CN117380255B - Preparation method and application of catalyst for purifying nitrogen oxides - Google Patents

Preparation method and application of catalyst for purifying nitrogen oxides Download PDF

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CN117380255B
CN117380255B CN202311650163.XA CN202311650163A CN117380255B CN 117380255 B CN117380255 B CN 117380255B CN 202311650163 A CN202311650163 A CN 202311650163A CN 117380255 B CN117380255 B CN 117380255B
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catalyst
sol
preparing
nitrogen oxides
uniformly mixing
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CN117380255A (en
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宋燕海
张春丽
赵宏义
段志青
王飞
庄忠再
郝晶晶
曹英才
张鹏
郑华
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Hebei Hwat Automobile Components Co ltd
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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
    • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
    • B01J29/76—Iron group metals or copper
    • 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
    • B01D53/9404—Removing only nitrogen compounds
    • B01D53/9409—Nitrogen oxides
    • B01D53/9413—Processes characterised by a specific catalyst
    • B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas

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  • Chemical Kinetics & Catalysis (AREA)
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  • Health & Medical Sciences (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

The invention relates to the technical field of automobile exhaust purification, and provides a preparation method and application of a catalyst for purifying nitrogen oxides, wherein the preparation method comprises the following steps: s1, preparing composite sol: uniformly mixing silica sol, nano aluminum sol and aluminum sol to obtain composite sol; the mass ratio of the silica sol to the nano aluminum sol is 4:6-12:13; s2, preparing catalyst slurry: adding deionized water into the composite sol, uniformly mixing, adding molecular sieve powder containing cerium hydroxide, and uniformly mixing to obtain catalyst slurry; s3, preparing a catalyst for purifying nitrogen oxides: and (3) coating the catalyst slurry on the surface of ceramic, and roasting to obtain the nitrogen oxide purifying catalyst. Through the technical scheme, the problems of low loading capacity and high falling rate of the catalyst for purifying nitrogen oxides in the prior art are solved.

Description

Preparation method and application of catalyst for purifying nitrogen oxides
Technical Field
The invention relates to the technical field of automobile exhaust purification, in particular to a preparation method and application of a catalyst for purifying nitrogen oxides.
Background
Nitrogen oxides are one of the main atmospheric pollutants. The nitrogen oxides in the automobile exhaust are very high. With the development of the automotive field, the emission of nitrogen oxides is increasing, which causes the continuous increase of atmospheric pollution. Therefore, the purification of nitrogen oxides in automobile exhaust is of great significance.
Currently, selective Catalytic Reduction (SCR) technology is considered as one of the most effective methods for purifying nitrogen oxides, and a catalyst is the core of the selective catalytic reduction technology. At present, the preparation of the catalyst for purifying nitrogen oxides mainly comprises the step of coating catalyst slurry on the surface of a ceramic carrier. However, at present, the catalyst has low loading and high shedding rate, and the purification rate of nitrogen oxides is affected. Therefore, research on a novel preparation method of a catalyst for purifying nitrogen oxides is needed to improve the loading and reduce the falling rate.
Disclosure of Invention
The invention provides a preparation method and application of a catalyst for purifying nitrogen oxides, which solve the problems of low loading capacity and high falling rate of the catalyst for purifying nitrogen oxides in the related technology.
The technical scheme of the invention is as follows:
the invention provides a preparation method of a catalyst for purifying nitrogen oxides, which comprises the following steps:
s1, preparing composite sol: uniformly mixing silica sol, nano aluminum sol and aluminum sol to obtain composite sol;
the mass ratio of the silica sol to the nano aluminum sol is 4:6-12:13;
s2, preparing catalyst slurry: adding deionized water into the composite sol, uniformly mixing, adding molecular sieve powder containing cerium hydroxide, and uniformly mixing to obtain catalyst slurry;
s3, preparing a catalyst for purifying nitrogen oxides: and coating the catalyst slurry on the surface of ceramic, and roasting to obtain the catalyst for purifying nitrogen oxides.
As a further technical scheme, in step S2, the mass ratio of the composite sol to the molecular sieve powder containing cerium hydroxide is 2:1.
In step S1, the nano-alumina sol is a lanthanum nitrate modified nano-alumina sol, and the alumina sol is a self-made alumina sol made of lanthanum nitrate, pseudo-boehmite and nitric acid.
As a further technical scheme, in step S2, the preparation method of the molecular sieve powder containing cerium hydroxide includes: and (3) dissolving cerium nitrate in a mixed solution of ammonia water and triethanolamine, uniformly mixing, adding a copper molecular sieve and nano aluminum oxide, uniformly mixing, and roasting to obtain the molecular sieve powder containing cerium hydroxide.
