CN102807192A - Potassium perchlorate production technology with zero wastewater discharge and products thereof - Google Patents
Potassium perchlorate production technology with zero wastewater discharge and products thereof Download PDFInfo
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- CN102807192A CN102807192A CN 201210280728 CN201210280728A CN102807192A CN 102807192 A CN102807192 A CN 102807192A CN 201210280728 CN201210280728 CN 201210280728 CN 201210280728 A CN201210280728 A CN 201210280728A CN 102807192 A CN102807192 A CN 102807192A
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Abstract
The invention relates to the technical fields of cleaner production and circulating production, in particular to a potassium perchlorate production technology with zero wastewater discharge and products of the potassium perchlorate production technology. The steps of electrolytic double decomposition are as follows: (1) electrolyzing sodium chlorate to sodium perchlorate; (2) taking potassium chlorate as a double decomposition raw material, and performing double decomposition reaction of potassium chlorate and sodium perchlorate to generate the potassium perchlorate crude materials; and (3) recrystallizing and purifying the potassium perchlorate crude materials to obtain the products, and electrolyzing and recycling double decomposition mother solution sodium chlorate. The invention has the following advantages that: the water in the production process can be recycled, the production wastewater is not discharged, the chromium-containing waste residues in the production are recycled after being extracted simultaneously, and the rest of solid waste residues are used for other purposes, so that the strategic requirements of the sustainable development of the social economy can be met, and the production technology is suitable for popularization; and moreover, the environmental protection problem is completely solved, the product quality is improved, the product purity is high, the firing is fast, the reaction is complete, no residue is caused; and the production technology is safer and more stable, the product cost performance is higher, and the competitive power is stronger.
Description
Technical field
The present invention relates to cleaner production and cyclic production technical field, be meant a kind of potassium perchlorate zero-discharge production process and products thereof especially.
Background technology
Potassium perchlorate is one of important kind of perchlorate, is mainly used in to make fireworks and firecrackers, safety match, explosive, meteorological rocket, the civilian coal of igniting, oxygenant etc.Hydrogen is mainly used in the industries such as manufacturing, Metal smelting, cutting and welding of oil, food, fine chemistry industry, glass and hard mass.Mostly traditional technology is that the Repone K method of completing the square is as shown in Figure 1; Its technical process is: with the VAL-DROP electrolysis is sodium perchlorate; Carry out replacement(metathesis)reaction with Repone K again; Cool off centrifugally, promptly make potassium perchlorate, the metathesis mother liquor after centrifugal is mainly sodium-chlor, also has the small amounts of chlorine hydrochlorate, perchlorate discharges behind freezing recoverys part potassium perchlorate.Therefore the process method of prior art is a kind of Repone K method of completing the square with waste water, waste discharge.According to " inorganic chemicals industry " 2007 the 7th phases " oxymuriate overview and future development trend analysis " literary composition; Because metathesis mother liquor (to traditional technology Repone K method of completing the square) recovery technology is not perfect at present; Or the economic benefit that investment brings is not remarkable; Thereby bringing environmental issue inevitably, this has caused showing great attention to of insider.The producer that has contains the waste water (being the metathesis mother liquor) of perchlorate, oxymuriate and other heavy metal for fear of discharging, once adopts vaporizer with the waste water evaporate to dryness, because the moisture content of evaporation too much (is produced 1 ton of potassium perchlorate 3m
3Waste water), the sodium chloride as impurity too high levels that makes of evaporation, no economic worth and energy consumption are high again and abandon.It is chloride hydrochlorate in the waste water, perchlorate and other a small amount of heavy metal (like lead) that discharge of wastewater causes the major cause of environmental issue; Perchlorate is difficult for decomposition environment is caused long-time pollution; Cause salting of soil; And oxymuriate and the perchlorate use of solution intersection in process of production cause damage system chlorate electrolyser anode, and in the work-ing life of having reduced anode electrolytic cell, there is special elaboration in the U.S. to its pollution " environmental science is with the technological " first phase in 2005.
