CN105540613B - A kind of method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid - Google Patents

A kind of method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid Download PDF

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CN105540613B
CN105540613B CN201510995121.9A CN201510995121A CN105540613B CN 105540613 B CN105540613 B CN 105540613B CN 201510995121 A CN201510995121 A CN 201510995121A CN 105540613 B CN105540613 B CN 105540613B
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ammonium thiocyanate
reaction
potassium
aqueous solution
potassium rhodanide
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CN105540613A (en
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张影
宋香哲
韩永晓
程雪莲
周进辉
张国栋
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Henan Chengxinjiutian Pharmaceutical Chemical Co Ltd
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Henan Chengxinjiutian Pharmaceutical Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C3/00—Cyanogen; Compounds thereof
    • C01C3/20—Thiocyanic acid; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a kind of method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid, it is related to thiocyanic acid salt preparing technical field, the ammonium thiocyanate aqueous solution is made by decolouring, membrane separation concentration in coking desulfurization waste liquor containing ammonium thiocyanate, metathesis reaction is carried out using potassium hydroxide aqueous solution and the ammonium thiocyanate aqueous solution, generate potassium rhodanide and ammoniacal liquor, obtain potassium rhodanide of the purity more than 99% by decolourizing, being dehydrated concentration, separation of solid and liquid, drying successively again.The advantages of present invention is simple and convenient to operate with technique, raw material type is few, side reaction is few, catalyst is not needed, obtained potassium rhodanide product purity is high, potassium rhodanide is prepared using the ammonium thiocyanate contained in coking desulfurization waste liquor, and ammoniacal liquor is made simultaneously as accessory substance, there is the characteristics of cheap cost, environmental protection and energy saving.

Description

A kind of method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid
Technical field
The present invention relates to thiocyanic acid salt preparing technical field, more particularly to one kind to prepare potassium rhodanide with coking waste liquid and join The method for producing ammoniacal liquor.
Background technology
Potassium rhodanate is a kind of chemicals, be mainly used in synthetic resin, insecticidal bactericide, mustard oil, Thiourea and Medicine etc., it is also possible to make chemical reagent, be the common indicator of ferric ion, the cotton-shaped complex compound of blood red is produced after addition； It is also used for preparing thiocyanate salt solution, calibrating ferric ion, copper and silver, urine test, tungsten developer, the finger of the legal titanium of capacity Show agent；It can be used as refrigerant, photograph intensifier.Uncommon for the preparation method of potassium rhodanide, coke-oven plant is carried out to coal gas Contain substantial amounts of ammonium sulfate, ATS (Ammonium thiosulphate) and ammonium thiocyanate during desulfuration and decyanation in caused waste liquid, if by these Waste liquid is used, and carrying out recovery will will play a positive role to environmental protection.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of side that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid Method, the characteristics of being simple and convenient to operate with technique, be particularly suitable for use in using the ammonium thiocyanate extracted from coking desulfurization waste liquor come Prepare potassium rhodanide co-production ammoniacal liquor.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid, step are as follows：
, in the coking desulfurization waste liquor containing ammonium thiocyanate add activated carbon decolourized, the feed liquid after decolouring is passed through again Nanofiltration membrane separation plant, the ammonium sulfate in feed liquid, ATS (Ammonium thiosulphate) are separated with ammonium thiocyanate, after nanofiltration UF membrane Ammonium thiocyanate solution be more pure ammonium thiocyanate solution, then by concentration enrichment be made there is certain density thiocyanic acid Aqueous ammonium；
, using ammonium thiocyanate prepare potassium rhodanide：The ammonium thiocyanate aqueous solution is added dropwise into potassium hydroxide aqueous solution, until The pH of feed liquid is neutrality after reaction, the ammonia water discharged in course of reaction is absorbed ammoniacal liquor is made；Feed liquid after reacting again Decolourize, separation of solid and liquid obtains potassium rhodanide sterling.
Preferably, in step A, addition activated carbon is decolourized in the coking desulfurization waste liquor containing ammonium thiocyanate；Decolourize Feed liquid afterwards passes through nanofiltration membrane separation plant again, and the ammonium sulfate in feed liquid, ATS (Ammonium thiosulphate) are separated with ammonium thiocyanate.
