CN105439091A - Environment-friendly chlorine dioxide preparing method and device by means of hydrogen peroxide - Google Patents
Environment-friendly chlorine dioxide preparing method and device by means of hydrogen peroxide Download PDFInfo
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Abstract
The invention discloses an environment-friendly chlorine dioxide preparing method and device by means of hydrogen peroxide. According to the method, the raw material hydrogen peroxide is evenly mixed with a sodium chlorate solution firstly and then delivered to a lower circulating tube of a generator, sulfuric acid is added through a pipe arranged on a top opening of a reboiler, and chlorine dioxide, oxygen, neutral mirabilite and water are generated through reaction in a reactor; chlorine dioxide mixed gas enters an intercooler from the top of the generator and then enters an absorption tower to be absorbed by chilled water, so that a ClO2 aqueous solution is formed; mirabilite crystals separated out from generator mother liquor are sent to a salt cake filter to be filtered by extracting part of the mother liquor, so that the mirabilite crystals are filtered and separated out; the mother liquor which is filtered out returns to the generator, and the mirabilite crystals which are filtered out enter a mirabilite drying system to be dried to form anhydrous sodium sulphate; gas discharged from each tank of the system is sucked into a washing tower to be washed with chilled water and then is discharged completely after meeting the standard. No waste acid is discharged, neutral mirabilite generated through reaction can be made into anhydrous sodium sulphate to be sold after being filtered and dried, no solid waste is discharged, and the production technology is clean and environmentally friendly.
Description
Technical field
The present invention relates to chlorine dioxide production technical field, specifically a kind of peroxide passivation dioxide peroxide preparation method of environment-friendly type and equipment.
Technical background
Dioxide peroxide is orange-yellow gas at normal temperatures and pressures, similar chlorine on outward appearance and smell, boiling point is 11 DEG C, and freezing point is-59 DEG C, 11 DEG C time, gaseous density is that 3.09g/m3. gaseous chlorine dioxide is unstable, is heated, by illumination or contact with organism to set off an explosion and decompose during high density.Dioxide peroxide is soluble in water, is to spread with molecular form, forms volatile yellow-green soln.Dioxide peroxide is hydrolyzed hardly in water, and is not combined with organism, does not generate trichloromethane carcinogenic substance, does not also react with ammonia.The danger that ClO 2 solution concentration is not exploded substantially at below 10g/l.
Dioxide peroxide is a kind of extremely strong oxygenant, and stable dioxide peroxide is considered to respond well, the sterilant of superior performance, sterilizing agent, SYNTHETIC OPTICAL WHITNER.Dioxide peroxide is widely used in the bleaching of paper pulp, fiber; Industrial sewage, hospital sewage, industrial circulating cooling water process; Soil virus killing, the aspect such as water body disinfection diseases prevention, oil production in aquaculture.Chlorine dioxide with high purity can also be applied to the aspect such as anti-corrosive fresh-keeping of sterilization in the disinfection of clinical treatment, food-processing, food (meat, fishery products, fruits and vegetables).
Always very active about the research preparing chlorine dioxide method, shaping production technique reaches tens kinds, but each method has its distinguished advantage, also has obvious defect simultaneously.Main employing R1 method, R3 method, R5 method, R8 method in current industrial production application.Namely be reductive agent with sulfurous gas, chlorion, methyl alcohol, react with sodium chlorate in acid condition and prepare dioxide peroxide.Take sulfurous gas as reduction method, agent prepares dioxide peroxide, transformation efficiency is not high, and the inconvenience of sulfurous gas source, can carry sulfurous gas, chlorine secretly in product, product purity is not high.Be that dioxide peroxide prepared by reductive agent with chlorion, raw material sources are convenient, but transformation efficiency is not high, and the dioxide peroxide often obtaining 1mol can produce the chlorine of 0.5mol simultaneously, needs to process especially product.Be that dioxide peroxide prepared by reductive agent with methyl alcohol, can obtain by the methyl alcohol of different generation formaldehyde, formic acid, carbonic acid gas and the non-complete reactions of reducing degree.Methyl alcohol, formaldehyde and formic acid are all toxic substances, and they can be restricted to the application of product.
