CN108579754A - A kind of preparation method and system of auto-exhaust catalyst - Google Patents
A kind of preparation method and system of auto-exhaust catalyst Download PDFInfo
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- CN108579754A CN108579754A CN201810474383.4A CN201810474383A CN108579754A CN 108579754 A CN108579754 A CN 108579754A CN 201810474383 A CN201810474383 A CN 201810474383A CN 108579754 A CN108579754 A CN 108579754A
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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
- B01J23/70—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
- B01J23/83—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 rare earths or actinides
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
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Abstract
The invention discloses a kind of preparation method of auto-exhaust catalyst and systems, this method introduces hydrolysis in supercritical carbon dioxide environment, and friendly, the unique chemical reaction environment that is capable of providing using the strong solubility energy of supercritical carbon dioxide, entrainment performance and supercritical fluid prepares copper cerium zirconium composite catalyst.Since the surface tension of supercritical carbon dioxide is relatively low, so as to reduce or substitute the addition of surfactant, green cleaning, the copper cerium zirconium composite catalyst of preparation reaches 92.3% to the conversion ratio of CO, HC and NO.
Description
Technical field
The present invention relates to auto-exhaust catalyst technical field, more particularly to a kind of preparation method of auto-exhaust catalyst
And system.
Background technology
With the increase of car ownership, CO, HC, NOX that automobile is discharged into air are more and more.Currently, many states
Family takes motor vehicle exhaust emission stringent control emission measure.Therefore the processing of vehicle exhaust has become important
Project.In the prior art, it is to be realized by installing catalytic cleaner additional to the control of motor vehicle exhaust emission, and catalytic cleaner
Key be catalyst.The preparation of traditional auto-exhaust catalyst is frequently with the precipitation method, and the precipitation method are needed using a large amount of
Solvent, operating process is comparatively laborious, and the dispersion performance and catalytic performance of prepared catalyst are to be improved.
Supercritical carbon dioxide is gradually replacing that some are conventional, have to environment as the cleaning solvent of " Green Chemistry "
The organic solvent of harm is permitted in extraction and separation, analytical technology, food industry, Chinese medicine extraction, biomaterial, environmental protection etc.
Various aspects are all applied, and have extensive foreground.Supercritical carbon dioxide have high diffusibility, low viscosity, density is adjustable (into
And solubility is adjustable), polarity it is small, the advantages that being not easy to cause the product purity of the chemical agglomeration of particle and preparation high, in car tail
There to be good application value in the preparation of gas catalyst.
Invention content
The purpose of the present invention is to provide a kind of preparation method of auto-exhaust catalyst and systems, and this method is overcritical
It is carried out in carbon dioxide, there is prepared copper cerium zirconium composite catalyst good dispersibility, catalytic performance also to greatly improve.
To achieve the goals above, the first aspect of the present invention provides a kind of preparation method of auto-exhaust catalyst, should
Method includes the following steps：
(1) carbon dioxide is passed through into first reactor so that it is default that the pressure in the first reactor reaches first
Pressure value, first preset pressure value are 8~15MPa；Then soluble-salt, the cerium of copper are added into the first reactor
Soluble-salt, the soluble-salt of zirconium and the mixed solution of absolute ethyl alcohol, warming while stirring is to 100~160 DEG C；
(2) carbon dioxide is passed through into second reactor so that it is default that the pressure in the second reactor reaches second
The difference of pressure value, first preset pressure value and second preset pressure value is 0.1~0.5MPa；Then to described
In two reactors be added deionized water, citric acid mixed solution, warming while stirring is to 100~160 DEG C；
(3) supercritical carbon dioxide for the mixed solution that deionized water and citric acid are entrained in step (2) is slowly led to
Enter into the first reactor, stir the first reactor so that the deionized water and citric acid and described first are instead
It answers the solution in device to be sufficiently mixed, controls the temperature of the first reactor at 130~160 DEG C, after reaction 5~10 hours, mistake
Filter, washing obtain solid product, and the solid product is dry, calcining obtains the auto-exhaust catalyst.
