CN203529949U - Device for dilution crystallization of coked rough ammonium sulfate - Google Patents
Device for dilution crystallization of coked rough ammonium sulfate Download PDFInfo
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- CN203529949U CN203529949U CN201320649766.3U CN201320649766U CN203529949U CN 203529949 U CN203529949 U CN 203529949U CN 201320649766 U CN201320649766 U CN 201320649766U CN 203529949 U CN203529949 U CN 203529949U
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- sulphur ammonium
- storage tank
- thick sulphur
- coking
- crystallizer
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Abstract
The utility model particularly relates to a device for dilution crystallization of coked rough ammonium sulfate. The device comprises a rough ammonium sulfate dissolving kettle, a filter, a crystalline mother solution storing tank, a crystallizing tank, a dissolving agent storing tank, a centrifugal separator, a boiling bed dryer, a dissolving agent regeneration tower and pipelines for connecting the equipment. The device has the characteristic of short production period; the ammonium sulfate product using the coked rough ammonium sulfate as the raw material not only is centralized in granularity distribution, controllable in average granularity, bright and clean in surface, high in purity and good in fluidity, but also can reach the specification of the industrial superior product, and is high in yield.
Description
Technical field
The utility model belongs to industrial crystallization technical field, is specifically related to the thick sulphur ammonium of a kind of coking dilution crystallization device.
Background technology
Coked thiamine is large industry byproduct that coke oven gas purification produces.7 meter 63,2 * 65 hole of a JN60-60 type coke oven of producing 2000000 t coke per year, sulphur ammonium output can reach 30,000 t/a.And China's coke output since nineteen ninety-three surely occupies first place in the world always, within 2011, break through 400,000,000 t, therefore the output of domestic coked thiamine is huge.Ammonium sulfate is important nitrogenous fertilizer, industrial agent, food catalyzer, the buffer reagent of also can printing and dyeing, leather deliming agent etc.
At present, most domestic coke-oven plant adopts saturex method to produce sulphur ammonium more.Coked thiamine is because the impact of impurity is often with grey, green, blueness, furvous or redness, and crystallization mostly is needle-like, sheet or Powdered, and the particle of moulding is very little, and median size is no more than 0.5mm; And moisture, acidity exceed standard.The easy moisture absorption of sulphur ammonium crystal caking, large in atmospheric moisture, the little and water content of crystal grain is particularly serious when high.Sulphur ammonium after the moisture absorption is all corrosive to iron and steel, cement and gunnysack etc., easily causes storage, transportation and uses difficulty.
At present, refining general evaporative crystallization or the first evaporative crystallization technique of crystallisation by cooling again that adopts of the thick sulphur ammonium of coking.But no matter evaporative crystallization or crystallisation by cooling, all easily form brilliant dirt at heat exchange surfaces such as coil pipe or chucks, significantly reduce heat transfer efficiency, make vaporator rate or rate of temperature fall wayward, crystallization time extends, thereby cause crystalline product size-grade distribution heterogeneity, production efficiency is low.And, for evaporation and crystal process, in crystallizer, solid-liquid suspension density is more and more higher, brilliant liquid mixes inhomogeneous, crystal easily sinks to the bottom, and the frictional impact between crystal and between crystal and stirring rake causes crystallisation process crystal fracture phenomenon serious, this also can aggravate crystalline product size-grade distribution heterogeneity.In addition, sulphur ammonium is solubleness large (0 ℃, 70g/100g water) in water, no matter evaporative crystallization or crystallisation by cooling, and crystallization at the end also has not crystallization of a large amount of sulphur ammoniums in mother liquor, causes unit volume crystallizer throughput on the low side.
Summary of the invention
The utility model is intended to overcome above-mentioned technological deficiency, the thick sulphur ammonium of a kind of coking dilution crystallization device is provided, this utility model crystallization apparatus has feature with short production cycle, not only concentrate, mean particle size is controlled by size-grade distribution for the ammonium sulfate products that the thick sulphur ammonium of the coking of take is raw material production, any surface finish, purity is high and good fluidity, can reach industrial premium grads specification, and yield is high.
For achieving the above object, the thick sulphur ammonium of the utility model coking dilution crystallization device, specifically comprise thick sulphur ammonium dissolution kettle, strainer, crystalline mother solution storage tank, crystallizer, dissolved agent storage tank, separating centrifuge, fluid bed dryer, dissolved agent regenerator column, between described thick sulphur ammonium dissolution kettle and strainer, between strainer and crystalline mother solution storage tank, between crystallizer and separating centrifuge, between separating centrifuge and fluid bed dryer, by pipeline, be connected respectively, between described crystalline mother solution storage tank and crystallizer, between crystallizer and dissolved agent storage tank, between separating centrifuge and dissolved agent regenerator column, between dissolved agent storage tank and dissolved agent regenerator column, by being provided with the pipeline of pump, be connected respectively.
