CN104311499A - Method for treating chlorine generated in production of metal lithium and application thereof - Google Patents
Method for treating chlorine generated in production of metal lithium and application thereof Download PDFInfo
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- CN104311499A CN104311499A CN201410512755.XA CN201410512755A CN104311499A CN 104311499 A CN104311499 A CN 104311499A CN 201410512755 A CN201410512755 A CN 201410512755A CN 104311499 A CN104311499 A CN 104311499A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/30—Only oxygen atoms
- C07D251/36—Only oxygen atoms having halogen atoms directly attached to ring nitrogen atoms
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Abstract
The invention discloses a method for treating chlorine generated in production of metal lithium and an application thereof. The method for treating chlorine generated in production of metal lithium comprises the following process flows: A, preparing a disodium cyanurate solution; B, carrying out chlorination; C, washing; and D, carrying out neutralization reaction. The method for treating chlorine generated in production of metal lithium disclosed by the invention has the advantages of being simple and practical in process, low in production cost, low in equipment investment, environment-friendly and the like.
Description
Technical field
The present invention relates to a kind for the treatment of process of chlorine, particularly relate to a kind of method processing during metallic lithium is produced the chlorine produced.
The invention still further relates to aforesaid method in the industrial application prepared in the chlorine produced in metallic lithium process of process.
Background technology
Electrolyzing fused lithium chloride, Repone K miscellany are the industrial main method preparing metallic lithium at present, and in preparing metal lithium by electrolyzing molten salt production process, the recycling problem that anode produces chlorine is a difficult problem for lithium Metal smelting industry always.Chlorine chemical property is active, soluble in water, has unpleasant irritating smell, serious harm HUMAN HEALTH, and has serious corrosion to hardware or buildings.The amount of chlorine that lithium electrolytic industry produces in producing is large, should effectively process, qualified discharge, otherwise can greatly welding.
At present, the recovery and treatment method of chlorine generally adopts sodium hydroxide solution absorption process, and the chlorine produced in electrolytic process is introduced reactor by induced draft fan, with sodium hydroxide solution by chlorine absorption preparation time sodium acid sodium, the method assimilation effect is better, after absorbing, and can qualified discharge.But, due to secondary sodium acid sodium solution concentration low (about 10%), very easily decompose (storage temperature≤30 DEG C) and selling price is low, the storage of clorox, transport and sale become the another hang-up of Kun Long enterprise, limit industrial scale, and it is high to result in cost absorption, reduce the profit of enterprise.
Summary of the invention
The present invention completes to solve in prior art problems such as adopting the added value of product of the chlorine technique existence produced in sodium hydroxide solution process metallic lithium production process is low, concentration is low, difficult storage, easily decomposition,
The object of this invention is to provide that a kind of cost is low, features simple and practical process, the added value of product that obtains be high, and the method for chlorine that the metallic lithium of easily Storage Box transport produces in producing.
A kind of method processing during metallic lithium is produced the chlorine produced of the present invention, comprises the following steps:
A. by cyanuric acid and mass percent be the caustic soda soln of 15% ~ 30% in molar ratio for 1:2 drops into reactor, stirring reaction 30 ~ 60min, obtains cyanuric acid two sodium solution;
B. pass into during metallic lithium is produced the chlorine produced in cyanuric acid two sodium solution obtained toward steps A and carry out chlorination reaction, controlling chlorination reaction temperature is 10 ~ 35 DEG C, when the pH of solution reaches 4 ~ 6, stopped reaction, obtains wet DICHLOROISOCYANURIC ACID slip and dichloro isocyanuric urine acid mother liquor after centrifugation;
C. adding with its mass ratio in the wet DICHLOROISOCYANURIC ACID slip obtained toward step B is the pure water of 1:1 ~ 1:3, and stir and wash 2 ~ 5 times, washing lotion returns in steps A step and recycles, and washing lotion main component is pure water and sodium-chlor;
D: adding with its mass ratio in the wet DICHLOROISOCYANURIC ACID slip that step C obtains is pure water or the Surchlor GR 60 mother liquor of 1:1 ~ 1:3, stir and form suspension liquid, the sodium hydroxide solution that mass percent is 10% ~ 30% is dripped in suspension liquid, the sodium hydroxide dripped and DICHLOROISOCYANURIC ACID mol ratio are 0.8 ~ 1.2, stirring reaction 30 ~ 60min, again through evaporation, cooling, crystallization, centrifugation obtains wet Surchlor GR 60 and Surchlor GR 60 mother liquor, Surchlor GR 60 powder-product is obtained after wet Surchlor GR 60 drying, described Surchlor GR 60 mother liquor returns the recycling of D step.
