CN111013660A - graphene-Schiff base nickel combustion catalyst and preparation method thereof - Google Patents
graphene-Schiff base nickel combustion catalyst and preparation method thereof Download PDFInfo
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- CN111013660A CN111013660A CN201911215567.XA CN201911215567A CN111013660A CN 111013660 A CN111013660 A CN 111013660A CN 201911215567 A CN201911215567 A CN 201911215567A CN 111013660 A CN111013660 A CN 111013660A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000002262 Schiff base Substances 0.000 title claims abstract description 57
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 44
- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003446 ligand Substances 0.000 claims abstract description 16
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003380 propellant Substances 0.000 abstract description 11
- 239000002585 base Substances 0.000 abstract description 6
- 239000004449 solid propellant Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 2
- 239000007822 coupling agent Substances 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 description 11
- 150000004753 Schiff bases Chemical class 0.000 description 6
- 239000013543 active substance Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 235000015842 Hesperis Nutrition 0.000 description 1
- 235000012633 Iberis amara Nutrition 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1608—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes the ligands containing silicon
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/04—Nickel compounds
- C07F15/045—Nickel compounds without a metal-carbon linkage
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02K—JET-PROPULSION PLANTS
- F02K9/00—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof
- F02K9/08—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof using solid propellants
- F02K9/28—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof using solid propellants having two or more propellant charges with the propulsion gases exhausting through a common nozzle
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23R—GENERATING COMBUSTION PRODUCTS OF HIGH PRESSURE OR HIGH VELOCITY, e.g. GAS-TURBINE COMBUSTION CHAMBERS
- F23R5/00—Continuous combustion chambers using solid or pulverulent fuel
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/847—Nickel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a graphene-Schiff base nickel combustion catalyst, and the structural formula of the catalyst is shown as I. The synthesis process comprises the following steps: (1) modifying graphene oxide by using a coupling agent to obtain surface-modified graphene oxide; (2) reacting the surface-modified graphene oxide with salicylaldehyde to synthesize a graphene-Schiff base ligand; (3) and reacting the graphene-Schiff base ligand with nickel nitrate to prepare the graphene-Schiff base nickel complex. The graphene-Schiff base nickel complex synthesized by the method can obviously improve the burning rate of the modified double-base propellant containing HMX, and is an efficient combustion catalyst of a solid propellant.
Description
Technical Field
The invention relates to a graphene-Schiff base nickel combustion catalyst and a preparation method thereof, and the synthesized graphene-Schiff base nickel can effectively adjust the combustion speed and the pressure index of a modified double-base solid propellant containing HMX and can be used as a combustion catalyst of the modified double-base propellant.
Background
The solid propellant has wide application in tactical missiles and rockets, and the comprehensive performance of the solid propellant is directly related to the accurate striking, high-energy damage and survival capability of modern weapon equipment systems. The energy characteristics of the propellant can be effectively improved by adding HMX, RDX and CL-20, but the burning rate of the propellant is reduced, and the addition of the lead-copper-nickel compound catalytic system is beneficial to the improvement of the burning rate of the propellant in a certain range, but the requirements of modern weapons and equipment systems on high burning rate, low pressure index and wide platform are still difficult to meet.
The Schiff base nickel complex is added on the basis of a lead-copper-nickel compound catalytic system, which is proved to have excellent catalytic action on the burning rate of the solid propellant, but the pressure index of the propellant is increased after the Schiff base nickel complex is added. The synthesis of the graphene-Schiff base nickel complex can combine the catalytic performance of catalytic active substances Schiff base nickel and graphene on a molecular level, the graphene can effectively promote the dispersion of the catalytic active substances nickel and nickel oxide, more catalytic active sites are provided, and the excellent lubricating, heat conducting and mechanical properties of the graphene are beneficial to the improvement of the comprehensive performance of the modified double-base propellant.
In view of the above, the preparation of the graphene-Schiff base nickel complex is designed and synthesized, the excellent catalytic performance of the graphene and the Schiff base nickel is combined, the variety of the combustion catalyst is expanded, and the requirements of modern weaponry systems on high combustion speed, low pressure index and wide platform are met.
Disclosure of Invention
In order to meet the requirements of modern weaponry systems on high burning rate, low pressure index and wide platform, the invention provides a graphene-Schiff base nickel combustion catalyst and a synthesis method thereof.
