CN106745064A - A kind of method that ammonium thiocyanate is removed in the crude salt from ammonium sulfate - Google Patents

A kind of method that ammonium thiocyanate is removed in the crude salt from ammonium sulfate Download PDF

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Publication number
CN106745064A
CN106745064A CN201611046411.XA CN201611046411A CN106745064A CN 106745064 A CN106745064 A CN 106745064A CN 201611046411 A CN201611046411 A CN 201611046411A CN 106745064 A CN106745064 A CN 106745064A
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CN
China
Prior art keywords
ammonium
ammonium sulfate
crude salt
liquid
thiocyanate
Prior art date
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Pending
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CN201611046411.XA
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Chinese (zh)
Inventor
郑翠红
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Anhui University of Technology AHUT
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Anhui University of Technology AHUT
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Publication date
Application filed by Anhui University of Technology AHUT filed Critical Anhui University of Technology AHUT
Priority to CN201611046411.XA priority Critical patent/CN106745064A/en
Publication of CN106745064A publication Critical patent/CN106745064A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/24Sulfates of ammonium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C3/00Cyanogen; Compounds thereof
    • C01C3/20Thiocyanic acid; Salts thereof
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C3/00Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

A kind of method the invention discloses ammonium thiocyanate is removed in crude salt from ammonium sulfate, belongs to technical field of fine.The method dissolves the ammonium thiocyanate in ammonium sulfate crude salt with ammonium sulfate saturated solution, after centrifuge separates solid and liquid, solid is the ammonium sulfate for removing ammonium thiocyanate, agricultural fertilizer can be directly used as, liquid adds moderate amount of sulfuric acid copper and ammoniacal liquor, generate the cuprous sulfocyanide precipitation of white, after centrifuge separates solid and liquid, liquid continuously adds ammonium sulfate crude salt, the ammonium thiocyanate in dissolving crude salt, such circulate operation.The present invention possesses low production cost, without waste water and dregs waste gas, without heating, and simple and reliable process, the characteristics of remarkable in economical benefits.

Description

A kind of method that ammonium thiocyanate is removed in the crude salt from ammonium sulfate
Technical field
The invention belongs to technical field of fine, and in particular to remove the side of ammonium thiocyanate in a kind of crude salt from ammonium sulfate Method.
Background technology
Domestic many coke-oven plants use HPF sulfur removal technologies desulfuration and decyanation from coal gas, daily must outer a part of desulfurization of row Waste liquid simultaneously keeps the skin wet to keep desulfuration efficiency higher.Desulfurization waste liquor can extract after being processed through Steppecd crystallization and isolate sulphur Ammonium cyanate, three kinds of salt of ATS (Ammonium thiosulphate) and ammonium sulfate, but the general all ammonium thiocyanates containing 1-20% of the ammonium sulfate isolated And the ATS (Ammonium thiosulphate) of 1-16%, referred to as ammonium sulfate crude salt.Because ammonium thiocyanate has larger harmfulness to plant, this A little ammonium sulfate crude salts could be used after must removing ammonium thiocyanate as agricultural fertilizer.
The content of the invention
To overcome the shortcomings of the existing technology, the invention provides the side that ammonium thiocyanate is eliminated from a kind of crude salt from ammonium sulfate Method, to simple and easy to apply, cost of investment is relatively low, the characteristic of three-waste free pollution.
The present invention realizes that the technical scheme of above-mentioned technical purpose is as follows:
The ammonium thiocyanate and ATS (Ammonium thiosulphate) in 2-5 tons of ammonium sulfate crude salt are dissolved with 1 cubic metre of ammonium sulfate saturated solution, from After scheming separates solid and liquid, solid is the ammonium sulfate for removing ammonium thiocyanate, can be directly used as agricultural fertilizer.Added in liquid suitable The amount of the material that amount copper sulphate and ammoniacal liquor, copper sulphate and ammoniacal liquor are added is respectively 95% He of the amount of ammonium thiocyanate material in filtrate 150%, react for:
(NH4)2S2O3+4CuSO4·5H2O+4NH4SCN+6NH3·H2O→4CuSCN↓+2(NH4)2SO3+4(NH4)2SO4+ 23H2O
The cuprous sulfocyanide precipitation of white is generated, after centrifuge separates solid and liquid, every cubic metre of filtrate continuously adds 2-5 tons of ammonium sulfate crude salt, the ammonium thiocyanate in dissolving crude salt, such circulate operation.
The innovation of the art of this patent be with ammonium sulfate saturated solution dissolve ammonium sulfate crude salt in ammonium thiocyanate without Dissolving ammonium sulfate, after centrifuge separates solid and liquid, liquid adds copper sulphate and ammoniacal liquor that ammonium thiocyanate is changed into thiocyanic acid Cuprous precipitation, so as to rhodanate be separated from filtrate, filtrate continues to dissolve the ammonium thiocyanate in ammonium sulfate crude salt.This Patented technology coke-oven plant is processed the ammonium sulfate crude salt produced during desulfurization waste liquor using method simple and easy to apply and removes sulphur Ammonium cyanate, possesses low production cost, without waste water and dregs waste gas, without heating, simple and reliable process, remarkable in economical benefits The characteristics of.
Specific embodiment
Below in conjunction with specific embodiment in detail the present invention is described in detail, but the present invention is not limited to following embodiments.
Embodiment 1
The ammonium sulfate crude salt of certain coke-oven plant offer is provided, is that ammonium thiocyanate content is 18.7wt%, thio sulphur through analysis ingredient Sour ammonium content is 13.5wt%, and ammonium sulphate content is 67.1wt%.10 liters of saturated ammonium sulfate solution when taking room temperature, add the sulfuric acid 20 kilograms of ammonium crude salt, stirring isolates undissolved solid after 30 minutes through centrifuge, is agricultural ammonium sulfate product, through analyzing sulphur Ammonium cyanate content is less than 0.7wt%.The liquid that centrifuge is isolated adds 11.7 kilograms of Salzburg vitriol, 25% industrial ammonia 5.6 liters of (13.33 mol/L), stirring isolates white solid after 30 minutes through centrifuge, is cuprous sulfocyanide product.Centrifugation The liquid that machine is isolated continues to add 20 kilograms of ammonium sulfate crude salt, and stirring is isolated undissolved solid through centrifuge after 30 minutes Body, is agricultural ammonium sulfate product.The liquid that centrifuge is isolated adds 11.7 kilograms of Salzburg vitriol, 25% industrial ammonia 5.6 liters of (13.33 mol/L), stirring isolates white solid after 30 minutes through centrifuge, is cuprous sulfocyanide product.It is above-mentioned Such circulate operation.
Embodiment 2
The ammonium sulfate crude salt of certain coke-oven plant offer is provided, is that ammonium thiocyanate content is 1.8wt%, thiosulfuric acid through analysis ingredient Ammonium content is 3.6wt%, and ammonium sulphate content is 94.0wt%.10 liters of saturated ammonium sulfate solution when taking room temperature, add the ammonium sulfate 50 kilograms of crude salt, stirring isolates undissolved solid after 30 minutes through centrifuge, is agricultural ammonium sulfate product, through analyzing sulphur cyanogen Sour ammonium content is less than 0.5wt%.The liquid that centrifuge is isolated adds 2.8 kilograms of Salzburg vitriol, 25% industrial ammonia 0.15 liter of (13.33 mol/L), stirring isolates white solid after 30 minutes through centrifuge, is cuprous sulfocyanide product.Centrifugation The liquid that machine is isolated continues to add 20 kilograms of ammonium sulfate crude salt, and stirring is isolated undissolved solid through centrifuge after 30 minutes Body, is agricultural ammonium sulfate product.The liquid that centrifuge is isolated adds 2.8 kilograms of Salzburg vitriol, 25% industrial ammonia 0.15 liter of (13.33 mol/L), stirring isolates white solid after 30 minutes through centrifuge, is cuprous sulfocyanide product.It is above-mentioned Such circulate operation.

