CN109529871B - Sea urchin-shaped copper-based catalyst and preparation method and application thereof - Google Patents
Sea urchin-shaped copper-based catalyst and preparation method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- 239000010949 copper Substances 0.000 title claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 40
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000002485 combustion reaction Methods 0.000 claims abstract description 11
- 241000257465 Echinoidea Species 0.000 claims abstract description 8
- 239000007800 oxidant agent Substances 0.000 claims abstract description 7
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000011572 manganese Substances 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 13
- 229910052748 manganese Inorganic materials 0.000 claims description 11
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- HPDFFVBPXCTEDN-UHFFFAOYSA-N copper manganese Chemical compound [Mn].[Cu] HPDFFVBPXCTEDN-UHFFFAOYSA-N 0.000 claims description 8
- 238000010335 hydrothermal treatment Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000012495 reaction gas Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000012691 Cu precursor Substances 0.000 claims description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- 230000002950 deficient Effects 0.000 claims description 5
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical group [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical group [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 238000007084 catalytic combustion reaction Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 206010021143 Hypoxia Diseases 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000005173 quadrupole mass spectroscopy Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- B01J35/51—
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C01B32/50—Carbon dioxide
Abstract
The invention belongs to the technical field of metal oxide materials, and particularly discloses a sea urchin-shaped copper-based catalyst which is of a spherical sea urchin structure, wherein a plurality of outwards-radiating columnar bodies are formed on spherical sea urchins. The invention also discloses a preparation method of the sea urchin-shaped copper-based catalyst. The invention also provides the application of the sea urchin-shaped copper-based catalyst in the preparation of O2As an oxidant, to catalyze the complete combustion of CO. The preparation method is simple, the prepared catalyst has unique shape, and CO is oxidized into CO at 30-40 DEG C2。
Description
Technical Field
The invention belongs to the technical field of metal oxide materials, and particularly discloses a sea urchin-shaped copper-based catalyst and a preparation method and application thereof.
Background
For hydrogen-fueled fuel cells, the hydrogen produced from lower alcohols and hydrocarbons often contains about 5X 105-2×106ppm (0.5-2%) of CO, which not only causes electrode poisoning of the fuel cell, but also competes with hydrogen to affect the reaction between hydrogen and oxygen, and finally results in a great reduction in the performance of the fuel cell, needs to be eliminated. Among various methods for eliminating CO, the elimination of CO by catalytic combustion is a simple, inexpensive, and easy-to-implement method.
Catalytic combustion is a technique of performing flameless combustion at a low light-off temperature with the aid of a catalyst and oxidatively decomposing an organic exhaust gas into carbon dioxide and water. The essence of catalytic combustion is a vigorous oxidation reaction involving active oxygen, the catalytically active component activates air oxygen, and when in contact with reactant molecules, energy transfer occurs, and the reactant molecules are activated, thereby accelerating the oxidation reaction. Catalytic combustion has incomparable advantages compared with general flame combustion, so that the application of catalytic combustion in the aspect of CO elimination is generally concerned.
Disclosure of Invention
The invention aims to provide a copper-based catalyst with a sea urchin-shaped structure and a preparation method thereof, and the copper-based catalyst is prepared by adding O2The catalyst is used for catalyzing the complete combustion of CO.
In order to achieve the purpose, the basic scheme of the invention is as follows:
a copper-based catalyst in the form of sea urchin is in the form of spherical sea urchin with multiple columns radiating outwards.
The invention also provides a preparation method of the sea urchin-shaped copper-based catalyst, which comprises the following steps:
(1) mixing the copper precursor solution and the manganese precursor solution to obtain a copper-manganese mixed solution;
(2) adding water, cetyl trimethyl ammonium bromide and absolute ethyl alcohol into the copper-manganese mixed solution, and stirring at room temperature at the stirring speed of 80-100 r/min;
(3) slowly dropwise adding ammonia water into the reaction mixed liquid obtained in the step (2), and stirring at room temperature at the stirring speed of 250-350 r/min;
(4) carrying out hydrothermal treatment on the reaction mixed solution obtained in the step (3);
(5) and (4) filtering the reaction mixed solution obtained in the step (4) to obtain a filtrate, and washing, drying and calcining the filtrate to obtain the sea urchin-shaped copper-based catalyst.
The principle and the beneficial effects of the sea urchin-shaped copper-based catalyst and the preparation method thereof are as follows:
the sea urchin-shaped catalyst can catalyze CO to be completely combusted at a lower temperature.
The room temperature referred to herein means 25 ℃ as is well known to those skilled in the art.
The preparation method takes cetyl trimethyl ammonium bromide as a structure directing agent, water, absolute ethyl alcohol and ammonia water as auxiliary agents, and prepares the copper-based catalyst with sea urchin-shaped structural characteristics by using a hydrothermal synthesis method.
The preparation method is only required to be carried out under the stirring conditions that the stirring speed is 80-100r/min and 250-350r/min respectively, and can be achieved by a magnetic stirrer which is common in laboratories.
