CN1098805C - Improvement of production method of sodium thiosulfate - Google Patents
Improvement of production method of sodium thiosulfate Download PDFInfo
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- CN1098805C CN1098805C CN99116880A CN99116880A CN1098805C CN 1098805 C CN1098805 C CN 1098805C CN 99116880 A CN99116880 A CN 99116880A CN 99116880 A CN99116880 A CN 99116880A CN 1098805 C CN1098805 C CN 1098805C
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- sulfothiorine
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Abstract
The present invention discloses a process improvement for preparing sodium thiosulfate by using alkali wastewater reduced by sodium sulfide as an aromatic nitro compound as a raw material, which comprises: non-settled oxidated materials, non-settled materials after decolorization of activated carbon and non-settled materials after evaporating concentration are completely and directly introduced into a filter press and filtered; crystalline water containing sodium thiosulfate contained in a filter cake is filtered out with saturated steam and/or hot water of higher than 95DEG C to activate active carbon residues. The activated active carbon residues can be reused in the working procedure of decolorization.
Description
The present invention relates to the production method of mineral compound, specifically is a kind of production method of Sulfothiorine.
Sulfothiorine popular name sodium thiosulfate is used in industries such as photograph, process hides, papermaking, weaving in a large number, and in agricultural chemicals, dyestuff etc. synthetic.
In prior art, the production method of Sulfothiorine, the method that from waste liquid, reclaims in commercial most employing, for example: from the factory effluent of sulphur black or other thioxine dyes by filtration, activated carbon decolorizing, filtrate concentrate, crystallization, centrifugation reclaim the five water Sulfothiorine that obtain purity about 96%.For another example, alkaline waste water with the aromatic nitro compound sodium sulfide reducing is a raw material, by add sulphur, oxidation, filtration, concentrate, to obtain purity be 96% five water Sulfothiorine raw product for heat filtering, activated carbon decolorizing, filtration, crystallization, centrifugation for the first time.It is five water Sulfothiorine industrial goods more than 98% that raw product dissolving, activated carbon decolorizing, filtration, crystallization, centrifugation are for the second time obtained purity.Again with industrial goods dissolvings, activated carbon decolorizing for the third time, it is photographic-grade five water Sulfothiorine more than 99% that filtration, crystallization, centrifugation obtain purity.
Alkaline waste water with the aromatic nitro compound sodium sulfide reducing is the prior art of five water Sulfothiorine of raw material production photographic-grade, except its two roads master operation adds sulphur, the oxidation, also needs through at least three activated carbon decolorizings and five filtration operations, producing a large amount of waste residues that contains Sulfothiorine and breeze thus needs to handle, as the breeze behind heat filtering slag after oxide slag, the evaporation concentration and three activated carbon decolorizings, singly amount is not big for these waste residues and breeze, and difficulty.How reclaiming Sulfothiorine contained in waste residue and the breeze to greatest extent, reduce the quantity of waste residue generation and the gac in the regeneration breeze as far as possible, to overcome the existing above-mentioned defective of prior art, is the problem that the inventor faces.
For this reason, the inventor is that the production method of raw material production Sulfothiorine has been done a large amount of research and improvement to the alkaline waste water with the aromatic nitro compound sodium sulfide reducing.Discover in prior art, alkaline waste water with the aromatic nitro compound sodium sulfide reducing is in the method for raw material production Sulfothiorine, and the material of the heat filtering of the material of oxidation operation and evaporation concentration operation and the material of activated carbon decolorizing operation all adopt the partly filtering technology of sedimentation.
As everyone knows, aromatic amine compound is oxidation very easily, and the time is grown the easier tarry polymer substance that aggregates into slightly, and its result not only makes filtration difficulty, and filter wash cloth is wanted in per tour, and the waste residue amount is big, and Sulfothiorine contained in the waste residue is also quite high.Therefore, the heat filtering material of the material of oxidation operation, evaporation concentration operation and the material of activated carbon decolorizing operation are without sedimentation, take directly all to enter the filtering method of pressure filter, can avoid the generation of tarry materials as far as possible, found that not single-filtering efficient height, waste residue is few, Sulfothiorine impure few, quality and yield all increase, and poisoning when having exempted sediment and needing regularly (5-7 days) manually to go out residual pin and operative employee's hard work.