Developing low-cost, high purity, pollution-free, safe and reliable chlorine dioxide production novel process and production equipment, substitute the old technology of high cost, maximum discharge, to alleviation environmental protection pressure, promotes national economic development, have important economic implications and social effect.At present, hydrogen peroxide method is prepared in the gaseous product that dioxide peroxide generates and is only had and form chlorine on a small quantity or not, and by-product oxygen is favourable to environmental protection to bleaching together with dioxide peroxide.And due to features such as the method raw material sources are convenient, cheaply, transformation efficiency is high, and product purity is high, and the speed that occurs is fast, deeply pay close attention to by people.The chemical principle of the method is:
6NaClO
3+3H
2O
2+H
2SO
4→6ClO
2+2Na
3H(SO
4)
2+3O
2+6H
2O
Hydrogen-peroxide reduction method is produced in chlorine dioxide, and the vitriol that sulfuric acid concentration difference is then formed is different.When sulfuric acid concentration is 1--2.5mol/L, can obtain higher speed of reaction and efficiency, produce neutral saltcake, reaction principle is:
2NaClO
3+H
2O
2+H
2SO
4→2ClO
2+Na
2SO
4+O
2+2H
2O
When sulfuric acid concentration is 2.5--5.5mol/L, speed of response and efficiency are very high, and can produce the little product of chlorine content, produce the acid saltcake of byproduct, its reaction principle is:
6NaClO
3+3H
2O
2+H
2SO
4→6ClO
2+2Na
3H(SO
4)
2+3O
2+6H
2O
When the concentration of sulfuric acid is greater than 5.5mol/L, the byproduct of generation is hydrosulfate.Its reaction principle is as follows:
2NaClO
3+H
2O
2+2H
2SO
4→2ClO
2+2NaHSO
4+O
2+2H
2O
Peroxide passivation chlorine dioxide preparing process domestic is at present substantially all adopt multi-stage aeration formula producer.Consider from economic benefits such as the transformation efficiency of sodium chlorate, purity of chlorine dioxide and yields, in multi-stage generator, sulfuric acid is with the excessive existence of different concns, so in manufacture chlorine dioxide, there is a large amount of spent acid discharges, causes severe contamination to environment.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of peroxide passivation dioxide peroxide preparation method of environment-friendly type.The method realizes preparation process does not have spent acid to discharge, clean environment firendly.
The present invention solves the problems of the technologies described above with following technical scheme:
The peroxide passivation dioxide peroxide preparation method of a kind of environment-friendly type of the present invention, adopt the vertical producer of single container as chlorine dioxide generator, be connected by circulation line between chlorine dioxide generator with reboiler, raw material hydrogen peroxide adds from the pipeline be connected between chlorine dioxide generator outlet at bottom and reboiler with after sodium chlorate solution's mixed diluting in advance again, sulfuric acid adds from the trunnion of reboiler top exit, the chemical added constantly circulates between reboiler and chlorine dioxide generator, react in chlorine dioxide generator, flash distillation, by controlling the sulfuric acid of reaction solution in chlorine dioxide generator at 1.75-2.0mol/L, under relatively low acidity condition, reaction generates dioxide peroxide, water, oxygen and neutral saltcake, dioxide peroxide, oxygen, water vapor discharge from liquid, and saltcake is dissolved in mother liquor, after reaching capacity, separate out with crystalline form, in order to keep produce continue carry out, by filter charging pump by connect chlorine dioxide generator outlet at bottom and reboiler pipeline in a part of liquor abstraction, deliver to filter to filter, saltcake crystal filtering separation out, the mother liquor leached returns this line segments and proceeds circulating reaction, the saltcake crystal leached enters saltcake dehumidification system, dries and makes Sodium sulfate anhydrous.min(99), the dioxide peroxide mixed gas being flashed out enters vapor pipe from chlorine dioxide generator top exit and enter absorption tower after inter cooler cooling, and absorption tower refrigerated water absorbs, and becomes ClO
2the aqueous solution, delivers to ClO with shifting pump
2solution storage tank is stored, the exhaust of each groove tank is introduced in washing tower through exhaust fan suction, up to standard rear emptying with refrigerated water washing, and washing tower dioxide peroxide dilute solution enters absorption tower through vacuum self-priming and absorbs ClO
2gas enrichment.
