CN108187649A - A kind of processing method of tail gas catalyzed agent carrier newly developed - Google Patents
A kind of processing method of tail gas catalyzed agent carrier newly developed Download PDFInfo
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- CN108187649A CN108187649A CN201711465332.7A CN201711465332A CN108187649A CN 108187649 A CN108187649 A CN 108187649A CN 201711465332 A CN201711465332 A CN 201711465332A CN 108187649 A CN108187649 A CN 108187649A
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/20—Carbon monoxide
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Abstract
The invention discloses a kind of processing methods of tail gas catalyzed agent carrier newly developed, include the following steps：Feedstock capture and parametric measurement；Experiment equipment prepares；Meerschaum pretreatment；Sepiolite difference acid concentration modification sequentially adds the HCL solution of different acid concentrations, and beaker acid concentration is set in arithmetic progression, obtains the modified sepiolite of different acid；The different sour handling duration modifications of sepiolite add in the HCL solution of identical acid concentration into beaker successively；Different durations are stood in water bath with thermostatic control respectively；Sepiolite calcination processing is calcined under conditions of different temperatures, different durations respectively, and the temperature of every part of sepiolite calcining is equal with duration product；The characterization test of sepiolite after processing.The present invention provides processing parameter for follow-up sepiolite as different catalysts carrier, accelerates the technological development process that sepiolite is applied to catalyst carrier by people.
Description
Technical field
The invention belongs to tail gas catalyzed Technical Development Areas, and in particular to a kind of place of tail gas catalyzed agent carrier newly developed
Reason method.
Background technology
At present, the pollution of air becomes an important environmental problem gradually.Due to the use of multiple fuel machinery, because
It is influenced by factors such as the sulfur phosphorus compounds in fuel qualities, lubricating oil, fuel oil easily generates carbon distribution and colloid, air inlet discrimination
Pipe has dust grease, leads to the discharge of more exhaust gas.
The major pollutants of vehicle exhaust for hydrocarbon, oxynitrides, carbon monoxide, sulfur dioxide, containing leaded
Close object, Benzpyrene and solid particulate matter etc..Most polluted gas is manufactured by vehicle exhaust in city, and carbon dioxide is more
It is one of the main reason for causing atmosphere pollution and greenhouse effects.CO, HC, NOx not only cause human body damage but also certain
Under conditions of generate the photochemical fog of blue, make vegetation dead, the environment of human survival is destroyed.
Catalyst converter is mounted at existing automobile exhaust, can reduce correlation in vehicle exhaust by catalyst converter endangers gas,
The catalyst carrier so more used now is mostly porous aluminum silicon materials, and thermal stability is poor, is susceptible in actual use
The problem of catalytic efficiency is low, therefore searching new material is particularly important as carrier.
Sepiolite is a kind of hydrous magnesium silicate of threadiness, opaque also not have usually in the colors such as white, light gray, pale yellow
It is glossy.The shape that they have is as soil block, and some is into a strange cot shape or concretion forms.It can see under an electron microscope
It is to be got together to line up sheet by countless filaments to them, there is good inner space and gap basis.
