CN117884192A - Preparation method of sewage treatment cracking reduction catalyst - Google Patents
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- CN117884192A CN117884192A CN202410288531.9A CN202410288531A CN117884192A CN 117884192 A CN117884192 A CN 117884192A CN 202410288531 A CN202410288531 A CN 202410288531A CN 117884192 A CN117884192 A CN 117884192A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- 239000010865 sewage Substances 0.000 title claims abstract description 45
- 230000009467 reduction Effects 0.000 title claims abstract description 25
- 238000005336 cracking Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 33
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 25
- 239000000661 sodium alginate Substances 0.000 claims abstract description 25
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 25
- 229910000514 dolomite Inorganic materials 0.000 claims abstract description 22
- 239000010459 dolomite Substances 0.000 claims abstract description 22
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- 230000008569 process Effects 0.000 claims abstract description 11
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- 239000000203 mixture Substances 0.000 claims description 52
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
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- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 238000004108 freeze drying Methods 0.000 claims description 12
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- 238000001035 drying Methods 0.000 claims description 11
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- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000002736 nonionic surfactant Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
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Abstract
The invention relates to a preparation method of a sewage treatment cracking reduction catalyst, and belongs to the technical field of catalysts. According to the method, dolomite is firstly roasted for the first time to improve the catalytic performance, alumina is used as a carrier, and then a lyophilization process and a secondary roasting process are combined to prepare the catalyst with uniform pore size distribution, high specific surface area and high dispersity; the adsorption performance of the catalyst is improved by adding pollution-free sodium alginate, and in addition, the addition of the sodium alginate can also prevent metal ions in the catalyst from migrating into water to cause secondary pollution.
Description
Technical Field
The invention belongs to the technical field of catalysts, and relates to a preparation method of a sewage treatment cracking reduction catalyst.
Background
The sewage reclamation refers to treating and purifying polluted water bodies such as industrial wastewater, domestic sewage, rainwater and the like in various modes to ensure that the water quality reaches a certain standard and can meet a certain use purpose, thereby being capable of being reused as a new water resource. The treatment of toxic and difficultly biodegradable organic wastewater, such as petroleum exploitation, pharmacy, pesticide, papermaking, printing and dyeing and other wastewater, is still lack of economical and effective practical technology. Such toxic, difficult to biodegrade substances are highly dangerous, some also have carcinogenic, teratogenic, mutagenic properties, which by themselves and their chemical composition pose a hazard to biological life or human health. At present, main pollutants are tar, sulfur, cyanogen, phenol, suspended matters, various organic matters and partial heavy metals.
In general, the sewage reuse technology needs to reasonably combine a plurality of sewage treatment technologies, namely, various water treatment methods are combined for advanced treatment. This is because it is generally difficult to meet the water quality requirements of the reuse water by a single water treatment process. Biological treatment (such as a traditional activated sludge method, a filler activated sludge method, an anaerobic-anoxic-aerobic activated sludge method, a contact oxidation method, an aeration filter tank, a biological fluidized bed method, a biological turntable method and the like) commonly used in the existing reclaimed water recycling and sewage centralized treatment recycling processes is performed by adopting a process of coagulating sedimentation, filtering, adsorption and disinfection (ultraviolet, chlorine, ozone or chlorine dioxide and the like) as a post-treatment technology after the secondary treatment so as to meet the requirement of sewage recycling, and the use of a catalyst in the method can effectively improve the sewage treatment efficiency, so that the development of a sewage treatment cracking reduction catalyst is necessary to solve the problems.
Disclosure of Invention
The invention aims to provide a preparation method of a sewage treatment cracking reduction catalyst, which has the characteristics of uniform pore size distribution, high specific surface area and high dispersity.
The aim of the invention can be achieved by the following technical scheme:
A preparation method of a sewage treatment cracking reduction catalyst, which comprises the following steps,
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
s2: roasting the precursor obtained by drying at 900-1300 ℃ for 4-6 hours to obtain a black solid product;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
s4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, carrying out secondary roasting on the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The catalytic activity of the calcined dolomite is greatly improved compared with that of the uncalcined dolomite, and the calcined dolomite can absorb H 2 S, HCl in gasification gas and destroy part of heavy tar. The complex of CaO-MgO is formed after the dolomite catalyst is roasted, and the complex is a mixed oxide catalyst, and the mixture of oxides causes the atomic array to generate a certain degree of distortion, so that more catalytic active centers are generated; tar contains a plurality of condensed ring compounds with electronegative pi electron systems, pi electron clouds are destroyed after being adsorbed on an activation site to lose stability, so that C-C bond and C-H bond are easy to break, and cracking activation energy is reduced, therefore, dolomite is roasted once in the preparation process.
