CN103864115B - The method that waste liquid reclaims crude product ammonium thiocyanate produces ammonium thiocyanate - Google Patents
The method that waste liquid reclaims crude product ammonium thiocyanate produces ammonium thiocyanate Download PDFInfo
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- CN103864115B CN103864115B CN201410084846.8A CN201410084846A CN103864115B CN 103864115 B CN103864115 B CN 103864115B CN 201410084846 A CN201410084846 A CN 201410084846A CN 103864115 B CN103864115 B CN 103864115B
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Abstract
The invention discloses a kind of method that waste liquid reclaims crude product ammonium thiocyanate production ammonium thiocyanate, crude product ammonium thiocyanate is added to the water, stirring heats up makes it to dissolve, be warmed up to 50 DEG C-95 DEG C, add the active carbon of 0.3%-2% and the cleaner of 50ppm-500ppm, insulated and stirred 5-60 minute, squeeze into filter press, circulating filtration 5-60 minute, is switched to and in cooling reactor, stirs coolingly, and centrifugation obtains fine work. Technique of the present invention is simple, directly cooling after material decolorization filtering, extremely short in the time of staying of high temperature section, avoid to greatest extent the pyrolytic of ammonium thiocyanate and ATS (Ammonium thiosulphate), Energy Intensity Reduction 60%, efficiency improves 50%, and with low cost, adding of cleaner significantly takes a turn for the better water-insoluble and chromaticity index, the contents on dry basis of the ammonium thiocyanate of output is more than 99%, outward appearance is white crystal, and colourity is less than 25, and water-insoluble and every impurity index all reach rower requirement.
Description
Technical field
The present invention relates to the energy-efficient new method of a kind of crude product ammonium thiocyanate reclaiming taking desulfuration and decyanation waste liquid as raw material production high-quality ammonium thiocyanate, belong to chemical technology field.
Background technology
What at present domestic a lot of coal chemical enterprise coke-oven-gas desulfurization and decyanations adopted is HPF method, the desulfuration and decyanation waste liquid producing cannot be arranged outward because of seriously polluted, the desulfuration and decyanation waste liquid that mostly started is carried salt device, the ammonium thiocyanate that the inside is rich in is reclaimed, but due to investment, the limitation of age and technology, it is all relatively backward three phase separation technology that a lot of enterprises take, although the rhodanate in desulfurization holder cyanogen waste liquid is reclaimed, but it is relatively poor to put forward product salt quality, the ammonium thiocyanate content of separating is mostly lower than 95%, contain in addition: ATS (Ammonium thiosulphate) 0.2%-5%, ammonium sulfate 0.2-5%, because not meeting industrial products index, cannot be sold to terminal client, customers are limited, price is lower.
And the main purification technique of crude product ammonium thiocyanate producing for coke-oven plant is at present: crude product ammonium thiocyanate filters through activated carbon decolorizing after dissolving, concentrated afterwards, cooling, crystallization, product after centrifugation, although the method can be brought up to the contents on dry basis of ammonium thiocyanate more than 98%, although product can be sold reluctantly, but due to long evaporation and concentration, inevitably make ammonium thiocyanate, ATS (Ammonium thiosulphate) is decomposed, produce water-fast particle and floccule, cause water-insoluble to increase, colourity and the water-insoluble index of product are affected, product quality does not obtain raising in essence, if colourity is all up to more than 200, water insoluble matter content is too high, aqueous solution muddiness, and owing to adopting evaporating and concentrating process, energy consumption is higher, production cycle is longer, the method still has significant limitation
How to find more energy-efficient, and make ammonium thiocyanate product mass-energy obtain essence promote new method, be a new research topic.
Summary of the invention
The technical issues that need to address of the present invention are just to overcome the defect of prior art, provide a kind of waste liquid to reclaim the method for crude product ammonium thiocyanate production ammonium thiocyanate, technique of the present invention is simple, compared with conventional method, remove " evaporation and concentration " this high energy consumption, macrocyclic production unit process, directly cooling after material decolorization filtering, the time of staying in high temperature section is extremely short, avoid to greatest extent the pyrolytic of ammonium thiocyanate and ATS (Ammonium thiosulphate), Energy Intensity Reduction 60%, efficiency improves 50%, and with low cost, adding of cleaner significantly takes a turn for the better water-insoluble and chromaticity index, the contents on dry basis of the ammonium thiocyanate of output is more than 99%, outward appearance is white crystal, colourity is less than 25, water-insoluble and every impurity index all reach rower requirement.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of method that waste liquid reclaims crude product ammonium thiocyanate production ammonium thiocyanate, described method is:
The crude product ammonium thiocyanate that desulfuration and decyanation waste liquid reclaims is added to the water, stirring heats up makes it to dissolve, it is 45 DEG C-90 DEG C that adjustment controls to crystalline temperature, continues to be warmed up to 50 DEG C-95 DEG C, adds the active carbon of 0.3%-2% and the cleaner of 50ppm-500ppm, insulated and stirred 5-45 minute, afterwards material is squeezed into filter press by circulating pump, Matter Transfer filters 5-45 minute, after the mechanical admixtures such as filtering active carbon, be switched to and in cooling reactor, stir coolingly, centrifugation obtains fine work.
In the present invention, solution circulation after centrifugation uses 1-6 time, must crude product ammonium thiocyanate after concentrated, removal of impurities, crystallization are centrifugal, and the system of getting back to is refined again.
