CN103072950B - Method for extracting high-purity sodium thiocyanate and sodium thiosulfate in gas desulfurization waste salt - Google Patents
Method for extracting high-purity sodium thiocyanate and sodium thiosulfate in gas desulfurization waste salt Download PDFInfo
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Abstract
The invention relates to a method for extracting high-purity sodium thiocyanate and sodium thiosulfate in coal gas desulfurization waste salt. The technical scheme is that the method comprises the following steps: preparing the desulfurization waste salt as well as water and crystal mixed salt into solution, adding activated carbon to discolor, filtering, adding a sodium thiosulfate crystal seed into a filtrate, reducing the temperature to 25-30 DEG C at a speed of 1-3 DEG C/hour after crystallization and filtering to obtain secondary crystallization mother liquor and a sodium thiosulfate crystal with a purity of more than 95 weight percent; then adding a sodium thiocyanate crystal seed into the secondary crystallization mother liquor, adding a solventing-out agent at a velocity flow of 1-10 mL/min after crystallization and filtering to obtain tertiary crystallization mother liquor and a sodium thiocyanate crystal with a purity of more than 95 weight percent; and then evaporating and crystallizing the tertiary crystallization mother liquor to obtain the crystal mixed salt. The method has the characteristics of simple process, mild operation condition, low production cost, easiness in realizing large-scale production and high quality.
Description
Technical field
The invention belongs to industrial solid castoff and process and resource technology field, be specifically related to extract in a kind of coal gas desulfurization abraum salt the method for high purity Sodium Thiocyanate 99 and Sulfothiorine.
Background technology
H in coke-oven gas
2s and HCN have stronger corrodibility, also easily cause synthesis gas reaction poisoning of catalyst; During as industry and domestic fuel, the SO in discharging waste gas
2and NO
xmust the strict environomental pollution source of controlling.At present, common coke-oven-gas desulfurization and decyanation adopts Wet-type oxidation sweetening technique more: first utilize the H in alkali liquor absorption coal gas
2s and HCN, then under the katalysis of oxygen carrier, by the H absorbing
2s is oxidized to elemental sulfur, then regeneration of absorption solution circulation.But in Wet-type oxidation sweetening decyanation technology process, can there are some side reactions and generate thiocyanate-, thiosulphate, vitriol etc., these industrial secondary salts can the enrichment gradually along with the circulation of doctor solution, cause the viscosity of desulphurization circulating liquid to increase, and then causing regenerator column, absorption tower, heat-exchange equipment resistance to increase, desulfuration efficiency reduces.In order to ensure the steady running of Wet-type oxidation sweetening decyanation technology, in the time that running up to a certain degree, the industrial secondary salt concentration in desulphurization circulating liquid has two large class methods of disposal, one large class is that direct extension desulphurization circulating liquid is carried salt, or high temperature pyrolysis (burning); Another large class is that these industrial secondary salts are separated from desulphurization circulating liquid, obtains so-called desulfurization abraum salt.Obviously, last class method of disposal process complexity is high, is mainly applicable to large-scale gas purification enterprise; Then a class method of disposal is simple, is applicable to some middle-size and small-size gas purification enterprises.
Desulfurization abraum salt is the filemot solid mixture with bad smell, wherein main component is Sodium Thiocyanate 99 (30 ~ 55wt%) and Sulfothiorine (40 ~ 65wt%), if but desulfurization alkali source is while being ammonia, the main component of desulfurization abraum salt is ammonium thiocyanate and ammonium thiosulfate.At present, the desulfurization abraum salt of many middle-size and small-size coal gas desulfurization decyanation enterprises is all to store up as industrial solid castoff, and both contaminate environment, occupy again factory building.But the main component Sodium Thiocyanate 99 in desulfurization abraum salt and Sulfothiorine are important Chemicals.Sodium Thiocyanate 99 not only can be used for acryl fibre spin solvent, chemical analysis reagent, colour cinefilm irrigation, certain plants defoliating agent and airport roadway weedkiller, also can be used for pharmacy, printing and dyeing, rubberized, black nickel plating and manufacture artificial mustard oil etc.Sodium Thiocyanate 99 is also the good mould sanitas that presses down, and share in raw milk fresh-keeping with hydrogen peroxide.At present, the highly purified NaSCN market requirement is very large, but chemosynthesis NaSCN needs highly purified HCN, and production cost is higher.Sulfothiorine can be used for fixing salt, the dechlorinating agent of cotton goods and association with pulp bleaching, washing composition, sterilizing agent and decolourant in medicine industry, and chemical analysis reagent.Therefore, separating-purifying high purity Sodium Thiocyanate 99 and Sulfothiorine from desulfurization abraum salt, be the effective way of disposal of resources industrial solid castoff desulfurization abraum salt, has important economic benefit and environmental benefit.