The alumina can react with the active component of the catalyst to disperse the active component of the catalyst into the carrier, and provide effective specific surface area and proper pore structure for the active component so as to improve the thermal stability and the antitoxic performance of the catalyst.
The invention also utilizes the characteristics of gel precipitation formed by sodium alginate, calcium ions, iron ions and the like and stronger adsorptivity thereof to be used as a water purifying agent. When the water is purified, the agglomeration condition is unfavorable, and when the turbidity is large, the sodium alginate with strong adsorption force is added to promote the agglomeration, so that the sewage purification rate is improved.
According to the invention, a freeze-drying method is used in the preparation process, and metal ions are fixed on a carrier in situ and uniformly through quenching of liquid nitrogen, so that the catalyst prepared later has more uniform active site distribution, and the prepared catalyst has more uniform pore size distribution, larger specific surface area and better catalytic performance by combining secondary roasting.
Further, the particle size of the dolomite powder obtained by crushing in the step S1 is 3-5 mu m.
Further, the molecular weight of the polyethylene glycol in the S1 is 200-600.
The polyethylene glycol with low molecular weight is used in the invention, and the polyethylene glycol with the molecular weight range has better permeability and viscosity, can be fully mixed with dolomite, and has good permeability and viscosity, thereby being beneficial to metal fixation in the freeze-drying process.
Further, the temperature rising rate of the roasting process in the step S2 is 10 ℃/min.
Further, in the step S3, the particle size of the mixture of aluminum oxide, nickel nitrate and sodium alginate is 3-5 μm.
Further, the temperature rising rate in the roasting process in the step S4 is 5 ℃/min.
The method comprises the steps of carrying out secondary roasting on the prepared catalyst, wherein the temperature of the first selection is 900-1300 ℃, when the roasting temperature is too low, mgCO 3、CaCO3 in dolomite cannot be completely decomposed to generate a complex, and when the roasting temperature is too high, mgO grains grow up and lose activity; and the roasting temperature is 400 ℃ in the secondary roasting process, and the nickel oxide obtained by roasting at the temperature has the optimal activity.
Further, the screen used in the screening in the step S4 is 1000 meshes.
Further, the sewage treatment cracking reduction catalyst prepared in the step S5 is spherical with the particle size of 10 mm.
According to the method, dolomite is roasted at 900-1300 ℃, the dolomite is decomposed to obtain a CaO-MgO complex without excessively large grains losing activity, sodium alginate is added to prevent migration of Ca and Mg metal elements, secondary pollution generated by a catalyst is reduced, metal ions are uniformly fixed on a carrier in situ through a quenching step of a freeze-drying method, so that the catalyst has more uniform active site distribution, and the secondary roasting is carried out at 400 ℃, so that sintering of the metal carrier at high temperature and collapse of holes generated by freeze-drying can be effectively avoided, and the prepared catalyst has optimal performance.
The invention has the beneficial effects that:
According to the method, dolomite is firstly roasted for the first time to improve the catalytic performance, alumina is used as a carrier, and then a lyophilization process and a secondary roasting process are combined to prepare the catalyst with uniform pore size distribution, high specific surface area and high dispersity; the adsorption performance of the catalyst is improved by adding pollution-free sodium alginate, and in addition, the addition of the sodium alginate can also prevent metal ions in the catalyst from migrating into water to cause secondary pollution.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description is given below with reference to the embodiments, structures, features and effects according to the present invention.
According to the invention, the measurement standard is HJ 91.1-2019, namely sewage monitoring technical Specification, untreated sewage and sewage treated by the catalyst are respectively sampled, and the components of the untreated sewage and the sewage treated by the catalyst are detected to obtain the purification rate of the sewage.
The raw material suppliers in the examples and comparative examples of the present invention are shown in the following table,
Example 1
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
s2: roasting the dried precursor at 900 ℃ for 6 hours to obtain a black solid product;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
s4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, carrying out secondary roasting on the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The purification rate of the catalyst for sewage in the embodiment is 98.5%.
Example 2
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
s2: roasting the dried precursor at 1300 ℃ for 4 hours to obtain a black solid product;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
s4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, carrying out secondary roasting on the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The purification rate of the catalyst for sewage in the embodiment is 98.2%.
Example 3
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
S2: roasting the dried precursor at 1200 ℃ for 4 hours to obtain a black solid product;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
s4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, carrying out secondary roasting on the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The purification rate of the catalyst of the embodiment to sewage is 99.9%.
Comparative example 1
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
s2: in the comparative example, dolomite is not subjected to primary roasting;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
S4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, roasting the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The purification rate of the catalyst for the comparative example on sewage is 94.8%.
Comparative example 2
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
S2: roasting the dried precursor at 1200 ℃ for 4 hours to obtain a black solid product;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
S4: drying the mixture prepared in the step S3 for 12 hours at 110 ℃, carrying out secondary roasting on the dried solid at 400 ℃ for 4 hours, crushing, grinding and sieving the solid obtained by roasting, wherein a freeze-drying method is not used in the comparative example;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The purification rate of the catalyst for the comparative example on sewage is 96.9%.
