CN101850989B - Preparation method of large-particle ammonium sulfate - Google Patents

Preparation method of large-particle ammonium sulfate Download PDF

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Publication number
CN101850989B
CN101850989B CN 200910081374 CN200910081374A CN101850989B CN 101850989 B CN101850989 B CN 101850989B CN 200910081374 CN200910081374 CN 200910081374 CN 200910081374 A CN200910081374 A CN 200910081374A CN 101850989 B CN101850989 B CN 101850989B
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ammonium sulfate
gas
weight part
preparation
washings
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CN101850989A (en
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王宝安
曹涛
聂景新
马杰文
刘峰
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HEBEI TOPRUN CHEMICAL INDUSTRY Co Ltd
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HEBEI TOPRUN CHEMICAL INDUSTRY Co Ltd
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Abstract

The invention relates to a preparation method of large-particle nitrogenous fertilizers, in particular to a preparation method of large-particle ammonium sulfate, which comprises the following steps: firstly, adding 25-60 parts by weight of sulfuric acid, 7.6-16.5 parts by weight of ammonia and washing liquid from a gas-liquid separator to a tubular reactor for neutralization reaction; spraying high-temperature slurry formed after the reaction into a pelletizer; wherein, simultaneously, a solid material bed which comprises 20-70 parts by weight of solid material and rolls together with returns in the pelletizer can be installed in the pelletizer; spraying a pelleting binder through a spray nozzle and spraying the ammonium through an ammonium spraying shaft for pelleting to form wet solid material; fractionating the dried material after entering a sieving machine to sieve qualified particles and then cooling the particles to obtain the product. The invention reduces the reaction load of the tubular reactor; the system returns ratio is reduced, and the water balance is easier to control; simultaneously, the production cost is reduced, and recycling and the high-value utilization of industrial byproducts are realized by utilizing by-product powdery ammonium sulfate.

Description

A kind of preparation method of large-particle ammonium sulfate
Technical field
The present invention relates to a kind of preparation method of macrobead nitrogenous fertilizer, particularly a kind of preparation method of large-particle ammonium sulfate.
Background technology
The technology of preparation large-particle ammonium sulfate has at present:
1. " producing ammonium sulfate byproduct solution condensing crystal production technique ": can produce with the by product ammoniumsulphate soln of preparation lactan.In process of production the by product ammoniumsulphate soln of preparation lactan is input to the crystallizer condensing crystal, and by tripping device reclaim(ed) sulfuric acid ammonium crystal from the slurry that contains the crystalline sulfuric acid ammonium, this arts demand makes the ammonia sulfate crystal quantity stayed in the crystallizer repeatedly increase/reduce in the scope between ammonia sulfate crystal upper content limit and the lower limit in the crystallizer that predetermines, with the large-particle ammonium sulfate crystallization of discharging at the bottom of the reclaim(ed) sulfuric acid crystalline ammonium tank, the small-particle ammonia sulfate crystal then is transmitted back to the ammonium sulfate crystallization tank together with the mother liquor after separating further grows up crystal.Cause energy consumption high, the particle size dispersion of ammonium sulfate is uneven and particle shape is irregular, is difficult to be fit to the needs of mechanized application and preparation bulk blended fertilizer (BB is fertile).Be the preparation method of disclosed large-particle ammonium sulfate in 90109065.4 the Chinese invention patent such as UBE Industries Ltd. in the patent No..
2. " extrinsion pressing ": a kind of technique of utilizing powdery ammonium sulfate to prepare ammonium sulphate grain, can utilize the secondary powdery ammonium sulfate production of desulfurization by-product.The production technique of this method is: powdery ammonium sulfate is added dry method rolling granulation unit push granulating by physical method; because the special crystal formation of ammonium sulfate powder; the mechanical energy that granulating needs is very large; energy consumption is very high; and product be shaped as sheet, be difficult to be fit to the needs of mechanized application and preparation bulk blended fertilizer (BB is fertile).
Therefore, provide a kind of returning charge reaction heat, drying load low, that take full advantage of sulfuric acid and the ammonia method for preparing large-particle ammonium sulfate little, that steam consumption is low, production efficiency is high just to become the technical barrier that this technical field urgent need will solve.
