CN107008459A - It is a kind of for catalyst of chlorinated organics low-temperature catalytic burning and its preparation method and application - Google Patents
It is a kind of for catalyst of chlorinated organics low-temperature catalytic burning and its preparation method and application Download PDFInfo
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- CN107008459A CN107008459A CN201710174632.3A CN201710174632A CN107008459A CN 107008459 A CN107008459 A CN 107008459A CN 201710174632 A CN201710174632 A CN 201710174632A CN 107008459 A CN107008459 A CN 107008459A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
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Abstract
The invention discloses a kind of catalyst for chlorinated organics low-temperature catalytic burning, it is the transition metal oxide that sulfuric acid is modified, described transition metal oxide is zirconium oxide, titanium oxide or iron oxide, sulfuric acid is present in transition metal oxide surface in the form of bidentate sulfate, and the mass fraction of element sulphur is 0.5~3wt%.The invention also discloses the preparation method of described catalyst and its application in chlorinated organics low-temperature catalytic burning.The catalyst of transition metal oxide of the sulfuric acid modification of the present invention not only has higher catalytic activity, combustion oxidation of the chlorinated organics including chloride aliphatic hydrocarbon and chloride aromatic hydrocarbon can be catalyzed at a lower temperature, primary combustion product is carbon dioxide, hydrogen chloride and chlorine, the chloro-product for not having secondary pollution is formed, and prepare simply, cost is low, long lifespan, it is adapted to the processing of complex industrial waste gas, the application prospect with industrial waste gas processing.
Description
Technical field
The invention belongs to organic compound catalytic combustion technology field, it is related specifically to a kind of for chlorinated organics low temperature
It is catalyzed catalyst of burning and preparation method thereof and the application in chlorinated organics low-temperature catalytic burning.
Background technology
Chlorinated organics mainly include aromatic hydrocarbon chloride (such as chlorobenzene, dichloro-benzenes) and non-aromatic hydro carbons chloride, such as two
Chloromethanes (DCM), chloroform (CHCl3), dichloroethanes (DCE) and trichloro ethylene (TCE) etc..Chlorinated organics can be to environment and people
The health of class causes serious harm, and the influence of lasting accumulation property can be caused to biosystem, and it is smelly to destroy air
Oxygen layer.It is all chlorine-containing organic to have 12 persistent organic pollutions for being classified as first place in united nations environment project international treaties
Compound.In 41 kinds of hazardous VOCs that American National Environmental Protection Agency (EPA) delimit, there are 32 kinds to fall within chlorinated organics.
Chlorinated organics are obtained extensively as conventional organic solvent, organic synthesis raw material and semi-finished product in Chemical Manufacture
General application, such as intermediate of thermal conductivity liquid, extinguishing chemical and chemical products and the accessory substance of power industry, and chloro oxidant
Wood pulp float white, chlorine industry oxygen chlorine method prepares the industries such as vinyl chloride process, process hides, washing, pharmacy.Due to above-mentioned generation
The process of chloride is involved in the basic industries of national economy, and the discharge of a large amount of chlorinated organics is inevitable, therefore, mesh
Before do not have the possibility that pollutes caused by chlorinated organics eliminated from source, post processing is approach and the side of unique feasible
Method.
In recent years, the comprehensive regulation for chlorinated organics receives more and more extensive concern.Production by Catalytic Combustion Process is mesh
The effective way of preceding most industrial industrialization prospect, with the characteristics of energy consumption is low, reactor is small, moreover it is possible to realize the complete of harmful substance
It totally disappeared except and do not cause secondary pollution.And realize the key of this purpose and be the performance and design of catalyst.Existing research
As a result show, noble metal catalyst has that price is relatively expensive, chlorination activity is high (and easily to form the bigger many chlorine pairs of harm
Product), easy fluorine poisoning, high temperature active component be lost in etc. deactivation prob so that the practical application of noble metal catalyst by
Limitation.So, the catalyst research for being catalyzed burning for chlorinated organics is concentrated mainly on transition metal oxide and with molecule
On solid acid catalyst based on sieve, such as MnO2、Co3O4、CrO2、CeO2With H-MOR, H-BEA, H-X, H-Y equimolecular sieve and
SiO2、Al2O3、TiO2And ZrO2Etc. common carrier.Representational patent has JP 2002219364, JP 2001286729, JP
10085559A2, US 4031149, US 58116628, US 4561969, US 4169862, US 7052663 etc..
The content of the invention
It is an object of the invention to provide a kind of high and low cost of catalytic activity, long lifespan be used for chlorinated organics low temperature
It is catalyzed the catalyst of burning.
