CN111450812A - Composition and method for preparing titanium dioxide molded product - Google Patents
Composition and method for preparing titanium dioxide molded product Download PDFInfo
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- CN111450812A CN111450812A CN201910058802.0A CN201910058802A CN111450812A CN 111450812 A CN111450812 A CN 111450812A CN 201910058802 A CN201910058802 A CN 201910058802A CN 111450812 A CN111450812 A CN 111450812A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000203 mixture Substances 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 32
- 241000219782 Sesbania Species 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 15
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004898 kneading Methods 0.000 claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims abstract description 6
- 238000007580 dry-mixing Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 3
- 150000001735 carboxylic acids Chemical class 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 8
- 239000008188 pellet Substances 0.000 description 8
- 239000012752 auxiliary agent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- SXAMGRAIZSSWIH-UHFFFAOYSA-N 2-[3-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,2,4-oxadiazol-5-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NOC(=N1)CC(=O)N1CC2=C(CC1)NN=N2 SXAMGRAIZSSWIH-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2 ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
Abstract
The invention provides a composition for preparing a titanium dioxide forming object, which comprises nano titanium dioxide powder, sesbania powder and polycarboxylic acid. The invention also provides a preparation method of the titanium dioxide forming object, which comprises the following steps: step S1, carrying out dry mixing on the nano titanium dioxide powder, the sesbania powder and the polycarboxylic acid to obtain mixed powder; step S2, adding water into the mixed powder obtained in the step S1, and stirring and kneading the mixture to obtain wet dough; and step S3, performing extrusion molding on the wet dough obtained in the step S2, and drying and calcining the wet dough to obtain a titanium dioxide molded product. The preparation method has the advantages of simple process, environmental protection and low cost, and the prepared titanium dioxide forming product can be used as a carrier in a catalyst.
Description
Technical Field
The invention belongs to the field of catalytic materials, and particularly relates to a composition and a method for preparing a titanium dioxide forming object.
Background
Titanium dioxide is one of main raw materials for realizing industrial production of Selective Catalytic Reduction (SCR) denitration catalysts, and practical experience shows that the cost of titanium dioxide accounts for more than 70% of the total production cost of the catalysts and is a primary factor for controlling the performance and the cost of the catalysts.
The localization of the denitration catalyst carrier titanium dioxide raw material is a restriction bottleneck for the development of the denitration industry in China, and is related to whether the energy-saving and emission-reducing engineering in China can be smoothly implemented. Therefore, the preparation technology of the denitration catalyst carrier raw material and the realization of the batch production of the raw material are extremely important for the production of the catalyst.
Titanium dioxide is used as a barren material, the forming of the titanium dioxide is difficult and the process is complex, and the forming research work of the titanium dioxide is an important basis for the wide application of the titanium dioxide carrier. The strip-shaped titanium dioxide carrier is used as a carrier of a low-temperature catalyst for flue gas denitration in the low-temperature and low-dust field, and the strip-shaped titanium dioxide carrier is required to have a proper specific surface area, a proper pore structure and a certain mechanical strength.
Disclosure of Invention
In order to achieve the above object, the present invention provides a composition for preparing a titanium dioxide molding, and a method for preparing a titanium dioxide molding.
According to a first aspect, the invention provides a composition for preparing titanium dioxide moldings, which comprises nano titanium dioxide powder, sesbania powder and polycarboxylic acid.
According to some embodiments of the present invention, the nano titanium dioxide powder is 80 to 90 wt%, the sesbania powder is 8 to 9 wt%, and the polycarboxylic acid is 1 to 12 wt%; preferably, the nano titanium dioxide powder is 85-88 wt%, the sesbania powder is 8.5-8.8 wt%, and the polycarboxylic acid is 3.2-6.5 wt%.
According to some embodiments of the invention, the nano-titania is anatase, rutile or P25 type.
According to some embodiments of the invention, the polycarboxylic acid is oxalic acid, citric acid or a mixture of both.
According to a second aspect, the present invention provides a method for preparing a titanium dioxide molding, comprising the steps of:
step S1, carrying out dry mixing on the nano titanium dioxide powder, the sesbania powder and the polycarboxylic acid to obtain mixed powder;
step S2, adding water into the mixed powder obtained in the step S1, and stirring and kneading the mixture to obtain wet dough;
and step S3, performing extrusion molding on the wet dough obtained in the step S2, and drying and calcining the wet dough to obtain a titanium dioxide molded product.