As a further technical scheme, the mass ratio of the cerium nitrate to the ammonia water to the triethanolamine to the copper molecular sieve to the nano alumina is 1:4:40:750-850:30.
As a further technical scheme, the preparation method of the lanthanum nitrate modified nano-alumina sol comprises the following steps: adding lanthanum nitrate into deionized water, uniformly mixing, adding nano aluminum sol dry powder, and mixing until the solution becomes light blue transparent solution, thus obtaining the lanthanum nitrate modified nano aluminum sol.
As a further technical scheme, the mass ratio of the lanthanum nitrate to the deionized water to the nano aluminum sol dry powder is 1-2:4:1.
As a further technical scheme, the preparation method of the self-made aluminum sol comprises the following steps: adding lanthanum nitrate into deionized water, uniformly mixing, adding pseudo-boehmite, uniformly mixing, finally adding nitric acid, and mixing until the solution becomes white semitransparent jelly-like solution, thereby obtaining the self-made aluminum sol.
As a further technical scheme, the mass ratio of the lanthanum nitrate to the deionized water to the pseudo-boehmite to the nitric acid is 4:18:3-5:1.
As a further technical scheme, the pseudo-boehmite comprises a first pseudo-boehmite and a second pseudo-boehmite, the pore capacities of the first pseudo-boehmite and the second pseudo-boehmite are different, and the mass ratio of the first pseudo-boehmite to the second pseudo-boehmite is 5:1.
As a further technical scheme, the average pore volume of the first pseudo-boehmite is 1mL/g, and the average pore volume of the second pseudo-boehmite is 0.6mL/g.
As a further technical scheme, in step S3, the coating is divided into a first-stage coating and a second-stage coating, wherein the first-stage coating is to coat the catalyst slurry on one end of the ceramic surface, and the second-stage coating is to coat the catalyst slurry on the other end of the ceramic surface, and the first-stage coating is to dry the catalyst slurry at 80-100 ℃ for 2-5min.
As a further technical scheme, the ceramic is one of cordierite, spodumene, mullite and zircon.
As a further technical scheme, in the step S3, the roasting temperature is 450-550 ℃ and the roasting time is 1-3h.
The invention also provides application of the nitrogen oxide purifying catalyst obtained by the preparation method of the nitrogen oxide purifying catalyst in purifying automobile exhaust.
The working principle and the beneficial effects of the invention are as follows:
1. in the invention, the molecular sieve powder containing cerium hydroxide is mixed with the composite sol, so that the uniformity of catalyst slurry is improved, and the loading capacity of the catalyst for purifying nitrogen oxides is increased in the subsequent coating process. Wherein, through the synergistic blending of silica sol, nano aluminum sol and aluminum sol, the shedding rate of the catalyst for purifying nitrogen oxides is reduced.
2. According to the invention, the lanthanum nitrate is used for modifying the nano aluminum sol, so that the loading capacity of the catalyst for purifying nitrogen oxides is further increased, and the purification rate of the catalyst for purifying nitrogen oxides is improved.
3. In the invention, lanthanum nitrate, pseudo-boehmite and nitric acid are utilized to self-prepare aluminum sol, so that the active components in the catalyst for purifying nitrogen oxides are increased, and the purification rate of the catalyst for purifying the nitrogen oxides is further improved.
4. In the invention, when the self-made aluminum sol is prepared, two pseudo-boehmite with different pore capacities are selected, which is favorable for uniformly dispersing lanthanum nitrate in the self-made aluminum sol, thereby further increasing the loading capacity of the catalyst for purifying nitrogen oxides and improving the purifying rate of the catalyst for nitrogen oxides.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following examples and comparative examples, the model of the copper molecular sieve was SSZ-13, the model of the nano alumina was LAE-5, the model of the silica sol was GSW-30, the model of the nano alumina sol was JHASH-15, the alumina sol was A-4 type alumina sol, the model of the first pseudo-boehmite was ZTL-MAH, and the model of the second pseudo-boehmite was ZTL-CAH.
