CN105439091B - The peroxide passivation chlorine dioxide preparation method and equipment of environment-friendly type - Google Patents
The peroxide passivation chlorine dioxide preparation method and equipment of environment-friendly type Download PDFInfo
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- CN105439091B CN105439091B CN201510873365.XA CN201510873365A CN105439091B CN 105439091 B CN105439091 B CN 105439091B CN 201510873365 A CN201510873365 A CN 201510873365A CN 105439091 B CN105439091 B CN 105439091B
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Abstract
The invention discloses the peroxide passivation chlorine dioxide preparation method and equipment of a kind of environment-friendly type, this method is that raw material hydrogen peroxide is first well mixed to the lower circulation pipe for being then sent through generator with sodium chlorate solution, sulfuric acid is added from the trunnion of reboiler top exit, and chlorine dioxide, oxygen, neutral saltcake and water are generated in reactor reaction.Chlorine dioxide mixed gas enters inter cooler at the top of generator, is absorbed subsequently into absorption tower with chilled water, turns into ClO2The aqueous solution.The saltcake crystal separated out from generator mother liquor, the filtering of salt-cake filter is sent to by the way that partial mother liquid is extracted out, saltcake crystal is separated by filtration out.The mother liquor filtered out returns to generator, and the saltcake crystal filtered out enters saltcake drying system, and glauber salt is made in drying.The each groove tank exhaust of system is attracted into scrubbing tower, with the rear emptying up to standard of freezing water washing.The inventive method does not have spent acid discharge, and glauber salt take-away is can be made into after the neutral filtered drying of saltcake caused by reaction, without solid waste discharge, belongs to the production technology of clean environment firendly.
Description
Technical field
The present invention relates to chlorine dioxide production technical field, prepared by the peroxide passivation chlorine dioxide of specifically a kind of environment-friendly type
Method and apparatus.
Technical background
Chlorine dioxide is orange-yellow gas at normal temperatures and pressures, and outward appearance chlorine similar with smell, boiling point is 11 DEG C, freezing point
For -59 DEG C, at 11 DEG C, gaseous density is that 3.09g/m3. gaseous chlorine dioxides are unstable, it is heated during high concentration, by illumination or with
Organic matter is in contact the decomposition that can set off an explosion.Chlorine dioxide is soluble in water, is spread with molecular forms, is formed volatile
Yellow-green soln.Chlorine dioxide hardly hydrolyzes in water, and is not combined with organic matter, does not generate chloroform carcinogenic substance
Matter, also do not reacted with ammonia.ClO 2 solution concentration is in the basic danger without blast of below 10g/l.
Chlorine dioxide is a kind of extremely strong oxidant, stable chlorine dioxide be considered as work well, superior performance
Bactericide, disinfectant, bleaching agent.Chlorine dioxide is widely used in the bleaching of paper pulp, fiber；Trade effluent, hospital sewage, industry follow
Ring cold water process；Water body disinfection diseases prevention, oil exploitation etc. in soil antivirus, aquaculture.Chlorine dioxide with high purity is also
It can apply to the anti-of the disinfection, the sterilization in food processing, food (meat, aquatic products, fruits and vegetables) of clinical treatment
It is rotten fresh-keeping etc..
Research on preparing chlorine dioxide method is very active always, and the production technology up to ten of shaping is several but each
Kind method has its distinguished advantage, while also has the defects of obvious.Mainly using R1 methods, R3 in industrial production application at present
Method, R5 methods, R8 methods.It is reducing agent i.e. with sulfur dioxide, chlorion, methanol, prepares two with sodium chlorate reaction in acid condition
Chlorine monoxid.Chlorine dioxide is prepared by reducing process, agent of sulfur dioxide, conversion ratio is not high, the inconvenience of sulfur dioxide source, meeting in product
Carry sulfur dioxide, chlorine secretly, product purity is not high.Chlorine dioxide is prepared by reducing agent of chlorion, raw material sources are convenient, but turn
Rate is not high, often obtains 1mol chlorine dioxide while can produce 0.5mol chlorine, it is necessary to especially be handled product.With
Methanol is that reducing agent prepares chlorine dioxide, can be obtained by the different generation formaldehyde of reducing degree, formic acid, carbon dioxide and not complete
The methanol of full response.Methanol, formaldehyde and formic acid are all noxious materials, and they can be restricted to the application of product.