Invention content
The purpose of the present invention is to provide a kind of processing method of tail gas catalyzed agent carrier newly developed, especially by following
Technical solution is realized：
A kind of processing method of tail gas catalyzed agent carrier newly developed, includes the following steps：
Step 1: feedstock capture and parametric measurement：
More complete sepiolite block is obtained as experimental subjects, sepiolite is measured by X-ray fluorescence spectra and is initialized
It studies and is grouped as, sepiolite starting material phase composition is measured by X-ray diffractometer；
Step 2: pretreatment equipment prepares：
Reagent needed for preparation and laboratory apparatus, experiment reagent is configured and laboratory apparatus is cleaned, is sterilized,
It is dried；
Step 3: meerschaum pretreatment：
It is 1 in mass ratio by sepiolite and deionized water：8 mixing are placed in reaction under high pressure stove in 100-200 DEG C of heat preservation
More than 1h；Washing filtering is placed in drying box dry more than 10h, and drying temperature is higher than 100 DEG C, the sepiolite after being purified
Object of experiment object；
Step 4: sepiolite difference acid concentration modification：
The object of experiment object in several pieces step 3 is taken, is respectively placed in experiment beaker；It is added in successively into beaker different
The HCL solution of acid concentration, beaker acid concentration are set in arithmetic progression；More than 12h is stood in 65-80 DEG C of water bath with thermostatic control；Washing
Water removal, is placed in 100 DEG C of dry 18h in drying box, obtains the modified sepiolite of different acid；
Step 5: the different sour handling duration modifications of sepiolite：
The object of experiment object in several pieces step 3 is taken, is respectively placed in experiment beaker, is added in successively into beaker identical
The HCL solution of acid concentration；Different durations are stood in 65-80 DEG C of water bath with thermostatic control respectively, washing water removal is placed in 100 in drying box
DEG C dry 18h, obtains the modified sepiolites of different acid；
Step 6: sepiolite calcination processing：
Modified meerschaum under standing duration same in step 5 is divided into several pieces, respectively in different temperatures, difference
It is calcined under conditions of duration, the temperature of every part of sepiolite calcining is equal with duration product；It takes out and stands, obtain difference
Temperature calcination sepiolite sample；
Step 7: processing after sepiolite characterization test：
Respectively pair Step 4: Step 5: the sample after the meerschaum pretreatment obtained in step 6 carries out specific surface area survey
Fixed, phase structure measures, surface topography measures, thermogravimetric analysis measures, and is determined by analysis, obtains sepiolite in different experiments
Under the conditions of modification variation tendency.
Further, five parts of object of experiment objects are taken in the step 4, every part of 12g is added in respectively into object of experiment object
Molar concentration difference is 0.5 five parts of HCL solution.
Further, it is described absolute ethyl alcohol washing to be used to go to remove water three times Step 4: the washing in step 5 removes water.
Further, five parts of object of experiment objects, every part of 12g, with solid-liquid mass ratio 1 are taken in the step 5；10 to five parts
The HCL solution of 1.0mol/L is added in object of experiment object, five parts of object of experiment objects stand duration difference in 70 DEG C of waters bath with thermostatic control and are
6h。
Further, the modified meerschaum under same standing duration is divided into three parts in the step 6, existed respectively
200 DEG C of heat preservation 5h, 500 DEG C of heat preservation 2h, 1000 DEG C of heat preservation 1h.
Further, the experiment equipment electronic balance for preparing in the step 2, reacting furnace, thermostat water bath, drying
Case.
Further, object of experiment object is filtered after standing in the step 4, and object of experiment is washed with deionized
Object easily detects washing effect after deionized water washing using the silver nitrate of 0.1mol/L.
The beneficial effects of the invention are as follows：
The present invention devises development process method of the sepiolite as catalyst carrier, by different acid concentrations, no
With under handling duration and different calcination conditions, to before processing, treated, and the every of sepiolite progress measures, and can be derived that
Modification process condition of the sepiolite as carrier provides processing ginseng for follow-up sepiolite as different catalysts carrier
Number accelerates the process that sepiolite is applied to catalyst carrier by people, realizes the exploitation and utilization of new technology.
Specific embodiment
The technical solution in the embodiment of the present invention will be clearly and completely described below, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's all other embodiments obtained without making creative work, belong to guarantor of the present invention
The range of shield.
It is the sepiolite under the conditions of different acid concentrations, different disposal duration and different calcining pretreatments individually below
The embodiment of modification.
