CN101269297B - Catalytic oxidation purification method for hydrogen cyanide in industrial waste gas - Google Patents

Catalytic oxidation purification method for hydrogen cyanide in industrial waste gas Download PDF

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Publication number
CN101269297B
CN101269297B CN200810058420XA CN200810058420A CN101269297B CN 101269297 B CN101269297 B CN 101269297B CN 200810058420X A CN200810058420X A CN 200810058420XA CN 200810058420 A CN200810058420 A CN 200810058420A CN 101269297 B CN101269297 B CN 101269297B
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hydrogen cyanide
palladium
gas
tail gas
mixed
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CN101269297A (en
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宁平
田森林
戴春皓
蒋蕾
瞿广飞
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The invention relates to a method of the catalytic oxidation and purification of tail gas containing hydrocyanic acid, in particular to a method for purifying the tail gas containing hydrocyanic acid by using a chemical method. The tail gas containing hydrocyanic acid is enabled to react with a prepared mixed catalyst solution containing palladium and copper under the temperature of 4 to 100 DEG C in a absorption tower, and the tail gas containing hydrocyanic acid is blown into the absorption tower in a gas-liquid negative-direction contact way, part of the hydrocyanic acid contacts and reacts with the palladium ions to form insoluble palladium simple substance, and part of the hydrocyanic acid reacts with the copper ions to form insoluble phosphor copper, part of the hydrocyanic acid is oxidized into phosphoric acid; all the generated substances enter into the liquid phase, and the mixed catalyst solution which absorbs the hydrocyanic acid and the purified and qualified tail gas not containing the hydrocyanic acid are acquired, the mixed hydrocyanic acid catalyst solution is oxidized into a by-product of the phosphoric acid to be used as resources again, the problems of hydrocyanic acid pollution is effectively eliminated, and the method provided by the invention provides a practical purifying method for the calcium carbide furnace gas and yellow phosphorus exhaust gas used as monocarbide chemical raw materials.