Preferably, the detailed step that potassium rhodanide is prepared in step B is as follows：
（One）Course of reaction：
1）Prefabricated concentration is 30%~55% potassium hydroxide aqueous solution, and concentration is 30% -60% ammonium thiocyanate aqueous solution：
It is 30%~55% that solid potassium hydroxide is mixed according to a certain percentage with water, stirs obtained concentration after being completely dissolved Potassium hydroxide solution；The coking desulfurization waste water containing ammonium thiocyanate is made into concentration by removal of impurities of decolourizing, membrane separation concentration is 30% -60% ammonium thiocyanate aqueous solution；
2) according to mol ratio 1:1, the ammonium thiocyanate aqueous solution is added dropwise into potassium hydroxide aqueous solution, until feed liquid after reaction PH is neutrality, while the ammonia water discharged in course of reaction is absorbed ammoniacal liquor is made；
3) reaction temperature control is at 40~100 DEG C；2~6 hours reaction time；
（Two）Decolorization：
Activated carbon is added after to reaction in feed liquid to be decolourized, bleaching temperature is 20~100 DEG C, and bleaching time is 0.5~3 Hour, the dosage of activated carbon is 1 ‰~8 ‰ of solution total amount after reaction；Decolouring completion is filtered, and it is transparent to obtain achromaticity and clarification The potassium rhodanide aqueous solution；
（Three）Dehydration：
Negative pressure is dehydrated to there is the precipitation of potassium rhodanide solid under feed liquid progress vacuum after decolouring, and feed temperature is 50~100 DEG C, Vacuum is 1~10KPa；
（Four）Separation of solid and liquid process：
The feed liquid that dehydration finishes is cooled to 10~40 DEG C and filtered, and solid potassium rhodanide separating and filtering is come out；
（Five）Dry：
The solid potassium rhodanide wet finished product separated is dried, drying temperature is 2 small in 80~100 DEG C, time When, potassium rhodanide sterling is produced after drying.
It is further preferred that in step（One）In, potassium hydroxide aqueous solution be 40%~50%, the ammonium thiocyanate aqueous solution it is dense Spend for 40%~50%, at 70~100 DEG C, the reaction time is 3~5 hours for reaction temperature control.
It is further preferred that in step（Two）In, bleaching temperature is 40~80 DEG C, and bleaching time is 2~3 hours, activity The dosage of charcoal is 2 ‰~the 6 ‰ of feed liquid total amount.
It is further preferred that in step（Four）In, it is dehydrated the material finished and is cooled to 30~40 DEG C and is filtered.
It is using beneficial effect caused by above-mentioned technical proposal：Coking desulfurization waste liquor containing ammonium thiocyanate is passed through The ammonium thiocyanate aqueous solution is made in activated carbon decolorizing, nanofiltration membrane separation concentration, water-soluble with ammonium thiocyanate using potassium hydroxide aqueous solution Liquid carries out metathesis reaction, generates potassium rhodanide and ammoniacal liquor, then obtained successively by decolourizing, being dehydrated concentration, separation of solid and liquid, drying To potassium rhodanide of the purity more than 99%.The advantages of present invention is simple and convenient to operate with technique, raw material type is few, side reaction It is few, it is not necessary to which that catalyst, obtained potassium rhodanide product purity is high, is made using the ammonium thiocyanate contained in coking desulfurization waste liquor Standby potassium rhodanide, and ammoniacal liquor is made simultaneously as accessory substance, there is the characteristics of cheap cost, environmental protection and energy saving.
Brief description of the drawings
Fig. 1 is the FB(flow block) of the present invention.
Embodiment
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
A kind of FB(flow block) of method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid as shown in Figure 1, step is such as Under：
, in the coking desulfurization waste liquor containing ammonium thiocyanate add activated carbon decolourized, the feed liquid after decolouring is passed through again Nanofiltration membrane separation plant, the ammonium sulfate in feed liquid, ATS (Ammonium thiosulphate) are separated with ammonium thiocyanate, after nanofiltration UF membrane Ammonium thiocyanate solution be more pure ammonium thiocyanate solution, then by concentration enrichment be made there is certain density thiocyanic acid Aqueous ammonium；
, using ammonium thiocyanate prepare potassium rhodanide：The ammonium thiocyanate aqueous solution is added dropwise into potassium hydroxide aqueous solution, until The pH of feed liquid is neutrality after reaction, and the ammonia discharged in course of reaction is collected or ammoniacal liquor is made with water absorption；Again will reaction Feed liquid is decolourized afterwards, separation of solid and liquid obtains potassium rhodanide sterling.