Embodiment 1：
A kind of processing method of tail gas catalyzed agent carrier newly developed, includes the following steps：
Step 1: feedstock capture and parametric measurement：
More complete sepiolite block is obtained as experimental subjects, sepiolite is measured by X-ray fluorescence spectra and is initialized
It studies and is grouped as, sepiolite starting material phase composition is measured by X-ray diffractometer；
Step 2: pretreatment equipment prepares：
Reagent needed for preparation and laboratory apparatus, experiment reagent is configured and laboratory apparatus is cleaned, is sterilized,
It is dried；Experiment equipment electronic balance, reacting furnace, thermostat water bath, drying box.
Step 3: meerschaum pretreatment：
It is 1 in mass ratio by sepiolite and deionized water：8 mixing, are placed in reaction under high pressure stove and keep the temperature 2h at 150 DEG C；It washes
Filtering is washed, is placed in drying box dry 10h, 120 DEG C of drying temperature position, the sepiolite object of experiment object after being purified；
Step 4: sepiolite difference acid concentration modification：
The object of experiment object in five parts of step 3 is taken, every part of 12g is respectively placed in experiment beaker；It is tested respectively to five parts
The HCL solution that molar concentration is 0.5,1.0,1.5,2.0,2.5 is added in object；12h is stood in 65 DEG C of waters bath with thermostatic control；
It filters, object of experiment object is washed with deionized, washing is easily detected using the silver nitrate of 0.1mol/L after deionized water washing
Effect；Washing water removal, washing water removal go to remove water three times, are placed in 100 DEG C of dry 18h in drying box, obtain using absolute ethyl alcohol washing
The sepiolite modified to different acid；
Step 5: processing after sepiolite characterization test：
Specific area measuring is carried out to the sample after the meerschaum pretreatment that is obtained in step 4 respectively, phase structure is surveyed
Fixed, surface topography measures, thermogravimetric analysis measures, and is determined by analysis, obtains sepiolite changing under the conditions of different acid concentrations
Property variation tendency.
Test obtains, acid solution increases, advantageously forms to the seriously corroded of sepiolite, sepiolite surface roughness
Composite material；And acid concentration, in 2-2.5mol/L, the thermal stability of sepiolite tends towards stability.
Embodiment 2：
A kind of processing method of tail gas catalyzed agent carrier newly developed, includes the following steps：
Step 1: feedstock capture and parametric measurement：
More complete sepiolite block is obtained as experimental subjects, sepiolite is measured by X-ray fluorescence spectra and is initialized
It studies and is grouped as, sepiolite starting material phase composition is measured by X-ray diffractometer；
Step 2: pretreatment equipment prepares：
Reagent needed for preparation and laboratory apparatus, experiment reagent is configured and laboratory apparatus is cleaned, is sterilized,
It is dried；Experiment equipment electronic balance, reacting furnace, thermostat water bath, drying box.
Step 3: meerschaum pretreatment：
It is 1 in mass ratio by sepiolite and deionized water：8 mixing, are placed in reaction under high pressure stove and keep the temperature 2h at 150 DEG C；It washes
Filtering is washed, is placed in drying box dry 10h, 120 DEG C of drying temperature position, the sepiolite object of experiment object after being purified；
Step 4: the different sour handling duration modifications of sepiolite：
The object of experiment object in five parts of step 3 is taken, every part of 12g is respectively placed in experiment beaker, with solid-liquid mass ratio 1；
10 add in the HCL solution of 1.0mol/L to five parts into beaker；Respectively in 70 DEG C of waters bath with thermostatic control stand 4.5h, 10.5h,
16.5h, 22.5h, 28.5h, washing water removal, washing water removal are gone to remove water three times, be placed in drying box using absolute ethyl alcohol washing
100 DEG C of dry 18h obtain the modified sepiolite of different acid；
Step 5: processing after sepiolite characterization test：
Specific area measuring is carried out to the sample after the meerschaum pretreatment that is obtained in step 4, phase structure measures, table
Face pattern measures, thermogravimetric analysis measures, and is determined by analysis, obtains modification of the sepiolite under the conditions of different sour handling durations
Variation tendency.
