CN112275285B - Promote CO 2 Catalyst for generating CO by hydrogenation and preparation method thereof - Google Patents
Promote CO 2 Catalyst for generating CO by hydrogenation and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 47
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 5
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 230000001737 promoting effect Effects 0.000 abstract description 11
- 239000002082 metal nanoparticle Substances 0.000 abstract description 10
- 239000013067 intermediate product Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 238000003795 desorption Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 150000002500 ions Chemical class 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000006004 Quartz sand Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- 229920002994 synthetic fiber Polymers 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/60—Platinum group metals with zinc, cadmium or mercury
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention relates to CO 2 The technical field of hydrogenation, in particular to a method for promoting CO 2 Catalyst for hydrogenation to produce CO and its useA preparation method and application. The catalyst is Cd 2+ Ion-modified supported catalyst Pt/TiO 2 (Pt/Cd‑TiO 2 ). The preparation method comprises the following steps: adding TiO into the mixture 2 Dispersing in deionized water, adding H 2 PtCl 6 Solution, cd (NO) 3 ) 2 .4H 2 Stirring and evaporating to dryness to obtain gray powder; the grey powder obtained is reacted with hydrogen 2 Reducing the catalyst in the atmosphere at the temperature of 300-400 ℃ to obtain the catalyst Pt/Cd-TiO 2 . By the reaction of Pt/TiO 2 Performing Cd 2+ Ion modification is carried out, the electron density of the surface of the Pt metal nano particle is reduced, and the CO is inhibited 2 The adsorption of the hydrogenation intermediate product CO (abs) promotes the desorption of CO (abs) to generate CO gas, thereby improving the CO gas 2 Selectivity of hydrogenation product CO.
Description
Technical Field
The invention relates to CO 2 The technical field of hydrogenation, in particular to a method for promoting CO 2 A catalyst for generating CO by hydrogenation and a preparation method thereof.
Background
Large amount of CO 2 And when the gas is generated, a series of environmental problems such as global gas temperature rise are caused. Wherein CO is passed through 2 The hydrogenation reaction can lead CO to 2 Conversion to CO, CH 4 、CH 3 A series of energy substances such as OH and the like, which can not only reduce CO in the atmosphere 2 The concentration of the (D) can be converted into a novel energy substance, and the (D) has important significance in relieving energy crisis and protecting environment.
Pt/TiO 2 Is catalyzing CO 2 One of the commonly used catalysts in hydrogenation reactions has been extensively studied due to its high conversion efficiency. With Pt/TiO 2 CO for catalyst 2 Hydrogenation reactions, the hydrogenation products of which are predominantly CH 4 And CO. Since CO is an important raw material in the chemical synthesis process, the improvement of the selectivity of CO in the product is of great significance, and researchers have improved the CO in the product through various waysAnd (4) selectivity.
Das et al enhanced the reducibility of the catalyst by incorporating Fe into the catalyst to promote CO formation and to increase CO selectivity in the product. Wang et al by regulating H in gas mixture 2 Inhibit further hydrogenation of the intermediate product CO (abs) to CH 4 Thereby improving the selectivity of CO in the product. However, the methods have the defects of complex synthetic process, poor catalyst stability and the like, and the wide application of the methods is greatly limited.
In CO 2 In the hydrogenated product, CO (abs) is CH 4 Are important intermediates in the synthesis of (A). However, the Pt metal nanoparticles have strong adsorption to CO (abs), so that the CO (abs) can be further subjected to hydrogenation reaction to generate CH 4 Resulting in lower selectivity of CO in the product.
Disclosure of Invention
Technical problem to be solved
In view of the above-mentioned disadvantages and drawbacks of the prior art, the present invention provides a method for promoting CO 2 Catalyst for the hydrogenation to CO by means of a Pt/TiO catalyst 2 Performing Cd 2+ Ion modification, reduction of electron density on the surface of Pt metal nanoparticles, and inhibition of Pt on CO 2 And (3) adsorbing CO serving as an intermediate product of hydrogenation, thereby promoting the generation of CO.