In the following examples and comparative examples, unless otherwise specified;
the preparation method of the cerium hydroxide-containing molecular sieve powder comprises the following steps: according to parts by weight, 1 part of cerium nitrate is dissolved in a mixed solution of 4 parts of ammonia water and 40 parts of triethanolamine, the mixed solution is uniformly mixed, 800 parts of copper molecular sieve and 30 parts of nano alumina are added, the mixed solution is uniformly mixed, evaporated to dryness, and the mixture is baked for 1.5 hours at 400 ℃ under the protection of inert gas and then ground to obtain cerium hydroxide-containing molecular sieve powder;
the preparation method of the lanthanum nitrate modified nano aluminum sol comprises the following steps: adding 4 parts of lanthanum nitrate into 16 parts of deionized water, uniformly mixing, adding 4 parts of nano aluminum sol dry powder, and mixing until the solution becomes light blue transparent solution to obtain lanthanum nitrate modified nano aluminum sol;
the preparation method of the self-made aluminum sol comprises the following steps: adding 12 parts of lanthanum nitrate into 54 parts of deionized water, uniformly mixing, adding 10 parts of first pseudo-boehmite and 2 parts of second pseudo-boehmite, uniformly mixing, finally adding 3 parts of nitric acid, and mixing until the solution becomes white semitransparent jelly-like solution, thus obtaining the self-made alumina sol.
Example 1
A method for preparing a catalyst for purifying nitrogen oxides, which comprises the following steps:
s1, preparing composite sol: according to the weight parts, 8 parts of silica sol, 12 parts of nano aluminum sol and 26 parts of aluminum sol are uniformly mixed to obtain composite sol;
s2, preparing catalyst slurry: adding 23 parts of deionized water into the composite sol according to parts by weight, uniformly mixing, adding 23 parts of cerium hydroxide-containing molecular sieve powder, and uniformly mixing to obtain catalyst slurry;
s3, preparing a catalyst for purifying nitrogen oxides: firstly, coating catalyst slurry on one end of the surface of cordierite ceramic, drying at 80 ℃ for 5min, coating catalyst slurry on the other end of the surface of cordierite ceramic, drying at 80 ℃ for 5min, and roasting at 450 ℃ for 3h to obtain the purified nitrogen oxide catalyst.
Example 2
A method for preparing a catalyst for purifying nitrogen oxides, which comprises the following steps:
s1, preparing composite sol: according to the weight parts, 8 parts of silica sol, 12 parts of lanthanum nitrate modified nano-alumina sol and 26 parts of self-made alumina sol are uniformly mixed to obtain composite sol;
s2, preparing catalyst slurry: adding 23 parts of deionized water into the composite sol according to parts by weight, uniformly mixing, adding 23 parts of cerium hydroxide-containing molecular sieve powder, and uniformly mixing to obtain catalyst slurry;
s3, preparing a catalyst for purifying nitrogen oxides: firstly, coating catalyst slurry on one end of the surface of cordierite ceramic, drying at 80 ℃ for 5min, coating catalyst slurry on the other end of the surface of cordierite ceramic, drying at 80 ℃ for 5min, and roasting at 450 ℃ for 3h to obtain the purified nitrogen oxide catalyst.
Example 3
A method for preparing a catalyst for purifying nitrogen oxides, which comprises the following steps:
s1, preparing composite sol: according to the weight parts, 8 parts of silica sol, 18 parts of lanthanum nitrate modified nano-alumina sol and 26 parts of self-made alumina sol are uniformly mixed to obtain composite sol;
s2, preparing catalyst slurry: adding 26 parts of deionized water into the composite sol according to parts by weight, uniformly mixing, adding 26 parts of cerium hydroxide-containing molecular sieve powder, and uniformly mixing to obtain catalyst slurry;
s3, preparing a catalyst for purifying nitrogen oxides: firstly, coating catalyst slurry on one end of the surface of cordierite ceramic, drying at 90 ℃ for 3.5min, coating catalyst slurry on the other end of the surface of cordierite ceramic, drying at 90 ℃ for 3.5min, and roasting at 500 ℃ for 2h to obtain the purified nitrogen oxide catalyst.
Example 4
A method for preparing a catalyst for purifying nitrogen oxides, which comprises the following steps:
s1, preparing composite sol: according to the weight parts, 8 parts of silica sol, 24 parts of lanthanum nitrate modified nano aluminum sol and 26 parts of self-made aluminum sol are uniformly mixed to obtain composite sol;
s2, preparing catalyst slurry: adding 29 parts of deionized water into the composite sol according to parts by weight, uniformly mixing, adding 29 parts of cerium hydroxide-containing molecular sieve powder, and uniformly mixing to obtain catalyst slurry;
s3, preparing a catalyst for purifying nitrogen oxides: firstly, coating catalyst slurry on one end of the surface of cordierite ceramic, drying for 2min at 100 ℃, then coating the catalyst slurry on the other end of the surface of cordierite ceramic, drying for 2min at 100 ℃, and roasting for 1h at 550 ℃ to obtain the purified nitrogen oxide catalyst.