Described catalyst is the transition metal oxide that sulfuric acid is modified, wherein described transition metal oxide is oxidation
Zirconium, titanium oxide or iron oxide, sulfuric acid are present in transition metal oxide surface, the quality of element sulphur in the form of bidentate sulfate
Fraction is 0.5~3wt%, preferably 0.5~1.5%.
Described catalyst belongs to solid oxidation species super acidic catalyst, and wherein transition metal oxide is preferably aoxidized
Iron.
Described catalyst can be prepared by the precipitation method and/or infusion process, and the presoma of transition metal oxide can select
Ferrous sulfate, ferric sulfate, nitre may be selected in the presoma of sulfate, carbonate or nitrate of transition metal etc., such as iron oxide
One kind in sour iron, iron chloride.The presoma of sulfuric acid may come from sulfate (such as ferrous sulfate or ferric sulfate) precipitation,
Remaining oxysulfide or the sulfuric acid using traditional infusion process load in roasting process.
A kind of preparation method for described catalyst that the present invention is provided is the precipitation method, specifically includes step：By transition gold
Category sulfate is dissolved in the water, and ammonia spirit is slowly added dropwise and adjusts pH value to 9~10, the hydroxide for forming transition metal sinks
Form sediment, stir 1~3h preferred 2h, the still aging preferred 8h of 6~10h, then suction filtration, Washing of Filter Cake, drying, roasting are obtained into sulfuric acid
The transition metal oxide of modification.
In the described precipitation method, transition metal sulfate is the presoma of transition metal oxide, and the presoma of sulfuric acid comes
From in sulfate oxysulfide remaining in precipitation, roasting process.
The preparation method for another described catalyst that the present invention is provided is infusion process, specifically includes step：Use sulphur
Dried after the hydroxide of acid solution or ammonium sulfate impregnated transition metal, standing, be calcined the transition gold for obtaining sulfuric acid modification
Belong to oxide.Wherein the hydroxide of transition metal can be before being calcined as made from transition metal sulfate in the above-mentioned precipitation method
Hydroxide or the precipitation that the precipitation method are obtained is used by nitrate or chloride.
Preferably, in the above-mentioned precipitation method and infusion process, drying temperature is 110~120 DEG C, preferably 110 DEG C.Sintering temperature is
350~650 DEG C, more preferably preferably 450~550 DEG C, 500 DEG C.
Calcination atmosphere is nitrogen or air, preferably air.
The present invention also aims to application of the catalyst described in disclosure in chlorinated organics low-temperature catalytic burning.
Specially a kind of method of chlorinated organics low-temperature catalytic burning of described application, the burning condition of this method is：
Catalyst is described catalyst, and reaction pressure is the preferred 0.1MPa of 0.1~0.5MPa, and the concentration of chlorinated hydrocarbon is 1
~10000ppm, oxygen concentration be 5~20vol%, reaction temperature be 150~500 DEG C preferably 300 DEG C, air speed be 1000~
100000/ hour.
Described chlorinated organics can be monochloro methane, dichloromethane, chloroform, dichloroethanes, vinyl chloride, trichlorine
Other chlorinated hydrocarbons such as the chlorinated aliphatic hydrocarbons such as ethene or chlorobenzene, dichloro-benzenes.
Beneficial effects of the present invention：The catalyst of transition metal oxide of the sulfuric acid modification of the present invention not only has higher
Catalytic activity, combustion oxidation of the chlorinated organics including chloride aliphatic hydrocarbon and chloride aromatic hydrocarbon can be catalyzed at a lower temperature, main
It is carbon dioxide, hydrogen chloride and chlorine to want combustion product, and the chloro-product without secondary pollution is formed, and preparation is simple, into
This low, long lifespan, is adapted to the processing of complex industrial waste gas, the application prospect with industrial waste gas processing.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.It should be understood that following examples are merely to illustrate this
Invention is not for restriction the scope of the present invention.
Embodiment 1
8.0g ferric sulfate is dissolved in 200mL deionized waters, ammonia spirit is slowly added dropwise, solution ph is adjusted to 9~10,
2h is stirred vigorously, suction filtration after ageing 8h is stored at room temperature, then is washed with deionized to filtrate in neutrality, filter cake is placed in baking oven
110 DEG C are dried overnight, and obtain orange FeOOH (confirming through XRD).Finally FeOOH is put into Muffle furnace, in air atmosphere
500 DEG C of roasting 4h, obtain Fe2O3- III catalyst.Photoelectron spectroscopy and plasma emission spectroscopy show Fe2O3-III
S containing 0.49wt% in catalyst, infrared spectrum (KBr tablettings) shows that S species are bidentate bridge-type sulphate form.