Wherein, the drying condition is：Dry 1~2h at 80~100 DEG C, calcination condition be 300~400 DEG C of calcinings 2~
4h。
Further, in step (1), the molar ratio of the soluble-salt of the soluble-salt of copper, the soluble-salt of cerium and zirconium is
(0.05~0.15)：(0.65~0.85)：(0.1~0.2).
Further, the soluble-salt of the soluble-salt of the copper, the soluble-salt of cerium and zirconium is copper nitrate, nitric acid respectively
Cerium and zirconium nitrate.
The second aspect of the present invention also provides a kind of preparation system of auto-exhaust catalyst, which includes：First is anti-
Answer device, second reactor, carbon dioxide storage tank, booster pump and triple valve, the carbon dioxide exported in the carbon dioxide storage tank
It is punished into two-way in the triple valve after booster pump supercharging, wherein be input to all the way in the first reactor, it is another
Road is input in second reactor；
Further include the first mixer and the first delivery pump being connected to first reactor, first mixer is used for copper
Soluble-salt, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol form mixed solution, first delivery pump is used for
The mixed solution is delivered in the first reactor；
Further include the second mixer and the second delivery pump being connected to second reactor, second mixer will be for that will go
Ionized water and citric acid form mixed solution, and second delivery pump is used to the mixed solution being delivered to second reactor
In.
Further, the soluble-salt of the copper, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol form mixing
In solution, the molar ratio of the soluble-salt of the soluble-salt of copper, the soluble-salt of cerium and zirconium is (0.05~0.15)：(0.65~
0.85)：(0.1~0.2).
Further, the soluble-salt of the soluble-salt of the copper, the soluble-salt of cerium and zirconium is copper nitrate, nitric acid respectively
Cerium and zirconium nitrate.
Further, the pressure difference value of the first reactor and second reactor is 0.1~0.5MPa.
The preparation method and system of a kind of auto-exhaust catalyst of the present invention have the advantages that：
The present invention introduces hydrolysis in supercritical carbon dioxide environment, utilizes the strong solubility of supercritical carbon dioxide
To prepare, copper cerium zirconium is compound to urge the close friend that energy, entrainment performance and supercritical fluid are capable of providing, unique chemical reaction environment
Agent.The surface tension of supercritical carbon dioxide is relatively low, so as to reduce or substitute the addition of surfactant, green
Cleaning, the copper cerium zirconium composite catalyst of preparation reach 92.3% to the conversion ratio of CO, HC and NO.
Description of the drawings
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical scheme of the present invention
The attached drawing used is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, right
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Its attached drawing.
Fig. 1 is a kind of structural schematic diagram of the preparation system of auto-exhaust catalyst provided by the invention.
Specific implementation mode
Technical scheme in the embodiment of the invention is clearly and completely described below in conjunction with the accompanying drawings, it is clear that described
Embodiment be only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained without making creative work, belongs to the present invention
The range of protection.
【Embodiment 1】
The present embodiment provides a kind of preparation systems of auto-exhaust catalyst, as shown in Figure 1, the system includes the first reaction
Device 1, second reactor 2, carbon dioxide storage tank 3, booster pump 4 and triple valve 5, the dioxy exported in the carbon dioxide storage tank 3
Change carbon to punish at two-way, wherein being input to the first reactor 1 all the way in the triple valve 5 after the supercharging of the booster pump 4
In, another way is input in second reactor 2.
The system further includes the first mixer 6 and the first delivery pump 7 being connected to first reactor 1, first mixing
Device 6 is used to the soluble-salt of copper, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol forming mixed solution, and described the
One delivery pump 7 is for the mixed solution to be delivered in the first reactor 1.
The system further includes the second mixer 8 and the second delivery pump 9 being connected to second reactor 2, second mixing
Device 8 is used to deionized water and citric acid forming mixed solution, and second delivery pump 9 is for the mixed solution to be delivered to
In second reactor 2.