Example 5
The difference between this embodiment and embodiment 2 is that in step S1, the self-made alumina sol is different, and in this embodiment, the preparation method of the self-made alumina sol is as follows: adding 12 parts of lanthanum nitrate into 54 parts of deionized water according to parts by weight, uniformly mixing, adding 12 parts of first pseudo-boehmite, uniformly mixing, finally adding 3 parts of nitric acid, and mixing until the solution becomes white semitransparent jelly-like solution, thus obtaining self-made aluminum sol.
Example 6
The difference between this embodiment and embodiment 2 is that in step S1, the self-made alumina sol is different, and in this embodiment, the preparation method of the self-made alumina sol is as follows: adding 12 parts of lanthanum nitrate into 54 parts of deionized water, uniformly mixing, adding 12 parts of second pseudo-boehmite, uniformly mixing, finally adding 3 parts of nitric acid, and mixing until the solution becomes white semitransparent jelly-like solution, thus obtaining self-made aluminum sol.
Comparative example 1
A method for preparing a catalyst for purifying nitrogen oxides, which comprises the following steps:
s1, preparing catalyst slurry: adding 23 parts of deionized water into 46 parts of silica sol, uniformly mixing, adding 23 parts of cerium hydroxide-containing molecular sieve powder, and uniformly mixing to obtain catalyst slurry;
s2, preparing a catalyst for purifying nitrogen oxides: firstly, coating catalyst slurry on one end of the surface of cordierite ceramic, drying at 80 ℃ for 5min, coating catalyst slurry on the other end of the surface of cordierite ceramic, drying at 80 ℃ for 5min, and roasting at 450 ℃ for 3h to obtain the purified nitrogen oxide catalyst.
Comparative example 2
The present comparative example differs from comparative example 1 only in that in step S1, the silica sol is replaced with an equivalent amount of lanthanum nitrate modified nano-alumina sol.
Comparative example 3
The present comparative example differs from comparative example 1 only in that in step S1, the silica sol is replaced with an equivalent amount of self-made alumina sol.
Comparative example 4
The present comparative example differs from comparative example 1 only in that in step S1, the silica sol was replaced with 14.5 parts of lanthanum nitrate modified nano-alumina sol and 31.5 parts of self-made alumina sol.
The purified nitrogen oxide catalysts prepared in examples 1-6 and comparative examples 1-4 were subjected to the following performance tests:
(1) loading amount: the weighing method is adopted for measurement, and the calculation formula is as follows:
loading= (weight of purified nitrogen oxide catalyst-weight of cordierite ceramic)/volume of cordierite ceramic;
(2) shedding rate: at a position 2cm away from the section of the catalyst for purifying the nitrogen oxide, uniformly purging with 10bar of compressed air, wherein the purging time is 2min, and the calculation formula is as follows:
the falling rate (%) = (weight of nitrogen oxide purifying catalyst before purging-weight of nitrogen oxide purifying catalyst after purging)/(weight of nitrogen oxide purifying catalyst-weight of cordierite ceramic) ×100;
(3) purification rate: at 400℃the exhaust model gas (NO 200ppm, NH by volume 3 200ppm、O 2 10vol%、H 2 O 5vol%、N 2 Residual) was passed over the nitrogen oxide-purifying catalyst at a space velocity of 50000/h, and the nitrogen oxide-purifying rate was measured.
The test results are shown in table 1 below.
Table 1 results of performance test of nitrogen oxide purifying catalyst
As shown in the table, the purified nitrogen oxide catalyst obtained by the preparation method has higher loading capacity, higher purification rate and lower shedding rate, wherein the loading capacity can reach 281g/L, the purification rate can reach 98.7% at the highest, and the shedding rate can reach 0.61% at the lowest, so that the catalyst can meet the industrial production and application. Examples 2-6 and comparative examples 1-4 show that compared with the combined use of single silica sol or lanthanum nitrate modified nano-alumina sol and self-made alumina sol, the silica sol, the lanthanum nitrate modified nano-alumina sol and the self-made alumina sol are cooperatively blended, so that the loading capacity and the purification rate of the nitrogen oxide purifying catalyst are greatly improved, and the falling rate is obviously reduced.