Developing low-cost, high-purity, pollution-free, safe and reliable chlorine dioxide production new technology and process units, substitute
High cost, the old technology of maximum discharge, to alleviating environmental protection pressure, promoting national economic development, there is important economic implications and society
Can meaning.At present, prepared by hydrogen peroxide method only has on a small quantity in the gaseous product of chlorine dioxide generation or does not form chlorine, by-product
Product oxygen is favourable to environmental protection to bleaching together with chlorine dioxide.And because this method raw material sources are convenient, cheap, high conversion rate,
Product purity is high, and the features such as speed is fast occurs, deep to be paid close attention to by people.The chemical principle of this method is：
6NaClO3+3H2O2+H2SO4→6ClO2+2Na3H(SO4)2+3O2+6H2O
In hydrogen-peroxide reduction method production chlorine dioxide, the sulfate that sulfuric acid concentration difference is then formed is different.Work as sulphur
When acid concentration is 1--2.5mol/L, higher reaction rate and efficiency can be obtained, produces neutral saltcake, reaction principle is：
2NaClO3+H2O2+H2SO4→2ClO2+Na2SO4+O2+2H2O
When sulfuric acid concentration is 2.5--5.5mol/L, reaction speed and efficiency are very high, and it is seldom to produce chlorine content
Product, byproduct acidity saltcake is produced, its reaction principle is：
6NaClO3+3H2O2+H2SO4→6ClO2+2Na3H(SO4)2+3O2+6H2O
When the concentration of sulfuric acid is more than 5.5mol/L, caused byproduct is disulfate.Its reaction principle is as follows：
2NaClO3+H2O2+2H2SO4→2ClO2+2NaHSO4+O2+2H2O
Domestic peroxide passivation chlorine dioxide preparing process is substantially using multi-stage aeration formula generator at present.From chloric acid
The economic benefits such as conversion ratio, purity of chlorine dioxide and the yield of sodium consider that sulfuric acid is excessive with various concentrations in multi-stage generator
In the presence of so in production prepares chlorine dioxide, substantial amounts of spent acid discharge being present, environment caused seriously to pollute.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of peroxide passivation chlorine dioxide preparation method of environment-friendly type.Should
Method realizes that preparation process does not have spent acid discharge, clean environment firendly.
The present invention solves above-mentioned technical problem with following technical scheme：
A kind of peroxide passivation chlorine dioxide preparation method of environment-friendly type of the present invention, using the vertical generator conduct of single container
Chlorine dioxide generator, connected between chlorine dioxide generator and reboiler by circulation line, raw material hydrogen peroxide is in advance and chlorine
After acid sodium solution mixed diluting again from connection chlorine dioxide generator outlet at bottom and reboiler between pipeline add, sulfuric acid from
The trunnion of reboiler top exit adds, and the chemicals of addition constantly circulates between reboiler and chlorine dioxide generator,
React, flash in chlorine dioxide generator, by control the sulfuric acid of reaction solution in chlorine dioxide generator 1.75-
2.0mol/L, reaction generation chlorine dioxide, water, oxygen and neutral saltcake under the conditions of relatively low acidity；Chlorine dioxide, oxygen gas and water
Steam is discharged from liquid, and saltcake is dissolved in mother liquor, after reaching saturation, is separated out with crystal form；In order to keep producing
Lasting progress, a part in the pipeline of chlorine dioxide generator outlet at bottom and reboiler will be connected by filter charging pump
Liquor abstraction, filter filtering is sent to, saltcake crystal is separated by filtration out, the mother liquor filtered out returns to the line segments and continued
Circular response, the saltcake crystal filtered out enter saltcake drying system, and glauber salt is made in drying；The chlorine dioxide for being flashed out mixes
Close gas to enter blast pipe from chlorine dioxide generator top exit and enter after inter cooler cools down absorption tower, absorption tower is with cold
Freeze water to absorb, turn into ClO2The aqueous solution, ClO is pumped to transfer2Solution storage tank is stored；Each groove tank exhaust is taken out through exhaust fan
It is attracted into scrubbing tower, with the rear emptying up to standard of freezing water washing, scrubbing tower chlorine dioxide weak solution enters through vacuum self-priming to be absorbed
Tower absorbs ClO2Gas enrichment.