Correspondingly, the invention also provides the promotion of CO 2 A preparation method of a catalyst for generating CO by hydrogenation.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the present invention provides a method for promoting CO 2 Catalyst for hydrogenation to CO, which is Cd 2+ Ion modified supported catalyst Pt/TiO 2 。
In a second aspect, the present invention provides a method for selectively promoting CO 2 A method for preparing a catalyst for the hydrogenation to CO comprising the steps of:
s1 reacting TiO with 2 Dispersing in deionized water, adding H 2 PtCl 6 Solution, cd (NO) 3 ) 2 .4H 2 Stirring and evaporating to dryness to obtain gray powder;
s2, adding the obtained gray powder to H 2 Reducing the catalyst in the atmosphere at the temperature of 300-400 ℃ to obtain the catalyst Pt/Cd-TiO 2 。
Optionally, it further comprises the steps of:
TiO 2 the preparation of (1): dissolving tetrabutyl titanate in an ethanol solution, stirring for 30min, dropwise adding into deionized water, continuously stirring until the solution is evaporated, and calcining the obtained white powder to obtain TiO 2 。
Optionally, the temperature of calcination is 400 to 500 ℃.
In a third aspect, the present invention provides a method for selectively promoting CO 2 Use of a catalyst for the production of CO by hydrogenation in the catalytic production of CO, comprising the steps of:
the obtained catalyst Pt/Cd-TiO 2 Fully mixing with quartz sand, filling into a reaction device, and adding CO 2 /H 2 the/Ar (3/12/85) mixed gas is filled into the reaction system to react for 4 to 6 hours at the temperature of between 300 and 400 ℃, and then the reaction is finished.
(III) advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
the invention selectively promotes CO 2 Catalyst for the hydrogenation to CO by means of a Pt/TiO catalyst 2 Performing Cd 2+ Ion modification is carried out, the electron density of the surface of the Pt metal nano particle is reduced, and the CO is inhibited 2 The adsorption of the intermediate product CO (abs) is hydrogenated, thereby promoting the desorption of CO (abs) to generate CO gas and improving the selectivity of CO in the product;
wherein Cd 2+ The ion is a cation with stronger positive electricity and has more stable chemical property. In Pt/TiO 2 In the synthesis process of (2), positive Cd 2+ The ion being capable of reacting with PtCl 6 2- Combined in PtCl 6 2- After being reduced into Pt metal simple substance, cd 2+ The ions will still be adsorbed on the surface of the Pt metal nanoparticles. Due to Cd 2+ Electropositivity of ions, which strongly adsorb Pt metal nanoparticlesElectrons on the surface of the particles, thereby making the Pt metal nanoparticles to CO (abs) Adsorption strength of (2) is reduced, CO (abs) The CO gas is easier to be desorbed and generated, thereby achieving the purpose of improving the CO selectivity in the product.
3. The invention selectively promotes CO 2 The preparation method of the catalyst for generating CO by hydrogenation is simple and easy, and the yield of the synthetic material is high, thereby being beneficial to large-scale application of the catalyst in practical production.
Drawings
FIG. 1 shows Pt/TiO 2 ，Pt/Cd-TiO 2 ，Cd-TiO 2 And TiO 2 An XRD pattern of (a);
FIG. 2 shows Pt/TiO 2 ，Pt/Cd-TiO 2 ，TiO 2 And Cd-TiO 2 H of (A) to (B) 2 -a TPR curve;
FIG. 3 shows Pt/TiO 2 And Pt/Cd-TiO 2 Catalyzing CO 2 The activity curve of the hydrogenation reaction.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present invention by way of specific embodiments thereof.
[ MEANS FOR CARRYING OUT THE INVENTION ]
The invention aims to reduce Pt/TiO 2 The electron density on the surface of the Pt metal nano-particles in the catalyst inhibits the adsorption of the Pt metal nano-particles on CO (abs) so as to improve CO 2 The selectivity of CO in the hydrogenation reaction product provides a selectivity promoting CO 2 Catalyst for hydrogenation to CO being Cd 2+ Ion-modified supported catalyst Pt/TiO 2 . Namely: pt/Cd-TiO 2 Catalyst and process for preparing same
It is Pt/TiO 2 Performing Cd 2+ Synthesizing Pt/Cd-TiO by ion modification 2 A catalyst.