Wherein, the pressure difference value of first reactor 1 and second reactor 2 is 0.1MPa.
The present embodiment also provides a kind of method that the preparation system using above-mentioned auto-exhaust catalyst prepares catalyst, should
Method includes the following steps：
(1) carbon dioxide is passed through into first reactor so that it is default that the pressure in the first reactor reaches first
Pressure value 8MPa；Then the mixing that copper nitrate, cerous nitrate, zirconium nitrate and absolute ethyl alcohol are added into the first reactor is molten
Liquid, warming while stirring is to 100 DEG C.
Wherein, the molar ratio of copper nitrate, cerous nitrate and zirconium nitrate is：0.05：0.85：0.1.
(2) carbon dioxide is passed through into second reactor so that it is default that the pressure in the second reactor reaches second
Pressure value 7.9MPa；Then into the second reactor be added deionized water, citric acid mixed solution, warming while stirring
To 100 DEG C；
(3) supercritical carbon dioxide for the mixed solution that deionized water and citric acid are entrained in step (2) is slowly led to
Enter into the first reactor, stir the first reactor so that the deionized water and citric acid and described first are instead
It answers the solution in device to be sufficiently mixed, controls the temperature of the first reactor at 130 DEG C, after reacting 5 hours, be filtered, washed
To solid product, the solid product is dry, calcining obtains copper cerium zirconium composite catalyst.
Wherein, drying condition is：Dry 1h at 80 DEG C, calcination condition are 300 DEG C of calcining 2h.
The copper cerium zirconium composite catalyst of above-mentioned preparation is tested for the property, the conversion ratio of CO, HC and NO are reached
90.6%.
【Embodiment 2】
The present embodiment provides a kind of preparation systems of auto-exhaust catalyst, as shown in Figure 1, the system includes the first reaction
Device 1, second reactor 2, carbon dioxide storage tank 3, booster pump 4 and triple valve 5, the dioxy exported in the carbon dioxide storage tank 3
Change carbon to punish at two-way, wherein being input to the first reactor 1 all the way in the triple valve 5 after the supercharging of the booster pump 4
In, another way is input in second reactor 2.
The system further includes the first mixer 6 and the first delivery pump 7 being connected to first reactor 1, first mixing
Device 6 is used to the soluble-salt of copper, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol forming mixed solution, and described the
One delivery pump 7 is for the mixed solution to be delivered in the first reactor 1.
The system further includes the second mixer 8 and the second delivery pump 9 being connected to second reactor 2, second mixing
Device 8 is used to deionized water and citric acid forming mixed solution, and second delivery pump 9 is for the mixed solution to be delivered to
In second reactor 2.
Wherein, the pressure difference value of first reactor 1 and second reactor 2 is 0.3MPa.
The present embodiment also provides a kind of method that the preparation system using above-mentioned auto-exhaust catalyst prepares catalyst, should
Method includes the following steps：
(1) carbon dioxide is passed through into first reactor so that it is default that the pressure in the first reactor reaches first
Pressure value 12MPa；Then the mixing that copper nitrate, cerous nitrate, zirconium nitrate and absolute ethyl alcohol are added into the first reactor is molten
Liquid, warming while stirring is to 130 DEG C.
Wherein, the molar ratio of copper nitrate, cerous nitrate and zirconium nitrate is：0.1：0.7：0.2.
(2) carbon dioxide is passed through into second reactor so that it is default that the pressure in the second reactor reaches second
Pressure value 11.7MPa；Then into the second reactor be added deionized water, citric acid mixed solution, rise while stirring
Temperature is to 130 DEG C；
(3) supercritical carbon dioxide for the mixed solution that deionized water and citric acid are entrained in step (2) is slowly led to
Enter into the first reactor, stir the first reactor so that the deionized water and citric acid and described first are instead
It answers the solution in device to be sufficiently mixed, controls the temperature of the first reactor at 150 DEG C, after reacting 8 hours, be filtered, washed
To solid product, the solid product is dry, calcining obtains copper cerium zirconium composite catalyst.