At present, existing patented technology focuses mostly in direct separation and Extraction Sodium Thiocyanate 99 and thiosulphate from desulfurization waste liquor, and such technique generally first adopts activated carbon decolorizing, evaporation concentration, multistep crystallization.Patent CN 102259894 A disclose the method for desulfurization abraum salt separation and Extraction vitriol, but the content of vitriol in desulfurization abraum salt is less.
Summary of the invention
The present invention is intended to overcome prior art defect; object is to provide a kind of low method taking coal gas desulfurization abraum salt as main raw material separation and Extraction high purity Sodium Thiocyanate 99 and Sulfothiorine with being easy to large-scale production of production cost; not only size-grade distribution is concentrated for the Sulfothiorine obtaining by the method and Sodium Thiocyanate 99 crystal product, controlled, any surface finish of mean particle size and good fluidity, and purity is high.
For achieving the above object, the concrete steps of the technical solution used in the present invention are:
Step 1, first the thick sodium salt of gained solids mixing in desulfurization abraum salt, water and step 4 is mixed with to solution, in gained solution, the concentration of Sodium Thiocyanate 99 is 30 ~ 50wt%, and the concentration of Sulfothiorine is 45 ~ 65wt%; Under the speed conditions of normal pressure, 40 ~ 60 DEG C and 300～500r/min, add while stirring the gac that accounts for desulfurization abraum salt 3 ~ 5wt% again, insulated and stirred decolouring 0.5 ~ 1h; Then under 40 ~ 60 DEG C of conditions, filter, with the water washings of 10 ~ 30 DEG C 1 ~ 2 time, gained filtrate I is primary crystallization mother liquor.
Step 2, first under the speed conditions of normal pressure, 40 ~ 60 DEG C and 300～500r/min, in the primary crystallization mother liquor of preparing to step 1, add the Sulfothiorine crystal seed that accounts for desulfurization abraum salt 0.5 ~ 1.5wt%, insulated and stirred growing the grain 15 ~ 30min, makes and is suspended magma I; Under the speed conditions of normal pressure and 300～500r/min, be cooled to 25 ~ 30 DEG C with the speed of 1 ~ 3 DEG C/h being suspended magma I again; Then filter, gained filtrate II is secondary crystal mother liquor, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes thiosulfuric acid sodium crystal.
Step 3, first under the speed conditions of normal pressure, 25 ~ 30 DEG C and 300～500r/min, in the secondary crystal mother liquor of preparing to step 2, add the Sodium Thiocyanate 99 crystal seed that accounts for desulfurization abraum salt 0.5 ~ 1.5wt%, insulated and stirred growing the grain 15 ~ 30min, makes and is suspended magma II; Under the speed conditions of normal pressure, 25 ~ 30 DEG C and 300～500r/min, add dissolved agent with the speed of 1 ~ 10mL/min to being suspended stream in magma II again, the add-on of dissolved agent is 3 ~ 5 times of quality that add water in step 1; Then filter, gained filtrate III is crystalline mother solution three times, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes Sodium Thiocyanate 99 crystal.
Step 4, be under 0.02 ~ 0.08MPa condition at normal pressure or vacuum tightness, three crystalline mother solution evaporative crystallizations prepared by step 3, filter and obtain the thick sodium salt of solids mixing.