Which can effectively improve the selectivity of CO in the product.
[ second embodiment ] to provide a medicine for treating diabetes
The invention provides a method for selectively promoting CO 2 The catalyst for generating CO by hydrogenation has a simple preparation method, and comprises the following steps:
S1mixing TiO with 2 Dispersing in deionized water, adding H 2 PtCl 6 Solution, cd (NO) 3 ) 2 .4H 2 Stirring and evaporating to dryness to obtain gray powder;
s2 the grey powder obtained is purified in H 2 Reducing the mixture in the atmosphere at the temperature of between 300 and 400 ℃ to obtain Pt/Cd-TiO 2 。
In order to improve the catalyst output and reduce the production cost, the invention also provides TiO 2 The preparation method comprises the steps of dissolving tetrabutyl titanate in ethanol solution, stirring for 30min, dropwise adding the solution into deionized water, continuously stirring until the solution is evaporated, and calcining the obtained white powder to obtain TiO 2 。
Preferably, the calcination temperature is 400 to 500 ℃.
[ third embodiment ]
The invention provides a method for selectively promoting CO 2 Catalyst for generating CO by hydrogenation in catalysis of CO 2 Use of hydrogenation to CO, comprising the steps of:
the obtained catalyst Pt/Cd-TiO 2 Fully mixing with quartz sand, filling into a reaction device, and adding CO 2 /H 2 Filling the mixed gas of/Ar (3/12/85) into the reaction system, reacting for 4-6 h at the temperature of 300-400 ℃, and finishing the reaction.
In order to better understand the above technical solutions, exemplary embodiments of the present invention will be described in more detail below. While the following shows exemplary embodiments of the invention, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1: tiO 2 2 Preparation of
15ml of tetrabutyl titanate was dissolved in 50ml of ethanol solution and stirred for 30min. The solution was added dropwise to 100ml of deionized water and the mixture was stirred for 3 hours and then evaporated. Calcining the obtained white powder at 450 ℃ for 3h to obtain TiO 2 。
Example 2: the other points are different from example 1 in that: the temperature of calcination was 400 ℃.
Example 3: the other points are different from example 1 in that: the temperature of calcination was 500 ℃.
Example 4
Pt/Cd-TiO 2 Preparation of
Mixing TiO with 2 (0.5 g) dissolved in 50ml deionized water solution, stirred for 30min by ultrasonic wave, and added with H 2 PtCl 6 Solution (0.67 ml), cd (NO) 3 ) 2 .4H 2 O (2.1 g), stirring for 3 hours and evaporating the solution to dryness to obtain a grey powder in H 2 Reducing for 3h at 350 ℃ in atmosphere to obtain Pt/Cd-TiO 2 。
Example 5: the other points are different from example 4 in that: the temperature of the reduction was 300 ℃.
Example 6: the other points are different from example 4 in that: the temperature of the reduction was 400 ℃.
Example 7
Catalyst Pt/Cd-TiO 2 Filling the mixture into a reaction device, and detecting CO and CH by using Aglient7820 chromatography 4 The yield of (2). The reaction process comprises the steps of adding a catalyst Pt/Cd-TiO 2 (0.2 g) was thoroughly mixed with quartz sand (1.2 g), and the mixture was packed in a reaction apparatus, and CO was added 2 /H 2 Charging the mixed gas of/Ar (3/12/85) into the reaction system, and reacting for 5 hours at the temperature of 350 ℃.
Example 8: the procedure is otherwise the same as in example 7, except that the reaction is terminated after 6 hours at 300 ℃.
Example 9: the reaction was conducted in the same manner as in example 7 except that the reaction was terminated after 4 hours at 390 ℃.