The good decolorizing effect of gac, but price is more expensive, and a large amount of uses certainly will influence the industrial cost of Sulfothiorine.Be used to the gac that decolours in traditional method, throw aside after the decolouring, real is very big loss.Though waste active carbon can be with the calcination method in 850 ℃ of-900 ℃ of thermal regenerations, its adsorption activity is still undesirable.Trace it to its cause, remove through calcination though may be organism, inorganics (being mainly Sulfothiorine) adsorbed in the gac still exists, and will influence its further performance adsorption and decoloration.The inventor is through discovering repeatedly, in the life of this product in this process of producing product, gac after the decolouring, by reduce to hot wash to sodium thiosulfate content more than 95 ℃ lower level (＜1%〉time, the activity of gac obtains regeneration, and its decolorizing ability can reach or the approaching gac level of newly purchasing.Find simultaneously at the above-mentioned oxide compound waste residue of press filtration, when heat filtering slag and breeze, easily produce grain during owing to the thiosulfuric acid sodium cooling, the eyelet of filter cloth will be stopped up, make filtration velocity more and more slower, per tour must be cleaned filter cloth, and the waste water of generation and operative employee's labour intensity increase greatly.The inventor takes to feed saturation steam extruding filter cake in pressure filter, with the hot wash filter cake more than 95 ℃, the contained Sulfothiorine that contains crystal water will be molten state and leach in the filter cake, not only filtration velocity is fast, and contained Sulfothiorine also reduces significantly in level of residue and the residue, per tour can be washed or filter wash cloth not less, greatly reduces the quantity and the unit consumption that produce waste water.Simultaneously, be surprised to find, the breeze that the decolouring after-filtration produces is through after feeding saturation steam and the hot wash more than 95 ℃, the content of Sulfothiorine reduced to very low level (＜1% 〉, and the activity of breeze has obtained regeneration, its decolorizing ability near or reach the level of newly purchasing gac, fully can recycle in bleaching process.
The object of the present invention is to provide a kind of production method of Sulfothiorine.
Above-mentioned purpose of the present invention realizes in the following manner: a kind of production method of Sulfothiorine, comprise that alkaline waste water with the aromatic nitro compound sodium sulfide reducing is as raw material, by adding sulphur, oxidation, filter, evaporation concentration, heat filtering, activated carbon decolorizing, filter, crystallization, centrifugal separation process, it is characterized in that described being filtered into: with the material of described oxidation operation, material and the material behind the activated carbon decolorizing after the evaporation concentration all enter the pressure filter direct filtration without sedimentation, filter cake in the pressure filter is molten state with saturated vapo(u)r and/or the hot water more than 95 ℃ with the Sulfothiorine that contains crystal water contained in the filter cake and leaches, and obtain the active breeze of activatory again reuse in described bleaching process.
It is characterized in that bleaching process carries out three times, with for the second time and the gac filter cake after the decolouring for the third time sodium thiosulfate content is less than 1% to the filter cake through hot wash more than 95 ℃, the active breeze that obtains activating and regenerating is back in the bleaching process again.
It is further characterized in that the active breeze filter cake after the decolouring for the third time behind the activating and regenerating is used for bleaching process for the second time; Active breeze filter cake after the second time behind the activating and regenerating of the decolouring is used for bleaching process for the first time.
Advantage of the present invention is tangible: without sedimentation, the residence time of material significantly shortens, the tarry materials that contained arylamine class oxidation of impurities polymerization is produced in the material significantly reduces, filtration velocity is obviously accelerated, without per tour washing filter cloth, thereby the wastewater flow rate that produces reduces significantly, and the waste residue amount also significantly reduces, and the quality of Sulfothiorine and yield improve a lot; The gac filter residue is used saturation steam and/or gac acquisition activation after the hot wash more than 95 ℃, its decolorizing ability of gac after the regeneration near or reach the level of newly purchasing gac, can be back to fully in the bleaching process of producing this product, thereby having reached that change " give up " is the purpose of treasured.
The present invention is described in further detail below with reference to specific embodiment.