The detailed step that potassium rhodanide is prepared in above-mentioned steps B is as follows：
（One）Course of reaction：
Chemical equation is：
1）Prefabricated potassium hydroxide aqueous solution and the ammonium thiocyanate aqueous solution, by solid potassium hydroxide and water according to a certain percentage Potassium hydroxide solution is made after being completely dissolved in mixing, stirring；Coking desulfurization waste water containing ammonium thiocyanate is cleaned by decolouring, The ammonium thiocyanate aqueous solution is made in membrane separation concentration；Potassium hydroxide aqueous solution concentration is 30%~55%, preferably 40%~50%；Thiocyanic acid Aqueous ammonium concentration is 30%~55%, preferably 40%~50%；
2) according to mol ratio 1:1, the ammonium thiocyanate aqueous solution is added dropwise into potassium hydroxide aqueous solution, until feed liquid after reaction PH is neutrality, while the ammonia water discharged in course of reaction is absorbed ammoniacal liquor is made；
3) reaction temperature control is at 40~100 DEG C, preferably 70~100 DEG C；In 2~6 hours reaction time, preferably 3~5 is small When；
（Two）Decolorization：
Activated carbon is added after to reaction in feed liquid to be decolourized, bleaching temperature is 20~100 DEG C, preferably 40~80 DEG C, is taken off The color time is 0.5~3 hour, and preferably 2~3 hours, the dosage of activated carbon was 1 ‰~8 ‰ of solution total amount after reaction, preferably 2 ‰~6 ‰；Decolouring completion is filtered, and obtains the transparent potassium rhodanide aqueous solution of achromaticity and clarification；
（Three）Dehydration：
Negative pressure is dehydrated to there is the precipitation of potassium rhodanide solid under feed liquid progress vacuum after decolouring, and feed temperature is 50~100 DEG C, Vacuum is 1~10KPa；
（Four）Separation of solid and liquid process：
The feed liquid that dehydration finishes is cooled to 10~40 DEG C and filtered, and preferably 30~40 DEG C, solid potassium rhodanide is separated Filter out；
（Five）Dry：
The solid potassium rhodanide wet finished product separated is dried, drying temperature is 2 small in 80~100 DEG C, time When, potassium rhodanide sterling is produced after drying.
The advantages of present invention is simple and convenient to operate with technique, by the coking desulfurization waste liquor containing ammonium thiocyanate by de- The ammonium thiocyanate aqueous solution is made in color removal of impurities, membrane separation concentration, is answered using potassium hydroxide aqueous solution and the ammonium thiocyanate aqueous solution Decomposition reaction, potassium rhodanide and ammoniacal liquor are generated, then obtain purity by decolourizing, being dehydrated concentration, separation of solid and liquid, drying successively and exist More than 99% potassium rhodanide.Raw material type is few needed for the present invention, and side reaction is few, it is not necessary to catalyst, obtained potassium rhodanide production Product purity is high, and potassium rhodanide is prepared using the ammonium thiocyanate contained in coking desulfurization waste liquor, and ammoniacal liquor is made simultaneously as secondary Product, coking desulfurization waste liquor is reused, there is the characteristics of cheap cost, environmental protection and energy saving.
Specific embodiment is as follows：
Embodiment 1：
Equipped with thermometer, mechanical agitation and dropping funel, reflux condenser（Condenser is followed by ammonia absorption device）'s The potassium hydroxide solution that 100g concentration is 30% is added in flask, the ammonium thiocyanate solution that 67g concentration is 60% is slowly added dropwise, then In 40 DEG C of insulation reactions 6 hours, the ammonia water discharged, which absorbs, was made ammoniacal liquor.Reaction terminates, and adds the work of feed liquid total amount 1 ‰ Property charcoal 20 DEG C decolourize 3 hours, filtering.Filtrate decompression dehydration is until potassium rhodanide solid separates out, and temperature reaches 100 DEG C, vacuum 10Kpa.Then 40 DEG C of filterings are cooled to, is dried within 2 hours in 80 DEG C of drying and obtains potassium rhodanide solid 25.5g, purity 99.5%, Filtrate 51g, potassium rhodanide purity：50%.Potassium rhodanide conversion ratio 99.2%.By-product ammoniacal liquor 45g, purity 20%.