Claims (1)

1. a kind of method that ammonium thiocyanate is removed in crude salt from ammonium sulfate, it is characterised in that comprise the following steps:
(1) ammonium thiocyanate and ATS (Ammonium thiosulphate) in 2~5 tons of ammonium sulfate crude salts are dissolved with 1 cubic metre of ammonium sulfate saturated solution, from After the heart is separated, solid is the ammonium sulfate for removing ammonium thiocyanate, can be directly used as agricultural fertilizer;
(2) moderate amount of sulfuric acid copper and ammoniacal liquor are added in the liquid that step (1) centrifugation goes out, the cuprous sulfocyanide for generating white sinks Form sediment;
The amount of the material that the copper sulphate and ammoniacal liquor are added is respectively the 95% and 150% of the amount of ammonium thiocyanate material in liquid;
(3) 2~5 tons of ammonium sulfate crude salt, such circulate operation are continuously added in the liquid after step (2) centrifugation.
CN201611046411.XA 2016-11-23 2016-11-23 A kind of method that ammonium thiocyanate is removed in the crude salt from ammonium sulfate Pending CN106745064A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611046411.XA CN106745064A (en) 2016-11-23 2016-11-23 A kind of method that ammonium thiocyanate is removed in the crude salt from ammonium sulfate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611046411.XA CN106745064A (en) 2016-11-23 2016-11-23 A kind of method that ammonium thiocyanate is removed in the crude salt from ammonium sulfate

Publications (1)

Publication Number Publication Date
CN106745064A true CN106745064A (en) 2017-05-31

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114408943A (en) * 2021-11-26 2022-04-29 安徽英瑞骐生物科技有限公司 Method for preparing cuprous thiocyanate nanoparticles through solid-phase synthesis

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101985359A (en) * 2009-07-29 2011-03-16 中国科学院过程工程研究所 Method for preparing thiocyanate and sulfate by utilizing desulfuration waste liquor in coking plant
CN102259894A (en) * 2011-05-27 2011-11-30 山东美科动力有限公司 Comprehensive recovery process of secondary salts from coking plant desulfurization waste liquid
CN102874845A (en) * 2012-10-15 2013-01-16 安徽工业大学 Extraction of ammonium thiocyanate from coking and desulfurization waste liquid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101985359A (en) * 2009-07-29 2011-03-16 中国科学院过程工程研究所 Method for preparing thiocyanate and sulfate by utilizing desulfuration waste liquor in coking plant
CN102259894A (en) * 2011-05-27 2011-11-30 山东美科动力有限公司 Comprehensive recovery process of secondary salts from coking plant desulfurization waste liquid
CN102874845A (en) * 2012-10-15 2013-01-16 安徽工业大学 Extraction of ammonium thiocyanate from coking and desulfurization waste liquid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114408943A (en) * 2021-11-26 2022-04-29 安徽英瑞骐生物科技有限公司 Method for preparing cuprous thiocyanate nanoparticles through solid-phase synthesis
CN114408943B (en) * 2021-11-26 2023-03-10 安徽英瑞骐生物科技有限公司 Method for preparing cuprous thiocyanate nanoparticles through solid-phase synthesis

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Application publication date: 20170531

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