The invention also provides the application of the echinoid copper-based catalyst for catalyzing O under the condition of oxygen deficiency2For complete combustion of CO as oxidant, the reaction gas in oxygen-deficient condition comprises 0.5-5% CO and 0.5-5% O2And argon gas. The sea urchin-shaped copper-based catalyst is very suitable for eliminating CO under the condition of oxygen deficiency.
Furthermore, the cross section of the columnar body is in a diamond shape, the length of the columnar body is more than 1 mu m, and the contact area between the catalyst and CO can be effectively increased, so that the catalyst can catalyze the complete combustion of CO at a lower temperature.
Further, the copper precursor is copper nitrate and the manganese precursor is manganese nitrate. NO in copper and manganese precursors3 -Can be removed by burning and heating, and can prevent the oxide from remaining on the surface of the oxide and influencing the catalytic performance of the oxide.
Further, the molar ratio of copper to manganese in the sea urchin-shaped copper-based catalyst is 0.5-1.65: 1. Under the above-mentioned conditions of the molar ratio of copper to manganese, the sea urchin-like structure of the catalyst obtained is preferred.
Further, for catalyzing with O under oxygen-deficient conditions2For complete combustion of CO as oxidant, the reaction gas in oxygen-deficient condition comprises 0.5-5% CO and 0.5-5% O2And argon, the sea urchin-like copper-based catalyst is very suitable for eliminating CO under the condition of oxygen deficiency.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a sea urchin-like copper-based catalyst obtained in example 1;
FIG. 2 shows the results obtained in example 1Catalysis of spherical sea urchin-shaped copper-based catalyst with O2The performance of the oxidant for complete combustion of CO;
FIG. 3 is an X-ray diffraction pattern of the catalysts prepared in example 1 and comparative examples 1 to 4.
Detailed Description
The following is a more detailed description of the present invention by way of specific embodiments. Cu (NO) mentioned in the following examples and comparative examples3)2、50％Mn(NO3)2The aqueous solution, CTAB, ammonia water, and absolute ethanol were purchased from shanghai tyntake technologies, inc, and used as received without further treatment before use. Reaction gas [ CO (0.5-5%) + O ] subjected to CO catalytic elimination reaction test2(0.5-5％)+Ar(90-99％)]Purchase of Chongqing Chaoyang gas from high purity O2High-purity Ar and high-purity CO. The element ratio (Cu: Mn) contained in the obtained catalyst was measured by the ICP method
Example 1
(1) Weighing 19.9gCu (NO)3)2And 5.9g 50% Mn (NO)3)2The aqueous solutions were mixed, and then 7.5ml of distilled water was added to the mixture and stirred until Cu (NO) was obtained3)2And completely dissolving to obtain copper-manganese mixed liquor.
(2) Adding 112.5gH into the copper-manganese mixed solution2O, 5.6g CTAB and 135.1g of absolute ethyl alcohol, and stirring at room temperature for 15 minutes (the stirring speed is 80-100 r/min).
(3) And (3) slowly dropwise adding 29.7g of ammonia water into the reaction mixed solution obtained in the step (2), and stirring the mixed solution at room temperature (250-.
(4) And (4) transferring the reaction mixed liquid obtained in the step (3) to a hydrothermal synthesis kettle for hydrothermal treatment, and carrying out hydrothermal treatment at 120 ℃ for 24 hours.
(5) After the hydrothermal treatment is finished, obtaining a solid by suction filtration, washing the solid by distilled water fully, drying the filtered solid in a rotary evaporator at 60 ℃, finally putting the dried solid in a muffle furnace, and calcining the dried solid for 4 hours at 550 ℃ in an air atmosphere to obtain the sea urchin-shaped copper-based catalyst.
80mg of the catalyst is filled into a quartz reaction tube of a fixed bed catalytic reaction furnace, and reaction gas with the mixture ratio of CO (0.5-5%) + O2 (0.5-5%) + Ar (90-99%) is introduced to test the performance of the catalyst in catalyzing the complete combustion of CO. The flow rate of the reaction gas is controlled at 25ml/min by using a mass flow meter, the temperature of the reaction tube is controlled by a temperature controller, and the heating rate is 10 ℃/min. Monitoring of the CO content in the reaction gas, the content of CO2 produced, was carried out using QIC-20 quadrupole mass spectrometry, produced by Hiden Analytical Ltd.
FIG. 1 is a Scanning Electron Microscope (SEM) image of a spherical sea urchin-like copper-based catalyst obtained in example 1. As can be seen from FIG. 1, the catalyst has a spherical sea urchin-like structure which is formed by columns with the length of more than 1 μm, wherein the columns are diverged outwards from the center, and the cross section of each column is in a diamond shape.