It is 50% to control the hydrogen peroxide solution concentration added, sodium chlorate solution's concentration mix with hydrogen peroxide for 640~
680g/L, 45~50 DEG C of temperature；The sulfuric acid of addition is first diluted with water to 60~65% concentration, same time control before trunnion is injected into
System is by controlling the sulfuric acid in reaction solution in 1.75-2.0mol/L.
The peroxide passivation chlorine dioxide Preparation equipment of environment-friendly type of the present invention, it include chlorine dioxide generator 8, reboiler 4,
Filter gas-liquid knockout drum 11, filter 12, inter cooler 23, absorption tower 22 and tail gas washing tower 16, chlorine dioxide generator 8 with
Connected between reboiler 4 by upper circular tube 7 and lower circulation pipe 25 and form circulation, lower circulation pipe 25 connects generator circulating pump
3rd, the liquid of the Hybrid connections pipe of connection hydrogen peroxide addition pipe 2 and sodium chlorate's addition pipe 1, filter charging pump 24 and filter 12
Body return duct, the outlet connection filter 12 of filter charging pump 24, filter 12 are connected with filter gas-liquid knockout drum 11, mistake
One end of filter knockout drum 11 is connected with filter vacuum pump 13, and the other end connects the liquid return tube of filter 12, mistake
Filter 12 is provided with saltcake discharging opening 10；Reboiler 4 adds pipe 6 with sulfuric acid with the junction of upper circular tube 7 and is connected, and chlorine dioxide occurs
The top exit of device 8 connection generator blast pipe 9, the outlet connection inter cooler 23 of generator blast pipe 9, the drainpipe of inter cooler 23
Absorption tower 22 is accessed, the top exit on absorption tower 22 connects generator vavuum pump 17 by the road, and the bottom on absorption tower 22 is through dioxy
Change chloride shift pump 21 and connect chlorine dioxide storagetank 20, generator vavuum pump 17, filter vacuum pump 13 access washing tail gas
The bottom of tower 16, the top of tail gas washing tower 16 and the top on absorption tower 22 are all connected with chilled water and add pipe 14, tail gas washing tower 16
Top connection exhaust fan 15.
The present invention has the advantages that：
1st, three big raw materials are respectively changed by evaporating in water tariff collection generator liquid level, mother liquor in the continuous circular response of generator
Product concentration, discharged without spent acid.
2nd, reaction generates neutral saltcake, is not acid saltcake, reduces the loss of acid；It can be made after the neutral filtered drying of saltcake
Taken out into glauber salt, without solid waste discharge.
3rd, tail gas from absorption tower is conveyed to scrubbing tower and carries out double absorption, and each groove tank exhaust is also aspirated through blower fan introduces washing
In tower, discharged after up to standard；Chlorine dioxide weak solution after washing returns to absorption tower and absorbs chlorine dioxide enrichment, without pernicious gas
And discharge of wastewater.
Brief description of the drawings
Fig. 1 is the device structure and process chart that the present invention uses.
