CN102583443B - Method for producing ammonium sulfate by using ammonium bicarbonate as main raw material - Google Patents
Method for producing ammonium sulfate by using ammonium bicarbonate as main raw material Download PDFInfo
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- CN102583443B CN102583443B CN201210099988.2A CN201210099988A CN102583443B CN 102583443 B CN102583443 B CN 102583443B CN 201210099988 A CN201210099988 A CN 201210099988A CN 102583443 B CN102583443 B CN 102583443B
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- ammonium sulfate
- ammonium
- phosphogypsum
- bicarbonate
- ammonia
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 42
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 42
- 235000012538 ammonium bicarbonate Nutrition 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 title claims abstract description 12
- 239000001099 ammonium carbonate Substances 0.000 title claims abstract description 12
- 239000002994 raw material Substances 0.000 title claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 31
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 4
- 239000012065 filter cake Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 12
- 239000012066 reaction slurry Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000007601 warm air drying Methods 0.000 claims description 3
- 235000015097 nutrients Nutrition 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000004254 Ammonium phosphate Substances 0.000 abstract 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 abstract 2
- 235000019289 ammonium phosphates Nutrition 0.000 abstract 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 abstract 2
- 238000005086 pumping Methods 0.000 abstract 2
- 238000005259 measurement Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000003337 fertilizer Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 210000003608 fece Anatomy 0.000 description 2
- 239000010871 livestock manure Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 235000010269 sulphur dioxide Nutrition 0.000 description 2
- 239000004291 sulphur dioxide Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QLULGSLAHXLKSR-UHFFFAOYSA-N azane;phosphane Chemical compound N.P QLULGSLAHXLKSR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000002015 leaf growth Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Fertilizers (AREA)
Abstract
The invention discloses a method for producing ammonium sulfate by using ammonium bicarbonate as a main raw material, comprising the following steps of: (1) adding solid ammonium bicarbonate, process water, liquid ammonia or gas ammonia into a dissolving tank according to a mass ratio through measurement to react to be prepared into an ammonium phosphate solution; (2) pumping the ammonium phosphate solution into a conversion reactor by using a pump, adding phosphogypsum according to a certain proportion to carry out conversion reaction, and controlling the density of reacting slurry to be 1.35-1.40g/cm<3>; (3) pumping the reacting slurry into a filtering machine by using the pump, filtering in vacuum, and separating ammonium sulfate filtrate and calcium carbonate dreg filter cakes; and (4) delivering the ammonium sulfate filtrate into a evaporative crystallization by using the pump to obtain ammonium sulfate slurry, and finally carrying out centrifugal separation and drying to obtain an ammonium sulfate product. By using the method, the ammonium bicarbonate and the phosphogypsum are consumed, the value of the ammonium bicarbonate is increased, and the pressure of the phosphogypsum to the environment is reduced; and the produced large-particle crystal ammonium sulfate has better market, low production cost and remarkable profit. The method is suitable for manufacturers for manufacturing both ammonium bicarbonate and the phosphogypsum.
Description
[technical field]
The present invention relates to the fertilizer that contains ammonium salt, relate in particular to bicarbonate of ammonia and ammonium sulfate, specifically, relate to the method for producing ammonium sulfate take bicarbonate of ammonia as main raw material.
[background technology]
The nitrogen content of ammonium sulfate, between 20%～21%, is widely used in the industries such as agricultural, metallurgy, medicine, leather, wood preservation, weaving, plating, makes fermention medium in bio-pharmaceuticals, also as foodstuff additive, dough conditioning agent, yeast nutriment.In agricultural, as acidic fertilizier, use, be suitable for neutral soil and alkaline soil, for general farm crop, can make shoot and leaf growth vigorous, improve fruit quality and output, strengthen the resistivity of crop to disaster, can be used as topdressing, base manure, seed manure.Ammonium sulfate, with being chemical fertilizer, contains nitrogen, two kinds of nutritive elements of sulphur, very favourable to farm crop, is generally relatively applicable to the crops such as wheat, corn, paddy rice, cotton, sweet potato, crudefiber crop, fruit tree, vegetables.Can be used alone, the production composite fertilizer of also can preparing burden together with nitrogen, phosphate fertilizer effective element.