Embodiment 2：
Equipped with thermometer, mechanical agitation and dropping funel, reflux condenser（Condenser is followed by ammonia absorption device）'s The potassium hydroxide solution that 100g concentration is 40% is added in flask, the ammonium thiocyanate solution that 108g concentration is 50% is slowly added dropwise, so Afterwards in 60 DEG C of insulation reactions 5 hours, the ammonia water discharged, which absorbs, is made ammoniacal liquor.Reaction terminates, and adds feed liquid total amount 2 ‰ Activated carbon decolourizes 2 hours at 40 DEG C, filtering.Filtrate decompression dehydration is until potassium rhodanide solid separates out, and temperature reaches 80 DEG C, vacuum 6Kpa.Then 30 DEG C of filterings are cooled to, potassium rhodanide solid 38g, purity 99.5%, filtrate are obtained within 1.5 hours in 90 DEG C of drying 62g, potassium rhodanide purity：50%.Potassium rhodanide conversion ratio 99.8%.By-product ammoniacal liquor 60g, purity 20%.
Embodiment 3：
Equipped with thermometer, mechanical agitation and dropping funel, reflux condenser（Condenser is followed by ammonia absorption device）'s The potassium hydroxide solution that 1000g concentration is 50% is added in flask, the ammonium thiocyanate solution that 1696g concentration is 40% is slowly added dropwise, Then in 70 DEG C of insulation reactions 3 hours, the ammonia water discharged, which absorbs, is made ammoniacal liquor.Reaction terminates, and adds feed liquid total amount 6 ‰ Activated carbon 80 DEG C decolourize 1 hour, filtering.Filtrate decompression dehydration is until potassium rhodanide solid separates out, and temperature reaches 70 DEG C, very Empty 3Kpa.Then 20 DEG C of filterings are cooled to, potassium rhodanide solid 493g, purity 99.5%, filtrate are obtained within 1 hour in 95 DEG C of drying 746g, potassium rhodanide purity：50%.Potassium rhodanide conversion ratio 99.7%.By-product ammoniacal liquor 758g, purity 20%.
Embodiment 4：
Equipped with thermometer, mechanical agitation and dropping funel, reflux condenser（Condenser is followed by ammonia absorption device）'s The potassium hydroxide solution that 1000g concentration is 55% is added in flask, the ammonium thiocyanate solution that 2488g concentration is 30% is slowly added dropwise, Then in 100 DEG C of insulation reactions 2 hours, the ammonia water discharged, which absorbs, is made ammoniacal liquor.Reaction terminates, and adds feed liquid total amount 8 ‰ activated carbon decolourizes 0.5 hour at 100 DEG C, filtering.Until potassium rhodanide solid separates out, temperature reaches for filtrate decompression dehydration 50 DEG C, vacuum 1Kpa.Then 10 DEG C of filterings are cooled to, potassium rhodanide solid 571g, purity are obtained within 1 hour in 100 DEG C of drying 99.5%, filtrate 762g, potassium rhodanide purity：50%.Potassium rhodanide conversion ratio 99.6%.By-product ammoniacal liquor 834g, purity 20%.