Test obtains, during acidification, sour effect is so that the duct of sepiolite is expanded；So with acid
Change the extension of time, the structure of sepiolite is destroyed；For acidificatoin time in 16.5h or so, sepiolite structure is preferable.
Embodiment 3：
Step 1: feedstock capture and parametric measurement：
More complete sepiolite block is obtained as experimental subjects, sepiolite is measured by X-ray fluorescence spectra and is initialized
It studies and is grouped as, sepiolite starting material phase composition is measured by X-ray diffractometer；
Step 2: pretreatment equipment prepares：
Reagent needed for preparation and laboratory apparatus, experiment reagent is configured and laboratory apparatus is cleaned, is sterilized,
It is dried；Experiment equipment electronic balance, reacting furnace, thermostat water bath, drying box.
Step 3: meerschaum pretreatment：
It is 1 in mass ratio by sepiolite and deionized water：8 mixing, are placed in reaction under high pressure stove and keep the temperature 2h at 150 DEG C；It washes
Filtering is washed, is placed in drying box dry 10h, 120 DEG C of drying temperature position, the sepiolite object of experiment object after being purified；
Step 4: the different sour handling duration modifications of sepiolite：
The object of experiment object in five parts of step 3 is taken, every part of 12g is respectively placed in experiment beaker, with solid-liquid mass ratio 1；
10 add in the HCL solution of 1.0mol/L to five parts into beaker；10.5h is stood in 70 DEG C of waters bath with thermostatic control, washing water removal is washed
It washs away water to go to remove water three times using absolute ethyl alcohol washing, is placed in 100 DEG C of dry 18h in drying box, obtain the modified Hai Pao of acid
Stone；
Step 5: sepiolite calcination processing：
The sour modified meerschaum obtained in step 4 is divided into three parts, keeps the temperature 5h, 500 DEG C of heat preservations at 200 DEG C respectively
2h, 1000 DEG C of heat preservation 1h.It takes out and stands, obtain different temperatures calcining sepiolite sample；
Step 6: processing after sepiolite characterization test：
Specific area measuring is carried out to the sample after the meerschaum pretreatment that is obtained in step 5 respectively, phase structure is surveyed
Fixed, surface topography measures, thermogravimetric analysis measures, and is determined by analysis, obtains sepiolite changing under the conditions of different acid concentrations
Property variation tendency.
Test obtains, with the raising of calcination temperature, the pore structure of sepiolite is caved in, and duct blocks, reduces, 1000
DEG C when, sepiolite structure is destroyed completely；For calcination temperature at 500 DEG C, sepiolite internal structure is preferable, and gap is clear.
Characterization measure in three above embodiment employs static n2 absorption apparatus, X-ray diffractometer, scanning electron microscope, red
External spectrum analyzer and thermogravimetric analyzer are measured accordingly.
The present invention devises preprocess method of the sepiolite as auto-exhaust catalyst carrier, by different acidity
Under concentration, different disposal duration and different calcination conditions, to before processing, treated, and the every of sepiolite progress measures, energy
It enough obtains modification process condition of the sepiolite as carrier, is provided for follow-up sepiolite as different catalysts carrier
Processing parameter accelerates the process that sepiolite is applied to catalyst carrier by people.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of processing method of tail gas catalyzed agent carrier newly developed, which is characterized in that include the following steps：
Step 1: feedstock capture and parametric measurement：
More complete sepiolite block is obtained as experimental subjects, by X-ray fluorescence spectra measure sepiolite original chemical into
It is grouped as, sepiolite starting material phase composition is measured by X-ray diffractometer；
Step 2: pretreatment equipment prepares：
Reagent needed for preparation and laboratory apparatus are configured experiment reagent and laboratory apparatus are cleaned, are sterilized, drying place
Reason；
Step 3: meerschaum pretreatment：
It is 1 in mass ratio by sepiolite and deionized water：8 mixing, be placed in reaction under high pressure stove 100-200 DEG C keep the temperature 1h with
On；Washing filtering is placed in drying box dry more than 10h, and drying temperature is higher than 100 DEG C, the sepiolite experiment after being purified