Embodiment 2
11.12g green vitriols are dissolved in 200mL deionized waters, ammonia spirit is slowly added dropwise, pH value of solution is adjusted
Value is stirred vigorously 2h to 9~10, is stored at room temperature suction filtration after ageing 8h, then is washed with deionized to filtrate in neutrality, and filter cake is put
Put in baking oven 110 DEG C to be dried overnight, obtain yellowish orange FeOOH (confirming through XRD).Finally FeOOH is put into Muffle furnace, in sky
The lower 500 DEG C of roastings 4h of gas atmosphere, obtains Fe2O3- II catalyst.Photoelectron spectroscopy and plasma emission spectroscopy show
Fe2O3S containing 1.15wt% in-II catalyst, infrared spectrum (KBr tablettings) shows that S species are that bidentate boils together sulphate form.
Embodiment 3
1.5mL 0.02g/mL sulfuric acid solutions are taken, 3g in embodiment 1 is impregnated in and dries on orange FeOOH powder, room temperature is quiet
Put 6h, place in baking oven 110 DEG C and be dried overnight, then 500 DEG C of roasting 4h under air atmosphere in Muffle furnace, finally give SO4 2-/
Fe2O3Catalyst.Photoelectron spectroscopy and plasma emission spectroscopy show SO4 2-/Fe2O3Containing 1.42wt%'s in catalyst
S, infrared spectrum (KBr tablettings) shows that S species are bidentate bridge-type sulphate form.
Comparative example 1
Using ammonium sulfate, as the commercially available iron oxide of maceration extract dipping, (average grain diameter 30nm, crystal structure is more advised
Whole, surface defect is less), subsequent treatment is identical with the method for embodiment 3, obtains SO4 2-/Fe2O3- N catalyst.Photoelectron spectroscopy and
Plasma emission spectroscopy shows SO4 2-/Fe2O3S containing 1.17wt% in-N catalyst, infrared spectrum (KBr tablettings) shows
It is monodentate sulphate form to show S species.
Comparative example 2
17.17g six is hydrated zirconium oxychloride and is dissolved in 200mL deionized waters, ammonia spirit is slowly added dropwise, pH value of solution is adjusted
Value is stirred vigorously 2h to 9~10, is stored at room temperature suction filtration after ageing 8h, then is washed with deionized to filtrate in neutrality, and filter cake is put
Put in baking oven 110 DEG C to be dried overnight, obtain white precipitate zirconium hydroxide Zr (OH)4.Finally sediment is put into Muffle furnace,
The lower 500 DEG C of roastings 4h of air atmosphere, obtains ZrO2Catalyst.
Embodiment 4
Zirconium hydroxide Zr (OH) before being calcined in comparative example 2 is impregnated as maceration extract using sulfuric acid solution4, by embodiment 3
Method carries out subsequent treatment, obtains SO4 2-/ZrO2Catalyst.Photoelectron spectroscopy and plasma emission spectroscopy show
SO4 2-/ZrO2S containing 1.11wt% in catalyst, infrared spectrum (KBr tablettings) shows that S species are bidentate bridge-type sulfate shape
Formula.
Comparative example 3
9.60g titanium sulfates are dissolved in 200mL deionized waters, ammonia spirit is slowly added dropwise, regulation solution ph to 9~
10,2h is stirred vigorously, suction filtration after ageing 8h is stored at room temperature, then be washed with deionized to filtrate in neutrality, filter cake places baking oven
Interior 110 DEG C are dried overnight, and obtain white titanium hydroxide Ti (OH)4.Finally by Ti (OH)4It is put into Muffle furnace, in air atmosphere
500 DEG C of roasting 4h, obtain TiO2Catalyst.
Embodiment 5
Titanium hydroxide Ti (OH) before being calcined in comparative example 3 is impregnated as maceration extract using sulfuric acid solution4, by embodiment 3
Method carries out subsequent treatment, obtains SO4 2-/TiO2Catalyst.Photoelectron spectroscopy and plasma emission spectroscopy show
SO4 2-/TiO2S containing 1.14wt% in catalyst, infrared spectrum (KBr tablettings) shows that S species are bidentate bridge-type sulfate shape
Formula.