A kind of method processing during metallic lithium is produced the chlorine produced of the present invention, adopt above-mentioned steps, in prior art, in above-mentioned steps, absorb during metallic lithium is produced the chlorine produced, obtain sodium dichloroisocyanate product, and this product is solid powdery, be convenient to store, transport and sell, and its value-added content of product is higher, and then reduce chlorine treatment cost, there is higher economic benefit.
The present invention also provides a kind of above-mentioned method processing during metallic lithium is produced the chlorine produced preparing the application in the chlorine produced in metallic lithium process in process industry.Utilize the method can obtain sodium dichloroisocyanate product, and this product is solid powdery, be convenient to store, transport and sell, and its value-added content of product is higher, and then reduces chlorine treatment cost, there is higher economic benefit.
Accompanying drawing explanation
A kind of process flow sheet processing during metallic lithium is produced the method for the chlorine produced of Fig. 1 the present invention.
Embodiment:
A kind of method processing during metallic lithium is produced the chlorine produced of the present invention, please refer to Fig. 1, comprises the following steps:
A. by cyanuric acid and mass percent be the caustic soda soln of 15% ~ 30% in molar ratio for 1:2 drops into reactor, stirring reaction 30 ~ 60min, obtains cyanuric acid two sodium solution;
B. pass into during metallic lithium is produced the chlorine produced in cyanuric acid two sodium solution obtained toward steps A and carry out chlorination reaction, controlling chlorination reaction temperature is 10 ~ 35 DEG C, when the pH of solution reaches 4 ~ 6, stopped reaction, obtains wet DICHLOROISOCYANURIC ACID slip and mother liquor after centrifugation;
C. adding with its mass ratio in the wet DICHLOROISOCYANURIC ACID slip obtained toward step B is the pure water of 1:1 ~ 1:3, and stir and wash 2 ~ 5 times, washing lotion returns in steps A step and recycles;
D: adding with its mass ratio in the wet DICHLOROISOCYANURIC ACID slip that step C obtains is pure water or the Surchlor GR 60 mother liquor of 1:1 ~ 1:3, stir and form suspension liquid, the sodium hydroxide solution that mass percent is 10% ~ 30% is dripped in suspension liquid, the sodium hydroxide dripped and DICHLOROISOCYANURIC ACID mol ratio are 0.8 ~ 1.2, stirring reaction 30 ~ 60min, obtain wet Surchlor GR 60 and Surchlor GR 60 mother liquor through evaporation, cooling, crystallization, centrifugation again, after wet Surchlor GR 60 drying, obtain Surchlor GR 60 powder-product.
Concrete analysis: the chemical equation of described steps A is as follows:
H
3(CNO)
3+2NaOH＝Na
2H(CNO)
3+2H
2O
In technique scheme, the reaction equation of step B is
Na
2H(CNO)
2+2Cl
2＝H(CNO)
3Cl
2+2NaCl
In technique scheme, the reaction equation of step D is
H(CNO)
3Cl
2+NaOH＝Na(CNO)
3Cl
2+H
2O
A kind of method processing during metallic lithium is produced the chlorine produced of the present invention, adopt above-mentioned steps, in terms of existing technologies, in above-mentioned steps, absorb during metallic lithium is produced the chlorine produced, obtain sodium dichloroisocyanate product, and this product is solid powdery, be convenient to store, transport and sell, and its value-added content of product is higher, and then reduce chlorine treatment cost, there is higher economic benefit.
A kind of method processing during metallic lithium is produced the chlorine produced of the present invention, please refer to Fig. 1, preferred technical scheme is further: the bake out temperature of described step D is 50 ~ 120 DEG C, and drying time is 1 ~ 3 hour.Can ensure that the available chlorine of product does not lose by controlling bake out temperature, and within the shortest time, obtain the product of having dried.
A kind of method processing during metallic lithium is produced the chlorine produced of the present invention is preparing the application in the chlorine produced in metallic lithium process in process industry.Utilize the method can obtain sodium dichloroisocyanate product, and this product is solid powdery, be convenient to store, transport and sell, and its value-added content of product is higher, and then reduces chlorine treatment cost, there is higher economic benefit.
Embodiment 1:
A, the caustic soda soln of 30% (wt%) of the cyanuric acid of 5Kg and 11Kg is dropped in reactor, after stirring reaction 30min, B, pass in solution metallic lithium produce in produce chlorine carry out chlorination reaction, controlling chlorination reaction temperature is 10 DEG C, when the pH of solution reaches 4, stopped reaction, 8.0Kg DICHLOROISOCYANURIC ACID solid and 8Kg mother liquor is obtained through centrifugation, C, add 8Kg pure water by the DICHLOROISOCYANURIC ACID solid obtained, repeatedly stir and wash 5 times, centrifugation obtains purer DICHLOROISOCYANURIC ACID solid, and washing lotion returns steps A and recycles.D, in purer DICHLOROISOCYANURIC ACID solid, add 8Kg pure water meter, drip 30% (wt%) NaOH of 5.2Kg, stirring reaction 60min, evaporation, crystallisation by cooling, at 50 DEG C, drying 1 hour, obtains Surchlor GR 60 product, by analysis, the assimilated efficiency of chlorine reaches 99.9%, and the tail gas of discharge meets discharging standards.
