CN110773229B - Polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2Method for producing particles - Google Patents
Polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2Method for producing particles Download PDFInfo
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- CN110773229B CN110773229B CN201911010375.5A CN201911010375A CN110773229B CN 110773229 B CN110773229 B CN 110773229B CN 201911010375 A CN201911010375 A CN 201911010375A CN 110773229 B CN110773229 B CN 110773229B
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- 239000002245 particle Substances 0.000 title claims abstract description 63
- 229920002125 Sokalan® Polymers 0.000 title claims abstract description 35
- 239000004584 polyacrylic acid Substances 0.000 title claims abstract description 35
- 229910000033 sodium borohydride Inorganic materials 0.000 title claims abstract description 27
- 239000012279 sodium borohydride Substances 0.000 title claims abstract description 27
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical class CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 37
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 20
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 20
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- -1 hydrogen Chemical class 0.000 claims abstract description 13
- 230000007062 hydrolysis Effects 0.000 claims abstract description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 125000003277 amino group Chemical group 0.000 claims abstract description 10
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 10
- 239000007822 coupling agent Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 1
- 150000001298 alcohols Chemical class 0.000 claims 1
- 150000008282 halocarbons Chemical class 0.000 claims 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 8
- 239000012153 distilled water Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 229910000077 silane Inorganic materials 0.000 abstract 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 238000003860 storage Methods 0.000 description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide Substances CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 description 2
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 description 2
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 description 2
- 229910000103 lithium hydride Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012360 testing method Methods 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
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/065—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents from a hydride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the field of composite catalysts, and relates to polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2A method for preparing the particles. The method comprises the following steps: (1) mixing SiO2Dissolving the particles and (amino) alkyl alkoxy silane in an organic solvent, and reacting to obtain SiO with amino on the surface2Particles; (2) SiO with amino group on the surface2Dissolving the particles, polyacrylic acid and coupling agent in distilled water, and reacting to obtain SiO containing polyacrylic acid on the surface2Particles; (3) modifying used polyacrylic acid with SiO2The particles are washed and dried, and then the particles can be activated again. Prepared polyacrylic acid modified SiO2The particles have the characteristics of high catalytic activity, low cost, easy recovery, reusability and the like in the hydrogen production reaction by catalyzing hydrolysis of sodium borohydride.
Description
Technical Field
The invention belongs to the field of composite catalysts, and particularly relates to polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2A method for preparing the particles.
Background
With the rapid development of society, the demand of human beings for energy is increasing. In order to overcome the problems of energy shortage and environmental pollution in the future, the search for renewable green energy is an important subject to be solved worldwide. At present, hydrogen energy is considered to be one of the most ideal clean energy sources in future energy structures, the energy density of hydrogen is high, and combustion products are nontoxic and are environment-friendly energy sources. The hydrogen is widely available, can be obtained by using solar energy hydrogen production and biomass cracking hydrogen production, and is a novel clean gas fuel which can potentially replace the traditional fossil energy. However, in the practical application of hydrogen energy, some technical problems exist, and the problems of convenience of hydrogen production mode, safety of hydrogen storage technology and the like are highlighted. With metal hydrides or borohydrides (e.g. lithium hydride (LiH), sodium aluminum hydride (NaAlH)4) Sodium borohydride (NaBH)4) Etc.), the hydrogen storage mode has the advantages of high hydrogen storage density, relatively high stability and high purity of prepared hydrogen, and the condition for releasing hydrogen is quite mild, so the hydrogen storage mode has good application prospect.
In order to meet the requirement of hydrogen energy, a catalyst for hydrogen production by sodium borohydride hydrolysis has been deeply explored. At present, sodium borohydride hydrolysis hydrogen production catalysts are mainly metal-based catalysts, and few non-metal catalysts are needed to be further developed.
Aiming at the problems, the invention aims to provide polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2The catalyst has the characteristics of high catalytic activity, low cost, easy recovery, reusability and the like.
Disclosure of Invention
The invention aims to provide polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2The preparation method of the particle is that polyacrylic acid is modified on SiO through chemical reaction2On the particles, SiO2The particles have a large number of carboxyl groups, so that the catalyst can effectively promote the hydrolysis of sodium borohydride to prepare hydrogen.
In order to achieve the purpose, the invention provides polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2A method of preparing particles comprising the steps of:
s1 preparation of SiO with amino groups on the surface2Particles
Weighing SiO in proportion2Mixing the particles with (amino) alkylalkoxysilane dissolved in organic solvent, stirring, centrifugal washing, and drying to obtain SiO with amino group on surface2Particles. The above SiO2The mass ratio of the particles to the (amino) alkylalkoxysilane is 1 (0.01-10).
S2 preparation of SiO having carboxyl groups on the surface2Particles
Weighing SiO with amino on the surface according to the proportion2Mixing the particles with polyacrylic acid and coupling agent dissolved in water, stirring, centrifugally washing, and drying to obtain SiO with carboxyl on the surface2And (3) particles. SiO having amino group on surface2The mass ratio of the particles to the polyacrylic acid is 1 (0.1-10), and the surface of the particles contains amino SiO2The mass ratio of the particles to the coupling agent is 1 (0.01-10).
S3 used polyacrylic acid modified SiO2Reactivation of the particles
In polyacrylic acid modified SiO2After the particles catalyze the hydrolysis of sodium borohydride, the used polyacrylic acid modified SiO2Washing the particles with water, and drying to obtain polyacrylic acid modified SiO2Particles.