Embodiment
The inventive method and equipment are further described with reference to Fig. 1：
The peroxide passivation of environment-friendly type of the present invention prepare chlorine dioxide plant mainly by generator circulating pump 3, reboiler 4, on
Circulation pipe 7, chlorine dioxide generator 8, lower circulation pipe 25, filter gas-liquid knockout drum 11, filter 12, filter vacuum pump
13rd, filter charging pump 24, inter cooler 23, absorption tower 22, tail gas washing tower 16 and related pipeline composition.Chlorine dioxide generator
Connected between 8 and reboiler 4 by upper circular tube 7 and lower circulation pipe 25 and form circulation, the bottom of reboiler 5 meets condensed water row
Water pipe, top connect steam and add pipe 5, and generator circulating pump 3, connection hydrogen peroxide add pipe 2 and sodium chlorate adds the mixing company of pipe 1
The liquid return tube of adapter, filter charging pump 24 and filter 12 is respectively connected to lower circulation pipe 25, filter charging pump 24
Outlet connection filter 12, filter 12 is connected with filter gas-liquid knockout drum 11, one end of filter gas-liquid knockout drum 11
It is connected with filter vacuum pump 13, the other end connects the liquid return tube of filter 12, and filter 12 is provided with saltcake discharging opening 10；
Reboiler 4 adds pipe 6 with sulfuric acid with the junction of upper circular tube 7 and is connected, the top exit of chlorine dioxide generator 8 connection generator
Blast pipe 9, the outlet connection inter cooler 23 of generator blast pipe 9, the drainpipe access absorption tower 22 of inter cooler 23, absorption tower 22
Top exit connect generator vavuum pump 17 by the road, the bottom on absorption tower 22 connects titanium dioxide through chlorine dioxide shifting pump 21
Chlorine storagetank 20, chlorine dioxide storagetank 20 connect chlorine dioxide delivery pipe 18 through chlorine dioxide delivery pump 19.Generator vacuum
Pump 17, filter vacuum pump 13 access the bottom of tail gas washing tower 16, the top of tail gas washing tower 16 and the top on absorption tower 22
It is all connected with chilled water and adds pipe 14, the top connection exhaust fan 15 of tail gas washing tower 16, the bottom of tail gas washing tower 16 is through pipe
The top on absorption tower 22 is accessed on road.
During preparation, sodium chlorate solution's (concentration be 640~680g/L, 45~50 DEG C of temperature) for coming from the pumping of sodium chlorate storage tank
Pipe 1 is added through sodium chlorate to add from lower circulation pipe 25, the concentrated sulfuric acid (concentration 98%, normal temperature) come from the pumping of concentrated sulfuric acid storage tank is through sulphur
Acid adds pipe 6 and sprays addition from the trunnion of the top exit of reboiler 4, is injected into before trunnion first with water diluting concentrated sulfuric acid to concentration
(highly exothermic cause local temperature to be diluted with water when preventing the concentrated sulfuric acid from entering after circulation pipe and being mixed with reaction solution for 60~65%
It is too high), circulation is mixed to form reaction mother liquor.Hydrogen peroxide solution (concentration 50%, the normal temperature) warp come from the pumping of hydrogen peroxide storage tank
Hydrogen peroxide adds pipe 2 and is added to the Hybrid connections pipe that connection hydrogen peroxide adds pipe 2 and sodium chlorate's addition pipe 1, makes hydrogen peroxide advance
It is sufficiently mixed with sodium chlorate solution and enters back into lower circulation pipe 25, the hydrogen peroxide for preventing from entering local concentration in circulation pipe is too high anti-
It excessively should acutely cause chlorine dioxide decomposition.Chemicals in the presence of circulating pump 3 constantly reboiler 4 and generator 8 it
Between circulate, reaction, flash distillation in the generator 8.As sodium chlorate solution, the concentrated sulfuric acid, hydrogen peroxide solution constantly add, mother liquor exists