Embodiment 1:
With the scale production Sulfothiorine of producing 36000 tons (100 ton per days) per year is example, waste water 250 ton per days with the aromatic nitro compound sodium sulfide reducing are raw material, heat sulphur, heated oxide operation according to common process, after oxidation finishes, oxidation material is all entered the pressure filter direct filtration without sedimentation, filter cake 2kg/cm
2Saturation steam the Sulfothiorine that contains crystal water in the filter cake be molten state leach, obtain the Sulfothiorine filtrate of high density, filter cake cleans with the hot water more than 95 ℃ again, filtrate merging enters the evaporation concentration operation, and the residue that press filtration obtains reduces more than 50% than traditional technology, and filtration velocity obviously improves; After an effect, two effects, three-effect evaporation and condensation, material is without sedimentation press filtration while hot, filter cake 2kg/cm in the evaporation concentration operation for filtrate
2Saturation steam the Sulfothiorine that contains crystal water in the filter cake be molten state leach, filter cake cleans with the hot water more than 95 ℃, washing lotion enters the evaporation concentration operation.The Sulfothiorine filtrate of the high density that obtains enters activated carbon decolorizing operation for the first time, and the material behind the activated carbon decolorizing all enters the pressure filter direct filtration without sedimentation, filter cake 2kg/cm for the first time
2Saturation steam the Sulfothiorine that contains crystal water in the filter cake be molten state leach, filter cake is used the hot wash more than 95 ℃ again, washing lotion enters enrichment process, residue is thrown aside, the merging of the Sulfothiorine filtrate of the high density that obtains enters Crystallization Procedure, and obtaining purity through crystallization, centrifugation again is five water Sulfothiorine raw product more than 96%.After the above-mentioned raw product dissolving that obtains, carry out the activated carbon decolorizing second time, the material after the decolouring all enters the pressure filter direct filtration without sedimentation, filter cake 2kg/cm
2Saturation steam the Sulfothiorine that contains crystal water in the cake be molten state leach, the merging of the Sulfothiorine filtrate of the high density that obtains enters Crystallization Procedure, filter cake is used hot water wash more than 95 ℃ again, and sodium thiosulfate content is less than 1% to the filter cake, and washing lotion enters the evaporation concentration operation.The decolorizing ability of the active breeze that obtains (in dried gac) is 90-110, and the gac rate of recovery is 90-95%.Crystallization is after centrifugation obtains purity is five water Sulfothiorine industrial goods more than 98%.After the industrial goods dissolving that obtains, carry out activated carbon decolorizing for the third time, the material after the decolouring all enters the pressure filter direct filtration without sedimentation, filter cake 2kg/cm
2Saturation steam the Sulfothiorine that contains crystal water in the filter cake be molten state leach, the merging of the Sulfothiorine filtrate of the high density that obtains enters Crystallization Procedure, filter cake uses the content of the hot water wash Sulfothiorine to the filter cake more than 95 ℃ less than 1% again, and washing lotion enters the evaporation concentration operation.The decolorizing ability of the active breeze that obtains (in dried gac) is 100-130, and the rate of recovery of gac is 95%, and crystallization is after centrifugation obtains purity at the five water Sulfothiorine of the photographic-grade more than 99%.
Embodiment 2:
Repeat the process of embodiment 1, except the used gac of the activated carbon decolorizing operation first time is used instead from the regeneration activity breeze that the second time, the activated carbon decolorizing operation reclaimed, the used gac of activated carbon decolorizing operation is used the active breeze of the activating and regenerating of activated carbon decolorizing operation recovery for the third time instead for the second time, the not enough gac of newly purchasing of partly using is supplied, and the used gac of activated carbon decolorizing operation is still used outside the gac of newly purchasing (decolorizing ability is 130) for the third time, the quantity of resulting five water Sulfothiorine is identical with embodiment 1 with quality, and the unit consumption of gac has saved about 60%, quality and yield that the quantity of waste residue has reduced about 50%, five water Sulfothiorine compared with prior art all increase.