Described thick sulphur ammonium dissolution kettle is the stirring tank of jacketed.
Described strainer can be plate-and-frame filter press or separating centrifuge.
Described crystalline mother solution storage tank is the storage tank of jacketed, can keep the temperature in storage tank consistent with in thick sulphur ammonium dissolution kettle.
Described crystallizer is the stirring tank of jacketed, interior guide shell and the baffle plate established.
Owing to adopting technique scheme, the utility model compared with prior art has following positively effect:
(1) the related thick sulphur ammonium of the coking dilution crystallization device of the utility model can first add alkali lye and gac in thick sulphur ammonium dissolution kettle, can remove the Al in the thick sulphur ammonium of coking
3+, Fe
3+, the insoluble thing such as the impurity such as arsenic and tar, coke tar refuse, improve ammonium sulfate products look level and purity.
(2) the related thick sulphur ammonium of the coking dilution crystallization device of the utility model, the crystal required degree of supersaturation of growing can regulate and control easily by changing the speed that adds of dissolved agent, and whole dilution crystallization process is less than 8h.And traditional evaporative crystallization or cooling and crystallizing process be due to the crystalline substance dirt forming on heat-transfer surface and coil pipe, evaporation or rate of temperature fall are difficult to control, and crystallization time is longer, therefore the utility model has significantly shortened the production cycle.
(3) the related thick sulphur ammonium of the coking dilution crystallization device of the utility model, avoided the ever-increasing drawback of crystalline mother solution suspension density in evaporative crystallization or crystallisation by cooling process, constantly adding of dissolved agent constantly increases liquid phase volume, the fragmentation of crystal product and clustering phenomena can greatly alleviate, and are conducive to concentrating of Granularity Distribution.
(4) the related thick sulphur ammonium of the coking dilution crystallization device of the utility model, can significantly improve sulphur crystalline ammonium process once through yield.In the time of 0 ℃, the solubleness of sulphur ammonium in water is 70g/100g water, and sulphur ammonium is dissolved in methyl alcohol, ethanol, Virahol, acetone and other organic solvent hardly.Traditional evaporative crystallization and cooling and crystallizing process all adopt water as solvent, also contain not crystallization of a large amount of sulphur ammoniums when crystallization completes in mother liquor, and product yield is lower; The related thick sulphur ammonium of the coking dilution crystallization once through yield of the utility model reaches more than 95%.
(5) the related thick sulphur ammonium of the coking dilution crystallization device of the utility model, dissolved agent regenerator column can be realized recycling of dissolved agent, has effectively saved production cost.
Therefore, the utlity model has production cost feature low and with short production cycle, not only concentrate, mean particle size is controlled by size-grade distribution for the ammonium sulfate products that the thick sulphur ammonium of the coking of take is raw material production, any surface finish, purity is high and good fluidity, can reach industrial premium grads specification, and yield is high.
Accompanying drawing explanation
Fig. 1 is the utility model schematic diagram
Embodiment
Below in conjunction with accompanying drawing the utility model is further explained explanation, the not restriction to its protection domain.
As shown in Figure 1, the thick sulphur ammonium of the coking dilution crystallization device that the utility model is related, comprises thick sulphur ammonium dissolution kettle 1, strainer 2, crystalline mother solution storage tank 3, crystallizer 4, dissolved agent storage tank 5, separating centrifuge 6, fluid bed dryer 7, dissolved agent regenerator column 8 and pump 9.Between thick sulphur ammonium dissolution kettle 1 and strainer 2, between strainer 2 and crystalline mother solution storage tank 3, between crystallizer 4 and separating centrifuge 6, be connected by pipeline respectively between separating centrifuge 6 and fluid bed dryer 7, between crystalline mother solution storage tank 3 and crystallizer 4, between crystallizer 4 and dissolved agent storage tank 5, between separating centrifuge 6 and dissolved agent regenerator column 8, be connected by being provided with the pipeline of pump 9 respectively between dissolved agent storage tank 5 and dissolved agent regenerator column 8.