FIG. 2 shows that the spherical sea urchin-like copper-based catalyst obtained in example 1 is catalyzed by O2Is the performance of the oxidant for complete combustion of CO. It can be seen that CO starts to oxidize CO to CO at 34 deg.C 250% of the CO is oxidized to CO at 108 DEG C2Complete oxidation of CO to CO at 175 deg.C2。
Examples 2 to 5 and comparative examples 1 to 4
Examples 2 to 5, comparative examples 1 to 4 differ from example 1 only in that the amounts of copper nitrate and manganese nitrate added in step (1) were different, resulting in different contents of Cu and Mn in the finally obtained catalyst, see table 1 below.
TABLE 1
And (4) conclusion:
(1) referring to comparative examples 1-4, when the molar ratio of copper nitrate to manganese nitrate is not in the range of 0.5-1.65:1, the finally prepared copper-based catalyst is not echinoid, and the initial CO oxidation temperature is 43-51 ℃, the 50% CO removal temperature is 130-142 ℃, and the 100% CO removal temperature is 190-219 ℃, which are all significantly higher than the relevant temperatures of examples 1-5, and in conclusion, we can conclude that the copper-based catalyst has an echinoid structure and is helpful for catalyzing at lower temperatures (30-40 ℃, 100-110 ℃ and 170-180 ℃) by using O2CO, which is an oxidant, is completely combusted.
(2) FIG. 3 is an X-ray diffraction pattern of the catalysts obtained in example 1 and comparative examples 1 to 4. As can be seen from fig. 3, the copper-based catalyst having a sea urchin-like structure prepared in example 1 is significantly different from the XRD patterns of comparative examples 1 to 4. This shows that the catalyst with a sea urchin-like structure Cu: Mn of 1.65:1 obtained in example 1 has a significantly different crystal phase structure from the catalysts obtained in comparative examples 1 to 4.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.
Claims (6)
1. A sea urchin-shaped copper-based catalyst is characterized in that the catalyst is of a spherical sea urchin structure, and a plurality of outwards-divergent columnar bodies are formed on the spherical sea urchin;
the catalyst is prepared by the following method:
(1) mixing the copper precursor solution and the manganese precursor solution to obtain a copper-manganese mixed solution;
(2) adding water, cetyl trimethyl ammonium bromide and absolute ethyl alcohol into the copper-manganese mixed solution, and stirring at room temperature at the stirring speed of 80-100 r/min;
(3) slowly dripping ammonia water into the reaction mixed liquid obtained in the step (2) until the ammonia water is excessive, and stirring at room temperature at the stirring speed of 250-350 r/min;
(4) carrying out hydrothermal treatment on the reaction mixed liquid obtained in the step (3); the temperature of the hydrothermal treatment is 120 ℃;
(5) filtering the reaction mixed solution obtained in the step (4) to obtain a filtrate, and washing, drying and calcining the filtrate to obtain the sea urchin-shaped copper-based catalyst; in the sea urchin-shaped copper-based catalyst, the molar ratio of copper to manganese is 0.5-1.65: 1.
2. A sea urchin-like copper-based catalyst according to claim 1, wherein the cross-section of the pillars is diamond-shaped, and the length of the pillars is > 1 μm.
3. The method for preparing a echinoid copper-based catalyst according to claim 1 or 2, characterized by comprising the steps of:
(1) mixing the copper precursor solution and the manganese precursor solution to obtain a copper-manganese mixed solution;
(2) adding water, cetyl trimethyl ammonium bromide and absolute ethyl alcohol into the copper-manganese mixed solution, and stirring at room temperature at the stirring speed of 80-100 r/min;
(3) slowly dripping ammonia water into the reaction mixed liquid obtained in the step (2) until the ammonia water is excessive, and stirring at room temperature at the stirring speed of 250-350 r/min;
(4) carrying out hydrothermal treatment on the reaction mixed liquid obtained in the step (3); the temperature of the hydrothermal treatment is 120 ℃;
(5) filtering the reaction mixed solution obtained in the step (4) to obtain a filtrate, and washing, drying and calcining the filtrate to obtain the sea urchin-shaped copper-based catalyst; in the sea urchin-shaped copper-based catalyst, the molar ratio of copper to manganese is 0.5-1.65: 1.
4. The method of claim 3, wherein the copper precursor is copper nitrate and the manganese precursor is manganese nitrate.
5. The use of a copper-based catalyst in the form of sea urchin according to claim 1, wherein O is used2As a catalyst, CO is oxidized to CO at 30-40 deg.C2Oxidizing 50% of CO into CO at 110 ℃ of 100-2Oxidizing all CO to CO at 170-180 DEG C2。
6. Use of a copper-based catalyst in the form of sea urchin according to claim 1 for catalyzing O under oxygen-deficient conditions2For complete combustion of CO as oxidant, the reaction gas in oxygen-deficient condition comprises 0.5-5% CO and 0.5-5% O2And argon gas.
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| Low-temperature CO oxidation over integrated;Shengpeng Mo et al.;《Catalysis Science & Technology》;The Royal Society of Chemistry;20180213(第8期);第1663-1676页 * |
| 铜锰氧化物制备改性及其CO催化氧化性能研究;蔡丽娜;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20150715(第7期);第B014-128页 * |
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