The hydrogen peroxide solution concentration controlling to add is 50%, and the sodium chlorate solution's concentration mixed with hydrogen peroxide is 640 ~ 680g/L, temperature 45 ~ 50 DEG C; The sulfuric acid added first to be diluted with water to the concentration of 60 ~ 65% before trunnion spraying, control by controlling sulfuric acid in reaction solution at 1.75-2.0mol/L simultaneously.
The peroxide passivation dioxide peroxide Preparation equipment of environment-friendly type of the present invention, it comprises chlorine dioxide generator 8, reboiler 4, filter gas-liquid separating tank 11, filter 12, inter cooler 23, absorption tower 22 and tail gas washing tower 16, be connected by upper circular tube 7 and lower circulation tube 25 and formed between chlorine dioxide generator 8 with reboiler 4 and circulate, lower circulation tube 25 connects producer recycle pump 3, be communicated with hydrogen peroxide and add the Hybrid connections pipe that pipe 2 and sodium chlorate add pipe 1, the liquid return tube of filter charging pump 24 and filter 12, the outlet of filter charging pump 24 connects filter 12, filter 12 is connected with filter gas-liquid separating tank 11, one end of filter gas-liquid separating tank 11 is connected with filter vacuum pump 13, the other end connects the liquid return tube of filter 12, filter 12 is provided with saltcake discharge port 10, reboiler 4 adds pipe 6 with upper circular tube 7 junction and sulfuric acid and is connected, chlorine dioxide generator 8 top exit connects producer vapor pipe 9, the outlet of producer vapor pipe 9 connects inter cooler 23, the water shoot access absorption tower 22 of inter cooler 23, the top exit on absorption tower 22 connects producer vacuum pump 17 by the road, the bottom on absorption tower 22 connects dioxide peroxide storagetank 20 through dioxide peroxide shifting pump 21, producer vacuum pump 17, filter vacuum pump 13 all accesses tail gas washing tower 16 bottom, the top of tail gas washing tower 16 is all connected refrigerated water with the top on absorption tower 22 and adds pipe 14, the top of tail gas washing tower 16 connects exhaust fan 15.
The present invention has following beneficial effect:
1, three large raw materials are at the continuous circulating reaction of producer, keep each chemical concentration in producer liquid level, mother liquor, do not have spent acid to discharge by transpiring moisture.
2, reaction generates neutral saltcake, is not acid saltcake, reduces the loss of acid; Neutral saltcake can be made into Sodium sulfate anhydrous.min(99) after drying after filtration and takes out, and does not have solid waste discharge.
3, tail gas from absorption tower is conveyed to washing tower and carries out double absorption, and the exhaust of each groove tank is also introduced in washing tower through blower fan suction, rear discharge up to standard; Dioxide peroxide dilute solution after washing returns to absorption tower and absorbs dioxide peroxide enrichment, does not have obnoxious flavour and discharge of wastewater.
Accompanying drawing explanation
Fig. 1 is the device structure that adopts of the present invention and process flow sheet.