Bicarbonate of ammonia was once widely used as nitrogenous fertilizer, but it has distinct disadvantage, was mainly that low, volatile, the easy caking of fertilizer efficiency, difficult keeping store, are not suitable for long-distance transport.Under the impact of the high-effective chemical fertilizers such as urea, phosphorus ammonium and composite fertilizer, bicarbonate of ammonia manufacturing enterprise must find another way in recent years.
Phosphogypsum is to discharge solid waste in Wet Phosphoric Acid Plant production process, and current treatment process is to deliver to phosphogypsum slag field to stack.Its purposes is except part is used as the raw material of phosphogypsum sheet material and cement setting retarder, ardealite brick etc., and the current less than 20% of regeneration rate, stores up pressure very big, seriously restricts the development of sulphur dioxide of phosphor chemical industry.
In Chinese patent database, the application part that relates to ammonium sulfate production method has mono-kind of No. 90105643 < < to produce the method > > of ammonium sulfate, the production method > > of a No. 01131599 < < ammonium sulfate, mono-kind of No. 200810068735 < < method > > take phosphogypsum as preparing ammonium sulfate, the production method > > of No. 200610130704 < < ammonium sulfate, No. 200810016300 < < preparing process of ammonia sulfate > >, 200910102690 < < produce the method > > of granular ammonium sulfate etc. by crystalline ammonium sulfate or powdery ammonium sulfate.These methods differ from one another, but there is no so far the technical scheme of utilizing bicarbonate of ammonia to produce ammonium sulfate for main raw material.
[summary of the invention]
The object of the invention is to overcome above-mentioned shortcoming and a kind of method of producing ammonium sulfate take bicarbonate of ammonia as main raw material is provided, to solve a difficult problem for restriction bicarbonate of ammonia manufacturing enterprise and sulphur dioxide of phosphor chemical industry development.
Contriver's thinking is: employing solid ammonium bicarbonate is basic material, is dissolved into the aqueous solution, adds in proportion water and liquefied ammonia or gas ammonia to react, and is prepared into sal volatile; Then by metering, in sal volatile, by proportioning, add phosphogypsum to carry out replacement(metathesis)reaction, reaction slurry, through filtering, is isolated ammoniumsulphate soln, then is passed through evaporative crystallization, and last, slurry obtains ammonium sulfate product after centrifugation goes out moisture content.
The method of producing ammonium sulfate take bicarbonate of ammonia as main raw material that contriver provides, comprises the following steps:
(1) get solid ammonium bicarbonate, process water, liquefied ammonia or gas ammonia, by metering, by the quality proportioning of 636: 1182: 134, add dissolving tank reaction, be prepared into sal volatile;
(2) with pump, throw the sal volatile of previous step into conversion reactor, by the mass ratio 727(butt of sal volatile and phosphogypsum): 1448(is containing CaSO
42H
2the phosphogypsum of O 90%) add phosphogypsum to carry out conversion reaction, controlling reaction slurry density is 1.35～1.40g/cm
3;
(3) reaction slurry is got to filter with pump, under vacuum, filter, isolate ammonium sulfate filtrate and calcium carbonate slag filter cake;
(4) ammonium sulfate filter pump is sent into evaporative crystallization, 58 ℃ of crystallization control temperature, draw the ammonium sulfate slurry containing promising particle diameter 2～4mm particle after crystallization, finally carry out centrifugation, and drying obtains ammonium sulfate product.
In above-mentioned (1) step, as the solid ammonium bicarbonate quality index of main raw material, be N >=17%, the massfraction of liquefied ammonia used or gas ammonia is >=99.5%; The waste water of the recirculated water that process water employing crystallization and evaporation enters, the massfraction that is prepared into sal volatile is 38%.