Summary of the invention
The purpose of this invention is to provide that a kind of returning charge is low, the tubular reactor process of the use sulfuric acid that reaction heat, drying load are little, steam consumption is low, production efficiency is high that takes full advantage of sulfuric acid and ammonia and ammonia prepares the method for large-particle ammonium sulfate.
The objective of the invention is to reach by the following technical programs:
A kind of preparation method of large-particle ammonium sulfate, its step is as follows:
(1) ammonia of the sulfuric acid of 25-60 weight part, 7.6-16.5 weight part and the washings from gas-liquid separator that accounts for liquid, the total charging capacity 30%-80% ratio of solid are added in the tubular reactor carry out neutralization reaction first, the slip that forms after reacting sprays into tablets press, together with the solid material bed that accounts for liquid, the total charging capacity 2-4 of solid returning charge formation rolling doubly; And in described solid material bed, spraying into the adhesive for granulating of 0.5-1.5 weight part through shower nozzle, the ammonia that sprays into the 0.4-7.5 weight part through spray ammonia axle carries out granulation, forms wet solid material and tail gas generated by granulation;
(2) described tail gas generated by granulation enter gas-liquid separator with from the washings of gas-liquid separator recycle pump in venturi-type eductors fully atomizing mix, gas-liquid mixture enters gas-liquid separator separates, washings mixes recovery ammonia and dust through recycle pump with tail gas generated by granulation, the washings that accounts for liquid, the total charging capacity 30%-80% ratio of solid is delivered to tubular reactor through transferpump, and the gas after the separation enters the eddy flow washing tower and further washs after the blower fan pressurization;
(3) dried tail gas from blower fan enters the eddy flow washing tower with the gas that gas-liquid separator comes, add simultaneously 2.5-15 weight part sulfuric acid and add entry according to the washings consumption, keep the gas-liquid separator liquid level equilibrium, form eddy flow washing tower washings, washings carries out spray washing through recycle pump to the tail gas that enters in the tower, spillway discharge is consistent with the total amount of liquid that adds the swirling flow washing tower, and the washings overflow is to gas-liquid separator, the exhaust gas evacuation after the washing;
(4) wet solid material of described step (1) formation enters drying machine and dry-heat air and fluidized drying, dried material enters sieve apparatus material is carried out classification, dried tail gas advances tornado dust collector and reclaims most of dust, the dust that reclaims returns tablets press as returning charge, and the gas after the separation enters the eddy flow washing tower through the blower fan pressurization and further washs;
(5) after the middle classification of described step (4), the macroparticle that sieves out returns tablets press together with sieving the fine powder that gets off as returning charge through crusher in crushing; Sieve out qualified particle except part return tablets press keep the returning charge amount stable, after all the other qualified particles cool off product.
A kind of prior technology scheme is characterized in that: when the slip that forms after the reaction in the step (1) sprays into tablets press, also add the filler of 20-70 weight part solid material or 20-70 weight part solid material and 1-2.5 weight part in tablets press.
Described solid material is the mixture of powdery ammonium sulfate or powdery ammonium sulfate and magnesium powder.
Filler adds according to nutrient requirement and the oarse-grained skeleton of formation ammonium sulfate, and described filler is pulverous wilkinite, kaolin, china clay, potter's clay.
A kind of optimal technical scheme is characterized in that: the phosphoric acid that also adds simultaneously the 0.5-1.5 weight part in the step (3) forms eddy flow washing tower washings.
The concentration of described phosphoric acid is 26%P 2O 5~51%P 2O 5
A kind of prior technology scheme is characterized in that: the slip amount of dry matter that sulfuric acid and ammonia neutralization reaction form in the described step (1) is the 30-75 weight part.
Described sulfuric acid concentration is 93-98%, and described ammonia can be liquefied ammonia, also can be gas ammonia.The sulfuric acid that adds in the described tubular reactor, the amount of ammonia make ammonia and the sulfuric acid neutralization reaction in the described tubular reactor complete, and the add-on of washings be used for to be regulated the optimal temperature of ammonium sulfate slurry and viscosity to satisfy the needs of large-particle ammonium sulfate granulation.
Described adhesive for granulating is urea-formaldehyde resin; The perhaps mixture prepared by a certain percentage of urea-formaldehyde resin and sodium lignosulfonate, treated starch, Mierocrystalline cellulose.Mixture type adhesive for granulating is 10-40 weight part treated starch as described, 5-20 weight part sodium lignosulfonate, 10-80 weight part urea-formaldehyde resin, the mixture that 5-15 weight part Mierocrystalline cellulose forms.