According to some embodiments of the present invention, the nano titanium dioxide powder is 80 to 90 wt%, the sesbania powder is 8 to 9 wt%, and the polycarboxylic acid is 1 to 12 wt%; preferably, the nano titanium dioxide powder is 85-88 wt%, the sesbania powder is 8.5-8.8 wt%, and the polycarboxylic acid is 3.2-6.5 wt%.
According to some embodiments of the invention, the nano-titania is anatase, rutile or P25 type.
According to some embodiments of the invention, the polycarboxylic acid is oxalic acid, citric acid or a mixture of both.
According to some embodiments of the invention, the wet mass is kneaded in a twin screw extruder in step S2 and/or extrusion molded using a twin screw extruder in step S3. Preferably, the molding is in the form of a strip.
According to some embodiments of the present invention, in step S2, the mass ratio of water to the mixed powder is 1: (1-5), preferably 1: (1.5-4), more preferably 1: (2-4).
According to some embodiments of the invention, in step S2, the kneading time is 0.5 to 1 h.
According to some embodiments of the invention, in step S3, the drying conditions are: the temperature is 80-120 ℃, and the time is 8-24 h.
According to some embodiments of the present invention, in step S3, the calcination is performed in two stages, wherein the first stage calcination temperature is 200 ℃ to 250 ℃, the temperature rise rate is 2 to 10 ℃/mim, and the time is 1 to 2 h; the second stage calcination temperature is 500-550 ℃, the heating rate is 2-10 ℃/mim, and the time is 4-6 h.
According to a third aspect, the invention provides a use of the shaped titanium dioxide prepared by the preparation method according to the second aspect as a carrier in a catalyst.
According to some embodiments of the invention, the catalyst is a selective catalytic reduction catalyst.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the invention, sesbania powder is used as an auxiliary agent, a lubricant and a binder, and polycarboxylic acid can be used as a mixing auxiliary agent together with sesbania powder, so that the performance of the product is improved.
(2) The method has simple process, reduces the addition of the auxiliary agent types compared with the prior art, reduces the production cost under the condition of keeping the same effect, simultaneously optimizes the preparation process, and has certain industrial application value.
(3) The active components and the forming auxiliary agents selected in the method are low-toxicity and environment-friendly products, and have low cost and good economic and environmental benefits.
(4) The titanium dioxide forming product prepared by the method is expected to be widely applied to the field of low-temperature denitration.
Drawings
Fig. 1 is a process flow for preparing a titanium dioxide molding according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail below by way of examples.
The test methods referred to in the following examples are as follows:
1. determination of crush Strength: and (3) carrying out crushing strength test on 100 strip-shaped carrier particles by using a particle strength tester, and averaging after removing extreme values to obtain the crushing strength of the particles.
2. Determination of specific surface area: the adsorption isotherm full analysis was performed on a full-automatic adsorption analyzer, ASAP2020, MICROMERITICS instruments, usa, and the specific surface area was calculated from the isotherm.
Example 1
A titanium dioxide carrier extrusion molding process comprises the following steps:
the method comprises the following steps: carrying out dry mixing on 30g of nano titanium dioxide powder, 3g of sesbania powder, 0.5g of oxalic acid and 1g of citric acid to obtain white mixed powder;
step two: adding 10g of distilled water into the mixed powder obtained in the step one, stirring to obtain a wet mass, and kneading for 0.5h in a double-screw extruder;
step three: and (3) extruding and molding the wet material mass by using a double-screw extruder to obtain the strip-shaped carrier. Drying the obtained strip-shaped carrier at 110 ℃ for 12h, heating to 200 ℃ at the heating rate of 5 ℃/min in a muffle furnace, calcining for 2h, heating to 550 ℃ at the heating rate of 5 ℃/min, and calcining for 5h to obtain a strip-shaped carrier finished product.
Example 2
The same as in example 1, except that the amount of distilled water added in step two was 15 g.
Example 3
The same as in example 1 except that the amount of distilled water added in step two was 17 g.
Example 4
The same as in example 1, except that the amount of distilled water added in step two was 20 g.
Example 5
The same as in example 1, except that the amount of distilled water added in step two was 25 g.