The applicant is because of being located in upper river, so can not pollute basin, place water body, if by the traditional technology route then can discharge the waste water that contains perchlorate, oxymuriate and other heavy metal, do not meet national environmental protection policy and STRATEGIES OF SUSTAINABLE DEVELOPMENT.In line with the spirit of being responsible for to society, to environment, the applicant drops into a large amount of human and material resources and financial resources and develops new environment-friendly type potassium perchlorate production technique and replace traditional technology.Through unremitting effort and keeping forging ahead; Finally problems such as the discharge of wastewater, exhaust gas emission and the coal consumption that occur in the production process be higher have been solved; Achieve success and realized closed operation; Non-wastewater discharge has been avoided the problem that the use of solution intersection causes anode electrolytic cell to damage in oxymuriate and the perchlorate production.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, and potassium perchlorate zero-discharge production process of a kind of suitable cleaner production and cyclic production and products thereof is provided.
The present invention realizes that through following technical scheme the step of electrolysis metathesis process is:
1. earlier VAL-DROP is electrolyzed to produce sodium perchlorate;
2. with Potcrate as metathesis feedstock, carry out replacement(metathesis)reaction with sodium perchlorate and generate the potassium perchlorate coarse fodder;
3. the potassium perchlorate coarse fodder obtains product after purifying through recrystallization; Said metathesis mother liquor VAL-DROP electrolysis cycle is used.
Replace Repone K as metathesis feedstock with Potcrate, the mother liquor that metathesis is extracted behind the potassium perchlorate is that VAL-DROP can return the perchlorate electrolytic tank electrolysis.
In the electrolytic process during said Potcrate is produced, the sub product that electrolytic sodium chloride system VAL-DROP produces contains chlorine, oxygen and hydrogen; Compression bottling after said hydrogen is purified through dechlorination, deoxygenation.
In the said Potcrate production process, the chromic salts mud waste residue that contains that produces is placed closed reactor, add sodium bicarbonate and water again and stir, with steam heating to 105 ℃, be incubated 4h, naturally cooling carries out solid-liquid separation subsequently.
The said saline solution that contains chromium that leaches is stored in the pond for recovering and recycles, and calcium magnesium slag places lauter tub to wash; Said washing water are used to handle the original chromic salts mud waste residue that contains, and the calcium magnesium slag after the washing is as material of construction.
Also comprise prepared potassium perchlorate and hydrogen.
Principle of work of the present invention does, is VAL-DROP with sodium chloride electrolysis earlier, and VAL-DROP makes Potcrate with the Repone K replacement(metathesis)reaction again, more than two process divisions following:
1. in electrosynthesis perchlorate process, can not regard the anodic reaction as oxymuriate direct oxygenation reaction and generate perchlorate.But secondary reaction comprises that the chlorate ion discharges, and follows to react near anode by radical and water, generates chlorous acid and perchloric acid, and emits oxygen, and unstable chlorous acid becomes chloric acid with regard to autoxidation.
The total reaction equation is:
2. sodium perchlorate electrolytic solution and potassium chlorate solution carry out replacement(metathesis)reaction.
Its reaction formula is following: NaClO
4+ KClO
3=KClO
4+ NaClO
3
This chemical reaction can obtain the potassium perchlorate crystallization, mainly be to utilize the solubleness of sodium perchlorate, Potcrate, VAL-DROP to vary in size to realize, because of the solubleness of potassium perchlorate low than sodium perchlorate, Potcrate.
The invention has the advantages that the water in the production process all is able to recycling, does not discharge factory effluent; Chromium residue in will producing simultaneously extracts the back and reuses, and all the other solid slags use it for anything else in addition, have satisfied social economy's STRATEGIES OF SUSTAINABLE DEVELOPMENT requirement; The suitable popularization not only solved environmental issue fully, and improved quality product; Product impurity is few, purity is high, start to exchange fire fast, reacts completely no residue; And safer stable, the product price ratio is higher, and is more competitive.To produce oxymuriate simultaneously and thoroughly separate, avoid the problem that the use of solution intersection causes (electrolytic sodium chloride system VAL-DROP) anode electrolytic cell to damage in oxymuriate and the perchlorate production with the solution system of producing perchlorate.
Description of drawings
Fig. 1 is the prior art processes flow diagram;
Fig. 2 is a technical matters flow diagram of the present invention;
Fig. 3 is an electrolysis tail gas process flow diagram;
Fig. 4 is a chromium residue processing technological flow skeleton diagram.
