CN103145149A - Method for purifying ammonium sulfate generated in flue gas desulfurization - Google Patents

Method for purifying ammonium sulfate generated in flue gas desulfurization Download PDF

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Publication number
CN103145149A
CN103145149A CN2013101011719A CN201310101171A CN103145149A CN 103145149 A CN103145149 A CN 103145149A CN 2013101011719 A CN2013101011719 A CN 2013101011719A CN 201310101171 A CN201310101171 A CN 201310101171A CN 103145149 A CN103145149 A CN 103145149A
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China
Prior art keywords
ammonium sulfate
ammonium
flue gas
gas desulfurization
cooling
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Pending
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CN2013101011719A
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Chinese (zh)
Inventor
刘飞
李天祥
郑润
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Wengfu Group Co Ltd
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Wengfu Group Co Ltd
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Priority to CN2013101011719A priority Critical patent/CN103145149A/en
Publication of CN103145149A publication Critical patent/CN103145149A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for purifying ammonium sulfate generated in flue gas desulfurization. The method comprises the following steps of: adding ammonium sulfate as a flue gas desulfurization byproduct into a reactor with a stirring blade, and adding water to stir, wherein the ammonium sulfate dissolves at the temperature of 20-80 DEG C; purifying the ammonium sulfate solution by using one of diatomite, active carbon, white carbon black and modified coal ash as a cleaning agent, decolorizing and filtering the purified ammonium sulfate solution; condensing filtrate under the condition that the vacuum degree ranges from 0.0MPa to 0.085MPa until a crystal coating appears in the solution; then, stopping heated condensation, cooling crystals in a programmed cooling way, wherein the stirring rotating speed ranges from 200rpm to 400rpm, the cooling rotating speed ranges from 2 DEG C/h to 8 DEG C/h, and the final cooling temperature ranges from 24 DEG C to 36 DEG C; and filtering and drying to obtain a crystal-shaped ammonium sulfate product. The method is simple in process flow, strong in operability, low in production cost, large in product particle, low in impurity content and favorable in economic benefit, and industrialization is easy to realize.