Described coal gas desulfurization abraum salt is the coal gas desulfurization waste liquid from adopting Wet-type oxidation sweetening decyanation technology, to separate the solid waste obtaining, and wherein main component is Sodium Thiocyanate 99 (30 ~ 55wt%) and Sulfothiorine (40 ~ 65wt%).
Described dissolved agent is the one in ethanol and acetone; Described Sodium Thiocyanate 99 crystal and the purity > 95wt% of thiosulfuric acid sodium crystal.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
(1) method taking coal gas desulfurization abraum salt as main raw material separation and Extraction high purity Sodium Thiocyanate 99 and Sulfothiorine involved in the present invention, according to the phase diagram data of our actual measurement, adopt respectively crystallisation by cooling separate sulfur sodium thiosulfate and dilution crystallization separating sodium thiocyanate in differing temps interval and concentration range, the purity > 95wt% of primary crystallization product, and crystalline product size-grade distribution is concentrated, controlled, any surface finish of mean particle size and good product mobility.
(2) method taking coal gas desulfurization abraum salt as main raw material separation and Extraction high purity Sodium Thiocyanate 99 and Sulfothiorine involved in the present invention, in the time of Crystallization Separation Sulfothiorine and Sodium Thiocyanate 99, service temperature is not higher than 60 DEG C, even if final step is carried out evaporative crystallization prepare mixing salt time, owing to having added dissolved agent acetone and the ethanol of boiling point lower than water in system, vaporization temperature obviously reduces, evaporation energy consumption reduces, therefore present method has operational condition gentleness, energy consumption is little, the low feature with being easy to accomplish scale production of production cost, can realize the concentrated processing of desulfurization abraum salt.
(3) method taking coal gas desulfurization abraum salt as main raw material separation and Extraction high purity Sodium Thiocyanate 99 and Sulfothiorine involved in the present invention, in processing consumption industrial by-product abraum salt, highly purified Sulfothiorine and Sodium Thiocyanate 99 crystalline product are prepared, turning waste into wealth, is a kind of effective way of the middle-size and small-size gas purification of disposal of resources enterprise desulfurization abraum salt.
Therefore, it is simple that the present invention has technique, and operational condition gentleness, production cost be low, be easy to the feature of accomplishing scale production and quality product is high.
Brief description of the drawings
Fig. 1 process flow diagram of the present invention
Embodiment
Below in conjunction with embodiment, the invention will be further described, not the restriction to its protection domain.
For avoiding repetition, first the main component unification of the desulfurization abraum salt described in this embodiment is described below: Sodium Thiocyanate 99 (30 ~ 55wt%) and Sulfothiorine (40 ~ 65wt%).In embodiment, repeat no more.
embodiment 1
In coal gas desulfurization abraum salt, extract a method for high purity Sodium Thiocyanate 99 and Sulfothiorine, its concrete steps are:
Step 1, first desulfurization abraum salt, water and crystallized mixed salt are mixed with to solution, wherein the concentration of Sodium Thiocyanate 99 is 30 ~ 40wt%, and the concentration of Sulfothiorine is 55 ~ 65wt%; Under the speed conditions of normal pressure, 40 ~ 50 DEG C and 300～500r/min, add while stirring the gac that accounts for desulfurization abraum salt 3 ~ 4wt% again, insulated and stirred decolouring 0.5 ~ 0.7h; Then under 40 ~ 50 DEG C of conditions, filter, with the water washings of 10 ~ 30 DEG C 1 ~ 2 time, gained filtrate I is primary crystallization mother liquor;
Step 2, first under the speed conditions of normal pressure, 40 ~ 50 DEG C and 300～500r/min, in the primary crystallization mother liquor of preparing to step 1, add the Sulfothiorine crystal seed that accounts for desulfurization abraum salt 0.5 ~ 1.0wt%, insulated and stirred growing the grain 15 ~ 20min, makes and is suspended magma I; Under the speed conditions of normal pressure and 300～500r/min, be cooled to 25 ~ 28 DEG C with the speed of 1 ~ 2 DEG C/h being suspended magma I again; Then filter, gained filtrate II is secondary crystal mother liquor, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes thiosulfuric acid sodium crystal;
Step 3, first under the speed conditions of normal pressure, 25 ~ 28 DEG C and 300～500r/min, in the secondary crystal mother liquor of preparing to step 2, add the Sodium Thiocyanate 99 crystal seed that accounts for desulfurization abraum salt 0.5 ~ 1.0wt%, insulated and stirred growing the grain 15 ~ 20min, makes and is suspended magma II; Under the speed conditions of normal pressure, 25 ~ 28 DEG C and 300～500r/min, add dissolved agent with the speed of 1 ~ 4mL/min to being suspended stream in magma II again, the add-on of dissolved agent is 3 ~ 4 times of quality that add water in step 1; Then filter, gained filtrate III is crystalline mother solution three times, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes Sodium Thiocyanate 99 crystal;
Step 4, under condition of normal pressure, three crystalline mother solution evaporative crystallizations prepared by step 3, gained solid phase prod is crystallized mixed salt.
