CN102602962A - Method for preparing ammonium sulfate by use of dilute acid generated by pyrite-based acid production - Google Patents

Method for preparing ammonium sulfate by use of dilute acid generated by pyrite-based acid production Download PDF

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Publication number
CN102602962A
CN102602962A CN2012101069170A CN201210106917A CN102602962A CN 102602962 A CN102602962 A CN 102602962A CN 2012101069170 A CN2012101069170 A CN 2012101069170A CN 201210106917 A CN201210106917 A CN 201210106917A CN 102602962 A CN102602962 A CN 102602962A
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CN
China
Prior art keywords
ammonium sulfate
pyrite
acid
dilute sulphuric
sulphuric acid
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Pending
Application number
CN2012101069170A
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Chinese (zh)
Inventor
饶轶晟
潘志云
杨毅
赵建勇
杨德贵
刘海
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Wengfu Group Co Ltd
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Wengfu Group Co Ltd
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Priority to CN2012101069170A priority Critical patent/CN102602962A/en
Publication of CN102602962A publication Critical patent/CN102602962A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for preparing ammonium sulfate by use of dilute acid generated by pyrite-based acid production. The method comprises the following steps of: adding a filtering process in a device to filter solid impurities in dilute acid, thus obtaining relatively pure dilute sulphuric acid; measuring and adding the dilute sulphuric acid into a neutralizing tank; proportionally adding ammonia to obtain an ammonium sulfate solution; performing evaporative crystallization on the ammonium sulfate liquid; separating moisture from the crystallized slurry by a centrifuge to obtain ammonium sulfate; and drying ammonium sulfate to obtain a qualified product. The method disclosed by the invention has the beneficial effects that the waste dilute sulphuric acid generated by pyrite-based acid production is recycled in an enterprise, the effects of energy conservation, emission reduction and circular economy are realized, and the produced ammonium sulfate has relatively good market and obvious profits; and the method is suitable for manufacturers with a pyrite-based acid production device and an ammonium sulfate device.

Description

The method for preparing ammonium sulfate with the diluted acid of pyrite-based sulfuric acid production generation
[technical field]
The present invention relates to sulfuric acid, also relate to ammonium sulfate, relating in particular to the dilute sulphuric acid that produces in the pyrite-based sulfuric acid production is the method for feedstock production ammonium sulfate.
[background technology]
With the sulfurous iron ore is raw material system vitriolic production equipment, is that roasting pyrite output sulfurous gas is converted into sulphur trioxide again to process sulfuric acid in fluidizing furnace.Because acid-scrubbing cleaning, diluted acid closed circulation process are adopted in the flue gas cleaning that produces in the technology, can produce a certain amount of diluted acid in the scavenging process.Contain more mine dust in this diluted acid.For this part diluted acid, most of enterprises are regarded as spent acid, efflux with the lime neutralization, and the lime expense and the working cost of annual labor have increased environmental protection pressure simultaneously, and the sulphur resource wastes in this part diluted acid.How with its recycling, turning waste into wealth, is one of difficult problem of reducing discharging of consumption reduction.In the Chinese patent DB, the application part that relates to pyrite-based sulfuric acid production has 25, but up to now, does not see the dilute sulphuric acid that uses in the pyrite-based sulfuric acid production technical scheme as feedstock production ammonium sulfate.
[summary of the invention]
The object of the present invention is to provide the diluted acid that produces with pyrite-based sulfuric acid production to prepare the method for ammonium sulfate, the dilute sulphuric acid that pyrite-based sulfuric acid production is produced can digest in enterprises, does not efflux.
Contriver's thinking is: in device, increase and filter operation, remove by filter the solid impurity in the diluted acid, obtain purified relatively dilute sulphuric acid; Add neutralizing well through measuring the back; Add ammonia in proportion, be prepared into ammoniumsulphate soln, send to evaporative crystallization to ammonium sulfate liquid then; Slurry obtains ammonium sulfate after isolating moisture content through whizzer, obtains specification product after the drying.
So far on the thinking basis, the useless dilute sulphuric acid of the utilization that the contriver provides is the method for feedstock production ammonium sulfate, may further comprise the steps:
(1) diluted acid that pyrite-based sulfuric acid production is produced removes by filter the solid impurity in the diluted acid, obtains purified relatively dilute sulphuric acid;
(2) get dilute sulphuric acid and ammonia behind the filtration, purification respectively through after the metering, add the neutralization reaction groove and react and obtain ammoniumsulphate soln, the mass ratio of dilute sulphuric acid and ammonia is 98: 34;
(3) ammoniumsulphate soln that will go up a step is thrown evaporative crystallizer into pump and is evaporated, and the control pulp density is 1.28~1.35g/cm 3In the scope, obtain qualified enriching slurry;
(4) get to whizzer to enriching slurry with pump and carry out solid-liquid separation, liquid mother liquor is sent to the evaporation reconcentration, and isolated solid obtains qualified large-particle ammonium sulfate product after fluidized drying.
In the first step of aforesaid method, the dilute sulphuric acid quality index behind the filtration, purification is: sulfuric acid massfraction 20%, proportion 1.15, solid impurity content≤0.1%.
In second step of aforesaid method, the pH of ammoniumsulphate soln is controlled at 4.5~5.5, has macrobead to generate to guarantee crystallization.
In the 3rd step of aforesaid method, the quality index of ammonium sulfate product is nutrient N>=21%, granularity (1-4mm)>=90%, moisture≤0.1%.
In the 4th step of aforesaid method, the dried tail gas temperature is 65 ℃~85 ℃.
The invention has the beneficial effects as follows: the useless dilute sulphuric acid that pyrite-based sulfuric acid production is produced digests in enterprises; Embodied the utilization of energy-saving and emission-reduction and recycling economy; The ammonium sulfate of producing has market preferably, and profit is remarkable, is applicable to the producer that existing pyrite-based sulfuric acid production device has ammonium sulfate device to produce again.
[embodiment]
Embodiment: certain factory's production of sulfur from pyrite acid and sulphur ammonium production equipment; To obtain massfraction be 20% dilute sulphuric acid through filter purifying the dilute sulphuric acid that produces in the pickling of sulfuric acid apparatus purification section; With ammonia through the metering after; Adding neutralization reaction groove reacts and obtains ammoniumsulphate soln, and the mass ratio of dilute sulphuric acid and ammonia is 98: 34; Threw the ammoniumsulphate soln in a last step into evaporative crystallizer with pump and evaporate, the control pulp density is 1.28~1.35g/cm 3In the scope, obtain qualified enriching slurry; Get to whizzer to enriching slurry with pump and carry out solid-liquid separation, liquid mother liquor is sent to the evaporation reconcentration, and isolated solid is after fluidized drying; Obtain qualified large-particle ammonium sulfate product; The quality index of product is nutrient N>=21%, granularity 1-4mm ()>=90%, moisture≤0.1%.