Embodiment 2:
A, the caustic soda soln of 15% (wt%) of the cyanuric acid of 15Kg and 63Kg is dropped in reactor, after stirring reaction 60min, B, pass in solution metallic lithium produce in produce chlorine carry out chlorination reaction, controlling chlorination reaction temperature is 35 DEG C, when the pH of solution reaches 6, stopped reaction, 24.0Kg DICHLOROISOCYANURIC ACID solid and 54Kg mother liquor is obtained through centrifugation, C, add 72Kg pure water by the DICHLOROISOCYANURIC ACID solid obtained, repeatedly stir and wash 2 times, centrifugation obtains purer DICHLOROISOCYANURIC ACID solid, and washing lotion returns steps A and recycles.D, in purer DICHLOROISOCYANURIC ACID solid, add 72Kg pure water meter, drip 15% (wt%) NaOH of 33Kg, stirring reaction 30min, evaporation, crystallisation by cooling, dry 30min at 120 DEG C, obtains Surchlor GR 60 product, by analysis, the assimilated efficiency of chlorine reaches 99.9%, and the tail gas of discharge meets discharging standards.
Embodiment 3:
A, the caustic soda soln of 20% (wt%) of the cyanuric acid of 10Kg and 31Kg is dropped in reactor, after stirring reaction 45min, B, pass in solution metallic lithium produce in produce chlorine carry out chlorination reaction, controlling chlorination reaction temperature is 23 DEG C, when the pH of solution reaches 7, stopped reaction, 16Kg DICHLOROISOCYANURIC ACID solid and 25Kg mother liquor is obtained through centrifugation, C, add 32Kg pure water by the DICHLOROISOCYANURIC ACID solid obtained, repeatedly stir and wash 3 times, centrifugation obtains purer DICHLOROISOCYANURIC ACID solid, and washing lotion returns steps A and recycles.D, in purer DICHLOROISOCYANURIC ACID solid, add 32Kg dichloro isocyanide mother liquid of sodium, drip the NaOH of 20% (wt%) of 15.5Kg, stirring reaction 45min, evaporation, crystallisation by cooling, dry 45min at 85 DEG C, obtains Surchlor GR 60 product, by analysis, the assimilated efficiency of chlorine reaches 99.9%, and the tail gas of discharge meets discharging standards.
In above-described embodiment, the technical indicator of dichlorocyanuric acid sodium is in table 1:
The technical indicator of table 1 dichlorocyanuric acid sodium
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Available chlorine (in Cl) content % | 60.17 | 60.99 | 60.65 |
| Moisture content, % | 2.74 | 0.97 | 1.25 |
| PH value (1% aqueous solution) | 5.73 | 6.27 | 6.81 |
| Water-insoluble, % | 0.091 | 0.083 | 0.072 |
| Arsenic content, %≤ | 0.0005 | 0.0005 | 0.0005 |
| Pb content, %≤ | 0.001 | 0.001 | 0.001 |
Above-described embodiment shows, uses method of the present invention, effectively can absorb the chlorine of metallic lithium production process output, the product obtained is pressed powder, be convenient to storage, transport, and the efficient height of product, quality is good, added value is high, all can realize goal of the invention of the present invention.
Foregoing is only illustrated several specific embodiments in the present invention; but can not as protection scope of the present invention; every according to the change of the equivalence done by design spirit in the present invention or to modify or equal proportion zooms in or out, all should think and fall into protection scope of the present invention.
Claims (3)
1. process during metallic lithium is produced a method for the chlorine produced, it is characterized in that: comprise the following steps:
A. by cyanuric acid and mass percent be the caustic soda soln of 15% ~ 30% in molar ratio for 1:2 drops into reactor, stirring reaction 30 ~ 60min, obtains cyanuric acid two sodium solution;
B. pass into during metallic lithium is produced the chlorine produced in cyanuric acid two sodium solution obtained toward steps A and carry out chlorination reaction, controlling chlorination reaction temperature is 10 ~ 35 DEG C, when the pH of solution reaches 4 ~ 6, stopped reaction, obtains wet DICHLOROISOCYANURIC ACID slip and dichloro isocyanuric urine acid mother liquor after centrifugation;
C. adding with its mass ratio in the wet DICHLOROISOCYANURIC ACID slip obtained toward step B is the pure water of 1:1 ~ 1:3, and stir and wash 2 ~ 5 times, washing lotion returns in steps A step and recycles, and washing lotion main component is pure water and sodium-chlor;
D: adding with its mass ratio in the wet DICHLOROISOCYANURIC ACID slip that step C obtains is pure water or the Surchlor GR 60 mother liquor of 1:1 ~ 1:3, stir and form suspension liquid, the sodium hydroxide solution that mass percent is 10% ~ 30% is dripped in suspension liquid, the sodium hydroxide dripped and DICHLOROISOCYANURIC ACID mol ratio are 0.8 ~ 1.2, stirring reaction 30 ~ 60min, again through evaporation, cooling, crystallization, centrifugation obtains wet Surchlor GR 60 and Surchlor GR 60 mother liquor, Surchlor GR 60 powder-product is obtained after wet Surchlor GR 60 drying, described Surchlor GR 60 mother liquor returns the recycling of D step.