Prilling temperature is 60~115 ℃ in the described step (1), and tablets press outlet wet solid material water content (free-water) is 2.5~4%; The dry-heat air temperature is 80~220 ℃ in the described step (4), and the dried tail gas temperature is 50~120 ℃, and the drying machine outlet material is moisture less than 1.0%.
Described returning charge comprises the finished product that dust, the granule behind the ultra-specification particle fragmentation, the part of the fine powder that sieves, recovery are returned.
Described tablets press returning charge than (charging capacity: returning charge amount, calculate take butt) as 1: 2~4.
The amount of the described sulfuric acid that enters the eddy flow washing tower and water guarantees that eddy flow washing tower washings pH is 1.5~3.5; Gas-liquid separator washings pH is controlled at 1~7.
The washings of described gas-liquid separator is delivered to the amount of tubular reactor and regulates according to the granulation needs through washing pump.
The reaction principle of tubular reactor
(1) ammonification of sulfuric acid
Violent neutralization reaction occurs and generates ammonium sulfate in the sulfuric acid that adds in tubular reactor and ammonia:
2NH 3+H 2SO 4=(NH 4) 2SO 4
The reaction of sulfuric acid and ammonia is to be achievable rapid reaction moment, and process speed depends on mixing velocity and the degree of mixing of sulfuric acid and ammonia.Use tubular reactor to carry out the sulfuric acid ammonification, utilize exactly strong mixing effect in the tubular reactor, make N-process shorten to about 1 second, take full advantage of simultaneously the moisture in a large amount of reacting heat evaporation slips.
(2) phosphoric acid by wet process ammonification
In washing device, tablets press, main chemical reaction is the reaction between phosphoric acid and the ammonia.Hydrogen ion in the phosphoric acid can be neutralized in moment and generate monoammonium phosphate (MAP), diammonium phosphate (DAP):
H 3PO 4+NH 3=NH 4H 2PO 4
H 3PO 4+2NH 3=(NH 4) 2HPO 4
Phosphoric acid and ammonia react directly generate (NH in the reaction process 4) 2HPO 4Less, that at first generate is NH 4H 2PO 4, following reaction occurs again:
NH 4H 2PO 4+NH 3=(NH 4) 2HPO 4
Pass into ammonia at the material bed, mainly reacting is the ammonification of free sulfuric acid and the further ammonification formation diammonium phosphate of minute quantity monoammonium phosphate:
2NH 3+H 2SO 4=(NH 4) 2SO 4
NH 4H 2PO 4+NH 3=(NH 4) 2HPO 4
Beneficial effect:
At first according to the nitrogen content requirement of producing large-particle ammonium sulfate; replace part tablets press tubular reactor reaction slurry with adding powdery ammonium sulfate; control reaction heat, the shortcoming of having avoided independent use tablets press tubular reactor reaction slurry heat too to concentrate makes the easier realization of system thermal balance.Reduced the reaction load of tubular reactor, corresponding amount of liquid phase reduces makes system's returning charge than further reducing the easier control of water balance.
The present invention is mainly for domestic coal electricity industry, abundant and the characteristics that are not easy to directly use of coking plant flue gas desulfurization and part organic chemical industry industry byproduct powdery ammonium sulfate, utilize tubular reactor process to provide take ammonium sulfate as main reaction slurry, with returning charge, powdery ammonium sulfate, filler and adhesive for granulating are base-material, realize the macrobead of ammonium sulfate, realizing under water balance and the thermally equilibrated prerequisite simultaneously, it is abundant to have kept the tubular reactor utilization of Heat of Reaction, reaction times is short, charging capacity is easy to adjust fast, tablets press outlet wet stock water content (free-water) low (2.5%~4%), returning charge lower (1: 2~4), the advantage that drying load is little, and then can suitably reduce the production cost of large-particle ammonium sulfate, certain direct economic benefit is arranged; Utilize the byproduct powdery ammonium sulfate to realize resource utilization and the high-value-use of industrial by-products, environmental benefit and the indirect economic effect of generation are limitless.