Through test determination:
1. the Pt/Cd-TiO obtained by the invention 2 And Pt/TiO 2 、Cd-TiO 2 、TiO 2 Measuring to obtain an XRD pattern shown in figure 1;
from fig. 1, we obtain: in Cd-TiO 2 And TiO 2 In the XRD pattern of (1), 25.1, 37.8, 47.9, 53.8, 55.0, 62.4, 70.1 and 75.5 DEG peaks correspond to sharp peaksTitanite type TiO 2 The (101), (004), (200), (105), (211), (204), (220) and (301) planes of (A), 30.6, 42.3 and 68.9 DEG peaks correspond to brookite-type TiO 2 The (211), (221), and (112) crystal planes of (a). In Pt/Cd-TiO 2 And Pt/TiO 2 Does not observe diffraction peaks corresponding to Pt species and Cd species in the XRD pattern, which is caused by the high dispersibility of low content of Pt species and Cd species on the surface of the carrier.
2. The Pt/Cd-TiO obtained by the invention 2 ，Pt/TiO 2 ，TiO 2 And Cd-TiO 2 Shown in FIG. 2, as shown in H 2 -TPR curve.
FIG. 2 can obtain Cd-TiO 2 And TiO 2 H of (A) to (B) 2 No H observed in TPR spectra 2 Peak of depletion, demonstrating Cd 2+ Ionic and bulk TiO 2 Are not reduced. Pt/Cd-TiO 2 H of (A) to (B) 2 Reduction peak temperature (118 ℃) of Pt species in TPR spectrum to Pt/TiO ratio 2 The temperature of the reduction peak of the middle Pt species (104 ℃) increased by 14 ℃, indicating Cd 2+ The introduction of ions increases the reduction temperature for the Pt species. H at 250 ℃ 2 Consumption peak corresponding to TiO in contact with Pt 2 Reduced peak of (2).
3. The Pt/Cd-TiO obtained by the invention 2 And Pt/TiO 2 Catalytic CO was carried out according to the method of example 7 2 Hydrogenation reaction, and sampling measurement at intervals of 30min gave the graph shown in FIG. 3.
As can be taken from FIG. 3, in CO 2 In the hydrogenation reaction, cd passes through 2+ The selectivity of CO in the modified product of the ion is improved by 98.1 percent from 87.5 percent. This is mainly due to Cd 2+ The introduction of ions can reduce the electron density on the surface of the Pt metal nano-particles and inhibit the Pt metal nano-particles from reacting on intermediate product CO (abs) The adsorption of (2) promotes the desorption of the CO gas to generate the CO gas, thereby improving the selectivity of CO in the product. Meanwhile, the yield of CO in the product is gradually reduced along with the prolonging of the reaction time, and CH 4 The yield of (2) was gradually increased, which indicates that CO is CO 2 An important intermediate product of the methanation process.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. Promote CO 2 A catalyst for generating CO by hydrogenation is characterized in that: it is Cd 2+ Ion-modified supported catalyst Pt/TiO 2 ；
The preparation method comprises the following steps:
s1 reacting TiO with 2 Dispersing in deionized water, adding H 2 PtCl 6 Solution, cd (NO) 3 ) 2 .4H 2 Stirring and evaporating to dryness to obtain gray powder;
s2, adding the obtained gray powder to H 2 Reducing the catalyst at the temperature of 300-400 ℃ in atmosphere to obtain the catalyst Pt/Cd-TiO 2 。
2. The CO promotion of claim 1 2 A catalyst for generating CO by hydrogenation is characterized in that: dissolving tetrabutyl titanate in an ethanol solution, stirring for 30min, dropwise adding into deionized water, continuously stirring until the solution is evaporated, and calcining the obtained white powder to obtain TiO 2 。
3. The CO promotion of claim 2 2 The catalyst for generating CO by hydrogenation is characterized in that: the calcining temperature is 400-500 ℃.
4. The CO-promoting catalyst of claim 1 2 Use of a catalyst for the hydrogenation to CO for the catalytic generation of CO, comprising the steps of:
the obtained catalyst Pt/Cd-TiO 2 After being fully mixed with quartz sandFilling into a reaction apparatus, and introducing CO 2 /H 2 Filling the/Ar (3/12/85) mixed gas into the reaction system, and reacting for 4 to 6 hours at the temperature of 300 to 400 ℃ to finish the reaction.
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