CN107115867A - A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas - Google Patents
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas Download PDFInfo
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- CN107115867A CN107115867A CN201710482025.3A CN201710482025A CN107115867A CN 107115867 A CN107115867 A CN 107115867A CN 201710482025 A CN201710482025 A CN 201710482025A CN 107115867 A CN107115867 A CN 107115867A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8678—Removing components of undefined structure
- B01D53/8687—Organic components
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/90—Injecting reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/48—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing arsenic, antimony, bismuth, vanadium, niobium tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention provides a kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprise the following steps：Solvent is dissolved in after soluble metallic salt is mixed, the mixed solution that mass fraction is 5 25% is prepared into；6 20h of placement are stirred at room temperature in mixed solution；Carrier is immersed into mass fraction in 5 25% acid solution, ultrasonically treated 5 25min is 67 with pure water to pH, in an oven 60~160 DEG C of dry for standby；Mass ratio (0.8~1.6) of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide：(0.8~1.6) is mixed, and stands 6 20h, and 60~160 DEG C of drying, are then calcined in an oven.Catalyst prepared by the present invention, can reduce the content of organic exhaust gas in the case where there is ozone, and with low cost, reproducibility is good, and reaction can be carried out at normal temperatures and pressures, with very bright application prospect.
Description
Technical field
The invention belongs to control atmosphere pollution technical field, more particularly, to a kind of catalyst of ozone oxidation organic exhaust gas
Preparation method.
Background technology
Organic exhaust gas species is various, due to its volatility be collectively referred to as more by force referred to as VOCs (VOC,
Volatile Organic Compounds abbreviation).It is entered after human body by respiratory tract and skin, the inside device that can be given people
Official causes temporary or permanent lesion, or even can also be through heredity injury health of future generation, such as brain paralysis youngster.Industrial production and family
Large quantity of exhaust gas can be all produced in the fitment process of front yard, mainly including various aldehydes, hydro carbons, ketone, amine, acids, alcohols etc., they
Human health is seriously endangered.
At present, the technology of processing organic exhaust gas mainly has condensation absorption method, absorption method, combustion method, absorption process etc., but they
The problem of all having various, such as investment cost are too high, operating process is complicated, energy consumption is larger, using being limited in scope.It is such as cold
Solidifying absorption method is applied to concentration height, the operating mode that temperature is low, air quantity is small；Adsorbing rule needs frequently to change activated carbon, adds dress
The link such as unload, transport, changing, operating cost is greatly increased；Combustion method needs to add auxiliary fuel, and energy consumption is larger, is suitable only for using
In the higher organic exhaust gas of concentration；Absorbing rule needs to be equipped with thermal analysis apparatus, and equipment volume is big, and investment cost is high.Exactly by
In organic exhaust gas, not only species is complicated, and organic compound concentrations scope is excessive in waste gas, it is difficult to be allowed to using single method
Effectively remove, realize qualified discharge, cause the problem of current VOCs treatment.As government supervises to air contaminant treatment
The further increasing of dynamics, the discharge standard of various regions every profession and trade is further improved, research and development VOCs treatment skill of new generation
Art is extremely urgent.
In recent years, increasing new technology is applied to the processing of organic exhaust gas, such as Purification biotechnology, photocatalysis skill
Art etc..Purification biotechnology equipment is simple, invests relatively low, but processing speed is slower, is of limited application；Photocatalysis technology energy
It is enough that directly catalytic organism is degraded in the presence of light, have the advantages that other technologies are incomparable, but the current technology is most
Big problem is that catalyst efficiency is too low.
Ozone oxidation can make the Some Organic Pollutants in waste gas are oxidized in the presence of catalyst to be completely converted into
Inorganic matter, inherently eliminates organic pollution, and this technology possesses the application prospect of light.
The content of the invention
In view of this, the present invention is directed to propose a kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, is passing through
In the presence of catalyst prepared by this method, ozone is passed through into organic exhaust gas, and organic pollution can be greatly reduced, and
Catalyst is with low cost, regenerability is good, reaction can be smoothed out at normal temperatures and pressures, preparation method amplify difficulty compared with
It is small, with very bright application prospect.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprises the following steps：
Step S1：It is dissolved in after soluble metallic salt is mixed in solvent, is prepared into the mixing that mass fraction is 5-25% molten
Liquid；Placement 6-20h is stirred at room temperature in mixed solution；
Step S2：Carrier is immersed into the mass fraction for preparing in 5-25% acid solution, ultrasonically treated 5-
25min, is 6-7 with pure water to pH, in an oven 60~160 DEG C of dry for standby；It is preferred that, drying temperature is 100 DEG C；
Step S3：Mass ratio of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide
(0.8~1.6)：(0.8~1.6) is mixed, and stands 6-20h, and 60~160 DEG C of drying, are then calcined in an oven；It is preferred that
, the mass ratio counted using oxide is 1：1 mixing, drying temperature is 100 DEG C.