Constantly circulated in the presence of circulating pump 3 between reboiler 5 and generator 9, reaction will be carried out constantly, while control reaction
The reaction under the conditions of 1.75-2.0mol/L low in acidity of sulfuric acid in liquid prepares chlorine dioxide, and caused neutral saltcake is occurring
In device can be separated out with crystal form, by filter charging pump 24 from lower circulation pipe 15 a part of liquor abstraction, be sent to filtering
Machine 12 is filtered, and saltcake crystal is separated by filtration out.The mother liquor filtered out returns in filter steam-water separation tank 11 from gravity to be occurred
The device circulatory system continues cycling through reaction, and saltcake enters saltcake drying system through saltcake discharging opening 13, and glauber salt is made in drying.Release
Chlorine dioxide mixed gas out comes out at the top of generator, is cooled down through generator blast pipe 10 into inter cooler 17, then
Absorbed into 19 chilled water of absorption tower, turn into ClO2The aqueous solution, ClO is delivered to shifting pump 212Solution storage tank 20 is stored.Occur
The gas and the exhaust of each groove tank of system that device vavuum pump 17, filter vacuum pump 13 eject aspirate through exhaust fan 15 to be introduced
In scrubbing tower, with the rear emptying up to standard of freezing water washing.The vacuum of system is provided by generator vavuum pump 17, the vacuum of filter 12
There is provided by filter vacuum pump 13.Enter wash tower bottoms, and scrubbing tower chlorine dioxide weak solution from vavuum pump discharge working solution
Through vacuum ClO is absorbed from inspiration absorption tower2Gas enrichment.Whole production process does not have pernicious gas and waste water, the discharge of spent acid,
Byproduct can directly be dried into glauber salt take-away.
The inventive method has been substantially carried out following improvement：
1st, feed way：Because hydrogen peroxide is a kind of metastable compound, easily decompose.So dioxygen is water-soluble
Liquid enters before generator, is diluted in advance with sodium chlorate solution, reduces the concentration of hydrogen peroxide, and hydrogen peroxide is equal through sodium chlorate dilution mixing
Enter after even from the front lower circulation pipe of generator circulating pump, form mother liquor.It can effectively prevent hydrogen peroxide from being decomposed because local excessive,
Suppress the generation foamed in generator system.Simultaneously and reduction moisture brings generation system into, reduces steam consumption.
2nd, reaction condition controls：
(1) system pressure controls：Present invention production preparation system operates under the conditions of using negative pressure of vacuum, in vacuum condition
Under, mother liquor boiling point is relatively low, further reduces the possibility that hydrogen peroxide decomposes in mother liquor, while improve sodium chloride crystal efficiency and reduce
ClO2The partial pressure of gas, improve the safety and stability of system.
(2) sulfuric acid concentration controls：By controlling the sulfuric acid in reaction solution under the conditions of 1.75-2.0mol/L low in acidity
Reaction prepares chlorine dioxide, the byproduct that reaction produces is all neutral saltcake, reduces the loss of acid.It is separated by filtration out simultaneously
Neutral saltcake can be with convection drying into glauber salt.
3rd, the type selecting of equipment：Chlorine dioxide generator uses the vertical generator of single container, collection reactor, evaporator and knot
Brilliant device is integrated.System is provided with emergent evacuation groove, and when long-term shutdown or system need maintenance, mother liquor can be transferred to urgent row
In dead slot.Avoid discharge from causing chemicals to lose, reduce environmental pollution.