Embodiment
Below in conjunction with Fig. 1, the inventive method and equipment are further described:
The peroxide passivation of environment-friendly type of the present invention prepares chlorine dioxide plant primarily of producer recycle pump 3, reboiler 4, upper circular tube 7, chlorine dioxide generator 8, lower circulation tube 25, filter gas-liquid separating tank 11, filter 12, filter vacuum pump 13, filter charging pump 24, inter cooler 23, absorption tower 22, tail gas washing tower 16 and relevant pipeline composition.Be connected by upper circular tube 7 and lower circulation tube 25 and formed between chlorine dioxide generator 8 with reboiler 4 and circulate, the bottom of reboiler 5 connects condensate draining pipe, top connects steam and adds pipe 5, producer recycle pump 3, be communicated with hydrogen peroxide and add the Hybrid connections pipe that pipe 2 and sodium chlorate add pipe 1, the liquid return tube of filter charging pump 24 and filter 12 accesses lower circulation tube 25 respectively, the outlet of filter charging pump 24 connects filter 12, filter 12 is connected with filter gas-liquid separating tank 11, one end of filter gas-liquid separating tank 11 is connected with filter vacuum pump 13, the other end connects the liquid return tube of filter 12, filter 12 is provided with saltcake discharge port 10, reboiler 4 adds pipe 6 with the junction of upper circular tube 7 with sulfuric acid and is connected, chlorine dioxide generator 8 top exit connects producer vapor pipe 9, the outlet of producer vapor pipe 9 connects inter cooler 23, the water shoot access absorption tower 22 of inter cooler 23, the top exit on absorption tower 22 connects producer vacuum pump 17 by the road, the bottom on absorption tower 22 connects dioxide peroxide storagetank 20 through dioxide peroxide shifting pump 21, and dioxide peroxide storagetank 20 connects dioxide peroxide transfer lime 18 through dioxide peroxide transferpump 19.Producer vacuum pump 17, filter vacuum pump 13 all access tail gas washing tower 16 bottom, the top of tail gas washing tower 16 is all connected refrigerated water with the top on absorption tower 22 and adds pipe 14, the top of tail gas washing tower 16 connects exhaust fan 15, and the bottom of tail gas washing tower 16 accesses the top on absorption tower 22 by the road.
During preparation, (concentration is 640 ~ 680g/L to the sodium chlorate solution come from the pumping of sodium chlorate storage tank, temperature 45 ~ 50 DEG C) add pipe 1 through sodium chlorate and add from lower circulation tube 25, from the vitriol oil (concentration 98% that the pumping of vitriol oil storage tank comes, normal temperature) add pipe 6 through sulfuric acid and to spray from the trunnion of reboiler 4 top exit and add, to spray before trunnion first with water diluting concentrated sulfuric acid to concentration be 60 ~ 65% (being diluted a large amount of heat release by water when mixing with reaction solution after entering circulation tube to prevent the vitriol oil causes local temperature too high), circulation is mixed to form reaction mother liquor.(concentration is 50% to the hydrogen peroxide solution come from the pumping of hydrogen peroxide storage tank, normal temperature) add pipe 2 through hydrogen peroxide and join and be communicated with hydrogen peroxide and add the Hybrid connections pipe that pipe 2 and sodium chlorate add pipe 1, hydrogen peroxide is fully mixed with sodium chlorate solution in advance and enters lower circulation tube 25 again, prevent the too high reaction of hydrogen peroxide partial concn in circulation tube entered from too acutely causing chlorine dioxide decomposition.Chemical constantly circulates under the effect of recycle pump 3 between reboiler 4 and producer 8, reaction, flash distillation in producer 8.Along with sodium chlorate solution, the vitriol oil, hydrogen peroxide solution constantly add, mother liquor constantly circulates under the effect of recycle pump 3 between reboiler 5 and producer 9, reaction will constantly be carried out, the sulfuric acid controlled in reaction solution reacts and prepares dioxide peroxide under the low acidic conditions of 1.75-2.0mol/L simultaneously, the neutral saltcake produced can be separated out with crystalline form in producer, by filter charging pump 24 a part of liquor abstraction from lower circulation tube 15, deliver to filter 12 to filter, saltcake crystal filtering separation out.The mother liquor leached returns the producer recycle system at filter steam-water separation tank 11 from gravity and continues circulating reaction, and saltcake enters saltcake dehumidification system through saltcake discharge port 13, dries and makes Sodium sulfate anhydrous.min(99).The dioxide peroxide mixed gas discharged from producer top out, enters inter cooler 17 through producer vapor pipe 10 and cools, and then enters absorption tower 19 and absorbs through refrigerated water, become ClO
2the aqueous solution, delivers to ClO with shifting pump 21
2solution storage tank 20 is stored.The exhaust of the gas that producer vacuum pump 17, filter vacuum pump 13 eject and each groove tank of system is aspirated through exhaust fan 15 and is introduced in washing tower, up to standard rear emptying with refrigerated water washing.The vacuum of system is provided by producer vacuum pump 17, and the vacuum of filter 12 is provided by filter vacuum pump 13.Discharge working fluid from vacuum pump and enter wash tower bottoms, and washing tower dioxide peroxide dilute solution absorbs ClO through vacuum from inspiration absorption tower
2gas enrichment.Whole production process does not have the discharge of obnoxious flavour and waste water, spent acid, and byproduct directly can be dried into Sodium sulfate anhydrous.min(99) and take out.