Description

A kind of method of flue desulfurization sulfur ammonium
Technical field
The present invention relates to the vitriol of ammonium, specifically a kind of method of flue desulfurization sulfur ammonium.
Background technology
The sulphur ammonium, as a kind of important Chemicals, is widely used in the industries such as fertilizer, weaving, leather, medicine bioengineering.At present, the waste gas that the production of sulphur ammonium mainly utilizes by product in industrial production or discharge with sulfuric acid or ammonia absorption (as the ammonia in the sulfuric acid absorption coke(oven)gas, ammonia absorption smeltery sulfur dioxide in flue gas, the ammonia of caprone in producing or the sulfuric acid method titanium pigment sulfuric acid waste in producing), also there is the gypsum of employing to take phosphogypsum, ammonia, carbonic acid gas and prepare the sulphur ammonium as raw material.The sulphur ammonium prepared by these methods is fully utilized resource, and is conducive to environment protection, but the general foreign matter content of ammonium sulfate products is high, need to be by after removal of impurities, purification, meeting industrial application.This patent is for this present situation, proposed flue gas desulfurization byproduct sulphur ammonium through purifying, and the combined soln crystallization technique, obtain the ammonium sulfate products that purity is higher, thereby meet the industrial application requirement, has higher economic benefit.
summary of the invention
The objective of the invention is for the deficiencies in the prior art, a kind of method of flue desulfurization sulfur ammonium is provided, to improve the purity of ammonium sulfate products.
Above-mentioned purpose of the present invention is achieved through the following technical solutions, and it comprises the following steps:
(1) flue gas desulfurization byproduct sulphur ammonium is added in the reactor with stirring rake, the water that adds 1.5 ~ 4 times of sulphur ammonium quality stirs, 20 ~ 80 ℃ of dissolvings, after dissolving, add wherein a kind of as scavenging agent of diatomite, gac, white carbon black, modified coal ash, the consumption of scavenging agent is 0.5 ~ 5% of sulphur ammonium quality, stir 10 ~ 25min, ammonium sulfate solution is carried out to purification and decoloration, and standing 5 ~ 30 min, filter;
(2) get filtrate and concentrated under 0.0 ~ 0.085MPa condition in vacuum tightness, be concentrated to solution and epitaxial occurs, stop heating concentrated;
(3) adopt the programmed cooling mode, decrease temperature crystalline, mixing speed is 200 ~ 400rpm, and rate of temperature fall is 2 ~ 8 ℃/h, and the cooling terminal temperature is 24 ~ 36 ℃, filters, and drying, obtain the lenticular ammonium sulfate products.
It is simple that the present invention has technical process, workable, easily industrialization, the advantage such as production cost is low, and product particle is large, foreign matter content is few.
The accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
embodiment 1
Getting 50.0g flue gas desulfurization byproduct sulphur ammonium adds in the reactor with stirring rake, with 75g water 80 ℃ of stirring and dissolving, after dissolving, add the 2.5g white carbon black to stir 15min, standing 5 min, filter, be to concentrate under the 0.085MPa condition until epitaxial appears in concentrated solution filtrate in vacuum tightness, concentrated solution is adopted to programmed cooling mode, decrease temperature crystalline, mixing speed is 300rpm, rate of temperature fall is 6 ℃/h, and the cooling terminal is 24 ℃, filters, dry, obtain the lenticular ammonium sulfate products, products obtained therefrom purity is high, and foreign matter content is few, crystal grain is large
Fe 3+the concentration clearance has reached 92.2%, and the water-insoluble clearance has reached 98.5%.
embodiment 2
Getting 50.0g flue gas desulfurization byproduct sulphur ammonium adds in the reactor with stirring rake, with 200g water 20 ℃ of stirring and dissolving, after dissolving, add 0.025g diatomite to stir 25min, standing 15 min, filter, be to concentrate under the 0.065MPa condition until epitaxial appears in concentrated solution filtrate in vacuum tightness, concentrated solution is adopted to programmed cooling mode, decrease temperature crystalline, mixing speed is 200rpm, rate of temperature fall is 2 ℃/h, and the cooling terminal is 36 ℃, filters, dry, obtain the lenticular ammonium sulfate products, products obtained therefrom purity is high, and foreign matter content is few, crystal grain is large
Fe 3+the concentration clearance has reached 91.3%, and the water-insoluble clearance has reached 96.2%.
embodiment 3
Getting 50.0g flue gas desulfurization byproduct sulphur ammonium adds in the reactor with stirring rake, with 100g water 40 ℃ of stirring and dissolving, after dissolving, add the 1.2g gac to stir 10min, standing 20 min, filter, be to concentrate under the 0.0MPa condition until epitaxial appears in concentrated solution filtrate in vacuum tightness, concentrated solution is adopted to programmed cooling mode, decrease temperature crystalline, mixing speed is 400rpm, rate of temperature fall is 8 ℃/h, and the cooling terminal is 30 ℃, filters, dry, obtain the lenticular ammonium sulfate products, products obtained therefrom purity is high, and foreign matter content is few, crystal grain is large, Fe 3+the concentration clearance has reached 90.1%, and the water-insoluble clearance has reached 97.3%.
embodiment 4
Getting 50.0g flue gas desulfurization byproduct sulphur ammonium adds in the reactor with stirring rake, with 150g water 60 ℃ of stirring and dissolving, after dissolving, add the 1.8g modified coal ash to stir 20min, standing 30 min, filter, by filtrate, in vacuum tightness, be under the 0.045MPa condition, to concentrate until epitaxial appears in concentrated solution, concentrated solution is adopted to the programmed cooling mode, decrease temperature crystalline, mixing speed is 250rpm, rate of temperature fall is 4 ℃/h, the cooling terminal is 28 ℃, filter, dry, obtain the lenticular ammonium sulfate products, products obtained therefrom purity is high, foreign matter content is few, crystal grain is large, Fe 3+the concentration clearance has reached 90.8%, and the water-insoluble clearance has reached more than 94.7%.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, any technical solution of the present invention content that do not break away from, any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all still belong in the scope of this bright technical scheme.