The structural formula of the graphene-Schiff base nickel combustion catalyst is shown as I:
the synthesis route of the graphene-Schiff base nickel combustion catalyst comprises the following steps:
in order to achieve the purpose, the synthesis method of the graphene-Schiff base nickel combustion catalyst provided by the invention comprises the following steps:
(1) synthesizing surface modified graphene oxide:
and (3) placing the dispersed graphene oxide ethanol dispersion liquid into a three-neck flask, dropwise adding a proper amount of gamma-mercaptopropyl trimethoxy silane KH590 ethanol solution, reacting for 2-4 h under a reflux condition, cooling to room temperature after the reaction is finished, centrifuging, collecting, and washing with ethanol to obtain the surface modified graphene oxide. Wherein the mass ratio of the KH590 to the graphene oxide is 10-15: 1.
(2) Synthesizing a graphene-Schiff base ligand:
and (2) placing the surface modified graphene oxide ethanol dispersion liquid synthesized in the step (1) into a three-neck flask, dropwise adding a proper amount of salicylaldehyde ethanol solution, reacting for 2-6 hours under a reflux condition, cooling to room temperature after the reaction is finished, centrifuging, collecting, and washing with ethanol to obtain the graphene-Schiff base ligand. Wherein the mass ratio of the salicylaldehyde to the surface-modified graphene oxide is 5-15: 1.
(3) Synthesis of graphene-Schiff base nickel combustion catalyst
And (3) dispersing the graphene-Schiff base ligand synthesized in the step (2) in ethanol, mixing with the prepared nickel nitrate aqueous solution, reacting at 50-70 ℃ for 6-12 h, cooling to room temperature after the reaction is finished, centrifugally collecting, and washing with ethanol to obtain the graphene-Schiff base nickel combustion catalyst. Wherein the mass ratio of the graphene-Schiff base ligand to the nickel nitrate is 0.1-1: 1, and the volume ratio of the ethanol to the water is 2-5: 1.
The invention has the advantages and positive effects that:
the graphene-Schiff base nickel complex realizes the assembly of catalytic active substances, namely Schiff base ligands, active metal nickel and two-dimensional structure graphene on a molecular level, when the synthesized graphene-Schiff base nickel complex is used as a combustion catalyst, uniform and nascent nickel oxide is generated by decomposition and is used as a main catalytic active component, and a large amount of carbon substances are generated and are used as auxiliary catalytic components, so that the catalytic combustion effect can be further improved.
Drawings
Fig. 1 SEM spectra of graphene-schiff base nickel combustion catalysts.
Figure 2 FTIR spectrum of graphene-schiff base nickel combustion catalyst.
Fig. 3 is a graph of burning rate versus pressure for a modified biradical propellant after addition of a graphene-schiff base nickel combustion catalyst of the present invention.
Detailed Description
The morphology is characterized by a Quanta600 scanning electron microscope of Quantachrome company in the United states, and an infrared spectrum is characterized by a Tensor 27 Fourier transform infrared spectrometer of Bruker company in Germany.
Synthesis of graphene-Schiff base nickel combustion catalyst
(1) Synthesizing surface modified graphene oxide:
and (3) placing the dispersed graphene oxide ethanol dispersion liquid into a three-neck flask, dropwise adding a proper amount of gamma-mercaptopropyl trimethoxy silane KH590 ethanol solution, reacting for 2 hours under a reflux condition, cooling to room temperature after the reaction is finished, centrifugally collecting, and washing with ethanol to obtain the surface modified graphene oxide. Wherein the mass ratio of the KH590 to the graphene oxide is 15.
(2) Synthesizing a graphene-Schiff base ligand:
and (2) placing the surface modified graphene oxide ethanol dispersion liquid synthesized in the step (1) into a three-neck flask, dropwise adding a proper amount of salicylaldehyde ethanol solution, reacting for 2-6 hours under a reflux condition, cooling to room temperature after the reaction is finished, centrifuging, collecting, and washing with ethanol to obtain the graphene-Schiff base ligand. Wherein the mass ratio of the salicylaldehyde to the surface-modified graphene oxide is 5-15: 1.
(3) Synthesis of graphene-Schiff base nickel combustion catalyst
And (3) dispersing the graphene-Schiff base ligand synthesized in the step (2) in ethanol, mixing with a prepared nickel nitrate aqueous solution, reacting at 65 ℃ for 6 hours, cooling to room temperature after the reaction is finished, centrifugally collecting, and washing with ethanol to obtain the graphene-Schiff base nickel combustion catalyst. Wherein the mass ratio of the graphene-Schiff base ligand to the nickel nitrate is 0.2, and the volume ratio of the ethanol to the water is 5.
Characterization of graphene-schiff base nickel combustion catalyst
(1) Scanning electron microscope:
the scanning electron microscope image of the graphene-schiff base nickel combustion catalyst is shown in fig. 1, the graphene-schiff base nickel keeps a better few-layer structure of graphene, schiff base ligands are combined on the surface of the graphene-schiff base nickel combustion catalyst, and the coordinated metal nickel serving as an active site has better dispersibility.