2. a kind of method processing during metallic lithium is produced the chlorine produced according to claim 1, is characterized in that: the bake out temperature of described step D is 50 ~ 120 DEG C, and drying time is 1 ~ 3 hour.
3. a kind of method processing during metallic lithium is produced the chlorine produced described in claim 1 or 2 prepares the application in the chlorine produced in metallic lithium process in process industry.
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| CN201410512755.XA CN104311499A (en) | 2014-09-29 | 2014-09-29 | Method for treating chlorine generated in production of metal lithium and application thereof |
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| CN201410512755.XA CN104311499A (en) | 2014-09-29 | 2014-09-29 | Method for treating chlorine generated in production of metal lithium and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110790716A (en) * | 2018-08-01 | 2020-02-14 | 中国科学院福建物质结构研究所 | Alkali metal cyanuric acid monohydrogen compound, crystal thereof, preparation method and application thereof |
| CN114014273A (en) * | 2021-10-27 | 2022-02-08 | 济南爱思医药科技有限公司 | Chlorine dioxide generation process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109053A (en) * | 1994-12-30 | 1995-09-27 | 南京师范大学 | Combination process for producing sodium dichloroisocyanurate and trichloroisocyanuric acid |
| CN101573296A (en) * | 2006-11-02 | 2009-11-04 | 株式会社三德 | Process for producing metallic lithium |
| CN102009958A (en) * | 2010-12-23 | 2011-04-13 | 何卫东 | Device and method for producing bleacher from waste chlorine generated in lithium production |
| CN102091527A (en) * | 2010-12-23 | 2011-06-15 | 何卫东 | Method and device for absorbing waste chlorine generated in lithium production process by utilizing iron powder |
| CN102206192A (en) * | 2011-04-09 | 2011-10-05 | 河北冀衡化学股份有限公司 | Method for continuously synthesizing sodium dichloro isocyanurate dihydrate by wet process |
-
2014
- 2014-09-29 CN CN201410512755.XA patent/CN104311499A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109053A (en) * | 1994-12-30 | 1995-09-27 | 南京师范大学 | Combination process for producing sodium dichloroisocyanurate and trichloroisocyanuric acid |
| CN101573296A (en) * | 2006-11-02 | 2009-11-04 | 株式会社三德 | Process for producing metallic lithium |
| CN102009958A (en) * | 2010-12-23 | 2011-04-13 | 何卫东 | Device and method for producing bleacher from waste chlorine generated in lithium production |
| CN102091527A (en) * | 2010-12-23 | 2011-06-15 | 何卫东 | Method and device for absorbing waste chlorine generated in lithium production process by utilizing iron powder |
| CN102206192A (en) * | 2011-04-09 | 2011-10-05 | 河北冀衡化学股份有限公司 | Method for continuously synthesizing sodium dichloro isocyanurate dihydrate by wet process |
Non-Patent Citations (3)
| Title |
|---|
| 李玉芳: "二氯异氰尿酸钠的生产及应用", 《贵州化工》, vol. 28, no. 1, 28 February 2003 (2003-02-28), pages 14 - 17 * |
| 韦礼宁 等: "二氯异氰尿酸及钠盐的研制", 《化工技术与开发》, vol. 35, no. 9, 15 September 2009 (2009-09-15), pages 8 - 10 * |
| 黄晋等: "电解法生产金属锂尾气回收工艺方法的探讨", 《新疆有色金属》, no. 4, 31 August 2009 (2009-08-31), pages 51 - 52 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110790716A (en) * | 2018-08-01 | 2020-02-14 | 中国科学院福建物质结构研究所 | Alkali metal cyanuric acid monohydrogen compound, crystal thereof, preparation method and application thereof |
| CN114014273A (en) * | 2021-10-27 | 2022-02-08 | 济南爱思医药科技有限公司 | Chlorine dioxide generation process |
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Application publication date: 20150128 |
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