Embodiment 6
The low-temperature catalytic burning for carrying out dichloromethane respectively using the catalyst of embodiment 1~5 and comparative example 1~3 is tested,
All combustion tests normal pressure in fixed-bed micro-reactor (internal diameter 4mm) is carried out.The consumption of catalyst is 200mg.It is chloride to have
Machine thing enters vaporizer using micro-injection pump injection, and is vaporized in vaporizer, enters after then being mixed with dry air
Reactor, gas flow is controlled with mass flowmenter, and total gas flow rate is 100mL/min.Concentration dichloromethane is
750ppm, oxygen concentration is 10.5vol%, and remaining is nitrogen.The relation of dichloromethane conversion ratio and reaction temperature is shown in Table 1, table
Middle T10、T50、T90Represent that conversion ratio reaches reaction temperature required when 10%, 50%, 90% respectively.On the catalyst of embodiment 5
Reaction product be mainly monochloro methane, hydrogen chloride, carbon monoxide；Reaction production on the catalyst of other embodiment and comparative example
If owner's hydrogen chloride, carbon dioxide and chlorine.As can be seen from Table 1, the Fe of sulfuric acid modification2O3-III、Fe2O3-II、SO4 2-/
Fe2O3And SO4 2-/TiO2Catalyst shows higher catalytic activity, T50Below 250 DEG C, and for CO/CO2Have compared with
High selectivity, does not cause the chloro accessory substance of secondary pollution to generate.
The catalytic combustion properties of dichloromethane in the different catalysts of table 1
Embodiment 7
According to the method for embodiment 6, testing example 1 and the catalyst of embodiment 2 respectively to dichloroethanes, trichloro ethylene,
The relation of chlorobenzene, dichloro-benzenes, the catalytic combustion activity of benzene, conversion ratio and reaction temperature is as shown in table 2.As shown in Table 2, sulfuric acid is repaiied
The Fe of decorations2O3Catalyst has higher activity to different chlorinated hydrocarbons, and especially for dichloroethanes, Examples 1 and 2 are urged
The T of agent90Only 317 and 253 DEG C.Product analysis shows, the further chloro-product of chlorinated aromatic hydrocarbon compound 10ppm with
Under；Chlorination does not occur for dichloroethanes, trichloro ethylene, shows the SO of sulfuric acid modification4 2-/Fe2O3Catalyst has higher
Activity, selectivity and broad spectrum activity.
The catalyst Fe of table 22O3The catalytic combustion properties of the upper chlorinated organics of-III
Embodiment 8
1500ppm vapor is added in reaction atmosphere, other reaction conditions are same as Example 6, have rated embodiment 1
With 2 catalyst in moist reaction gas dichloromethane catalytic combustion activity, the relation of reaction-ure conversion-age and reaction temperature is shown in Table
3.As shown in Table 3, the Fe of sulfuric acid modification2O3Catalyst shows good moisture-proof, T50It is below 300 DEG C.Product analysis table
Bright primary product is carbon dioxide and hydrogen chloride, and no chlorine and chlorinated hydrocarbon secondary pollution accessory substance is formed.
Under the aqueous conditions of table 3 in different catalysts dichloromethane catalytic combustion properties
Embodiment 9
Reaction temperature is set to 300 DEG C, other reaction conditions are same as Example 6, have rated the catalyst of embodiment 2 two
Stability in chloromethanes catalyst combustion reaction, as a result showed in 12 hours, the conversion ratio of dichloromethane be maintained at 90% with
On, last a long time.Product analysis shows that primary product is carbon dioxide, hydrogen chloride and chlorine, the chloro production without secondary pollution
Thing is formed, and complete combustion tail gas is vented after being absorbed using dilute alkaline soln.
To sum up the burn results of embodiment 6~9 show, the transition metal oxide of sulfuric acid modification of the invention not only has
Higher catalytic activity, burning oxygen of the chlorinated organics including chloride aliphatic hydrocarbon and chloride aromatic hydrocarbon can be catalyzed at a lower temperature
Change, primary combustion product is carbon dioxide, hydrogen chloride and chlorine, and the chloro-product without secondary pollution is formed, and prepare letter
Single, cost is low, and long lifespan is adapted to the processing of complex industrial waste gas, the application prospect with industrial waste gas processing.
Claims (8)
1. a kind of catalyst for chlorinated organics low-temperature catalytic burning, it is characterised in that it is the transition gold that sulfuric acid is modified
Belong to oxide, wherein described transition metal oxide is zirconium oxide, titanium oxide or iron oxide, sulfuric acid is with the shape of bidentate sulfate
Formula is present in transition metal oxide surface, and the mass fraction of element sulphur is 0.5~3wt%.