The present invention will be further described below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1
Total prescription is sulfuric acid 1.41m 3/ h, liquefied ammonia 0.848t/h, phosphoric acid 0.1m 3/ h, powdery ammonium sulfate 4t/h, magnesium powder 0.09t/h, adhesive for granulating 0.065t/h, returning charge 30t/h.
As shown in Figure 1, be process flow diagram of the present invention.Concentration is 46% (P 2O 5Content) phosphoric acid is forced into 1MPa through the phosphoric acid pump, after under meter and variable valve measure control with 0.1m 3/ h enters the eddy flow washing tower.The sulfuric acid of concentration 95% is forced into 1MPa through sulfuric acid pump, respectively after under meter and variable valve measure control with 1.25m 3/ h and 0.16m 3The amount of/h enters respectively tubular reactor and eddy flow washing tower.Liquefied ammonia (concentration 99.5%) enters tubular reactor and spray ammonia axle with 0.773t/h and 0.075t/h respectively after under meter and variable valve measure control, powdery ammonium sulfate (N21.2%,) 4t/h, magnesium powder 0.09t/h, adhesive for granulating urea-formaldehyde resin 0.065t/h, add tablets press; 80~100 ℃ of prilling temperatures.
Dried tail gas drying exhaust fan after the tornado dust collector dedusting enters the eddy flow washing tower, and is emptying after the washing water spray washing cooling dedusting from the washing water recycle pump.From the tail gas that tablets press is discharged, contain a large amount of steam, a small amount of ammonia and dust etc., spray wherein fully atomizing with circulating cleaning solution from gas-liquid separator at Venturi and mixes recovery ammonia, dust.Gas-liquid mixture separates in gas-liquid separator, the part washings washs tail gas generated by granulation through recycle pump, the part washings enters tubular reactor according to the granulation needs, gas after the separation enters the eddy flow washing tower through blower fan, through coming the further spray washing of washings of spin current washing tower detergent circulator, washings in the eddy flow washing tower partly enters recycle pump, and all the other washings overflows are to gas-liquid separator, the exhaust gas evacuation after the washing.
In eddy flow washing tower and gas-liquid separator, by Flux Valve Control sulfuric acid, phosphoric acid, process water add-on, the pH of control eddy flow washing tower and gas-liquid separator is respectively 1.5~3.5 and 1~7, and the liquid level of assurance gas-liquid separator is normal.The washings that forms in the eddy flow washing tower to gas-liquid separator, in the washing tail gas generated by granulation, is delivered to tubular reactor with washings through transferpump according to the granulation needs through overflow.
In tubular reactor; sulfuric acid; ammonia and washings carry out fast neutralization reaction; the high temperature slip that generates about 120-150 ℃ after the reaction sprays into tablets press; with solid material; granule after the macroparticle fragmentation of returning; the dust that reclaims with dedusting that sieves out; and the finished product that partly returns granulation in the revolution tablets press; go out the wet solid material moisture about 3% of tablets press; enter drying machine and temperature and be 100~180 ℃ dry-heat air and fluidized drying; material is moisture is down to~and 0.6%; dried material enters sieve apparatus; the dried tail gas temperature that goes out drying machine is 80~105 ℃; advance tornado dust collector and reclaim most of dust; the dust that reclaims returns tablets press as returning charge, and the gas drying exhaust fan pressurization after the separation enters the eddy flow washing tower and further washs.
Dried material enters sieve apparatus and carries out classification, sieves out macroparticle, and it is macroparticle that particle diameter surpasses 4.75mm, becomes small-particle through crusher in crushing, turns back to tablets press together with sieving the fine powder that gets off as returning charge; Sieve out qualified particle (particle diameter is 1-4.75mm), part is returned tablets press as returning charge, keeps the returning charge amount about 30t/h, obtains product after all the other qualified particles cool off, and product large-particle ammonium sulfate nitrogen nutrient specification is 20.5%.