Example 6
A titanium dioxide carrier extrusion molding process comprises the following steps:
the method comprises the following steps: dry-mixing 40g of nano titanium dioxide powder, 4g of sesbania powder, 0.67g of oxalic acid and 1.3g of citric acid to obtain white mixed powder;
step two: adding 20g of distilled water into the mixed powder obtained in the step one, stirring to obtain a wet mass, and kneading for 0.5h in a double-screw extruder;
step three: and (3) extruding and molding the wet material mass by using a double-screw extruder to obtain the strip-shaped carrier. Drying the obtained strip-shaped carrier at 110 ℃ for 12h, heating to 200 ℃ at the heating rate of 5 ℃/min in a muffle furnace, calcining for 2h, heating to 550 ℃ at the heating rate of 5 ℃/min, and calcining for 5h to obtain a strip-shaped carrier finished product.
Example 7
The same as in example 6, except that the amount of distilled water added in the second step was 21 g.
Example 8
The same as in example 6, except that the amount of distilled water added in the second step was 23 g.
TABLE 1 crush Strength and specific surface area of moldings with different Water-to-powder ratios
| Molded article | Water to powder ratio | Crush strength | Specific surface area |
| Example 1 | 1:3.45 | 5.1 kg/pellet | 88.3m2/g |
| Example 2 | 1:2.30 | 3.3 kg/pellet | 87.9m2/g |
| Example 3 | 1:2.03 | 2.8 kg/pellet | 89.1m2/g |
| Example 4 | 1:1.73 | 2.74 kg/pellet | 89.3m2/g |
| Example 5 | 1:1.38 | 2.6 kg/pellet | 87.6m2/g |
| Example 6 | 1:2.30 | 3.8 kg/pellet | 88.4m2/g |
| Example 7 | 1:2.19 | 3.4 kg/pellet | 87.9m2/g |
| Example 8 | 1:2.00 | 3.1 kg/pellet | 88.5m2/g |
As can be seen from the results shown in Table 1, the titanium dioxide molded product obtained by the preparation method of the present invention has high mechanical strength while ensuring a suitable specific surface area.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A composition for preparing titanium dioxide forming objects comprises nano titanium dioxide powder, sesbania powder and polycarboxylic acid.
2. A method for preparing titanium dioxide forming objects comprises the following steps:
step S1, carrying out dry mixing on the nano titanium dioxide powder, the sesbania powder and the polycarboxylic acid to obtain mixed powder;
step S2, adding water into the mixed powder obtained in the step S1, and stirring and kneading the mixture to obtain wet dough;
and step S3, performing extrusion molding on the wet dough obtained in the step S2, and drying and calcining the wet dough to obtain a titanium dioxide molded product.
3. The composition of claim 1 or the preparation method of claim 2, wherein the nano titanium dioxide powder is 80-90 wt%, the sesbania powder is 8-9 wt%, and the polycarboxylic acid is 1-12 wt%; preferably, the nano titanium dioxide powder is 85-88 wt%, the sesbania powder is 8.5-8.8 wt%, and the polycarboxylic acid is 3.2-6.5 wt%.
4. The composition according to claim 1 or the preparation process according to claim 2 or 3, characterized in that the nano-titania is anatase, rutile or P25 type; and/or the polybasic carboxylic acid is oxalic acid, citric acid or a mixture of the two.
5. The production method according to any one of claims 2 to 4,
the wet mass is kneaded in a twin-screw extruder in step S2, and/or extrusion-molded using a twin-screw extruder in step S3.
6. The production method according to any one of claims 2 to 5, wherein in step S2, the mass ratio of water to the mixed powder is 1: (1-5), preferably 1: (1.5-4), more preferably 1: (2-4).
7. The production method according to any one of claims 2 to 6, wherein in step S2, the kneading time is 0.5 to 1 h.
8. The production method according to any one of claims 2 to 7, wherein in step S3, the drying conditions are: the temperature is 80-120 ℃, and the time is 8-24 h.
9. The method as claimed in any one of claims 2 to 8, wherein in step S3, the calcination is carried out in two stages, the first stage calcination temperature is 200 ℃ and 250 ℃, the temperature rise rate is 2 to 10 ℃/mm, and the time is 1 to 2 h; the second stage calcination temperature is 500-550 ℃, the heating rate is 2-10 ℃/mim, and the time is 4-6 h.
10. Use of the shaped titanium dioxide product prepared by the preparation method according to any one of claims 2 to 9 as a carrier in a catalyst, preferably a selective catalytic reduction catalyst.
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| CN101195087A (en) * | 2007-12-21 | 2008-06-11 | 中国石化扬子石油化工有限公司 | Method for producing titanium dioxide preformed catalyst carrier with titanium dioxide aqua compound |
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2019
- 2019-01-22 CN CN201910058802.0A patent/CN111450812A/en active Pending
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Application publication date: 20200728 |