Described in the present embodiment, dissolved agent is ethanol.The purity > 95wt% of the present embodiment gained Sodium Thiocyanate 99 crystal and thiosulfuric acid sodium crystal.
embodiment 2
In coal gas desulfurization abraum salt, extract a method for high purity Sodium Thiocyanate 99 and Sulfothiorine, its concrete steps are:
Step 1, first desulfurization abraum salt, water and crystallized mixed salt are mixed with to solution, wherein the concentration of Sodium Thiocyanate 99 is 35 ~ 45wt%, and the concentration of Sulfothiorine is 50 ~ 60wt%; Under the speed conditions of normal pressure, 45 ~ 55 DEG C and 300～500r/min, add while stirring the gac that accounts for desulfurization abraum salt 3.5 ~ 4.5wt% again, insulated and stirred decolouring 0.7 ~ 0.9h; Then under 45 ~ 55 DEG C of conditions, filter, with the water washings of 10 ~ 30 DEG C 1 ~ 2 time, gained filtrate I is primary crystallization mother liquor;
Step 2, first under the speed conditions of normal pressure, 45 ~ 55 DEG C and 300～500r/min, in the primary crystallization mother liquor of preparing to step 1, add the Sulfothiorine crystal seed that accounts for desulfurization abraum salt 0.8 ~ 1.3wt%, insulated and stirred growing the grain 20 ~ 25min, makes and is suspended magma I; Under the speed conditions of normal pressure and 300～500r/min, be cooled to 27 ~ 29 DEG C with the speed of 1.5 ~ 2.5 DEG C/h being suspended magma I again; Then filter, gained filtrate II is secondary crystal mother liquor, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes thiosulfuric acid sodium crystal;
Step 3, first under the speed conditions of normal pressure, 27 ~ 29 DEG C and 300～500r/min, in the secondary crystal mother liquor of preparing to step 2, add the Sodium Thiocyanate 99 crystal seed that accounts for desulfurization abraum salt 0.8 ~ 1.3wt%, insulated and stirred growing the grain 20 ~ 25min, makes and is suspended magma II; Under the speed conditions of normal pressure, 27 ~ 29 DEG C and 300～500r/min, add dissolved agent with the speed of 3 ~ 7mL/min to being suspended stream in magma II again, the add-on of dissolved agent is 3.5 ~ 4.5 times of quality that add water in step 1; Then filter, gained filtrate III is crystalline mother solution three times, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes Sodium Thiocyanate 99 crystal;
Step 4, under condition of normal pressure, three crystalline mother solution evaporative crystallizations prepared by step 3, gained solid phase prod is crystallized mixed salt.