Embodiment 2
Total prescription is sulfuric acid 1.24m 3/ h, liquefied ammonia 0.744t/h, phosphoric acid 0.15m 3/ h, powdery ammonium sulfate 4.5t/h, the intercalation native 0.2t/h of Powdered Peng, mixture type (40 weight part treated starches, 20 weight part sodium lignosulfonates, 30 weight part urea-formaldehyde resins, 10 weight part Mierocrystalline celluloses) adhesive for granulating 0.04t/h, returning charge 20t/h.Other is identical with embodiment 1, and the identical type specifications of raw materials is with embodiment 1, and different is not add the magnesium powder in the tablets press, filled swollen intercalation soil.Sulfuric acid concentration 95%, tubular reactor sulfuric acid 1.08m 3/ h, liquefied ammonia (concentration 99.5%) enter tubular reactor and spray ammonia axle, eddy flow washing tower sulfuric acid 0.16m with 0.707t/h and 0.037t/h respectively after under meter and variable valve measure control 3/ h, gas-liquid separator 51% phosphoric acid (P 2O 5Content) 0.15m 3/ h; powdery ammonium sulfate 4.5t/h; swollen intercalation native 0.2t/h, adhesive for granulating 0.04t/h, returning charge amount 20t/h; 85~100 ℃ of prilling temperatures; 120~160 ℃ of dry-heat air temperature, 80~95 ℃ of dried tail gas temperature, the tablets press outlet material is moisture~and 4%; the drying machine outlet material is moisture~and 0.8%, product large-particle ammonium sulfate nitrogen nutrient specification is 20.5%.
Embodiment 3
Total prescription is sulfuric acid 2.35m 3/ h, liquefied ammonia 1.41t/h, powdery ammonium sulfate 5t/h, Powdered kaolin 0.11t/h, mixture type (10 weight part treated starches, 5 weight part sodium lignosulfonates, 80 weight part urea-formaldehyde resins, 5 weight part Mierocrystalline celluloses) adhesive for granulating 0.06t/h, returning charge 25t/h.
Other is identical with embodiment 1, and the identical type specifications of raw materials is with embodiment 1, and different is not add magnesium powder, filled kaolin in the tablets press.Sulfuric acid concentration 93%, tubular reactor sulfuric acid 2.15m 3/ h, gas ammonia 1.0t/h.The logical ammonia 0.41t/h of tablets press spray ammonia axle, eddy flow washing tower sulfuric acid 0.2m 3/ h; powdery ammonium sulfate 5t/h; kaolin 0.25t/h, adhesive for granulating 0.06t/h, returning charge amount 25t/h; 90~100 ℃ of prilling temperatures; 110~150 ℃ of dry-heat air temperature, 75~90 ℃ of dried tail gas temperature, the tablets press outlet material is moisture~and 3%; the drying machine outlet material is moisture~and 0.5%, product large-particle ammonium sulfate nitrogen nutrient specification is 20.5%.
Embodiment 4
Total prescription is sulfuric acid 4.17m 3/ h, liquefied ammonia 2.48t/h, phosphoric acid 0.1m 3/ h, mixture type (25 weight part treated starches, 10 weight part sodium lignosulfonates, 50 weight part urea-formaldehyde resins, 15 weight part Mierocrystalline celluloses) adhesive for granulating 0.09t/h, returning charge 35t/h.
Other is identical with embodiment 1, and the identical type specifications of raw materials is with embodiment 1, and different is not filled in the tablets press and magnesium powder.Sulfuric acid concentration 98%, tubular reactor sulfuric acid 3.75m 3/ h, gas ammonia enter tubular reactor and spray ammonia axle, eddy flow washing tower sulfuric acid 0.42m with 1.61t/h and 0.87t/h respectively after under meter and variable valve measure control 3/ h, gas-liquid separator 26% phosphoric acid (P 2O 5Content) 0.10m 3/ h; adhesive for granulating 0.09t/h; returning charge amount 35t/h; 80~105 ℃ of prilling temperatures; 100~150 ℃ of dry-heat air temperature, 85~110 ℃ of dried tail gas temperature, the tablets press outlet material is moisture~and 3%; the drying machine outlet material is moisture~and 0.9%, product large-particle ammonium sulfate nitrogen nutrient specification is 21%.
The quality index of above-described embodiment products obtained therefrom sees the following form 1.