Comparative example 3
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
S2: roasting the dried precursor at 1200 ℃ for 4 hours to obtain a black solid product;
S3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide and nickel nitrate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2, sodium alginate is not added in the comparative example;
s4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, carrying out secondary roasting on the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
The purification rate of the catalyst for the comparative example on sewage is 96.5%.
The invention is used when in use:
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (8)
1. A preparation method of a sewage treatment cracking reduction catalyst is characterized by comprising the following steps of,
S1: pulverizing dolomite into powder by using a jet mill, wherein the mass ratio of the powder obtained by pulverizing to the nonionic surfactant polyethylene glycol is (3): 1, after being uniformly stirred, carrying out ultrasonic treatment for 1h, and drying the obtained mixture at 110 ℃ for 24h;
s2: roasting the precursor obtained by drying at 900-1300 ℃ for 4-6 hours to obtain a black solid product;
s3: grinding the black solid product obtained in the step S2, dispersing 5g in 1L of deionized water, adding a mixture of aluminum oxide, nickel nitrate and sodium alginate, stirring at a rotating speed of 300r/min, and carrying out ultrasonic treatment for 1h to obtain a uniform mixture, wherein the mass ratio of the black solid product to the mixture is 1:1, the mass ratio of the aluminum oxide, the nickel nitrate and the sodium alginate in the mixture is 4:2:1, a step of;
s4: putting the mixture prepared in the step S3 into liquid nitrogen to be frozen for 10min, transferring to a freeze dryer to carry out freeze-drying treatment, carrying out secondary roasting on the freeze-dried solid at 400 ℃ for 4h, and crushing, grinding and sieving the solid obtained by roasting;
S5: and (3) putting the product prepared in the step (S4) into a press machine for pressing, granulating and forming to obtain the sewage treatment cracking reduction catalyst.
2. The method for preparing a sewage treatment cracking reduction catalyst according to claim 1, wherein the particle size of dolomite powder obtained by crushing in the step S1 is 3-5 μm.
3. The method for preparing a catalyst for sewage treatment and pyrolysis reduction according to claim 1, wherein the molecular weight of polyethylene glycol in the S1 is 200-600.
4. The method for preparing a catalyst for sewage treatment and pyrolysis reduction according to claim 1, wherein the heating rate of the roasting process in S2 is 10 ℃/min.
5. The method for preparing a catalyst for sewage treatment and pyrolysis reduction according to claim 1, wherein the particle size of the mixture of alumina, nickel nitrate and sodium alginate in the step S3 is 3-5 μm.
6. The method for preparing a catalyst for sewage treatment and pyrolysis reduction according to claim 1, wherein the heating rate of the roasting process in S4 is 5 ℃/min.
7. The method for preparing a catalyst for sewage treatment and pyrolysis reduction according to claim 1, wherein the screen used in the screening in the step S4 is 1000 mesh.
8. The method for preparing a catalyst for sewage treatment and pyrolysis reduction according to claim 1, wherein the catalyst for sewage treatment and pyrolysis reduction obtained by pressing in the step S5 is spherical with a particle size of 10 mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410288531.9A CN117884192B (en) | 2024-03-14 | 2024-03-14 | Preparation method of sewage treatment cracking reduction catalyst |
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| CN202410288531.9A CN117884192B (en) | 2024-03-14 | 2024-03-14 | Preparation method of sewage treatment cracking reduction catalyst |
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| CN117884192A true CN117884192A (en) | 2024-04-16 |
| CN117884192B CN117884192B (en) | 2024-05-10 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101396660A (en) * | 2008-10-22 | 2009-04-01 | 中国林业科学研究院林产化学工业研究所 | Biomass gasification tar cracking composite catalyst and preparation method thereof |
| CN111151232A (en) * | 2018-11-08 | 2020-05-15 | 营口市向阳催化剂有限责任公司 | Preparation method of spherical alumina |
| CN113304752A (en) * | 2021-06-11 | 2021-08-27 | 上海复沅环保工程有限公司 | Cracking reduction catalyst for sewage treatment and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101396660A (en) * | 2008-10-22 | 2009-04-01 | 中国林业科学研究院林产化学工业研究所 | Biomass gasification tar cracking composite catalyst and preparation method thereof |
| CN111151232A (en) * | 2018-11-08 | 2020-05-15 | 营口市向阳催化剂有限责任公司 | Preparation method of spherical alumina |
| CN113304752A (en) * | 2021-06-11 | 2021-08-27 | 上海复沅环保工程有限公司 | Cracking reduction catalyst for sewage treatment and preparation method thereof |
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