Described in the present embodiment, dissolved agent is acetone.The purity > 95wt% of the present embodiment gained Sodium Thiocyanate 99 crystal and thiosulfuric acid sodium crystal.
embodiment 3
In coal gas desulfurization abraum salt, extract a method for high purity Sodium Thiocyanate 99 and Sulfothiorine, its concrete steps are:
Step 1, first desulfurization abraum salt, water and crystallized mixed salt are mixed with to solution, wherein the concentration of Sodium Thiocyanate 99 is 40 ~ 50wt%, and the concentration of Sulfothiorine is 45 ~ 55wt%; Under the speed conditions of normal pressure, 50 ~ 60 DEG C and 300～500r/min, add while stirring the gac that accounts for desulfurization abraum salt 4 ~ 5wt% again, insulated and stirred decolouring 0.8 ~ 1.0h; Then under 50 ~ 60 DEG C of conditions, filter, with the water washings of 10 ~ 30 DEG C 1 ~ 2 time, gained filtrate I is primary crystallization mother liquor;
Step 2, first under the speed conditions of normal pressure, 50 ~ 60 DEG C and 300～500r/min, in the primary crystallization mother liquor of preparing to step 1, add the Sulfothiorine crystal seed that accounts for desulfurization abraum salt 1.0 ~ 1.5wt%, insulated and stirred growing the grain 25 ~ 30min, makes and is suspended magma I; Under the speed conditions of normal pressure and 300～500r/min, be cooled to 28 ~ 30 DEG C with the speed of 2 ~ 3 DEG C/h being suspended magma I again; Then filter, gained filtrate II is secondary crystal mother liquor, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes thiosulfuric acid sodium crystal;
Step 3, first under the speed conditions of normal pressure, 28 ~ 30 DEG C and 300～500r/min, in the secondary crystal mother liquor of preparing to step 2, add the Sodium Thiocyanate 99 crystal seed that accounts for desulfurization abraum salt 1.0 ~ 1.5wt%, insulated and stirred growing the grain 25 ~ 30min, makes and is suspended magma II; Under the speed conditions of normal pressure, 28 ~ 30 DEG C and 300～500r/min, add dissolved agent with the speed of 6 ~ 10mL/min to being suspended stream in magma II again, the add-on of dissolved agent is 4 ~ 5 times of quality that add water in step 1; Then filter, gained filtrate III is crystalline mother solution three times, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes Sodium Thiocyanate 99 crystal;
Step 4, under condition of normal pressure, three crystalline mother solution evaporative crystallizations prepared by step 3, gained solid phase prod is crystallized mixed salt.
Described in the present embodiment, dissolved agent is ethanol.The purity > 95wt% of the present embodiment gained Sodium Thiocyanate 99 crystal and thiosulfuric acid sodium crystal.
embodiment 4
In coal gas desulfurization abraum salt, extract a method for high purity Sodium Thiocyanate 99 and Sulfothiorine, its concrete steps are:
The evaporative crystallization of the present embodiment in the step 4 of embodiment 1 be vacuum tightness be under 0.02 ~ 0.05MPa condition, carry out, all the other are with embodiment 1.
embodiment 5
In coal gas desulfurization abraum salt, extract a method for high purity Sodium Thiocyanate 99 and Sulfothiorine, its concrete steps are:
The evaporative crystallization of the present embodiment in the step 4 of embodiment 2 be vacuum tightness be under 0.03 ~ 0.06MPa condition, carry out, all the other are with embodiment 2.
embodiment 6
In coal gas desulfurization abraum salt, extract a method for high purity Sodium Thiocyanate 99 and Sulfothiorine, its concrete steps are:
The evaporative crystallization of the present embodiment in the step 4 of embodiment 3 be vacuum tightness be under 0.05 ~ 0.08MPa condition, carry out, all the other are with embodiment 3.
Owing to illustrating and describing in detail the preferred embodiments of the invention, the present invention is carried out various amendments and improved will be obvious to those skilled in the art.Therefore, reply the spirit and scope of the invention are carried out the explanation of broad sense, and scope appended claim of the present invention instead of the restriction of specification sheets above.