Table 1
Figure G200910081374XD00061

Claims (10)

1. the preparation method of a large-particle ammonium sulfate, its step is as follows:
(1) ammonia of the sulfuric acid of 25-60 weight part, 7.6-16.5 weight part and the washings from gas-liquid separator that accounts for liquid, the total charging capacity 30%-80% ratio of solid are added in the tubular reactor carry out neutralization reaction first, the slip that forms after reacting sprays into tablets press, together with the solid material bed that accounts for liquid, the total charging capacity 2-4 of solid returning charge formation rolling doubly; And in described solid material bed, spraying into the adhesive for granulating of 0.5-1.5 weight part through shower nozzle, the ammonia that sprays into the 0.4-7.5 weight part through spray ammonia axle carries out granulation, forms wet solid material and tail gas generated by granulation;
(2) described tail gas generated by granulation enter gas-liquid separator with from the washings of gas-liquid separator recycle pump in venturi-type eductors fully atomizing mix, gas-liquid mixture enters gas-liquid separator separates, washings mixes recovery ammonia and dust through recycle pump with tail gas generated by granulation, the washings that accounts for liquid, the total charging capacity 30%-80% ratio of solid is delivered to tubular reactor through transferpump, and the gas after the separation enters the eddy flow washing tower and further washs after the blower fan pressurization;
(3) dried tail gas from blower fan enters the eddy flow washing tower with the gas that gas-liquid separator comes, add simultaneously 2.5-15 weight part sulfuric acid and add entry according to the washings consumption, keep the gas-liquid separator liquid level equilibrium, form eddy flow washing tower washings, washings carries out spray washing through recycle pump to the tail gas that enters in the tower, spillway discharge is consistent with the total amount of liquid that adds the swirling flow washing tower, and the washings overflow is to gas-liquid separator, the exhaust gas evacuation after the washing;
(4) wet solid material of described step (1) formation enters drying machine and dry-heat air and fluidized drying, dried material enters sieve apparatus material is carried out classification, dried tail gas advances tornado dust collector and reclaims most of dust, the dust that reclaims returns tablets press as returning charge, and the gas after the separation enters the eddy flow washing tower through the blower fan pressurization and further washs;
(5) after the middle classification of described step (4), the macroparticle that sieves out returns tablets press together with sieving the fine powder that gets off as returning charge through crusher in crushing; Sieve out qualified particle except part return tablets press keep the returning charge amount stable, after all the other qualified particles cool off product.
2. the preparation method of large-particle ammonium sulfate as claimed in claim 1; it is characterized in that: when the slip that forms after the reaction in the described step (1) sprays into tablets press, in tablets press, also add the filler of 20-70 weight part solid material or 20-70 weight part solid material and 1-2.5 weight part.
3. the preparation method of large-particle ammonium sulfate as claimed in claim 2, it is characterized in that: described solid material is the mixture of powdery ammonium sulfate or powdery ammonium sulfate and magnesium powder; Described filler is pulverous wilkinite or kaolin.
4. the preparation method of large-particle ammonium sulfate as claimed in claim 1 is characterized in that: in the described step (3), the phosphoric acid that also adds simultaneously the 0.5-1.5 weight part forms eddy flow washing tower washings, and the concentration of described phosphoric acid is 26%P 2O 5~51%P 2O 5
5. the preparation method of large-particle ammonium sulfate as claimed in claim 1 is characterized in that: sulfuric acid is the 30-75 weight part with the slip amount of dry matter of ammonia neutralization reaction formation in the described step (1).
6. such as the preparation method of each described large-particle ammonium sulfate of claim 1-5, it is characterized in that: described sulfuric acid concentration is 93-98%; Described ammonia is liquefied ammonia or gas ammonia.
7. the preparation method of large-particle ammonium sulfate as claimed in claim 6 is characterized in that: described adhesive for granulating is the mixture of urea-formaldehyde resin or 10-80 weight part urea-formaldehyde resin, 5-20 weight part sodium lignosulfonate, 10-40 weight part treated starch and the preparation of 5-15 weight part Mierocrystalline cellulose.
8. the preparation method of large-particle ammonium sulfate as claimed in claim 7 is characterized in that: prilling temperature is 60~115 ℃ in the described step (1), and tablets press outlet wet solid material water content is 2.5~4%; The dry-heat air temperature is 80~220 ℃ in the described step (4), and the dried tail gas temperature is 50~120 ℃, and the drying machine outlet material is moisture less than 1.0%.
9. the preparation method of large-particle ammonium sulfate as claimed in claim 8 is characterized in that: described tablets press returning charge is than being charging capacity: the returning charge amount, with butt be calculated as 1: 2~4.
10. the preparation method of large-particle ammonium sulfate as claimed in claim 9, it is characterized in that: described eddy flow washing tower washings pH is 1.5~3.5; The washings pH of gas-liquid separator is 1~7.
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