Embodiment
Be described further below in conjunction with 2 to 4 pairs of the preferred embodiments of the present invention of accompanying drawing, the step of electrolysis metathesis process is:
1. earlier VAL-DROP is electrolyzed to produce sodium perchlorate;
2. with Potcrate as metathesis feedstock, carry out replacement(metathesis)reaction with sodium perchlorate and generate the potassium perchlorate coarse fodder;
3. the potassium perchlorate coarse fodder obtains product after purifying through recrystallization; Said metathesis mother liquor VAL-DROP electrolysis cycle is used.
Replace Repone K as metathesis feedstock with Potcrate, the mother liquor that metathesis is extracted behind the potassium perchlorate is that VAL-DROP can return the perchlorate electrolytic tank electrolysis.
The Repone K metathesis is produced the traditional technology of potassium perchlorate because contain perchlorate (have go back fluoride ion) in the by product sodium chloride solution after the metathesis, if produce VAL-DROP as electrolysis, is shortened dramatically in the anode electrolytic cell coating life-span; Make and produce inconvenience, cost raises, in addition; If salt solution reclaims electrolysis again and is used for producing VAL-DROP; Because the VAL-DROP poor quality who produces, power consumption was quite high when electrolysis was sodium perchlorate again, and production cost is raise.This is the difficult problem on oxymuriate, the perchlorate production history, and the environmental issue that potassium perchlorate metathesis mother liquor exhaust emission water body causes fails effectively to be solved always; And the by product after the novel process metathesis of Potcrate metathesis production potassium perchlorate is a VAL-DROP; Can return the perchlorate electrolyzer recycles; This technology has thoroughly been separated with the solution system of producing perchlorate producing oxymuriate technically, thereby has avoided in oxymuriate and the perchlorate production solution to intersect the chlorate electrolyser anode problem of making of damaging that causes of using.
In the electrolytic process during said Potcrate is produced, the sub product that electrolytic sodium chloride system VAL-DROP produces contains chlorine, oxygen and hydrogen; Compression bottling after said hydrogen is purified through dechlorination, deoxygenation.
In the said Potcrate production process, the chromic salts mud waste residue that contains that produces is placed closed reactor, add sodium bicarbonate and water again and stir, with steam heating to 105 ℃, be incubated 4h, naturally cooling carries out solid-liquid separation subsequently.
The said saline solution that contains chromium that leaches is stored in the pond for recovering and recycles, and calcium magnesium slag places lauter tub to wash; Said washing water are used to handle the original chromic salts mud waste residue that contains, and the calcium magnesium slag after the washing is as material of construction.
Also comprise prepared potassium perchlorate and hydrogen.
Innovative point of the present invention is:
1) adopt the reaction of Potcrate and sodium perchlorate to produce potassium perchlorate, metathesis mother liquor VAL-DROP is able to recycle, and has avoided the discharge of wastewater in the traditional technology process, starting material Repone K, VAL-DROP utilization ratio height, and consuming has the traditional technology of discharge of wastewater little.To produce oxymuriate simultaneously and thoroughly separate, avoid the problem that the use of solution intersection causes (electrolytic sodium chloride system VAL-DROP) anode electrolytic cell to damage in oxymuriate and the perchlorate production with the solution system of producing perchlorate.
2) tail gas of discharging in the electrolytic process is administered.In Potcrate (as the raw material of producing potassium perchlorate) production process, the process of electrolytic sodium chloride system VAL-DROP can produce the hydrogen that contains chlorine, oxygen, and we are with hydrogen purification, and the compression bottling is sold.Process is following: hydrogen is got into tail gas washing tower, absorb with salt solution earlier and use alkali cleaning and washing again.Remove that chlorine is laggard goes into water sealed tank.Salt solution after the washing, alkali lye and water are sent electrolysis workshop section respectively back to and brine section fully utilizes again, have realized zero release.Hydrogen after the dechlorination adopts Root's blower to send into the water cooler cooling, get into de-aerator plant then carries out deoxidation, gets into the water cooler cooling again, gets into gas holder recompression bottling then and sells, referring to accompanying drawing 3.