(2) Infrared spectrum:
IR (ATR, cm) as shown in FIG. 2-1):3244,1628,1047,910,761,692.
Application of graphene-Schiff base nickel combustion catalyst
The basic formulation of the modified biradical propellant sample used in the experiment was: 63.4% of double-base adhesive (NC + NG), 26% of HMX and 10.6% of functional auxiliary agent. The medicine materials are prepared according to 500 g. The catalyst is added, the Pb-Cu-C compound catalyst is 3.9 percent, the graphene-Schiff base nickel combustion catalyst is 0.5 percent, and the control group is a formula containing 3.9 percent of the Pb-Cu-C catalyst.
The solid propellant sample is prepared by adopting a conventional solvent-free extrusion molding process of absorbing, driving water, cooking and cutting into medicine strips. The burning rate of the sample was measured by the target line method. Coating the side surface of the treated small grain of phi 5mm multiplied by 150mm with polyvinyl alcohol solution for 6 times, drying, and then carrying out burning rate test in a nitrogen-filled slow-acting burning rate instrument. The experimental temperature is 20 ℃, and the pressure intensity is 2-20 MPa.
The burning rate and pressure index of the graphene-schiff base-containing nickel combustion catalyst are shown in table 1 and fig. 3. Wherein u is the burning rate, p is the pressure, a is the formula of a Pb-Cu-C catalyst containing 3.9 percent, and b is the formula of a modified bi-based propellant added with 0.5 percent of graphene-Schiff base nickel combustion catalyst on the basis of a. The prepared graphene-Schiff base nickel has a remarkable improvement effect on the burning rate of the modified double-base propellant, and has a good reduction effect on the pressure index, and n is 0.21 within the pressure intensity range of 10-20 MPa.
TABLE 1 burning rate and pressure index for graphene-Schiff base-containing nickel combustion catalysts
Claims (2)
1. A graphene-Schiff base nickel combustion catalyst is characterized in that the structural formula is shown as I:
2. the method for preparing a graphene-schiff base nickel combustion catalyst according to claim 1, comprising the steps of:
(1) synthesizing surface modified graphene oxide:
placing the dispersed graphene oxide ethanol dispersion liquid into a three-neck flask, dropwise adding a proper amount of gamma-mercaptopropyl trimethoxy silane KH590 ethanol solution, reacting for 2-4 h under a reflux condition, cooling to room temperature after the reaction is finished, centrifugally collecting, and washing with ethanol to obtain surface-modified graphene oxide; wherein the mass ratio of the KH590 to the graphene oxide is 10-15: 1;
(2) synthesizing a graphene-Schiff base ligand:
placing the surface modified graphene oxide ethanol dispersion liquid synthesized in the step (1) into a three-neck flask, dropwise adding a proper amount of salicylaldehyde ethanol solution, reacting for 2-6 hours under a reflux condition, cooling to room temperature after the reaction is finished, centrifugally collecting, and washing with ethanol to obtain a graphene-Schiff base ligand; wherein the mass ratio of the salicylaldehyde to the surface-modified graphene oxide is 5-15: 1;
(3) synthesis of graphene-Schiff base nickel combustion catalyst
Dispersing the graphene-Schiff base ligand synthesized in the step (2) in ethanol, mixing with a prepared nickel nitrate aqueous solution, reacting at 50-70 ℃ for 6-12 h, cooling to room temperature after the reaction is finished, centrifugally collecting, and washing with ethanol to obtain a graphene-Schiff base nickel combustion catalyst; wherein the mass ratio of the graphene-Schiff base ligand to the nickel nitrate is 0.1-1: 1, and the volume ratio of the ethanol to the water is 2-5: 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010885A (en) * | 2020-08-28 | 2020-12-01 | 西安近代化学研究所 | Preparation method of 3-mercaptopropyltriethoxysilane-modified graphene oxide/nitrocotton compound |
| CN112169723A (en) * | 2020-09-03 | 2021-01-05 | 中国航天空气动力技术研究院 | Method for preparing high-temperature high-pressure gas and application |
| CN112919997A (en) * | 2021-02-05 | 2021-06-08 | 西安近代化学研究所 | graphene-Schiff base energetic MOFs and preparation method thereof |
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| CN112169723B (en) * | 2020-09-03 | 2022-05-24 | 中国航天空气动力技术研究院 | Method for preparing high-temperature high-pressure gas and application |
| CN112919997A (en) * | 2021-02-05 | 2021-06-08 | 西安近代化学研究所 | graphene-Schiff base energetic MOFs and preparation method thereof |
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Application publication date: 20200417 |