CN105498742A - Potassium-based soot combustion catalyst and preparation method thereof - Google Patents

Potassium-based soot combustion catalyst and preparation method thereof Download PDF

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CN105498742A
CN105498742A CN201510584483.9A CN201510584483A CN105498742A CN 105498742 A CN105498742 A CN 105498742A CN 201510584483 A CN201510584483 A CN 201510584483A CN 105498742 A CN105498742 A CN 105498742A
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ethanolic solution
combustion catalyst
soot combustion
potassium
cook
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CN105498742B (en
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王�华
于鹤
李孔斋
魏永刚
祝星
翟康
曾春华
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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 potassium-based soot combustion catalyst and a preparation method thereof and belongs to the technical field of environment catalysis. The potassium-based soot combustion catalyst comprises a KCL particle as a core and a Al2O3 coating on the KCL particle. The preparation method comprises respectively dissolving CH3COOK, AlCl3 and KOH in ethanol to obtain ethanol solutions, adding the ethanol solution of CH3COOK into the ethanol solution of AlCl3, carrying out stirring to obtain a uniform solution, dropwisely adding the ethanol solution of KOH into the mixed solution, carrying out stirring, carrying out standing, carrying out filtration and washing to obtain slurry and solids, putting the slurry into a high pressure reactor under conditions of a temperature of 80-120 DEG C and pressure intensity of 5-12Mpa, carrying out a reaction process for 16-48h to obtain mixed slurry, filtering and washing the mixed slurry to obtain solids and a filtrate, standing the solids over night and carrying out drying and roasting to obtain the potassium-based soot combustion catalyst. The potassium-based soot combustion catalyst can effectively prevent a sylvite loss in a catalytic process and substantially improve catalyst catalytic activity.