Comparison of the embodiment 1 and the embodiment 2 shows that compared with the conventional three-component blend of silica sol, nano aluminum sol and aluminum sol, the three-component blend of silica sol, lanthanum nitrate modified nano aluminum sol and self-made aluminum sol can further improve the loading amount and the purification rate of the nitrogen oxide purifying catalyst and further reduce the falling rate.
Comparison of example 2 with examples 5-6 shows that when preparing self-made alumina sol, the purification rate of the catalyst to nitrogen oxides can be further improved by selecting two pseudo-boehmite with different pore capacities.
The purified nitrogen oxide catalyst prepared in example 2 was applied to Xu Gong T4 engines and subjected to steady state NRSC and transient NRTC bench experiments, the test results of which are shown in table 2 below.
Table 2 example 2 catalyst bench test results for purifying nitrogen oxides
As can be seen from Table 2, the purified nitrogen oxide catalyst prepared in example 2 of the present invention can be successfully applied to Xu Gong T4 engines, wherein NRSC steady-state bench test NO x Conversion is 96.77%, NRTC transient bench test NO x The conversion rate is 95.85%, which shows that the purified nitrogen oxide catalyst prepared in the example 2 has good catalytic activity and meets the national non-road T4 stage emission requirements.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (7)

1. The preparation method of the catalyst for purifying nitrogen oxides is characterized by comprising the following steps:
s1, preparing composite sol: uniformly mixing silica sol, nano aluminum sol and aluminum sol to obtain composite sol;
the mass ratio of the silica sol to the nano aluminum sol to the aluminum sol is 4:6-12:13;
the nanometer aluminum sol is lanthanum nitrate modified nanometer aluminum sol, and the aluminum sol is self-made aluminum sol prepared from lanthanum nitrate, pseudo-boehmite and nitric acid;
s2, preparing catalyst slurry: adding deionized water into the composite sol, uniformly mixing, adding molecular sieve powder containing cerium hydroxide, and uniformly mixing to obtain catalyst slurry; the mass ratio of the composite sol to the cerium hydroxide-containing molecular sieve powder is 2:1; the preparation method of the cerium hydroxide-containing molecular sieve powder comprises the following steps: dissolving cerium nitrate in a mixed solution of ammonia water and triethanolamine, uniformly mixing, adding a copper molecular sieve and nano alumina, uniformly mixing, and roasting to obtain the molecular sieve powder containing cerium hydroxide; the model of the copper molecular sieve is SSZ-13;
s3, preparing a catalyst for purifying nitrogen oxides: and coating the catalyst slurry on the surface of ceramic, and roasting to obtain the catalyst for purifying nitrogen oxides.
2. The method for preparing the catalyst for purifying nitrogen oxides according to claim 1, wherein the method for preparing the lanthanum nitrate modified nano-alumina sol is as follows: adding lanthanum nitrate into deionized water, uniformly mixing, adding nano aluminum sol dry powder, and mixing until the solution becomes light blue transparent solution, thus obtaining the lanthanum nitrate modified nano aluminum sol.
3. The method for preparing the catalyst for purifying nitrogen oxides according to claim 1, wherein the method for preparing the self-made aluminum sol is as follows: adding lanthanum nitrate into deionized water, uniformly mixing, adding pseudo-boehmite, uniformly mixing, finally adding nitric acid, and mixing until the solution becomes white semitransparent jelly-like solution, thereby obtaining the self-made aluminum sol.
4. A method for preparing a catalyst for purifying nitrogen oxides according to claim 3, wherein the pseudo-boehmite comprises a first pseudo-boehmite and a second pseudo-boehmite, the pore capacities of the first pseudo-boehmite and the second pseudo-boehmite are different, and the mass ratio of the first pseudo-boehmite to the second pseudo-boehmite is 5:1.
5. The method for preparing a catalyst for purifying nitrogen oxides according to claim 1, wherein in the step S3, the coating is divided into a first stage coating and a second stage coating, the first stage coating is to coat the catalyst slurry on one end of the ceramic surface, the first stage coating is to dry the ceramic surface at 80-100 ℃ for 2-5min, and the second stage coating is to coat the catalyst slurry on the other end of the ceramic surface, and the second stage coating is to dry the ceramic surface at 80-100 ℃ for 2-5min.
6. The method for preparing a catalyst for purifying nitrogen oxides according to claim 1, wherein in the step S3, the roasting temperature is 450-550 ℃ and the roasting time is 1-3 hours.
7. Use of a purified nitrogen oxide catalyst obtained by a method for preparing a purified nitrogen oxide catalyst according to any one of claims 1 to 6 for purifying automobile exhaust.
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