Claims (3)

  1. A kind of 1. method that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid, it is characterised in that step is as follows：
    , will in the coking desulfurization waste liquor containing ammonium thiocyanate add activated carbon be decolourized, the feed liquid after decolouring passes through nanofiltration again Membrane separation plant, the ammonium sulfate in feed liquid, ATS (Ammonium thiosulphate) are separated with ammonium thiocyanate, the thiocyanic acid after membrane separation Ammonium salt solution is more pure ammonium thiocyanate solution, then being made by concentration enrichment has certain density ammonium thiocyanate water-soluble Liquid；
    , using ammonium thiocyanate prepare potassium rhodanide：The ammonium thiocyanate aqueous solution is added dropwise into potassium hydroxide aqueous solution, until reaction The pH of feed liquid is neutrality afterwards, the ammonia water discharged in course of reaction is absorbed ammoniacal liquor is made；Feed liquid after reaction is decolourized again, Separation of solid and liquid obtains potassium rhodanide sterling；The step of preparing potassium rhodanide is as follows：
    （One）Course of reaction：
    1）Prefabricated concentration is 30%~55% potassium hydroxide aqueous solution, and concentration is 30% -60% ammonium thiocyanate aqueous solution：
    Solid potassium hydroxide is mixed according to a certain percentage with water, stirs the hydrogen-oxygen for being made that concentration is 30%~55% after being completely dissolved Change potassium solution；By containing ammonium thiocyanate coking desulfurization waste water through decolouring removal of impurities, membrane separation concentration be made concentration be 30%- The 60% ammonium thiocyanate aqueous solution；
    2) according to mol ratio 1:1, the ammonium thiocyanate aqueous solution is added dropwise into potassium hydroxide aqueous solution, until the pH of feed liquid is after reaction Neutrality, while the ammonia water discharged in course of reaction is absorbed ammoniacal liquor is made；
    3) reaction temperature control is at 40~100 DEG C；2~6 hours reaction time；
    （Two）Decolorization：
    Activated carbon is added after to reaction in feed liquid to be decolourized, bleaching temperature is 40~80 DEG C, and bleaching time is 2~3 hours, living Property charcoal dosage for reaction after solution total amount 2 ‰~6 ‰；Decolouring completion is filtered, and obtains the transparent sulphur cyanogen of achromaticity and clarification Sour aqueous solutions of potassium；
    （Three）Dehydration：
    Negative pressure is dehydrated to there is the precipitation of potassium rhodanide solid under feed liquid progress vacuum after decolouring, and feed temperature is 50~100 DEG C, vacuum Spend for 1~10KPa；
    （Four）Separation of solid and liquid process：
    The feed liquid that dehydration finishes is cooled to 10~40 DEG C and filtered, and solid potassium rhodanide separating and filtering is come out；
    （Five）Dry：
    The solid potassium rhodanide wet finished product separated is dried, drying temperature is 2 hours in 80~100 DEG C, time, is dried Potassium rhodanide sterling is produced after dry.
  2. 2. the method according to claim 1 that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid, it is characterised in that：In step Suddenly（One）In, the concentration of potassium hydroxide aqueous solution is 40%~50%, and the concentration of the ammonium thiocyanate aqueous solution is 40%~50%, reaction temperature At 70~100 DEG C, the reaction time is 3~5 hours for degree control.
  3. 3. the method according to claim 1 that potassium rhodanide coproduction ammoniacal liquor is prepared with coking waste liquid, it is characterised in that：In step Suddenly（Four）In, it is dehydrated the feed liquid finished and is cooled to 30~40 DEG C and is filtered.
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CN109052429B (en) * 2018-10-16 2020-04-17 河北诚信九天医药化工有限公司 Production process of high-quality sodium thiocyanate

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CN1062884A (en) * 1990-12-29 1992-07-22 湖南省农药工业公司 Preparation process for high-content sodium rhodanide
JP3412637B2 (en) * 1992-11-19 2003-06-03 日本エクスラン工業株式会社 Recovery of rodan salt
CN101125644A (en) * 2007-08-09 2008-02-20 上海泽因工程设计有限公司 Production technique for reclaiming ammonium thiosulfate and ammonium thiocyanate from desulfurization waste liquor
CN101306885B (en) * 2008-06-30 2010-11-10 南京工业大学 Resource treatment method for coking sulfur-containing wastewater
EP2301886A1 (en) * 2009-09-03 2011-03-30 Ammonia Casale S.A. Waste heat recovery in a chemical process and plant, particularly for the synthesis of ammonia
CN102259896A (en) * 2011-06-21 2011-11-30 安徽工业大学 Method for extracting sodium thiocyanate from coking desulfurization waste liquid
CN102502709A (en) * 2011-11-13 2012-06-20 泰安金塔化工机械有限公司 Method for extracting secondary salt from coking desulphurized waste liquid
CN104071807B (en) * 2014-06-18 2015-11-25 黄进前 The technique of ammonium thiocyanate is extracted from coking desulfurization waste liquor

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