In above-mentioned (2) step, the quality index of powdery phosphogypsum used is CaSO
42H
2o>=90%; Described conversion reaction temperature is 61 ℃～65 ℃, and the reaction times is 2.5～3 hours.
In above-mentioned (3) step, the vacuum degree control of described filtration is 35～50kpa(absolute pressure).
In above-mentioned (4) step, the speed of rotation control of described centrifugation is 1000～1100 r/min; Described being dried as warm air drying, hot blast temperature control is 120 ℃～140 ℃; The quality index of described ammonium sulfate product is nutrient N >=21%, granularity 2～4mm particle ratio >=90%, moisture≤0.1%.
Contriver points out: in material, adding liquefied ammonia or gas ammonia, is after bicarbonate of ammonia dissolves, all to generate volatile salt in order to guarantee, so that phosphogypsum conversion reaction can normally be carried out.
The invention has the beneficial effects as follows: consume bicarbonate of ammonia and phosphogypsum, promote the use value of bicarbonate of ammonia, reduce the pressure of phosphogypsum to environment; The macrobead crystal ammonium sulfate of producing has good market, and production cost is low, and profit is remarkable.Be applicable to the producer that existing bicarbonate of ammonia has again phosphogypsum to produce.
[embodiment]
Embodiment:
Certain factory produces in the device of ammonium sulfate, gets solid ammonium bicarbonate, process water, liquefied ammonia or gas ammonia, by metering, by the quality proportioning of 636: 1182: 134, adds dissolving tank, is prepared into concentration and is 38% volatile salt.Sal volatile is thrown conversion reactor into pump, by the mass ratio 727(butt of sal volatile and phosphogypsum): 1448(is containing CaSO
42H
2the phosphogypsum of O 90%) add phosphogypsum to carry out conversion reaction, control pulp density is 1.35～1.40g/cm
3in scope, 61 ℃～65 ℃ of temperature of reaction, in 2.5～3 hours reaction times, obtain reaction slurry; Reaction slurry is got to filter with pump, through isolated by vacuum filtration, obtain ammonium sulfate filtrate and calcium carbonate slag filter cake.The filtrate ammonium sulfate of separating from filter with being pumped into evaporative crystallization, drawing the ammonium sulfate slurry containing promising particle diameter 2～4mm particle, then carries out centrifugation, through 120 ℃～140 ℃ warm air dryings, obtains ammonium sulfate product.
Claims (2)
1. the method for producing ammonium sulfate take bicarbonate of ammonia as main raw material, its feature comprises the following steps:
(1) get solid ammonium bicarbonate, process water, liquefied ammonia or gas ammonia, by metering, by the quality proportioning of 636: 1182: 134, add dissolving tank reaction, be prepared into sal volatile; Solid ammonium bicarbonate quality index used is N >=17%, and the massfraction of liquefied ammonia used or gas ammonia is >=99%;
(2) with pump, throw the sal volatile of previous step into conversion reactor, by sal volatile in the quality of butt with containing CaSO
42H
2the ratio of the phosphogypsum quality of O 90% adds powdery phosphogypsum to carry out conversion reaction at 727: 1448, and controlling reaction slurry density is 1.35～1.40g/cm
3; Described conversion reaction temperature is 61 ℃～65 ℃, and the reaction times is 2.5～3 hours;
(3) reaction slurry is got to filter with pump, under vacuum, filter, isolate ammonium sulfate filtrate and calcium carbonate slag filter cake; The vacuum tightness of described filtration is take absolute manometer control as 35～50KPa;
(4) ammonium sulfate filter pump is sent into evaporative crystallization, 58 ℃ of crystallization control temperature, show after crystallization and contain the ammonium sulfate slurry that particle diameter is 2～4mm particle, finally carry out centrifugation, drying obtains ammonium sulfate product; The speed of rotation control of described centrifugation is 1000～1100r/min; Described being dried as warm air drying, hot blast temperature control is 120 ℃～140 ℃; The quality index of described ammonium sulfate product is nutrient N >=21%, ratio >=90% of granularity 2～4mm particle, moisture≤0.1%.