Object；
Step 4: sepiolite difference acid concentration modification：
The object of experiment object in several pieces step 3 is taken, is respectively placed in beaker；Different acid concentrations are added in into beaker successively
HCL solution, beaker acid concentration are set in arithmetic progression；More than 12h is stood in 65-80 DEG C of water bath with thermostatic control；Washing water removal, is placed in
100 DEG C of dry 18h in drying box obtain the modified sepiolite of different acid；
Step 5: the different sour handling duration modifications of sepiolite：
The object of experiment object in several pieces step 3 is taken, is respectively placed in beaker, adds in identical acid concentration into beaker successively
HCL solution；Different durations are stood in 65-80 DEG C of water bath with thermostatic control respectively, washing water removal is placed in 100 DEG C of dryings in drying box
18h obtains the modified sepiolite of different acid；
Step 6: sepiolite calcination processing：
Modified meerschaum under standing duration same in step 5 is divided into several pieces, respectively in different temperatures, different durations
Under conditions of calcined, the temperature of every part of sepiolite calcining is equal with duration product；It takes out and stands, obtain different temperatures and forge
Burn sepiolite sample；
Step 7: processing after sepiolite characterization test：
Respectively pair Step 4: Step 5: the sample after the meerschaum pretreatment obtained in step 6 carries out specific area measuring, object
Phase structure measures, surface topography measures, thermogravimetric analysis measures, and is determined by analysis, obtains sepiolite changing at different conditions
Property variation tendency.
2. a kind of processing method of tail gas catalyzed agent carrier newly developed according to claim 1, it is characterised in that：The step
Five parts of object of experiment objects are taken in rapid four, every part of 12g adds in five parts of HCL that molar concentration difference is 0.5 into object of experiment object respectively
Solution.
3. a kind of processing method of tail gas catalyzed agent carrier newly developed according to claim 1, it is characterised in that：The step
Rapid four, the washing water removal in step 5 goes to remove water three times using absolute ethyl alcohol washing.
4. a kind of processing method of tail gas catalyzed agent carrier newly developed according to claim 1, it is characterised in that：The step
Five parts of object of experiment objects, every part of 12g, with solid-liquid mass ratio 1 are taken in rapid five；10 add in 1.0mol/L into five parts of object of experiment objects
HCL solution, five parts of object of experiment objects stand duration difference as 6h in 70 DEG C of waters bath with thermostatic control.
5. a kind of processing method of tail gas catalyzed agent carrier newly developed according to claim 1, it is characterised in that：The step
In rapid six by it is same standing duration under modified meerschaum be divided into three parts, respectively 200 DEG C keep the temperature 5h, 500 DEG C heat preservation 2h,
1000 DEG C of heat preservation 1h.
6. a kind of processing method of tail gas catalyzed agent carrier newly developed according to claim 1, it is characterised in that：The step
Experiment equipment electronic balance, reacting furnace, thermostat water bath, the drying box prepared in rapid two.
7. a kind of processing method of tail gas catalyzed agent carrier newly developed according to claim 1, it is characterised in that：The step
Object of experiment object is filtered after standing in rapid four, and object of experiment object is washed with deionized, is used after deionized water washing
The silver nitrate of 0.1mol/L easily detects washing effect.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112439384A (en) * | 2020-10-31 | 2021-03-05 | 湘潭大学 | Modified preparation method of low-grade sepiolite for synchronously removing nitrogen and phosphorus |
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| CN106732592A (en) * | 2016-12-14 | 2017-05-31 | 湘潭大学 | A kind of method that the method for modifying and microwave irradiation of sepiolite prepare Cu sepiolites |
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| CN112439384A (en) * | 2020-10-31 | 2021-03-05 | 湘潭大学 | Modified preparation method of low-grade sepiolite for synchronously removing nitrogen and phosphorus |
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