Claims (2)
- A kind of 1. peroxide passivation chlorine dioxide preparation method of environment-friendly type, it is characterised in that：Using the vertical generator of single container As chlorine dioxide generator, connected between chlorine dioxide generator and reboiler by circulation line, raw material hydrogen peroxide is advance With being added again from the pipeline being connected between chlorine dioxide generator outlet at bottom and reboiler after sodium chlorate solution's mixed diluting, sulphur Acid adds from the trunnion of reboiler top exit, and the chemicals of addition constantly follows between reboiler and chlorine dioxide generator Ring, react, flash in chlorine dioxide generator, by control the sulfuric acid of reaction solution in chlorine dioxide generator 1.75- 2.0mol/L, make reaction generation chlorine dioxide, water, oxygen and neutral saltcake under the conditions of relatively low acidity；Chlorine dioxide, oxygen, Water vapour is discharged from liquid, and saltcake is dissolved in mother liquor, after reaching saturation, is separated out with crystal form；In order to keep raw The lasting progress of production, by filter charging pump by one in the pipeline for connecting chlorine dioxide generator outlet at bottom and reboiler Decomposition mother solution extract out, be sent to filter filtering, saltcake crystal is separated by filtration out, the line segments that the mother liquor filtered out return to continue into Row circular response, the saltcake crystal filtered out enter saltcake drying system, and glauber salt is made in drying；The chlorine dioxide for being flashed out Mixed gas enters blast pipe from chlorine dioxide generator top exit and enters absorption tower after inter cooler cools down, and absorption tower is used Chilled water absorbs, and turns into ClO2The aqueous solution, ClO is pumped to transfer2Solution storage tank is stored；Each groove tank exhaust is through exhaust fan Suction is introduced into scrubbing tower, and with the rear emptying up to standard of freezing water washing, scrubbing tower chlorine dioxide weak solution enters through vacuum self-priming inhales Receive tower and absorb ClO2Gas enrichment；The hydrogen peroxide solution concentration of the addition is 50%, the sodium chlorate solution mixed with hydrogen peroxide Concentration is 640~680g/L, 45~50 DEG C of temperature；The sulfuric acid of addition is first diluted with water to 60~65% before trunnion is injected into Concentration, while the sulfuric acid in reaction solution is controlled in 1.75-2.0mol/L.
- 2. the peroxide passivation chlorine dioxide Preparation equipment of environment-friendly type, it is characterised in that：It includes chlorine dioxide generator (8), again Boil device (4), filter gas-liquid knockout drum (11), filter (12), inter cooler (23), absorption tower (22) and tail gas washing tower (16), it is connected and is formed by upper circular tube (7) and lower circulation pipe (25) between chlorine dioxide generator (8) and reboiler (4) Circulation, lower circulation pipe (25) connection generator circulating pump (3), connection hydrogen peroxide add pipe (2) and sodium chlorate adds the mixed of pipe (1) The liquid return tube of connecting tube, filter charging pump (24) and filter (12) is closed, the outlet of filter charging pump (24) connects Filter (12) is taken over, filter (12) is connected with filter gas-liquid knockout drum (11), one end of filter gas-liquid knockout drum (11) It is connected with filter vacuum pump (13), the liquid return tube of other end connection filter (12), filter (12) goes out provided with saltcake Material mouth (10)；Reboiler (4) adds pipe (6) with sulfuric acid with upper circular tube (7) junction and is connected, chlorine dioxide generator (8) top Portion's outlet connection generator blast pipe (9), the outlet connection inter cooler (23) of generator blast pipe (9), the row of inter cooler (23) Water pipe accesses absorption tower (22), and the top exit of absorption tower (22) connects generator vavuum pump (17), absorption tower (22) by the road Bottom through chlorine dioxide shifting pump (21) connect chlorine dioxide storagetank (20), generator vavuum pump (17), filter vacuum Pump (13) accesses tail gas washing tower (16) bottom, and the top of tail gas washing tower (16) and the top of absorption tower (22) are all connected with cold Freeze water and add pipe (14), the top connection exhaust fan (15) of tail gas washing tower (16).
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| 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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| CN101544354A (en) * | 2009-05-06 | 2009-09-30 | 广西大学 | A method for preparing clo2 using combined BSC reducing reagent |
| CN101746731B (en) * | 2009-12-16 | 2011-09-14 | 广西博世科环保科技股份有限公司 | Method for producing chlorine dioxide with high purity by adopting combined reducing agent |
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