesis that nitrocalcite vaporizer realizes nitrocalcite, ammonium nitrate and magnesium nitrate concentrates, and two steam boilers provide steam respectively to nitrocalcite, magnesium nitrate vaporizer.Single steel band granulation flaker that steel band tablets press adopts upper Nereid's great waves steel band Science and Technology Ltd. to produce, device numbering: JT3000-1.5-17.5.
Claims (1)
1. the method for a steel band granulation production full water-soluble calcium ammonium nitrate magnesium, it is characterized in that, comprise the following steps: (1), the dilute nitric acid solution being 40% by calcium oxide and concentration add reactor and carry out neutralization reaction, wherein the mol ratio of calcium oxide and nitric acid is 1:2, temperature controls at 70 ~ 80 DEG C of stirring reaction 1.5 ~ 2h, regulate reaction solution pH to 6.5 ~ 7.5 with calcium oxide afterwards, the nitrocalcite neutralizer obtained enters plate and frame(type)filter press and filters, and obtains clear filtrate; Filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380 ~ 1.510g/cm
3;
(2) ca nitrate soln, after concentrated quantitatively adds ammonium nitrate solid, and ammonium nitrate solid content is calculated by quality ratio and accounted for 3 ~ 8.5% of nitrocalcite quality, and carry out double evaporation-cooling after stirring and concentrate, concentrate to proportion is 1.440 ~ 1.640g/cm
3, vaporization temperature is 150 ~ 180 DEG C, generates calcium ammonium nitrate concentrated solution, for subsequent use;
(3) dilute nitric acid solution being, 40% by magnesium oxide and concentration adds reactor and carries out neutralization reaction, magnesium oxide and nitric acid mol ratio are 1:2, temperature controls at 70 ~ 80 DEG C of stirring reaction 1.5 ~ 2h, reaction solution pH to 6.5 ~ 7.5 are regulated afterwards with magnesium oxide, the magnesium nitrate neutralizer obtained enters plate and frame(type)filter press and filters, obtain clear filtrate, filtrate is pumped into vaporizer and carry out evaporation concentration, being evaporated to proportion is 1.380 ~ 1.430g/cm
3, for subsequent use;
(4), by the magnesium nitrate concentrated solution that step (3) obtains pump in the calcium ammonium nitrate concentrated solution in step (2), calcium ammonium nitrate concentrated solution and magnesium nitrate concentrated solution mass ratio are 1:2.8 ~ 3.5, evaporation concentration, and concentrate to proportion is 1.150 ~ 1.540g/cm
3, vaporization temperature is 150 ~ 180 DEG C;
(5), the concentrated solution that step (4) obtains is pumped into cooling reactor; add boric acid, EDTA-copper, EDTA-iron, EDTA-zinc, EDTA-manganese, ammonium molybdate trace element; trace element quality summation is more than or equal to 0.2% of the concentrated solution total mass obtained in step (4); be stirred to above-mentioned concentrated solution after dissolving and enter steel band tablets press, generate grass green semi-spherical shape nitrocalcite magnesium finished product through steel band tablets press.
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CN108147859A (en) * | 2016-12-02 | 2018-06-12 | 贵州芭田生态工程有限公司 | Nitric acid ca and mg fertilizer and preparation method thereof |
CN110668847A (en) * | 2019-11-04 | 2020-01-10 | 山西华鑫肥业股份有限公司 | Production method of large-particle magnesium nitrate |
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Effective date of registration: 20191108 Address after: 030599 Shanxi city of Lvliang province Jiaocheng Yiwang Village Patentee after: Shanxi Jiaocheng Hongxing Chemicals Co., Ltd. Address before: 030006, Shanxi, Taiyuan Province, No. 368 Yin Jie north water building, 14 floor Patentee before: Lu Yongkuan |