Wherein, drying condition is：Dry 2h at 90 DEG C, calcination condition are 350 DEG C of calcining 4h.
The copper cerium zirconium composite catalyst of above-mentioned preparation is tested for the property, the conversion ratio of CO, HC and NO are reached
91.2%.
【Embodiment 3】
The present embodiment provides a kind of preparation systems of auto-exhaust catalyst, as shown in Figure 1, the system includes the first reaction
Device 1, second reactor 2, carbon dioxide storage tank 3, booster pump 4 and triple valve 5, the dioxy exported in the carbon dioxide storage tank 3
Change carbon to punish at two-way, wherein being input to the first reactor 1 all the way in the triple valve 5 after the supercharging of the booster pump 4
In, another way is input in second reactor 2.
The system further includes the first mixer 6 and the first delivery pump 7 being connected to first reactor 1, first mixing
Device 6 is used to the soluble-salt of copper, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol forming mixed solution, and described the
One delivery pump 7 is for the mixed solution to be delivered in the first reactor 1.
The system further includes the second mixer 8 and the second delivery pump 9 being connected to second reactor 2, second mixing
Device 8 is used to deionized water and citric acid forming mixed solution, and second delivery pump 9 is for the mixed solution to be delivered to
In second reactor 2.
Wherein, the pressure difference value of first reactor 1 and second reactor 2 is 0.5MPa.
The present embodiment also provides a kind of method that the preparation system using above-mentioned auto-exhaust catalyst prepares catalyst, should
Method includes the following steps：
(1) carbon dioxide is passed through into first reactor so that it is default that the pressure in the first reactor reaches first
Pressure value 15MPa；Then the mixing that copper nitrate, cerous nitrate, zirconium nitrate and absolute ethyl alcohol are added into the first reactor is molten
Liquid, warming while stirring is to 160 DEG C.
Wherein, the molar ratio of copper nitrate, cerous nitrate and zirconium nitrate is：0.15：0.65：0.2.
(2) carbon dioxide is passed through into second reactor so that it is default that the pressure in the second reactor reaches second
Pressure value 14.5MPa；Then into the second reactor be added deionized water, citric acid mixed solution, rise while stirring
Temperature is to 160 DEG C；
(3) supercritical carbon dioxide for the mixed solution that deionized water and citric acid are entrained in step (2) is slowly led to
Enter into the first reactor, stir the first reactor so that the deionized water and citric acid and described first are instead
It answers the solution in device to be sufficiently mixed, controls the temperature of the first reactor at 160 DEG C, after reacting 10 hours, be filtered, washed
To solid product, the solid product is dry, calcining obtains copper cerium zirconium composite catalyst.
Wherein, drying condition is：Dry 2h at 90 DEG C, calcination condition are 400 DEG C of calcining 2h.
The copper cerium zirconium composite catalyst of above-mentioned preparation is tested for the property, the conversion ratio of CO, HC and NO are reached
92.3%.
To sum up, the present invention introduces hydrolysis in supercritical carbon dioxide environment, utilizes the strong of supercritical carbon dioxide
Friendly, unique chemical reaction environment that solubility property, entrainment performance and supercritical fluid are capable of providing prepares copper cerium zirconium
Ternary complex catalyst.The surface tension of supercritical carbon dioxide is relatively low, so as to reduce or substitute surfactant
Addition, green cleaning, the copper cerium zirconium composite catalyst of preparation reaches 92.3% to the conversion ratio of CO, HC and NO.