2. in accordance with the method for claim 1, it is characterized in that in (1) step, the massfraction that is prepared into sal volatile is 38%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210099988.2A CN102583443B (en) | 2012-04-09 | 2012-04-09 | Method for producing ammonium sulfate by using ammonium bicarbonate as main raw material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210099988.2A CN102583443B (en) | 2012-04-09 | 2012-04-09 | Method for producing ammonium sulfate by using ammonium bicarbonate as main raw material |
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| Publication Number | Publication Date |
|---|---|
| CN102583443A CN102583443A (en) | 2012-07-18 |
| CN102583443B true CN102583443B (en) | 2014-05-07 |
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|---|---|---|---|
| CN201210099988.2A Active CN102583443B (en) | 2012-04-09 | 2012-04-09 | Method for producing ammonium sulfate by using ammonium bicarbonate as main raw material |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107583466A (en) * | 2017-09-27 | 2018-01-16 | 四川恒泰环境技术有限责任公司 | A kind of method that wet desulphurization gypsum is converted into ammonium sulfate and calcium carbonate and recycled |
| CN113336242A (en) * | 2021-05-11 | 2021-09-03 | 太仓市业洪净水新材料有限公司 | Preparation method of phosphogypsum solid-phase ball milling of ammonium sulfate for water treatment |
| CN114350952B (en) * | 2021-11-29 | 2024-02-23 | 攀钢集团研究院有限公司 | Method for recycling gypsum slag in calcified vanadium extraction process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1114635A (en) * | 1995-02-20 | 1996-01-10 | 李永 | Process for producing potassium sulfate by plaster stone conversion method |
| US5980848A (en) * | 1995-06-23 | 1999-11-09 | Airborne Industrial Minerals Inc. | Method for production of sodium bicarbonate, sodium carbonate and ammonium sulfate from sodium sulfate |
| CN101269823A (en) * | 2008-05-07 | 2008-09-24 | 瓮福（集团）有限责任公司 | Method for producing ammonium sulphate with phosphogypsum as raw material |
| CN101318668A (en) * | 2008-07-05 | 2008-12-10 | 甘肃锦世化工有限责任公司 | Method for preparing agricultural ammonium sulphate and calcined soda for industry with salt cake ammonia soda process |
| CN101492178A (en) * | 2009-03-06 | 2009-07-29 | 瓮福（集团）有限责任公司 | Method for joint production of ammonium sulphate and calcium carbonate with phosphogypsum |
| CN101585547A (en) * | 2009-06-23 | 2009-11-25 | 西南科技大学 | Method for preparing ammonium sulfate as fertilizer by phosphogypsum through ball milling |
-
2012
- 2012-04-09 CN CN201210099988.2A patent/CN102583443B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1114635A (en) * | 1995-02-20 | 1996-01-10 | 李永 | Process for producing potassium sulfate by plaster stone conversion method |
| US5980848A (en) * | 1995-06-23 | 1999-11-09 | Airborne Industrial Minerals Inc. | Method for production of sodium bicarbonate, sodium carbonate and ammonium sulfate from sodium sulfate |
| CN101269823A (en) * | 2008-05-07 | 2008-09-24 | 瓮福（集团）有限责任公司 | Method for producing ammonium sulphate with phosphogypsum as raw material |
| CN101318668A (en) * | 2008-07-05 | 2008-12-10 | 甘肃锦世化工有限责任公司 | Method for preparing agricultural ammonium sulphate and calcined soda for industry with salt cake ammonia soda process |
| CN101492178A (en) * | 2009-03-06 | 2009-07-29 | 瓮福（集团）有限责任公司 | Method for joint production of ammonium sulphate and calcium carbonate with phosphogypsum |
| CN101585547A (en) * | 2009-06-23 | 2009-11-25 | 西南科技大学 | Method for preparing ammonium sulfate as fertilizer by phosphogypsum through ball milling |
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