Claims (4)
1. a method of extracting high purity Sodium Thiocyanate 99 and Sulfothiorine in coal gas desulfurization abraum salt, is characterized in that, specifically completes according to the following steps:
Step 1, first the thick sodium salt of gained solids mixing in desulfurization abraum salt, water and step 4 is mixed with to solution, in gained solution, the concentration of Sodium Thiocyanate 99 is 30 ~ 50wt%, and the concentration of Sulfothiorine is 45 ~ 65wt%; Under the speed conditions of normal pressure, 40 ~ 60 DEG C and 300～500r/min, add while stirring the gac that accounts for desulfurization abraum salt 3 ~ 5wt% again, insulated and stirred decolouring 0.5 ~ 1h; Then under 40 ~ 60 DEG C of conditions, filter, with the water washings of 10 ~ 30 DEG C 1 ~ 2 time, gained filtrate I is primary crystallization mother liquor;
Step 2, first under the speed conditions of normal pressure, 40 ~ 60 DEG C and 300～500r/min, in the primary crystallization mother liquor of preparing to step 1, add the Sulfothiorine crystal seed that accounts for desulfurization abraum salt 0.5 ~ 1.5wt%, insulated and stirred growing the grain 15 ~ 30min, makes and is suspended magma I; Under the speed conditions of normal pressure and 300～500r/min, be cooled to 25 ~ 30 DEG C with the speed of 1 ~ 3 DEG C/h being suspended magma I again; Then filter, gained filtrate II is secondary crystal mother liquor, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes thiosulfuric acid sodium crystal;
Step 3, first under the speed conditions of normal pressure, 25 ~ 30 DEG C and 300～500r/min, in the secondary crystal mother liquor of preparing to step 2, add the Sodium Thiocyanate 99 crystal seed that accounts for desulfurization abraum salt 0.5 ~ 1.5wt%, insulated and stirred growing the grain 15 ~ 30min, makes and is suspended magma II; Under the speed conditions of normal pressure, 25 ~ 30 DEG C and 300～500r/min, add dissolved agent with the speed of 1 ~ 10mL/min to being suspended stream in magma II again, the add-on of dissolved agent is 3 ~ 5 times of quality that add water in step 1; Then filter, gained filtrate III is crystalline mother solution three times, and the water washing of 10 ~ 30 DEG C 1 ~ 2 time for filter cake is dried, and makes Sodium Thiocyanate 99 crystal;
Step 4, be under 0.02 ~ 0.08MPa condition at normal pressure or vacuum tightness, three crystalline mother solution evaporative crystallizations prepared by step 3, filter and obtain the thick sodium salt of solids mixing.
2. in coal gas desulfurization abraum salt according to claim 1, extract the method for high purity Sodium Thiocyanate 99 and Sulfothiorine, it is characterized in that described coal gas desulfurization abraum salt is the coal gas desulfurization waste liquid from adopting Wet-type oxidation sweetening decyanation technology, to separate the solid waste obtaining, wherein main component is: Sodium Thiocyanate 99 is 30 ~ 55wt%, and Sulfothiorine is 40 ~ 65wt%.
3. in coal gas desulfurization abraum salt according to claim 1, extract the method for high purity Sodium Thiocyanate 99 and Sulfothiorine, it is characterized in that described dissolved agent is the one in ethanol and acetone.
4. in coal gas desulfurization abraum salt according to claim 1, extract the method for high purity Sodium Thiocyanate 99 and Sulfothiorine, it is characterized in that described Sodium Thiocyanate 99 crystal and the purity > 95wt% of thiosulfuric acid sodium crystal.
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| CN106006674B (en) * | 2016-05-23 | 2017-11-21 | 定州旭阳科技有限公司 | The method for producing potassium rhodanide, potassium sulfate and ammonium carbonate simultaneously with desulfurization waste liquor |
| CN107814396A (en) * | 2017-11-27 | 2018-03-20 | 云南煤业能源股份有限公司 | A kind of method of PDS desulfurization waste liquors extraction sodium sulfocyanate |
| CN108408740A (en) * | 2018-06-07 | 2018-08-17 | 江苏燎原环保科技股份有限公司 | A method of extracting sodium sulfocyanate from ADA desulfurization waste liquors |
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