It is preferred that, the carrier in the step S2 is aerosil, ZSM-5 molecular sieve, S-1 molecular sieves, TS-1 point
Any one in sub- sieve, Woelm Alumina, SAPO molecular sieve.
It is preferred that, the soluble metallic salt in the step S1 is nitrate, sulfate, carbonate, the chlorine of transition metal
One or both of compound, vanadate, acetate and more than.
It is preferred that, the soluble metallic salt is cerous nitrate, cobalt nitrate, the mixture of ammonium tungstate three, and three rubs
You are than being (0.1~0.2):(0.2~0.6):(0.4~0.6)；It is preferred that, mol ratio is 0.15：0.45：0.4.
It is preferred that, the soluble metallic salt is iron chloride, cadmium nitrate, the mixture of chromic nitrate three, mole of three
Than for (0.2~0.5):(0.2~0.5):(0.2~0.5)；It is preferred that, mol ratio is 0.3：0.4：0.3.
It is preferred that, the soluble metallic salt is cobalt chloride, manganese nitrate, cerous nitrate, the mixture of ferric sulfate, four
Mol ratio be (0.2~0.5):(0.2~0.5):(0.05~0.2):(0.05~0.2)；It is preferred that, mol ratio is 0.3：
0.4：0.15：0.15.
It is preferred that, the soluble metallic salt is the mixture of both cobalt nitrate, cerous nitrate, and both mol ratios are (0.3
~0.6):(0.4~0.8)；It is preferred that, mol ratio is 0.45：0.55.
It is preferred that, the solvent in the step S1 is methanol, ethanol, propyl alcohol, isopropanol, the tert-butyl alcohol, glycerine, second two
Any one or two kinds in alcohol, chloroform, carbon tetrachloride and more than.
It is preferred that, the acid solution in the step S2 is any one in sulfuric acid, nitric acid, hydrochloric acid.
It is preferred that, the temperature of the roasting in the step S3 is 400~700 DEG C, and the time is 6~20h.
Relative to prior art, the preparation method of the catalyst of ozone oxidation organic exhaust gas of the present invention has following
Advantage：
The preparation method of the catalyst of ozone oxidation organic exhaust gas of the present invention, is matched somebody with somebody by largely screening catalyst
Side, is prepared for efficient organic exhaust gas ozone oxidation catalyst,
1) catalyst preparation of organic exhaust gas ozone oxidation prepared by the present invention is simple, and technological process is short, with low cost；
2) in the presence of catalyst prepared by the present invention, the organic pollution in waste gas can be in ozone under normal temperature and pressure
Rapid degraded, with good economic prospect；
3) various solvents can be recycled in catalyst preparation process of the present invention, it is to avoid catalyst production process
Secondary pollution.
Embodiment
In addition to being defined, technical term used has universal with those skilled in the art of the invention in following examples
The identical meanings of understanding.Test reagent used, is routine biochemistry reagent unless otherwise specified in following examples；It is described
Experimental method, is conventional method unless otherwise specified.
The present invention is described in detail with reference to embodiment.
Embodiment 1
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprises the following steps：
Step S1：By cerous nitrate, cobalt nitrate, ammonium tungstate with mol ratio 0.15：0.45：It is dissolved in methanol, makes after 0.4 mixing
Standby is 5% mixed solution into mass fraction, and mixed solution is stirred at room temperature into placement 6h.
Step S2：Aerosil is immersed into the mass fraction for preparing in 5% sulfuric acid solution, it is ultrasonically treated
5min, is 6-7 with pure water to pH, in an oven dry for standby at 100 DEG C.
Step S3：Matter of the mixed solution that step step S1 is prepared with the carrier after step S2 processing in terms of oxide
Amount compares 1：1 mixing, stands 6h, dries in an oven at 100 DEG C, then 400 DEG C of roasting 6h in Muffle furnace.