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (7)
1. a kind of preparation method of auto-exhaust catalyst, which is characterized in that include the following steps：
(1) carbon dioxide is passed through into first reactor so that the pressure in the first reactor reaches the first preset pressure
Value, first preset pressure value are 8~15MPa；Then be added into the first reactor soluble-salt of copper, cerium can
The mixed solution of soluble, the soluble-salt of zirconium and absolute ethyl alcohol, warming while stirring is to 100~160 DEG C；
(2) carbon dioxide is passed through into second reactor so that the pressure in the second reactor reaches the second preset pressure
The difference of value, first preset pressure value and second preset pressure value is 0.1~0.5MPa；Then anti-to described second
Answer in device be added deionized water, citric acid mixed solution, warming while stirring is to 100~160 DEG C；
(3) by the supercritical carbon dioxide for the mixed solution for being entrained with deionized water and citric acid in step (2) be slowly introducing to
In the first reactor, the first reactor is stirred so that the deionized water and citric acid and the first reactor
Interior solution is sufficiently mixed, and is controlled the temperature of the first reactor at 130~160 DEG C, after reacting 5~10 hours, is filtered, washes
It washs to obtain solid product, the solid product is dry, calcining obtains the auto-exhaust catalyst.
2. the preparation method of auto-exhaust catalyst according to claim 1, which is characterized in that in step (1), copper can
The molar ratio of the soluble-salt of soluble, the soluble-salt of cerium and zirconium is (0.05~0.15)：(0.65~0.85)：(0.1~
0.2)。
3. the preparation method of auto-exhaust catalyst according to claim 1, which is characterized in that the solubility of the copper
The soluble-salt of salt, the soluble-salt of cerium and zirconium is copper nitrate, cerous nitrate and zirconium nitrate respectively.
4. a kind of preparation system of auto-exhaust catalyst, which is characterized in that including：First reactor, second reactor, dioxy
Change carbon storage tank, booster pump and triple valve, the carbon dioxide exported in the carbon dioxide storage tank after booster pump supercharging
The triple valve punishment is at two-way, wherein being input to all the way in the first reactor, another way is input in second reactor；
Further include the first mixer and the first delivery pump being connected to first reactor, first mixer for by copper can
Soluble, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol form mixed solution, and first delivery pump is used for institute
Mixed solution is stated to be delivered in the first reactor；
Further include the second mixer and the second delivery pump being connected to second reactor, second mixer is used for deionization
Water and citric acid form mixed solution, and second delivery pump is for the mixed solution to be delivered in second reactor.
5. the preparation system of auto-exhaust catalyst according to claim 4, which is characterized in that the solubility of the copper
Salt, the soluble-salt of cerium, the soluble-salt of zirconium and absolute ethyl alcohol are formed in mixed solution, the soluble-salt of copper, the solubility of cerium
The molar ratio of the soluble-salt of salt and zirconium is (0.05~0.15)：(0.65~0.85)：(0.1~0.2).
6. the preparation system of auto-exhaust catalyst according to claim 4, which is characterized in that the solubility of the copper
The soluble-salt of salt, the soluble-salt of cerium and zirconium is copper nitrate, cerous nitrate and zirconium nitrate respectively.
7. the preparation system of auto-exhaust catalyst according to claim 4, which is characterized in that the first reactor and
The pressure difference value of second reactor is 0.1~0.5MPa.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1600418A (en) * | 2003-09-25 | 2005-03-30 | 昆明贵研催化剂有限责任公司 | Catalyst for decontaminating tail gas of motorcar and preparation method |
| CN107042112A (en) * | 2017-04-21 | 2017-08-15 | 黑龙江大学 | Selective catalyst reduction of nitrogen oxides catalyst, preparation method and applications |
-
2018
- 2018-05-17 CN CN201810474383.4A patent/CN108579754A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1600418A (en) * | 2003-09-25 | 2005-03-30 | 昆明贵研催化剂有限责任公司 | Catalyst for decontaminating tail gas of motorcar and preparation method |
| CN107042112A (en) * | 2017-04-21 | 2017-08-15 | 黑龙江大学 | Selective catalyst reduction of nitrogen oxides catalyst, preparation method and applications |
Non-Patent Citations (2)
| Title |
|---|
| 徐鹏: "超临界水解制备金属氧化物微粒的实验研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 * |
| 蒋阳等主编: "《粉体工程》", 31 December 2008, 武汉理工大学出版社 * |
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