2. the preparation method of catalyst as claimed in claim 1, it is characterised in that it includes step：By transition metal sulfuric acid
Salt is dissolved in the water, and ammonia spirit is slowly added dropwise and adjusts pH value to 9~10, stirs 1~3h, still aging 6~10h, then takes out
Filter, Washing of Filter Cake, drying, roasting is obtained the transition metal oxide of sulfuric acid modification.
3. method as claimed in claim 2, it is characterised in that drying temperature is 110~120 DEG C, sintering temperature is 350~
650℃。
4. the preparation method of catalyst as claimed in claim 1, it is characterised in that it includes step：Using sulfuric acid solution or
Dried after the hydroxide of ammonium sulfate impregnated transition metal, standing, be calcined the transition metal oxide for obtaining sulfuric acid modification.
5. method as claimed in claim 4, it is characterised in that drying temperature is 110~120 DEG C, sintering temperature is 350~
650℃。
6. application of the catalyst as claimed in claim 1 in chlorinated organics low-temperature catalytic burning.
7. application as claimed in claim 6, it is characterised in that specially a kind of chlorinated organics of described application are low-temperature catalyzed
The method of burning, the burning condition of this method is：Catalyst be claim 1 described in catalyst, reaction pressure be 0.1~
0.5MPa, the concentration of chlorinated hydrocarbon is 1~10000ppm, and oxygen concentration is 5~20vol%, reaction temperature is 150~
500 DEG C, air speed is 1000~100000/ hours.
8. application as claimed in claim 6, it is characterised in that described chlorinated organics are monochloro methane, dichloromethane, three
Chloromethanes, dichloroethanes, vinyl chloride, trichloro ethylene, chlorobenzene or dichloro-benzenes.
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| CN107442102A (en) * | 2017-08-16 | 2017-12-08 | 杭州更蓝生物科技有限公司 | A kind of catalyst for chlorinated organics catalysis burning and preparation method thereof |
| CN107552013A (en) * | 2017-10-29 | 2018-01-09 | 桂林电子科技大学 | A kind of preparation and its application of bagasse cellulose matrix chemistry carbon sequestration post |
| CN109224761A (en) * | 2017-11-09 | 2019-01-18 | 新昌县以琳环保科技有限公司 | The technique of VOCs treatment containing chlorine |
| CN110756160A (en) * | 2019-11-05 | 2020-02-07 | 北京泷涛环境科技有限公司 | Modified molecular sieve, preparation method, material and use method |
| CN112717955A (en) * | 2020-12-31 | 2021-04-30 | 武汉理工大学 | Preparation method and application of surface sulfur modified iron oxide nanodisk |
| CN113117699A (en) * | 2021-04-19 | 2021-07-16 | 福州大学 | Sulfate radical modified iridium-based methane combustion catalyst, and preparation and application thereof |
| CN114029057A (en) * | 2021-12-06 | 2022-02-11 | 华东理工大学 | Preparation method of catalyst for catalytic purification of chlorine-containing volatile organic compounds |
| CN114768836A (en) * | 2022-04-19 | 2022-07-22 | 浙江师范大学 | Catalyst for catalytic oxidation of dichloromethane and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107442102A (en) * | 2017-08-16 | 2017-12-08 | 杭州更蓝生物科技有限公司 | A kind of catalyst for chlorinated organics catalysis burning and preparation method thereof |
| CN107552013A (en) * | 2017-10-29 | 2018-01-09 | 桂林电子科技大学 | A kind of preparation and its application of bagasse cellulose matrix chemistry carbon sequestration post |
| CN109224761A (en) * | 2017-11-09 | 2019-01-18 | 新昌县以琳环保科技有限公司 | The technique of VOCs treatment containing chlorine |
| CN110756160A (en) * | 2019-11-05 | 2020-02-07 | 北京泷涛环境科技有限公司 | Modified molecular sieve, preparation method, material and use method |
| CN110756160B (en) * | 2019-11-05 | 2022-07-26 | 北京泷涛环境科技有限公司 | Modified molecular sieve, preparation method, material and using method |
| CN112717955A (en) * | 2020-12-31 | 2021-04-30 | 武汉理工大学 | Preparation method and application of surface sulfur modified iron oxide nanodisk |
| CN113117699A (en) * | 2021-04-19 | 2021-07-16 | 福州大学 | Sulfate radical modified iridium-based methane combustion catalyst, and preparation and application thereof |
| CN114029057A (en) * | 2021-12-06 | 2022-02-11 | 华东理工大学 | Preparation method of catalyst for catalytic purification of chlorine-containing volatile organic compounds |
| CN114768836A (en) * | 2022-04-19 | 2022-07-22 | 浙江师范大学 | Catalyst for catalytic oxidation of dichloromethane and preparation method thereof |
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