Claims (5)

1. a diluted acid that produces with pyrite-based sulfuric acid production prepares the method for ammonium sulfate, and its characteristic may further comprise the steps:
(1) diluted acid that pyrite-based sulfuric acid production is produced removes by filter the solid impurity in the diluted acid;
(2) get dilute sulphuric acid and ammonia behind the filtration, purification respectively through after the metering, add the neutralization reaction groove and react and obtain ammoniumsulphate soln, the mass ratio of dilute sulphuric acid and ammonia is 98: 34;
(3) ammoniumsulphate soln that will go up a step is thrown evaporative crystallizer into pump and is evaporated, and the control pulp density is 1.28~1.35g/cm 3In the scope, obtain qualified enriching slurry;
(4) get to whizzer to enriching slurry with pump and carry out solid-liquid separation, liquid mother liquor is sent to the evaporation reconcentration, and isolated solid obtains ammonium sulfate product after fluidized drying.
2. according to the described method of claim 1, it is characterized in that in the first step that the dilute sulphuric acid quality index behind the filtration, purification is: sulfuric acid massfraction 20%, proportion 1.15, solid impurity content≤0.1%.
3. according to the described method of claim 1, it is characterized in that the pH of ammoniumsulphate soln is controlled at 4.5~5.5 in second step.
4. according to the described method of claim 1, it is characterized in that the quality index of ammonium sulfate product is nutrient N>=21% in the 3rd step, granularity be 1-4mm>=90%, moisture≤0.1%.
5. according to the described method of claim 1, it is characterized in that the dried tail gas temperature is 65 ℃~85 ℃ in the 4th step.
CN2012101069170A 2012-04-13 2012-04-13 Method for preparing ammonium sulfate by use of dilute acid generated by pyrite-based acid production Pending CN102602962A (en)

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CN2012101069170A CN102602962A (en) 2012-04-13 2012-04-13 Method for preparing ammonium sulfate by use of dilute acid generated by pyrite-based acid production

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Application Number Priority Date Filing Date Title
CN2012101069170A CN102602962A (en) 2012-04-13 2012-04-13 Method for preparing ammonium sulfate by use of dilute acid generated by pyrite-based acid production

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102897730A (en) * 2012-10-11 2013-01-30 瓮福(集团)有限责任公司 Method for recycling waste dilute sulphuric acid
CN103395803A (en) * 2013-08-01 2013-11-20 瓮福(集团)有限责任公司 Production method for powdery ammonium sulfate
CN103936032A (en) * 2014-04-08 2014-07-23 攀钢集团西昌钢钒有限公司 Method for producing large granular ammonium sulfate product

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB898851A (en) * 1960-03-05 1962-06-14 Carves Simon Ltd Improvements in and relating to the treatment of waste acid pickle liquor
US3167390A (en) * 1961-05-17 1965-01-26 Carves Simon Ltd Treatment of waste acid liquor
CN101177284A (en) * 2007-11-02 2008-05-14 北京化工大学 Method for reclaiming sulfuric ammonium and ferric oxide from sulfuric acid pickling waste fluid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB898851A (en) * 1960-03-05 1962-06-14 Carves Simon Ltd Improvements in and relating to the treatment of waste acid pickle liquor
US3167390A (en) * 1961-05-17 1965-01-26 Carves Simon Ltd Treatment of waste acid liquor
CN101177284A (en) * 2007-11-02 2008-05-14 北京化工大学 Method for reclaiming sulfuric ammonium and ferric oxide from sulfuric acid pickling waste fluid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李东光: "《工业废弃物回收利用实例》", 31 July 2010, 中国纺织出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102897730A (en) * 2012-10-11 2013-01-30 瓮福(集团)有限责任公司 Method for recycling waste dilute sulphuric acid
CN103395803A (en) * 2013-08-01 2013-11-20 瓮福(集团)有限责任公司 Production method for powdery ammonium sulfate
CN103936032A (en) * 2014-04-08 2014-07-23 攀钢集团西昌钢钒有限公司 Method for producing large granular ammonium sulfate product
CN103936032B (en) * 2014-04-08 2016-02-03 攀钢集团西昌钢钒有限公司 A kind of production method of large-particle ammonium sulfate product

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Application publication date: 20120725