Description

The catalyzing, oxidizing and purifying method of hydrogen cyanide in a kind of industrial waste gas
One, affiliated technical field: the present invention relates to the method that a kind of catalyzing, oxidizing and purifying contains hydrogen cyanide tail gas, particularly relate to the method that contains hydrogen cyanide tail gas with the chemical method purification.
Two, background technology: hydrogen cyanide (HCN) suppresses respiratory enzyme, causes in the cell and suffocates, and acute poisoning sucks high concentration hydrogen cyanide gas in the short time, immediately breath stopped and death.In calcium carbide, fiber, phosphorus production process, can produce.For example in calcium carbide was produced, closed calcium carbide furnace calcium carbide per ton produced furnace gas 400Nrn 3, the about 2500Nm of closed calcium carbide furnace generation furnace gas amount that capacity is 25500KVA 3/ h.Calcium carbide furnace gas, its main component percent by volume consists of CO80%~85%, H 26%~8%, CO 21%~3%, O 21.5%~3.5%, N 26%~8%, HCN1500~3000mg/Nm 3, H 2S300~900mg/Nm 3Owing to be rich in CO in the calcium carbide furnace gas, can be used for carbon one chemical industry, but it is very high that carbon one chemical products require material purity, and the purity of these raw materials, productive rate and yield all have substantial connection with the height of CO concentration, so also very high to the concentration requirement of basic material gas CO.Under the situation that current energy shortage, industrial chemicals shortage, particularly petroleum resource consumption speed up, countries in the world constantly increase the demand of high-purity CO.Seek a kind of efficiently, process for separation and purification is recycled the CO in the production discharging waste gas economically, make it become the cheap raw material of carbon one chemical industry, the important topic that has become reasonable use resource, eliminated the three wastes, turns waste into wealth has crucial meaning to the development of carbon one chemical industry and hydroxyl compound probability.Utilization contains the enclosed calcium carbide furnace gas of carbon monoxide nearly 85%, by purifying the synthetic carbonizer's product in back, has both avoided environmental pollution, can reduce the production cost of calcium carbide again, and it is too high because of cost to change present calcium carbide production, nocompetitive situation on market.HCN can produce in processes such as calcium carbide production as difficult purifying contaminated thing, has not only caused environmental pollution, endangered health but also has restricted production process control, safety in production and comprehensive utilization of waste materials.At present, the purification of HCN waste gas has methods such as burning, absorption method, chemical absorbing.Firing method purifies HCN and is more common in the traditional treatment method of calcium carbide furnace gas, and it is to utilize calcium carbide furnace gas to have higher calorific value, under the high temperature of burning with HCN and other pollutant oxidation, purification.This method can not reclaim CO in the calcium carbide furnace gas, and the energy resource waste is big.
Removal method for hydrogen cyanide, disclose in the Chinese patent 02821744.6 a kind of can be with the catalyst of its decomposition, be that the chromium compound solution impregnation is gone in the silica-alumina carriers, this carrier is prepared and is contained the silica with respect to vehicle weight 1~5wt% by aluminium oxide, thereby obtain a kind of decomposition catalyst, supported with Cr on this catalyst 2O 3The form meter is with respect to the chromated oxide of this catalyst weight 10~15wt%.Contact with this decomposition catalyst by the mist that partial oxidation heavy oil and/or coal are obtained, COS and HCN that mist contains are decomposed/remove.In this case, aluminium oxide exists owing to silica and chromated oxide the time to the conversion of boehmite and is suppressed, thereby can pass through highly active catalytic reaction decomposes COS and HCN in long-time.This method is very high to the requirement of catalyst, and catalyst loses effect very soon after the use of a period of time, and cost is very high, the product after transforming simultaneously still difficulty remove.A kind of HCN of removing from gas stream is disclosed in the Chinese patent 85108796., this method is that HCN is shunted from gas with two-step method, for example remove in the synthetic air, wherein, gas stream is contacted with special oxidation agent, remove most of HCN, then, this air-flow contacts with polysulfide solution, reduces the hydrogen cyanide content in this air-flow again.This method is not good to the hydrogen cyanide removal effect of low concentration.
Three, summary of the invention
1, the object of the present invention is to provide a kind of catalyzing, oxidizing and purifying to contain the method for hydrogen cyanide tail gas, adopt hydrogen cyanide to absorb the technology of carrying out step by step with oxidation, from contain hydrogen cyanide tail gas, remove hydrogen cyanide, hydrogen cyanide is oxidized to the phosphoric acid byproduct again and realizes resource, also effectively remove the pollution problem of hydrogen cyanide, also provide practical purification method as carbonizer's raw material simultaneously for calcium carbide furnace gas, yellow phosphoric tail gas etc.
2, technical scheme of the present invention
Catalyst preparation:
1. Cu-contained catalyst comprises a kind of in elemental copper, cupric oxide, copper sulphate, copper nitrate, copper chloride, the Schweinfurt green;
2. palladium-containing catalyst comprises a kind of in simple substance palladium, palladium oxide, palladium sulfate, palladium nitrate, palladium, the palladium bichloride;
3. solvent comprises hydrochloric acid, nitric acid or sulfuric acid.
Get cupric and palladium-containing catalyst respectively stirring and dissolving in concentration is 0~30% solvent, mix, filter the mixed catalytic agent solution.Wherein the palladium mass concentration is 0.05~50g/L, and copper mass concentration is 0.1~150g/L.
The process for purifying process that contains hydrogen cyanide in the hydrogen cyanide tail gas:
To contain hydrogen cyanide tail gas in the absorption tower in 4~100 ℃ with the palladium of being prepared that contains, the mixed catalytic agent solution of copper reacts, employing contains hydrogen cyanide tail gas from lower to upper, the gas-liquid conversed from top to bottom way of contact of mixed catalytic agent solution feeds the absorption tower, generate the palladium simple substance of indissoluble after part hydrogen cyanide and the palladium ion haptoreaction, part hydrogen cyanide and copper ion generate the phosphor-copper of indissoluble, the part hydrogen cyanide is oxidized to phosphoric acid, they all enter liquid phase, be absorbed hydrogen cyanide the mixed catalytic agent solution and do not contain the qualified tail gas of purification of hydrogen cyanide, palladium simple substance, the generation of phosphor-copper can make mixed catalyst solution become black suspension.Described absorption tower can be a kind of in turbulent contact absorber, tray absorption columns, bubble absorbing tower, venturi scrubber, the stirring bubble absorbing tower.
Be rich in carbon monoxide in enclosed calcium carbide furnace gas, the yellow phosphoric tail gas, after purifying, can be used as carbonizer's unstripped gas.If by purifying again after the oxygenating, then may also reduce the selectivity of catalyzing, oxidizing and purifying simultaneously owing to the oxygenating process is sneaked into more foreign gas.Therefore, adopt hydrogen cyanide to absorb the technology of carrying out step by step with oxidation to removing of hydrogen cyanide in the enclosed calcium carbide furnace gas, purified gas also is used as the raw material of other production links.
The mixed catalytic agent solution that will absorb hydrogen cyanide is then sent into oxidizing tower and is carried out oxidation, in oxidizing tower, blast air or oxygen, make the hydrogen cyanide that is absorbed in the solution and oxygen generation oxidation reaction and become carbon dioxide, nitrogen G﹠W, palladium simple substance then is oxidized to the divalence palladium ion.Mixed solution after the oxidation is discharged from oxidizing tower, sends into the absorption tower again and recycles.Oxidizing tower can be a kind of in packed column reactor, rapid ball absorption reactor thermally, plate-type reactor, bubbling reactor, falling film reactor, the stirring bubbling reactor.
Catalytic oxidation principle:
4HCN+5O 2→2N 2+4CO 2+2H 2O
3, the advantage that is compared with prior art had
1. the active height of catalyst, good stability, selectivity are good.The hydrogen cyanide that contains in enclosed calcium carbide furnace gas, the yellow phosphoric tail gas is its difficult point of carrying out recycling as carbonizer's unstripped gas, and catalyst of the present invention can make the removal efficiency of hydrogen cyanide keep 100% for a long time in the purification of enclosed calcium carbide furnace gas, yellow phosphoric tail gas, the enclosed calcium carbide furnace gas after the purification satisfy as in carbonizer's unstripped gas to the requirement of hydrogen cyanide content.The high activity, high stability and the high selectivity that possess as good catalyst have been shown;
2. catalyst is prepared easily, can adapt to the hydrogen cyanide concentration range of broad, and what can be applicable to produce in yellow phosphoric tail gas, enclosed calcium carbide furnace gas, the fiber production process contains removing of hydrogen cyanide in the hydrogen cyanide tail gas;
3. catalyst can be recycled, and has reduced the purification cost.
Five, the specific embodiment
Embodiment 1: the tail gas of processing is calcium carbide furnace gas, and its main component percent by volume is CO80~85%, H 26~8%, CO 21~3%, O 21.5~3.5%, N 26~8%, HCN1500~3000mg/Nm 3, H 2S300~900mg/Nm 3Get 2.1kg copper sulphate (being equivalent to 840g copper) and be dissolved in the 5L water, the 0.2kg palladium sulfate is dissolved in the hydrochloric acid of 5L10%, both is mixed again, and filters, and discards filter residue, obtains 10L mixed catalyst solution for standby.
Will be through being that main component, hydrogen cyanide content are 1500~3000mg/Nm with CO after washing and the alkali cleaning 3Calcium carbide furnace gas with 10m 3/ h flow velocity feeds in the tower from spraying bottom, absorption tower, and the mixed catalytic agent solution for preparing sprays into from spraying top, absorption tower with 2L/h, and gas-liquid conversed contact is in 40 ℃ of reactions down of tower temperature.The mixed catalytic agent solution that has absorbed hydrogen cyanide is sent into to stir in the bubbling reactor and is carried out oxidation, and the feeding flow velocity is 5m 3It is recycling that the air of/h, the absorption liquid after the oxidation pump into the spraying absorption tower with pump again.After measured, hydrogen cyanide content is 0mg/m in the yellow phosphoric tail gas behind the absorption cleaning of spraying absorption tower 3
Embodiment 2: the tail gas of processing is yellow phosphoric tail gas, and its main component percent by volume is CO85~95%, H 21~8%, CO 21~4%, O 20~1%, N 22~5%, HCN100~300mg/Nm 3, H 2S800~3000mg/Nm 3, PH 3500~1300mg/Nm 3Get the 2.1kg copper chloride and be dissolved in the 5L water, the 0.2kg palladium oxide is dissolved in the sulfuric acid of 5L10%, both is mixed again, and filters, and discards filter residue, obtains 10L mixed catalyst solution for standby.
Will be through being that main component, hydrogen cyanide content are 100~300mg/Nm with CO after washing and the alkali cleaning 3Yellow phosphoric tail gas with 30m 3/ h flow velocity feeds in the tower from spraying bottom, absorption tower, and the mixed catalytic agent solution for preparing sprays into from spraying top, absorption tower with 2L/h, and gas-liquid conversed contact is in 20 ℃ of reactions down of tower temperature.The mixed catalytic agent solution that has absorbed hydrogen cyanide is sent into to stir in the bubbling reactor and is carried out oxidation, and the feeding flow velocity is 8m 3It is recycling that the air of/h, the absorption liquid after the oxidation pump into the spraying absorption tower with pump again.After measured, hydrogen cyanide content is 0mg/m in the yellow phosphoric tail gas behind the absorption cleaning of spraying absorption tower 3