3) waste residue that produces in the production process is administered.Produce chromyl magnesium calcium body refuse in the salt refining process that Potcrate is produced, we add mineralizer high temperature alligatoring nano particle with chromium residue, and Separation and Recovery contains chromic salts water (returning the salt refining process).To pass through the magnesium calcium body refuse that mineralizer handle to reclaim behind exhausted most sexavalent chrome and use the washing water repeated washing; Sexavalent chrome is accumulated to finite concentration and just is used to handle original chromium residue in washing water; Finally make washing water be able to recycle; Significantly reduced the consumption of arsenic, eliminated the pollution of sexavalent chrome environment.Detoxification magnesium calcium slag after the washing can be used for preparing coating, refractory materials, poromerics etc., referring to accompanying drawing 4.
4) adopt this technology, need not the degree of depth electrolysis during electrolysis VAL-DROP system sodium perchlorate, electrolytic power consumption is compared traditional technology and is reduced 400-800 degree/ton.
5) whole process water has been accomplished to recycle, and has accomplished no waste water,waste gas and industrial residue discharging simultaneously.
The key technical index that the present invention can reach sees table:
| Project | Index |
| Outward appearance | White crystalline powder |
| Potassium perchlorate (KClO 4）%≥ | 99.2 |
| Moisture %<= | 0.03 |
| Oxymuriate (in KCl) %<= | 0.14 |
| Muriate (in KCl) %<= | 0.003 |
| Hypochlorite (in Cl) %<= | Do not have |
| Bromate is (with KBrO 3Count) %<= | 0.002 |
| Water-insoluble %<= | 0.0 |
| Sodium is (with NaClO 3Count) %<= | 0.20 |
1) with Potcrate be starting material, carry out replacement(metathesis)reaction with sodium perchlorate, metathesis mother liquor VAL-DROP recycles, and no longer discharging had not only reduced raw-material consumption but also free from environmental pollution;
2) hydrogen that produces in the electrolytic process compresses bottling after removal of impurities, absorption liquid during the hydrogen removal of impurities and washings reclaim comprehensive utilization;
3) waste residue that produces in the production process passes through to add mineralizer high temperature alligatoring nano particle, and Separation and Recovery sexavalent chrome and effective salinity are used as material of construction after the solid slag washing detoxification.
4) electrolysis waste heat, dissolving waste heat are utilized, avoided because of having increased the steam consumption problem of too that evaporation, purification process bring newly.
In sum, the gordian technique of this project is to be starting material with Potcrate, and the sodium perchlorate that makes with electrolysis carries out replacement(metathesis)reaction acquisition potassium perchlorate; Bottle behind the hydrogen cleaning that electrolysis produces; Mother liquor gets into electrolysis after through concentrating and impurity removing and carries out recycle; After filter residue reacts through the adding mineralizer, the Separation and Recovery sexavalent chrome.Solid slag is mainly magnesium calcium carbonate, can fully utilize.Whole production is accomplished zero release.
Claims (6)
1. potassium perchlorate zero waste water discharging production technique and products thereof is characterized in that the step of electrolysis metathesis process is: 1. earlier VAL-DROP is electrolyzed to produce sodium perchlorate;
2. with Potcrate as metathesis feedstock, carry out replacement(metathesis)reaction with sodium perchlorate and generate the potassium perchlorate coarse fodder;
3. the potassium perchlorate coarse fodder obtains product after purifying through recrystallization; Said metathesis mother liquor VAL-DROP electrolysis cycle is used.
2. potassium perchlorate zero waste water discharging production technique according to claim 1 and products thereof; It is characterized in that: replace Repone K as metathesis feedstock with Potcrate, the mother liquor that metathesis is extracted behind the potassium perchlorate is that VAL-DROP can return the perchlorate electrolytic tank electrolysis.
3. potassium perchlorate zero waste water discharging production technique according to claim 1 and products thereof is characterized in that: in the electrolytic process during said Potcrate is produced, the sub product that electrolytic sodium chloride system VAL-DROP produces contains chlorine, oxygen and hydrogen; Compression bottling after said hydrogen is purified through dechlorination, deoxygenation.