Embodiment 3:
Repeat the process of embodiment 2, except will be for the second time and the active breeze after the decolouring for the third time without the saturation steam purge, sodium thiosulfate content is less than 1% to the filter cake only to use hot wash more than 95 ℃, washing lotion enters the evaporation concentration operation.The rate of recovery and the decolorizing ability of the active breeze that obtains are as follows: the gac of recyclable 90% quantity of active slag after decolouring from the second time, and decolorizing ability is 90-110 (in a dried gac); The gac of recyclable 95% quantity of active breeze after the decolouring for the third time, decolorizing ability is 100-130 (in a dried gac).The quantity of the five water Sulfothiorine that obtain is identical with embodiment 1 or 2 with quality.
In the above-described embodiments,, reclaim activatory gac 550-600kg every day, count 180 tons the whole year by improvement to the prior art production method; Simultaneously, the Sulfothiorine yield improves 10-15%, and the foreign matter content in its quality index also descends to some extent.
Above-mentioned elaboration and embodiment only for illustrative purposes, protection scope of the present invention will embody in the claims.
Claims (3)
1, a kind of production method of Sulfothiorine, comprise that alkaline waste water with the aromatic nitro compound sodium sulfide reducing is as raw material, by adding sulphur, oxidation, filter, evaporation concentration, heat filtering, activated carbon decolorizing, filter, crystallization, centrifugal separation process, it is characterized in that described being filtered into: with the material of described oxidation operation generation, material and the material behind the activated carbon decolorizing after the evaporation concentration all enter the pressure filter direct filtration without sedimentation, filter cake in the pressure filter is molten with saturation steam and/or the hot water more than 95 ℃ with the Sulfothiorine that contains crystal water contained in the filter cake and leaches, and obtain the active breeze of activatory again reuse in described bleaching process.
2, the production method of Sulfothiorine according to claim 1, it is characterized in that bleaching process carries out three times, with for the second time and the gac filter cake after the decolouring for the third time through the content of the Sulfothiorine to the filter cake of hot wash more than 95 ℃ less than 1%, the active breeze by above-mentioned activating and regenerating is back in the bleaching process again.
3, the production method of Sulfothiorine according to claim 2, it is characterized in that the gac filter cake after the decolouring for the third time behind the activating and regenerating is used for bleaching process for the second time, the gac filter cake after the decolouring second time behind the activating and regenerating is used for bleaching process for the first time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99116880A CN1098805C (en) | 1999-09-16 | 1999-09-16 | Improvement of production method of sodium thiosulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99116880A CN1098805C (en) | 1999-09-16 | 1999-09-16 | Improvement of production method of sodium thiosulfate |
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| CN1245775A CN1245775A (en) | 2000-03-01 |
| CN1098805C true CN1098805C (en) | 2003-01-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN99116880A Expired - Fee Related CN1098805C (en) | 1999-09-16 | 1999-09-16 | Improvement of production method of sodium thiosulfate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102895962A (en) * | 2012-05-31 | 2013-01-30 | 山东新华制药股份有限公司 | Activated carbon recycling process in aspirin production |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1284942A1 (en) * | 1984-12-03 | 1987-01-23 | Предприятие П/Я М-5400 | Method of producing sodium thiosulfate |
| CN1031360A (en) * | 1987-08-08 | 1989-03-01 | 渭南市染料化工厂 | From thioxine dyes waste water, reclaim sodium thiosulfate |
| CN1154945A (en) * | 1995-11-24 | 1997-07-23 | 深州市津深联营颜料化工厂 | Method for prepn. of sodium thio sulfate from sodium sulfite contained in waste liquid from production of 2-naphthol |
-
1999
- 1999-09-16 CN CN99116880A patent/CN1098805C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1284942A1 (en) * | 1984-12-03 | 1987-01-23 | Предприятие П/Я М-5400 | Method of producing sodium thiosulfate |
| CN1031360A (en) * | 1987-08-08 | 1989-03-01 | 渭南市染料化工厂 | From thioxine dyes waste water, reclaim sodium thiosulfate |
| CN1154945A (en) * | 1995-11-24 | 1997-07-23 | 深州市津深联营颜料化工厂 | Method for prepn. of sodium thio sulfate from sodium sulfite contained in waste liquid from production of 2-naphthol |
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