Claims (3)

1. the catalyzing, oxidizing and purifying method of hydrogen cyanide in the industrial waste gas, it is characterized in that: it is finished according to the following steps,
1), get cupric and palladium-containing catalyst respectively stirring and dissolving in concentration is 0~30% solvent, mix, filter the mixed catalytic agent solution, wherein the palladium mass concentration is 0.05~50g/L, copper mass concentration is 0.1~150g/L; Described Cu-contained catalyst comprises a kind of in elemental copper, cupric oxide, copper sulphate, copper nitrate, copper chloride and the Schweinfurt green; Described palladium-containing catalyst comprises a kind of in simple substance palladium, palladium oxide, palladium sulfate, palladium nitrate, palladium and the palladium bichloride; Described solvent comprises hydrochloric acid, nitric acid or sulfuric acid;
2), will contain hydrogen cyanide tail gas reacts with the mixed catalytic agent solution in 4~100 ℃ in the absorption tower, contain hydrogen cyanide tail gas from lower to upper, the gas-liquid conversed from top to bottom contact of mixed catalytic agent solution, feed the absorption tower, the reaction back generates palladium simple substance, phosphor-copper and phosphoric acid enter liquid phase, and the mixed catalytic agent solution of the hydrogen cyanide that has been absorbed reaches the qualified tail gas of purification that does not contain hydrogen cyanide, and the described hydrogen cyanide tail gas that contains is calcium carbide furnace gas or yellow phosphoric tail gas;
3), the mixed catalytic agent solution that will absorb hydrogen cyanide is sent into oxidizing tower and is carried out oxidation, blast air or oxygen, make the hydrogen cyanide that is absorbed in the solution and oxygen generation oxidation reaction and become carbon dioxide, nitrogen G﹠W, mixed solution after the oxidation is discharged from oxidizing tower, sends into the absorption tower again and recycles.
2. the catalyzing, oxidizing and purifying method of hydrogen cyanide in the industrial waste gas according to claim 1 is characterized in that: the tail gas of processing is calcium carbide furnace gas, and its HCN content is 1500~3000mg/Nm 3, get 2.1kg copper sulphate and be dissolved in the 5L water, the 0.2kg palladium sulfate is dissolved in the hydrochloric acid of 5L10%, both is mixed again, and filters, and discards filter residue, obtains 10L mixed catalyst solution for standby, with calcium carbide furnace gas with 10m 3/ h flow velocity feeds in the tower from spraying bottom, absorption tower, the mixed catalytic agent solution for preparing sprays into from spraying top, absorption tower with 2L/h, and gas-liquid conversed contact is in 40 ℃ of reactions down of tower temperature, the mixed catalytic agent solution that has absorbed hydrogen cyanide is sent into to stir in the bubbling reactor and is carried out oxidation, and the feeding flow velocity is 5m 3The air of/h, the absorption liquid after the oxidation pump into the spraying absorption tower with pump again and recycle.
3. the catalyzing, oxidizing and purifying method of hydrogen cyanide in the industrial waste gas according to claim 1 is characterized in that: the tail gas of processing is yellow phosphoric tail gas, and its HCN content is 100~300mg/Nm 3, get the 2.1kg copper chloride and be dissolved in the 5L water, the 0.2kg palladium oxide is dissolved in the sulfuric acid of 5L10% and obtains 10L mixed catalyst solution for standby, with yellow phosphoric tail gas with 30m 3/ h flow velocity feeds in the tower from spraying bottom, absorption tower, the mixed catalytic agent solution for preparing sprays into from spraying top, absorption tower with 2L/h, in the reaction down of 20 ℃ of tower temperature, the mixed catalytic agent solution that has absorbed hydrogen cyanide is sent into to stir in the bubbling reactor and is carried out oxidation, and the feeding flow velocity is 8m 3The air of/h, the absorption liquid after the oxidation pump into the spraying absorption tower with pump again and recycle.
CN200810058420XA 2008-05-21 2008-05-21 Catalytic oxidation purification method for hydrogen cyanide in industrial waste gas Expired - Fee Related CN101269297B (en)