In the present invention, described cleaner is a kind of reducing substances.
Preferably, in the present invention, described reducing substances is ammonium sulfite, sulfur dioxide, hydrazine hydrate and kin material.
Technique of the present invention is simple, compared with conventional method, remove " evaporation and concentration " this high energy consumption, macrocyclic production unit process, directly cooling after material decolorization filtering, the time of staying in high temperature section is extremely short, avoid to greatest extent the pyrolytic of ammonium thiocyanate and ATS (Ammonium thiosulphate), Energy Intensity Reduction 60%, efficiency improves 50%, and with low cost, adding of cleaner significantly takes a turn for the better water-insoluble and chromaticity index, the contents on dry basis of the ammonium thiocyanate of output is more than 99%, outward appearance is white crystal, colourity is less than 25, water-insoluble and every impurity index all reach rower requirement.
Detailed description of the invention
Embodiment 1
The crude product ammonium thiocyanate 1000g(ammonium thiocyanate that desulfuration and decyanation waste liquid reclaims: 93%; ATS (Ammonium thiosulphate): 0.9% ammonium sulfate: 0.6%) join in the water of 290g, stirring heats up makes it to dissolve, adjustment controls to crystalline temperature and is 55 DEG C degrees Celsius, continue to be warmed up to 65 DEG C, add 0.5% active carbon and the ammonium sulfite of 50PM, insulated and stirred 15 minutes, afterwards material is squeezed into filter press by circulating pump, Matter Transfer filters 15 minutes, after the mechanical admixtures such as filtering active carbon, be switched to and in cooling reactor, stir coolingly, reach after 25 DEG C, centrifugation obtains fine work ammonium thiocyanate 398g, mother liquid recycle. The product contents on dry basis 99.35% obtaining, outward appearance is white crystals body, colourity: 22, the aqueous solution is clarified other index and is all reached rower standard.
Embodiment 2
The crude product ammonium thiocyanate 1000g(ammonium thiocyanate that desulfuration and decyanation waste liquid reclaims: 91.5%; ATS (Ammonium thiosulphate): 1.4% ammonium sulfate: 1.1%) join in the water of 300g, stirring heats up makes it to dissolve, adjustment controls to crystalline temperature and is 53 DEG C degrees Celsius, continue to be warmed up to 65 DEG C, add 0.5% active carbon and the ammonium sulfite of 50PM, insulated and stirred 15 minutes, afterwards material is squeezed into filter press by circulating pump, Matter Transfer filters 15 minutes, after the mechanical admixtures such as filtering active carbon, be switched to and in cooling reactor, stir coolingly, reach after 27 DEG C, centrifugation obtains fine work ammonium thiocyanate 378g, mother liquid recycle. The product contents on dry basis 99.19% obtaining, outward appearance is white crystals body, colourity: 23, the aqueous solution is clarified other index and is all reached rower standard.
In the present embodiment, described cleaner is a kind of reducing substances, as: as ammonium sulfite, sulfur dioxide, hydrazine hydrate and kin material.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment. For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description. Here without also giving exhaustive to all embodiments. And the apparent variation of being amplified out thus or variation are still among protection scope of the present invention.
Claims (2)
1. waste liquid reclaims a method for crude product ammonium thiocyanate production ammonium thiocyanate, it is characterized in that, described method is:
The crude product ammonium thiocyanate that desulfuration and decyanation waste liquid reclaims is added to the water, stirring heats up makes it to dissolve, it is 45 DEG C-90 DEG C that adjustment controls to crystalline temperature, continues to be warmed up to 50 DEG C-95 DEG C, adds the active carbon of 0.3%-2% and the cleaner of 50ppm-500ppm, insulated and stirred 5-45 minute, afterwards material is squeezed into filter press by circulating pump, Matter Transfer filters 5-45 minute, after filtering active carbon, be switched to and in cooling reactor, stir coolingly, centrifugation obtains fine work;
Described cleaner is ammonium sulfite, sulfur dioxide or hydrazine hydrate.
2. the method that waste liquid as claimed in claim 1 reclaims crude product ammonium thiocyanate and produces ammonium thiocyanate, is characterized in that, the solution circulation after centrifugation uses 1-6 time, after concentrated, removal of impurities, crystallization are centrifugal, obtains crude product ammonium thiocyanate, and the system of getting back to is refined again.
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| CN103864115B true CN103864115B (en) | 2016-05-04 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034349A (en) * | 1988-01-21 | 1989-08-02 | 化学工业部上海化工研究院 | The recovery method of ammonium thiocyanate |
| CN102126732A (en) * | 2011-01-23 | 2011-07-20 | 陈琳 | Method for extracting ammonium thiocyanate from coking desulfurization waste liquid |
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- 2014-03-10 CN CN201410084846.8A patent/CN103864115B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034349A (en) * | 1988-01-21 | 1989-08-02 | 化学工业部上海化工研究院 | The recovery method of ammonium thiocyanate |
| CN102126732A (en) * | 2011-01-23 | 2011-07-20 | 陈琳 | Method for extracting ammonium thiocyanate from coking desulfurization waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 运用三元相图理论回收煤焦化废水中的硫氰酸铵;袁桂梅等;《应用化工》;20080930;第37卷(第9期);第1070-7073页 * |
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