The inventive method has mainly carried out following improvement:
1, feed way: because hydrogen peroxide is a kind of metastable compound, easily decompose.So before hydrogen peroxide solution enters producer, in advance with sodium chlorate solution's dilution, reduce the concentration of hydrogen peroxide, hydrogen peroxide through sodium chlorate dilution mixture evenly after enter from the front lower circulation tube of producer recycle pump, form mother liquor.Effectively can prevent hydrogen peroxide from decomposing because local is excessive, suppress the generation of foaming in generator system.Also be reduce moisture to bring generation systems into simultaneously, reduce steam consumption.
2, reaction conditions controls:
(1) system pressure controls: manufacture system of the present invention operates under adopting negative pressure of vacuum condition, and under vacuum, mother liquor boiling point is lower, reduces the possibility that hydrogen peroxide decomposes in mother liquor further, improves sodium chloride crystal efficiency simultaneously and reduce ClO
2the pressure component of gas, improves the safety and stability of system.
(2) sulfuric acid concentration controls: reacted under the low acidic conditions of 1.75-2.0mol/L by the sulfuric acid controlled in reaction solution and prepare dioxide peroxide, and the byproduct that reaction is produced is neutral saltcake entirely, reduces the loss of acid.Filtering separation neutral saltcake out can become Sodium sulfate anhydrous.min(99) by convection drying simultaneously.
3, the type selecting of equipment: chlorine dioxide generator adopts the vertical producer of single container, integrates reactor, vaporizer and crystallizer.Operation system setting has emergent evacuation groove, when lengthy shut down or system need to overhaul, mother liquor can be transferred in emergent evacuation groove.Avoid discharge to cause chemical to lose, reduce environmental pollution.
Claims (3)
1. the peroxide passivation dioxide peroxide preparation method of an environment-friendly type, it is characterized in that: adopt the vertical producer of single container as chlorine dioxide generator, be connected by circulation line between chlorine dioxide generator with reboiler, raw material hydrogen peroxide adds from the pipeline be connected between chlorine dioxide generator outlet at bottom and reboiler with after sodium chlorate solution's mixed diluting in advance again, sulfuric acid adds from the trunnion of reboiler top exit, the chemical added constantly circulates between reboiler and chlorine dioxide generator, react in chlorine dioxide generator, flash distillation, by controlling the sulfuric acid of reaction solution in chlorine dioxide generator at 1.75-2.0mol/L, reaction under relatively low acidity condition is made to generate dioxide peroxide, water, oxygen and neutral saltcake, dioxide peroxide, oxygen, water vapor discharge from liquid, and saltcake is dissolved in mother liquor, after reaching capacity, separate out with crystalline form, in order to keep produce continue carry out, by filter charging pump by connect chlorine dioxide generator outlet at bottom and reboiler pipeline in a part of liquor abstraction, deliver to filter to filter, saltcake crystal filtering separation out, the mother liquor leached returns this line segments and proceeds circulating reaction, the saltcake crystal leached enters saltcake dehumidification system, dries and makes Sodium sulfate anhydrous.min(99), the dioxide peroxide mixed gas being flashed out enters vapor pipe from chlorine dioxide generator top exit and enter absorption tower after inter cooler cooling, and absorption tower refrigerated water absorbs, and becomes ClO
2the aqueous solution, delivers to ClO with shifting pump
2solution storage tank is stored, the exhaust of each groove tank is introduced in washing tower through exhaust fan suction, up to standard rear emptying with refrigerated water washing, and washing tower dioxide peroxide dilute solution enters absorption tower through vacuum self-priming and absorbs ClO
2gas enrichment.