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* Cited by examiner, † Cited by third party
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CN102019141A (en) * 2010-12-20 2011-04-20 昆明理工大学 Process for purifying tail gas containing hydrothion by using liquid phase catalytic oxidation method
CN102921285B (en) * 2012-11-08 2015-02-25 南京大学 Method for processing waste gases containing hydrogen cyanide
CN103071370B (en) * 2013-01-24 2014-09-03 昆明理工大学 Method and device for purifying hydrogen cyanide industrial waste gas by electrodialysis
CN104190429B (en) * 2014-09-04 2016-07-20 昆明理工大学 A kind of preparation method of HCN hydrolyst
CN105057100B (en) * 2015-08-03 2016-09-21 昆明理工大学 A kind of dust purified in coal gas and the method for HCN
CN106492627B (en) * 2016-11-28 2019-09-10 永康市禄祥环保科技有限公司 Organic exhaust gas solubilising is catalyzed solvent
CN108144438A (en) * 2017-12-04 2018-06-12 佛山杰致信息科技有限公司 A kind of preparation method of hydrogen cyanide cleanser

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EP0757969A1 (en) * 1995-08-08 1997-02-12 Exxon Research And Engineering Company Process for removing hydrogen cyanide from synthesis gas
CN1176737C (en) * 2002-09-27 2004-11-24 中国科学院山西煤炭化学研究所 Method for removing waste gas containing HCN by platinum-rhodium-palladium catalyst
CN1203918C (en) * 2003-04-30 2005-06-01 中国科学院山西煤炭化学研究所 Catalyst with Cu being loaded for taking off waste gas containing HCN and its preparing method as well as application
CN1830773A (en) * 2006-02-24 2006-09-13 昆明理工大学 Method of purifying furnace gas of closed calcium carbide furnace
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Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4521530A (en) * 1983-06-15 1985-06-04 Teledyne Industries, Inc., Teledyne Water Pik Catalyst of palladium, copper and nickel on a substrate
US4474739A (en) * 1983-06-29 1984-10-02 Teledyne Industries, Inc. Method for removing gaseous pollutants in highly dilute concentrations from air at room temperatures
EP0757969A1 (en) * 1995-08-08 1997-02-12 Exxon Research And Engineering Company Process for removing hydrogen cyanide from synthesis gas
CN1176737C (en) * 2002-09-27 2004-11-24 中国科学院山西煤炭化学研究所 Method for removing waste gas containing HCN by platinum-rhodium-palladium catalyst
CN1203918C (en) * 2003-04-30 2005-06-01 中国科学院山西煤炭化学研究所 Catalyst with Cu being loaded for taking off waste gas containing HCN and its preparing method as well as application
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WO2007124865A1 (en) * 2006-04-28 2007-11-08 Haldor Topsøe A/S Process for the removal of hydrogen cyanide and formic acid from synthesis gas

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