Description

A kind of potassium basis soot combustion catalyst and preparation method thereof
Technical field
The present invention relates to a kind of potassium basis soot combustion catalyst and preparation method thereof, belong to environmental catalysis technical field.
Background technology
Soot particulate is the important pollutant of a class of diesel emission.Carbon soot particles pollutant energy long-term suspension forms aerosol in atmosphere, reduce the visibility of air, not only affect sight line, visibility is reduced, simultaneously carbon smoke pollution thing also can stimulate lung, causes human body anoxia, slow poisoning, occur anaemia, nervous, feel sick, the various disease conditions such as headache, respiratory disease, pulmonary edema, skin disease and allergic disease, cause bronchitis and pneumonia, reduce people's respiratory system to the resistance infected; Also may make conjunctival congestion, shed tears, ophthalmodynia, have sore throat, pant, cough, even have difficulty in breathing.The more important thing is, these harmful substances are enough to carcinogenic! As low latitude mobile pollution source, carbon smoke pollution thing is floating apart from about 1.2 meters, ground, with the respiratory tract of people at same horizontal line, people is easy to the particle inspiration lung of emission by exhaust pipe, and contain a lot of carcinogen in the dissolved organic matter that carbon granule adsorbs (SOF) component as BaP etc., directly jeopardize health.In addition, black smoke with stink give direct offending detest sense.Therefore, the control of diesel emission carbon smoke pollution thing always is the emphasis of policies of various countries management and technical research, and the process of carbon smoke pollution thing more and more receives the concern of people.
Filtering the mode be combined with catalytic combustion is the mode the most effectively processing soot at present.Due to soot discharge time, first will adhere on the filter, therefore the catalytic oxidation of soot is the regeneration issues of exhaust gas from diesel vehicle filter in fact.The regeneration of filter, maximum problem is operation inconvenience, or expense is too high.If catalyst attachment on the filter, by effectively reducing the burning-point of soot, make it can burn under usual delivery temperature, just can realize not needing dismounting and continuous reproducible, not only easy to maintenance, simple to operate, and while raising the efficiency reduction energy consumption, can also secondary pollution be reduced.Thus develop the high activated catalyst of soot low-temperature burning, problem can be made perfectly to be solved, therefore the key of problem is just the catalyst finding a kind of like this function admirable.
Catalyst for the process of carbon smoke pollution thing comprises noble metal catalyst and non-precious metal catalyst etc., noble metal catalyst passes through active and stability is all higher, but its development of the price limit of its costliness, the non-precious metal catalyst developing a kind of superior performance is the focus paid close attention to of researcher both at home and abroad at present.Large quantity research shows, sylvite possesses good catalysis soot combustion activity, but sylvite very easily runs off in catalytic process, makes the stability of its catalysis be difficult to ensure.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the invention provides a kind of potassium basis soot combustion catalyst and preparation method thereof.The nucleocapsid structure potassium basis soot combustion catalyst that the present invention prepares not only effectively can stop the loss of sylvite in catalytic process, the catalytic activity of catalyst can also be significantly improved, can while significantly reducing costs, improve the treatment effeciency of pollutant, the present invention is achieved through the following technical solutions.
A kind of potassium basis soot combustion catalyst, this catalytic inner core is KCl particle, and KCl particle outer layer covers Al 2o 3.
A preparation method for above-mentioned potassium basis soot combustion catalyst, its concrete steps are as follows:
(1) first by CH 3cOOK, AlCl 3, KOH is dissolved in respectively in ethanol and is configured to the CH that concentration is 0.01 ~ 0.03mol/L 3cOOK ethanolic solution, 0.5 ~ 1.5mol/LAlCl 3ethanolic solution, 0.5 ~ 1.5mol/LKOH ethanolic solution;
(2) by CH that step (1) obtains 3cOOK ethanolic solution adds the AlCl of step (1) 3ethanolic solution, after stirring, drips the KOH ethanolic solution of step (1), stirs after 2 ~ 5 hours and leaves standstill 10h, obtains slurries and solids after having left standstill rear filtration washing (washing adopts conventional alcohol washing);
(3) slurries step (2) obtained temperature be 80 ~ 120 DEG C, pressure load under being 5 ~ 12Mpa condition autoclave reaction 16 ~ 48h obtain mixed slurry, obtain solids and filtrate after being washed after filtration by mixed slurry, solids prepares potassium basis soot combustion catalyst after hold over night, drying (110 DEG C drying 24 hours), roasting.
The CH added in described step (2) 3cOOK ethanolic solution, AlCl 3the amount of ethanolic solution, KOH ethanolic solution is for keeping CH 3cOOK:AlCl 3: KOH mol ratio is 3:1:3.
Sintering temperature in described step (3) is 450 ~ 600 DEG C.
At 900 DEG C of aging 2h after described step (3) roasting.
The invention has the beneficial effects as follows:
1, sylvite wraps up by superficial oxidation aluminium completely, can effectively stop sylvite in the loss of catalytic process.
2, sylvite and superficial oxidation aluminium form strong interaction, effectively improve catalysis and remember catalytic activity.
3, cheaper starting materials that this catalyst uses is easy to get, and greatly reduces the production cost of catalyst.
4, the dependence of COMPARATIVE CATALYST's surface area is low, especially at the material sintering that high heat release environment causes, and then still can keep higher activity when causing specific surface to reduce.
Accompanying drawing explanation
Fig. 1 is present invention process flow chart.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
This potassium basis soot combustion catalyst, this catalytic inner core is KCl particle, and KCl particle outer layer covers Al 2o 3.
As shown in Figure 1, the preparation method of this above-mentioned potassium basis soot combustion catalyst, its concrete steps are as follows:
(1) first by CH 3cOOK, AlCl 3, KOH is dissolved in respectively in ethanol and is configured to the CH that concentration is 0.01mol/L 3cOOK ethanolic solution, 0.5mol/LAlCl 3ethanolic solution, 1.5mol/LKOH ethanolic solution;
(2) by 1LCH that step (1) obtains 3cOOK ethanolic solution adds the AlCl of step (1) 3ethanolic solution, after stirring, drips the KOH ethanolic solution of step (1), stirs after 5 hours and leaves standstill 10h, obtains slurries and solids after having left standstill rear filtration washing (washing adopts conventional alcohol washing); Wherein CH 3cOOK ethanolic solution, AlCl 3ethanolic solution, KOH ethanolic solution addition are for keeping CH 3cOOK:AlCl 3: KOH mol ratio is 3:1:3.
(3) slurries step (2) obtained temperature be 120 DEG C, pressure load under being 12Mpa condition autoclave reaction 16h obtain mixed slurry, obtain solids and filtrate after being washed after filtration by mixed slurry, solids prepares potassium basis soot combustion catalyst through hold over night, drying (110 DEG C drying 24 hours), 600 DEG C of roastings after 3 hours; Potassium basis soot combustion catalyst is divided into two parts, a at 900 DEG C of aging 2h.
The potassium basis soot combustion catalyst burn results of aging front and back, T i(initiation temperature) and T p(summit temperature) is respectively 293 DEG C and 380 DEG C, and the average selectivity of carbon dioxide is 97.8%.
Embodiment 2
This potassium basis soot combustion catalyst, this catalytic inner core is KCl particle, and KCl particle outer layer covers Al 2o 3.
As shown in Figure 1, the preparation method of this above-mentioned potassium basis soot combustion catalyst, its concrete steps are as follows:
(1) first by CH 3cOOK, AlCl 3, KOH is dissolved in respectively in ethanol and is configured to the CH that concentration is 0.03mol/L 3cOOK ethanolic solution, 0.5mol/LAlCl 3ethanolic solution, 0.5mol/LKOH ethanolic solution;
(2) by 1LCH that step (1) obtains 3cOOK ethanolic solution adds the AlCl of step (1) 3ethanolic solution, after stirring, drips the KOH ethanolic solution of step (1), stirs after 5 hours and leaves standstill 10h, obtains slurries and solids after having left standstill rear filtration washing (washing adopts conventional alcohol washing); Wherein CH 3cOOK ethanolic solution, AlCl 3ethanolic solution, KOH ethanolic solution addition are for keeping CH 3cOOK:AlCl 3: KOH mol ratio is 3:1:3;
(3) slurries step (2) obtained temperature be 80 DEG C, pressure load under being 5Mpa condition autoclave reaction 48h obtain mixed slurry, obtain solids and filtrate after being washed after filtration by mixed slurry, solids prepares potassium basis soot combustion catalyst through hold over night, drying (110 DEG C drying 24 hours), 600 DEG C of roastings after 3 hours; Potassium basis soot combustion catalyst is divided into two parts, a at 900 DEG C of aging 2h.
The potassium basis soot combustion catalyst burn results of aging front and back, T i(soot initiation temperature) and T p(soot conversion summit temperature) is respectively 321 DEG C and 362 DEG C, and the average selectivity of carbon dioxide is 98.5%.
Embodiment 3
This potassium basis soot combustion catalyst, this catalytic inner core is KCl nano particle, and KCl particle outer layer covers Al 2o 3nano particle.
As shown in Figure 1, the preparation method of this above-mentioned potassium basis soot combustion catalyst, its concrete steps are as follows:
(1) first by CH 3cOOK, AlCl 3, KOH is dissolved in respectively in ethanol and is configured to the CH that concentration is 0.02mol/L 3cOOK ethanolic solution, 1.5mol/LAlCl 3ethanolic solution, 1.0mol/LKOH ethanolic solution;
(2) by 1LCH that step (1) obtains 3cOOK ethanolic solution adds the AlCl of step (1) 3ethanolic solution, after stirring, drips the KOH ethanolic solution of step (1), stirs after 2 hours and leaves standstill 10h, obtains slurries and solids after having left standstill rear filtration washing (washing adopts conventional alcohol washing); Wherein CH 3cOOK ethanolic solution, AlCl 3ethanolic solution, KOH ethanolic solution addition are for keeping CH 3cOOK:AlCl 3: KOH mol ratio is 3:1:3;
(3) slurries step (2) obtained temperature be 100 DEG C, pressure load under being 7Mpa condition autoclave reaction 40h obtain mixed slurry, obtain solids and filtrate after being washed after filtration by mixed slurry, solids prepares potassium basis soot combustion catalyst through hold over night, drying (110 DEG C drying 24 hours), 450 DEG C of roastings after 3 hours; Potassium basis soot combustion catalyst is divided into two parts, a at 900 DEG C of aging 2h.
The potassium basis soot combustion catalyst burn results of aging front and back, T i(soot initiation temperature) and T p(soot conversion summit temperature) is respectively 318 DEG C and 384 DEG C, and the average selectivity of carbon dioxide is 99.3%.
Embodiment 4
This potassium basis soot combustion catalyst, this catalytic inner core is KCl particle, and KCl particle outer layer covers Al 2o 3.
As shown in Figure 1, the preparation method of this above-mentioned potassium basis soot combustion catalyst, its concrete steps are as follows:
(1) first by CH 3cOOK, AlCl 3, KOH is dissolved in respectively in ethanol and is configured to the CH that concentration is 0.02mol/L 3cOOK ethanolic solution, 1.0mol/LAlCl 3ethanolic solution, 0.8mol/LKOH ethanolic solution;
(2) by 1LCH that step (1) obtains 3cOOK ethanolic solution adds the AlCl of step (1) 3ethanolic solution, after stirring, drips the KOH ethanolic solution of step (1), stirs after 4 hours and leaves standstill 10h, obtains slurries and solids after having left standstill rear filtration washing (washing adopts conventional alcohol washing); Wherein CH 3cOOK ethanolic solution, AlCl 3ethanolic solution, KOH ethanolic solution addition are for keeping CH 3cOOK:AlCl 3: KOH mol ratio is 3:1:3;
(3) slurries step (2) obtained temperature be 100 DEG C, pressure load under being 6Mpa condition autoclave reaction 40h obtain mixed slurry, obtain solids and filtrate after being washed after filtration by mixed slurry, solids prepares potassium basis soot combustion catalyst through hold over night, drying (110 DEG C drying 24 hours), 500 DEG C of roastings after 3 hours; Potassium basis soot combustion catalyst is divided into two parts, a at 900 DEG C of aging 2h.
The potassium basis soot combustion catalyst burn results of aging front and back, T i(soot initiation temperature) and T p(soot conversion summit temperature) is respectively 310 DEG C and 344 DEG C, and the average selectivity of carbon dioxide is 99.6%.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.