2. the peroxide passivation dioxide peroxide preparation method of environment-friendly type according to claim 1, it is characterized in that: the hydrogen peroxide solution concentration added is 50%, the sodium chlorate solution's concentration mixed with hydrogen peroxide is 640 ~ 680g/L, temperature 45 ~ 50 DEG C; The sulfuric acid added first to be diluted with water to the concentration of 60 ~ 65% before trunnion spraying, control by controlling sulfuric acid in reaction solution at 1.75-2.0mol/L simultaneously.
3. the peroxide passivation dioxide peroxide Preparation equipment of environment-friendly type, it is characterized in that: it comprises chlorine dioxide generator (8), reboiler (4), filter gas-liquid separating tank (11), filter (12), inter cooler (23), absorption tower (22) and tail gas washing tower (16), be connected by upper circular tube (7) and lower circulation tube (25) and formed between chlorine dioxide generator (8) with reboiler (4) and circulate, lower circulation tube (25) connects producer recycle pump (3), be communicated with hydrogen peroxide and add the Hybrid connections pipe that pipe (2) and sodium chlorate add pipe (1), the liquid return tube of filter charging pump (24) and filter (12), the outlet of filter charging pump (24) connects filter (12), filter (12) is connected with filter gas-liquid separating tank (11), one end of filter gas-liquid separating tank (11) is connected with filter vacuum pump (13), the other end connects the liquid return tube of filter (12), filter (12) is provided with saltcake discharge port (10), reboiler (4) and upper circular tube (7) junction and sulfuric acid add manages (6) and is connected, chlorine dioxide generator (8) top exit connects producer vapor pipe (9), the outlet of producer vapor pipe (9) connects inter cooler (23), water shoot access absorption tower (22) of inter cooler (23), the top exit on absorption tower (22) connects producer vacuum pump (17) by the road, the bottom on absorption tower (22) connects dioxide peroxide storagetank (20) through dioxide peroxide shifting pump (21), producer vacuum pump (17), filter vacuum pump (13) all accesses tail gas washing tower (16) bottom, top and the top of absorption tower (22) of tail gas washing tower (16) are all connected refrigerated water and add pipe (14), the top of tail gas washing tower (16) connects exhaust fan (15).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107511029A (en) * | 2017-09-15 | 2017-12-26 | 广西博世科环保科技股份有限公司 | A kind of apparatus and method of chlorine dioxide tail gas absorption |
| CN108439341A (en) * | 2018-05-18 | 2018-08-24 | 广西大学 | A kind of method and device producing chlorine dioxide with high purity gas |
| CN110382409A (en) * | 2018-08-30 | 2019-10-25 | 广西博世科环保科技股份有限公司 | A kind of methanol combines the method that reduction prepares chlorine dioxide with high purity with hydrogen peroxide |
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| CN101746731A (en) * | 2009-12-16 | 2010-06-23 | 广西博世科环保科技有限公司 | Method for producing chlorine dioxide with high purity by adopting combined reducing agent |
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| CN101544354A (en) * | 2009-05-06 | 2009-09-30 | 广西大学 | A method for preparing clo2 using combined BSC reducing reagent |
| CN101746731A (en) * | 2009-12-16 | 2010-06-23 | 广西博世科环保科技有限公司 | Method for producing chlorine dioxide with high purity by adopting combined reducing agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107511029A (en) * | 2017-09-15 | 2017-12-26 | 广西博世科环保科技股份有限公司 | A kind of apparatus and method of chlorine dioxide tail gas absorption |
| CN108439341A (en) * | 2018-05-18 | 2018-08-24 | 广西大学 | A kind of method and device producing chlorine dioxide with high purity gas |
| CN110382409A (en) * | 2018-08-30 | 2019-10-25 | 广西博世科环保科技股份有限公司 | A kind of methanol combines the method that reduction prepares chlorine dioxide with high purity with hydrogen peroxide |
| WO2020041916A1 (en) * | 2018-08-30 | 2020-03-05 | 广西博世科环保科技股份有限公司 | Method for preparing high-purity chlorine dioxide using combination of methyl alcohol and hydrogen peroxide as reducing agent |
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