In conjunction with concrete technology operational condition, the thick sulphur ammonium of the related coking of the utility model dilution crystallization device implementation process is described as follows: to the thick sulphur ammonium dissolution kettle thick sulphur ammonium of 1 interior input and water, open thick sulphur ammonium dissolution kettle 1 and stir, and pass into heating steam to the chuck of thick sulphur ammonium dissolution kettle 1; Until thick sulphur ammonium dissolution kettle 1 interior temperature, reach after technique preset temp, to thick sulphur ammonium dissolution kettle 1, interior input NaOH regulates pH=7 ~ 9, then to the interior input gac of thick sulphur ammonium dissolution kettle 1, insulated and stirred 0.5 ~ 1h; Open the valve of thick sulphur ammonium dissolution kettle 1 bottom, strainer 2 centrifugations, filtrate is sent into the crystalline mother solution storage tank 3 of jacketed, keeps crystalline mother solution storage tank 3 consistent with thick sulphur ammonium dissolution kettle 1 interior temperature; With pump, to a certain amount of crystalline mother solution of the interior conveying of crystallizer 4, then add acid regulator, make its mother liquor pH=5 ~ 7; In mother liquor, add crystal habit modifier citric acid and crystal seed again, insulated and stirred growing the grain 15 ~ 30min, by regulating the valve between dissolved agent storage tank 5 and crystallizer 4, adds dissolved agent ethanol with various flows rate of acceleration stage by stage, amount of alcohol added is 6 times of water-content in mother liquor, and it is 7h that stream adds the time; After adding, opens dissolved agent stream crystallizer 4 bottom valves, magma is sent into separating centrifuge 6, the filtrate that separating centrifuge 6 is discharged is sent into dissolved agent regenerator column 8, dissolved agent after regeneration is sent into dissolved agent storage tank 5 in order to recycling, the crystal that separating centrifuge 6 is discharged is sent into fluid bed dryer 7, after dry, obtain sulphur ammonium crystal, sulphur ammonium one way crystallization yield is 96.8%, can reach industrial premium grads specification.
Claims (5)
1. the thick sulphur ammonium of a coking dilution crystallization device, it is characterized in that, specifically comprise thick sulphur ammonium dissolution kettle, strainer, crystalline mother solution storage tank, crystallizer, dissolved agent storage tank, separating centrifuge, fluid bed dryer, dissolved agent regenerator column, between described thick sulphur ammonium dissolution kettle and strainer, between strainer and crystalline mother solution storage tank, between crystallizer and separating centrifuge, between separating centrifuge and fluid bed dryer, by pipeline, be connected respectively, between described crystalline mother solution storage tank and crystallizer, between crystallizer and dissolved agent storage tank, between separating centrifuge and dissolved agent regenerator column, between dissolved agent storage tank and dissolved agent regenerator column, by being provided with the pipeline of pump, be connected respectively.
2. the thick sulphur ammonium of coking as claimed in claim 1 dilution crystallization device, is characterized in that, described thick sulphur ammonium dissolution kettle is the stirring tank of jacketed.
3. the thick sulphur ammonium of coking as claimed in claim 1 dilution crystallization device, is characterized in that, described strainer can be plate-and-frame filter press or separating centrifuge.
4. the thick sulphur ammonium of coking as claimed in claim 1 dilution crystallization device, is characterized in that, described crystalline mother solution storage tank is the storage tank of jacketed.
5. the thick sulphur ammonium of coking as claimed in claim 1 dilution crystallization device, is characterized in that, described crystallizer is the stirring tank of jacketed, interior guide shell and the baffle plate established.
Priority Applications (1)
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CN201320649766.3U CN203529949U (en) | 2013-10-22 | 2013-10-22 | Device for dilution crystallization of coked rough ammonium sulfate |
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CN201320649766.3U CN203529949U (en) | 2013-10-22 | 2013-10-22 | Device for dilution crystallization of coked rough ammonium sulfate |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103908797A (en) * | 2014-04-10 | 2014-07-09 | 攀钢集团西昌钢钒有限公司 | Feeding system and feeding method of crystallizer |
CN108992965A (en) * | 2018-08-17 | 2018-12-14 | 张家港清澄纳米科技有限公司 | A kind of uniform one is hydrated sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process and device |
-
2013
- 2013-10-22 CN CN201320649766.3U patent/CN203529949U/en not_active Expired - Fee Related
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103908797A (en) * | 2014-04-10 | 2014-07-09 | 攀钢集团西昌钢钒有限公司 | Feeding system and feeding method of crystallizer |
CN103908797B (en) * | 2014-04-10 | 2015-12-30 | 攀钢集团西昌钢钒有限公司 | The feed system of crystallizer and feed process |
CN108992965A (en) * | 2018-08-17 | 2018-12-14 | 张家港清澄纳米科技有限公司 | A kind of uniform one is hydrated sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process and device |
CN108992965B (en) * | 2018-08-17 | 2021-07-27 | 张家港清澄纳米科技有限公司 | Continuous cooling crystallization preparation process and device for large particles of uniform sodium hypophosphite monohydrate |
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C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140409 Termination date: 20141022 |
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EXPY | Termination of patent right or utility model |