Claims (5)

1. a potassium basis soot combustion catalyst, is characterized in that: this catalytic inner core is KCl particle, and KCl particle outer layer covers Al 2o 3.
2. a preparation method for potassium basis soot combustion catalyst according to claim 1, is characterized in that concrete steps are as follows:
(1) first by CH 3cOOK, AlCl 3, KOH is dissolved in respectively in ethanol and is configured to the CH that concentration is 0.01 ~ 0.03mol/L 3cOOK ethanolic solution, 0.5 ~ 1.5mol/LAlCl 3ethanolic solution, 0.5 ~ 1.5mol/LKOH ethanolic solution;
(2) by CH that step (1) obtains 3cOOK ethanolic solution adds the AlCl of step (1) 3ethanolic solution, after stirring, drips the KOH ethanolic solution of step (1), leaves standstill, obtain slurries and solids after having left standstill rear filtration washing after stirring;
(3) slurries step (2) obtained temperature be 80 ~ 120 DEG C, pressure load under being 5 ~ 12Mpa condition autoclave reaction 16 ~ 48h obtain mixed slurry, obtain solids and filtrate after being washed after filtration by mixed slurry, solids prepares potassium basis soot combustion catalyst after hold over night, drying, roasting.
3. the preparation method of potassium basis soot combustion catalyst according to claim 2, is characterized in that: the CH added in described step (2) 3cOOK ethanolic solution, AlCl 3the amount of ethanolic solution, KOH ethanolic solution is for keeping CH 3cOOK:AlCl 3: KOH mol ratio is 3:1:3.
4. the preparation method of potassium basis soot combustion catalyst according to claim 2, is characterized in that: the sintering temperature in described step (3) is 450 ~ 600 DEG C.
5. the preparation method of potassium basis soot combustion catalyst according to claim 2, is characterized in that: at 900 DEG C of aging 2h after described step (3) roasting.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111804294A (en) * 2020-04-24 2020-10-23 济南大学 Preparation method of stable potassium-based carbon smoke combustion catalyst and obtained product

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63224838A (en) * 1987-03-13 1988-09-19 Mazda Motor Corp Core for pressurized casting
CN102658122A (en) * 2012-02-22 2012-09-12 华东理工大学 Catalyst for combustion of soot particles in diesel vehicle exhaust, and preparation method thereof

Non-Patent Citations (3)

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Title
KONG ZHAI LI等: "Selective Oxidation of Carbon Using Iron-Modified Cerium Oxide", 《J. PHYS. CHEM. C》 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111804294A (en) * 2020-04-24 2020-10-23 济南大学 Preparation method of stable potassium-based carbon smoke combustion catalyst and obtained product
CN111804294B (en) * 2020-04-24 2022-08-09 济南大学 Preparation method of stable potassium-based carbon smoke combustion catalyst and obtained product

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