Embodiment 2
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprises the following steps：
Step S1：By iron chloride, cadmium nitrate, chromic nitrate with mol ratio 0.3：0.4：It is dissolved in propyl alcohol, prepares after 0.3 mixing
Into the mixed solution that mass fraction is 25%, placement 20h is stirred at room temperature in mixed solution.
Step S2：ZSM-5 molecular sieve is immersed into the mass fraction for preparing in 25% hydrochloric acid solution, it is ultrasonically treated
25min, is 6-7 with pure water to pH, in an oven dry for standby at 100 DEG C.
Step S3：Mass ratio of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide
1：1 mixing, stands 20h, dries in an oven at 100 DEG C, then 700 DEG C of roasting 20h in Muffle furnace.
Embodiment 3
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprises the following steps：
Step S1：By cobalt chloride, manganese nitrate, cerous nitrate, ferric sulfate with mol ratio 0.3：0.4：0.15：It is molten after 0.15 mixing
In isopropanol, the mixed solution that mass fraction is 10% is prepared into, placement 10h is stirred at room temperature in mixed solution.
Step S2：TS-1 molecular sieves are immersed into the mass fraction for preparing in 10% hydrochloric acid solution, it is ultrasonically treated
20min, is 6-7 with pure water to pH, in an oven 95 DEG C of dry for standby.
Step S3：Mass ratio of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide
1：1 mixing, stands 15h, in an oven 105 DEG C of drying, then 600 DEG C of roasting 10h in Muffle furnace.
Embodiment 4
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprises the following steps：
Step S1：By cobalt nitrate, cerous nitrate with mol ratio 0.45：It is dissolved in after 0.55 mixing in chloroform, is prepared into quality point
Number is 15% mixed solution, and mixed solution is stirred at room temperature into placement 8h.
Step S2：S-1 molecular sieves are immersed into the mass fraction for preparing in 15% salpeter solution, it is ultrasonically treated
20min, is 6-7 with pure water to pH, in an oven 100 DEG C of dry for standby.
Step S3：Mass ratio of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide
1：1 mixing, stands 12h, in an oven 100 DEG C of drying, then 500 DEG C of roasting 10h in Muffle furnace.
Embodiment 5
A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, comprises the following steps：
Step S1：Cobalt nitrate is dissolved in glycerine, the mixed solution that mass fraction is 8% is prepared into, by mixed solution
Placement 10h is stirred at room temperature.
Step S2：Aerosil is immersed into the mass fraction for preparing in 10% hydrochloric acid solution, it is ultrasonically treated
20min, is 6-7 with pure water to pH, in an oven 105 DEG C of dry for standby.
Step S3：Mass ratio of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide
1：1 mixing, stands 10h, in an oven 105 DEG C of drying, then 400 DEG C of roasting 10h in Muffle furnace.
Comparative example
Comparative example tests the removal effect of organic exhaust gas not put catalyst only in the presence of appreciation condition ozone.
Evaluating catalyst is tested：
The catalyst 20g that embodiment 1~5 is prepared is placed in the internal 50L closed reactors equipped with aerofoil fan, wind
Fan power is 10W.0.05g organic exhaust gas is then passed to, 0.1mol ozone gas stops instead after opening fan, reaction 30min
Should, with the content of organic matter in gas chromatographic detection now ozone, as a result as shown in table 1.
Table 1 not be the same as Example prepared catalyst to organic matter removal effect in waste gas
By above-mentioned experimental data, catalyst prepared by the present invention is played during ozone catalytic organic exhaust gas
Larger facilitation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of the catalyst of ozone oxidation organic exhaust gas, it is characterised in that：Comprise the following steps：
Step S1：It is dissolved in after soluble metallic salt is mixed in solvent, is prepared into the mixed solution that mass fraction is 5-25%；Will
Placement 6-20h is stirred at room temperature in mixed solution；
Step S2：Carrier is immersed to the mass fraction prepared in 5-25% acid solution, ultrasonically treated 5-25min is used
Pure water to pH be 6-7, in an oven 60~160 DEG C of dry for standby；It is preferred that, drying temperature is 100 DEG C；
Step S3：Mass ratio (0.8 of the mixed solution that step S1 is prepared with the carrier after step S2 processing in terms of oxide
~1.6)：(0.8~1.6) is mixed, and stands 6-20h, and 60~160 DEG C of drying, are then calcined in an oven；It is preferred that, with
The mass ratio of oxide meter is 1：1 mixing, drying temperature is 100 DEG C.
2. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 1, it is characterised in that：The step
Carrier in rapid S2 is aerosil, ZSM-5 molecular sieve, S-1 molecular sieves, TS-1 molecular sieves, Woelm Alumina, SAPO point
Son sieve in any one.
3. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 1, it is characterised in that：The step
Soluble metallic salt in rapid S1 is in the nitrate of transition metal, sulfate, carbonate, chloride, vanadate, acetate
It is one or two kinds of and more than.
4. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 3, it is characterised in that：It is described can
Soluble metal salts is cerous nitrate, cobalt nitrate, the mixture of ammonium tungstate three, and the mol ratio of three is (0.1~0.2):(0.2
~0.6):(0.4~0.6)；It is preferred that, mol ratio is 0.15：0.45：0.4.
5. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 3, it is characterised in that：It is described can
Soluble metal salts is iron chloride, cadmium nitrate, the mixture of chromic nitrate three, and the mol ratio of three is (0.2~0.5):(0.2~
0.5):(0.2~0.5)；It is preferred that, mol ratio is 0.3：0.4：0.3.
6. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 3, it is characterised in that：It is described can
Soluble metal salts is cobalt chloride, manganese nitrate, cerous nitrate, the mixture of ferric sulfate, and four mol ratio is (0.2~0.5):
(0.2~0.5):(0.05~0.2):(0.05~0.2)；It is preferred that, mol ratio is 0.3：0.4：0.15：0.15.
7. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 3, it is characterised in that：It is described can
Soluble metal salts is the mixture of both cobalt nitrate, cerous nitrate, and both mol ratios are (0.3~0.6):(0.4~0.8)；It is excellent
Choosing, mol ratio is 0.45：0.55.
8. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 1, it is characterised in that：The step
Solvent in rapid S1 is times in methanol, ethanol, propyl alcohol, isopropanol, the tert-butyl alcohol, glycerine, ethylene glycol, chloroform, carbon tetrachloride
Meaning it is one or two kinds of and more than.
9. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 1, it is characterised in that：The step
Acid solution in rapid S2 is any one in sulfuric acid, nitric acid, hydrochloric acid.
10. the preparation method of the catalyst of ozone oxidation organic exhaust gas according to claim 1, it is characterised in that：It is described
The temperature of roasting in step S3 is 400~700 DEG C, and the time is 6~20h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109701546A (en) * | 2017-10-25 | 2019-05-03 | 万华化学集团股份有限公司 | A kind of ozone catalytic oxidation catalyst and its method for handling biochemical waste gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104624198A (en) * | 2015-01-28 | 2015-05-20 | 博天环境集团股份有限公司 | Preparation method of catalyst for ozone oxidization |
| CN105170199A (en) * | 2015-09-18 | 2015-12-23 | 中国天辰工程有限公司 | Regeneration method for deep oxidation catalyst of coal gasification waste water |
| CN105170135A (en) * | 2015-09-18 | 2015-12-23 | 中国天辰工程有限公司 | Preparing method for deep oxidation catalyst of coal gasification waste water |
| CN105363465A (en) * | 2015-07-07 | 2016-03-02 | 博天环境集团股份有限公司 | Preparation method of ozone oxidation catalyst loaded with polymetallic oxide |
-
2017
- 2017-06-22 CN CN201710482025.3A patent/CN107115867A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104624198A (en) * | 2015-01-28 | 2015-05-20 | 博天环境集团股份有限公司 | Preparation method of catalyst for ozone oxidization |
| CN105363465A (en) * | 2015-07-07 | 2016-03-02 | 博天环境集团股份有限公司 | Preparation method of ozone oxidation catalyst loaded with polymetallic oxide |
| CN105170199A (en) * | 2015-09-18 | 2015-12-23 | 中国天辰工程有限公司 | Regeneration method for deep oxidation catalyst of coal gasification waste water |
| CN105170135A (en) * | 2015-09-18 | 2015-12-23 | 中国天辰工程有限公司 | Preparing method for deep oxidation catalyst of coal gasification waste water |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109701546A (en) * | 2017-10-25 | 2019-05-03 | 万华化学集团股份有限公司 | A kind of ozone catalytic oxidation catalyst and its method for handling biochemical waste gas |
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