4. potassium perchlorate zero waste water discharging production technique according to claim 1 and products thereof; It is characterized in that: in the said Potcrate production process, the chromic salts mud waste residue that contains that produces is placed closed reactor, add sodium bicarbonate and water again and stir; With steam heating to 105 ℃; Insulation 4h, naturally cooling carries out solid-liquid separation subsequently.
5. potassium perchlorate zero waste water according to claim 4 discharging production technique and products thereof is characterized in that: the said saline solution that contains chromium that leaches is stored in the pond for recovering and recycles, and calcium magnesium slag places lauter tub to wash; Said washing water are used to handle the original chromic salts mud waste residue that contains, and the calcium magnesium slag after the washing is as material of construction.
6. according to each described potassium perchlorate zero waste water discharging production technique of claim 1 to 4 and products thereof, it is characterized in that: also comprise prepared potassium perchlorate and hydrogen.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265404A (en) * | 2013-05-23 | 2013-08-28 | 耒阳金悦科技发展有限公司 | Technical method for preparing 1,4-butylene glycol by hydrogen gas purified from electrolysis brine waste gas |
| CN105271125A (en) * | 2015-11-09 | 2016-01-27 | 大连高佳化工有限公司 | Spherical potassium perchlorate production technology |
| CN108793199A (en) * | 2018-05-24 | 2018-11-13 | 汶川县湘宁氯酸盐有限责任公司 | A method of recycling sodium chloride in preparing potassium chlorate waste water |
| CN109248465A (en) * | 2018-09-27 | 2019-01-22 | 茂县鑫盐化工有限公司 | Potassium hyperchlorate the systematic stock solution and wastewater recycling process |
| CN109574042A (en) * | 2018-12-21 | 2019-04-05 | 中国科学院过程工程研究所 | The separation method of potassium sodium in a kind of mixed chlorinated salt containing potassium and sodium |
| CN110129820A (en) * | 2019-06-25 | 2019-08-16 | 山东瑞克环境科技有限公司 | Calcium hypochlorite, calcium chlorate, Calcium perchlorate preparation facilities and method |
| CN110759568A (en) * | 2019-10-24 | 2020-02-07 | 广东闻扬环境科技有限公司 | Recovery system and recovery method for potassium perchlorate and sodium chloride crystal salt in wastewater |
| CN112028024A (en) * | 2020-08-27 | 2020-12-04 | 耒阳金悦科技发展有限公司 | Potassium perchlorate zero-wastewater discharge method |
-
2012
- 2012-08-08 CN CN 201210280728 patent/CN102807192A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265404A (en) * | 2013-05-23 | 2013-08-28 | 耒阳金悦科技发展有限公司 | Technical method for preparing 1,4-butylene glycol by hydrogen gas purified from electrolysis brine waste gas |
| CN105271125A (en) * | 2015-11-09 | 2016-01-27 | 大连高佳化工有限公司 | Spherical potassium perchlorate production technology |
| CN108793199A (en) * | 2018-05-24 | 2018-11-13 | 汶川县湘宁氯酸盐有限责任公司 | A method of recycling sodium chloride in preparing potassium chlorate waste water |
| CN108793199B (en) * | 2018-05-24 | 2020-06-12 | 台州市杰龙风机厂 | Method for recycling sodium chloride from potassium chlorate preparation wastewater |
| CN109248465A (en) * | 2018-09-27 | 2019-01-22 | 茂县鑫盐化工有限公司 | Potassium hyperchlorate the systematic stock solution and wastewater recycling process |
| CN109574042A (en) * | 2018-12-21 | 2019-04-05 | 中国科学院过程工程研究所 | The separation method of potassium sodium in a kind of mixed chlorinated salt containing potassium and sodium |
| CN110129820A (en) * | 2019-06-25 | 2019-08-16 | 山东瑞克环境科技有限公司 | Calcium hypochlorite, calcium chlorate, Calcium perchlorate preparation facilities and method |
| CN110759568A (en) * | 2019-10-24 | 2020-02-07 | 广东闻扬环境科技有限公司 | Recovery system and recovery method for potassium perchlorate and sodium chloride crystal salt in wastewater |
| CN112028024A (en) * | 2020-08-27 | 2020-12-04 | 耒阳金悦科技发展有限公司 | Potassium perchlorate zero-wastewater discharge method |
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Application publication date: 20121205 |