Claims (5)

1. the method for a flue desulfurization sulfur ammonium, comprise the steps:
(1) by flue gas desulfurization byproduct sulphur ammonium, add water and stir, at 20 ~ 80 ℃, dissolved, add scavenging agent after dissolving, and stir 10 ~ 25min, standing 5 ~ 30 min, filter;
(2) get filtrate, concentrated under 0.0 ~ 0.085MPa condition in vacuum tightness, be concentrated to solution and epitaxial occurs, stop heating concentrated;
(3) adopt the programmed cooling mode, to the concentrated solution decrease temperature crystalline, be down to 24 ~ 36 ℃, filter, drying, obtain the lenticular ammonium sulfate products.
2. the method for flue desulfurization sulfur ammonium according to claim 1, the quality that it is characterized in that the water in step (1) is 1.5 ~ 4 times of sulphur ammonium quality; Scavenging agent is wherein a kind of of diatomite, gac, white carbon black, modified coal ash.
3. according to the method for claim 1,2 described flue desulfurization sulfur ammoniums, the consumption that it is characterized in that the scavenging agent of step (1) is 0.5 ~ 5% of sulphur ammonium quality.
4. the method for flue desulfurization sulfur ammonium according to claim 1, is characterized in that the mixing speed of crystallization in step (3) is 200 ~ 400 rpm.
5. the method for flue desulfurization sulfur ammonium according to claim 1, is characterized in that the rate of temperature fall of step (3) Program cooling is 2 ~ 8 ℃/h.
CN2013101011719A 2013-03-27 2013-03-27 Method for purifying ammonium sulfate generated in flue gas desulfurization Pending CN103145149A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103708502A (en) * 2014-01-03 2014-04-09 武汉科技大学 Method for purifying ammonium sulfate serving as desulfuration byproduct
CN103771455A (en) * 2014-01-08 2014-05-07 瓮福(集团)有限责任公司 Method for preparing large particle ammonium sulfate from ardealite
CN104475050A (en) * 2014-11-13 2015-04-01 安徽凤凰滤清器股份有限公司 Activated carbon diatomite particles capable of rapid purification of flue gas and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1066826A (en) * 1996-08-29 1998-03-10 Chiyoda Corp Flue gas desulfurization method and apparatus therefor
CN102674398A (en) * 2012-05-11 2012-09-19 北京旭阳化工技术研究院有限公司 Method for recovering ammonium sulfate and ammonium thiocyanate from desulfuration waste liquor
CN102976361A (en) * 2012-12-10 2013-03-20 北京旭阳化工技术研究院有限公司 Method for extracting high-purity ammonium thiocyanate and ammonium sulphate from coking desulfurization/decyanation waste liquor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1066826A (en) * 1996-08-29 1998-03-10 Chiyoda Corp Flue gas desulfurization method and apparatus therefor
CN102674398A (en) * 2012-05-11 2012-09-19 北京旭阳化工技术研究院有限公司 Method for recovering ammonium sulfate and ammonium thiocyanate from desulfuration waste liquor
CN102976361A (en) * 2012-12-10 2013-03-20 北京旭阳化工技术研究院有限公司 Method for extracting high-purity ammonium thiocyanate and ammonium sulphate from coking desulfurization/decyanation waste liquor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103708502A (en) * 2014-01-03 2014-04-09 武汉科技大学 Method for purifying ammonium sulfate serving as desulfuration byproduct
CN103708502B (en) * 2014-01-03 2015-12-30 武汉科技大学 A kind of method of desulfuration byproduct ammonium sulfate purifying
CN103771455A (en) * 2014-01-08 2014-05-07 瓮福(集团)有限责任公司 Method for preparing large particle ammonium sulfate from ardealite
CN103771455B (en) * 2014-01-08 2015-09-09 瓮福(集团)有限责任公司 A kind of phosphogypsum sulphur ammonium increases the method for sulphur ammonium granularity
CN104475050A (en) * 2014-11-13 2015-04-01 安徽凤凰滤清器股份有限公司 Activated carbon diatomite particles capable of rapid purification of flue gas and preparation method thereof

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Application publication date: 20130612