The invention has the beneficial effects that:
1. the invention provides polyacrylic acid modified SiO2The particles are a non-metal catalyst, and the utilization of metal resources is avoided.
2. The invention provides polyacrylic acid modified SiO2The preparation method of the particles is simple and easy to implement, has low cost and is beneficial to industrial production.
3. The invention provides polyacrylic acid modified SiO2The hydrogen production rate of the particles can reach 12.49mL min per gram of the catalyst when the particles catalyze the hydrolysis of sodium borohydride to produce hydrogen-1The activation energy of which is 30.18kJ mol-1And after being recovered, the catalyst is activated again and used again, and the catalytic efficiency is more than 95% of that of the first catalyst after 5 times of circulation.
Drawings
FIG. 1 shows polyacrylic acid-modified SiO prepared by the method2Transmission Electron Microscope (TEM) photographs of the particles;
FIG. 2 shows polyacrylic acid-modified SiO prepared by the method at 20 deg.C2A hydrogen production rate curve graph when the particle-catalyzed sodium borohydride is hydrolyzed to produce hydrogen;
FIG. 3 shows the polyacrylic acid modified SiO prepared by the method2A cycle performance test curve diagram of hydrogen production by hydrolyzing sodium borohydride under particle catalysis.
Detailed Description
Example 1
Preparation of polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2The preparation method of the particles comprises the following steps:
weighing 4g of SiO2Dissolving the particles and 0.4g of 3-aminopropyltriethoxysilane in toluene, stirring at 60 deg.C for 24h, washing with toluene and distilled water, centrifuging, and drying in a vacuum oven for 12h to obtain SiO with amino groups on the surface2Particles.
Taking the obtained SiO with amino groups on the surface22g of particles, 18g of polyacrylic acid, 3g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 2g N-hydroxysuccinimide are weighed and dissolved in distilled water, stirred for 24h at 25 ℃, washed by water, centrifuged, and placed in a vacuum oven for drying for 12h to prepare SiO with carboxyl on the surface2Particles, denoted as PAA-SiO2-1。
Example 2
Preparation of polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze and prepare hydrogen2The preparation method of the particles comprises the following steps:
6g of SiO are weighed2Dissolving the particles and 1g of 3-aminopropyltriethoxysilane in toluene, stirring at 60 deg.C for 24h, washing with toluene and distilled water, centrifuging, and drying in a vacuum oven for 12h to obtain SiO with amino groups on the surface2Particles.
Taking the obtained SiO with amino groups on the surface22g of particles, 18g of polyacrylic acid, 6g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4g N-hydroxysuccinimide are weighed and dissolved in distilled water, stirred for 24h at 25 ℃, washed by water, centrifuged, and placed in a vacuum oven for drying for 12h to prepare SiO with carboxyl on the surface2Particles, denoted as PAA-SiO2-2。
Example 3
Polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2The application of the particles is as follows:
50mg of PAA-SiO2-1 catalyst was dissolved in 40g of aqueous solution and added to the flask, which contained 15mg of NaBH by syringe with stirring410g of an aqueous solution was injected into the flask while timing was started and the test temperature was 20 ℃.
The catalyst PAA-SiO is treated by the method2The experimental results of the kinetic performance test of hydrogen production by hydrolysis of sodium borohydride under catalysis of the catalyst are shown in FIG. 2. Therefore, the hydrogen production rate by sodium borohydride hydrolysis catalyzed by the catalyst is 12.49 mL/g of catalyst for min-1。
Washing the reacted catalyst in water solution, drying and usingUsed PAA-SiO2-1 the catalyst is activated again.
Repeating all the above operations 4 times to obtain PAA-SiO catalyst2The cycle curve of the catalyst-catalyzed sodium borohydride hydrolysis hydrogen production is shown in figure 3. The catalytic efficiency after 5 times of circulation is more than 95 percent of that of the first time.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (4)
1. Polyacrylic acid modified SiO for catalyzing sodium borohydride to hydrolyze to prepare hydrogen2A method for producing particles, characterized by comprising the steps of:
s1: preparation of SiO having amino groups on the surface2Particles
Weighing SiO in proportion2Mixing the particles with (amino) alkylalkoxysilane dissolved in organic solvent, stirring, centrifugal washing, and drying to obtain SiO with amino group on surface2Particles;
s2: preparation of SiO with polyacrylic acid on the surface2Particles
Weighing SiO with amino on the surface according to the proportion2Mixing the particles with polyacrylic acid and coupling agent dissolved in water, stirring, centrifugal washing, and drying to obtain SiO containing polyacrylic acid on surface2Particles;
s3: used polyacrylic acid-modified SiO2Reactivation of the particles
In polyacrylic acid modified SiO2After the particles catalyze the hydrolysis of sodium borohydride, the used polyacrylic acid modified SiO2Washing the particles with water, and drying to obtain polyacrylic acid modified SiO2Particles.
2. The polyacrylic acid-modified SiO for catalyzing the hydrolysis of sodium borohydride to produce hydrogen according to claim 12ParticlesThe preparation method is characterized by comprising the following steps: and step S1, the organic solvent comprises toluene, N-dimethylformamide, tetrahydrofuran, halogenated hydrocarbon and alcohols.
3. The polyacrylic acid-modified SiO for catalyzing the hydrolysis of sodium borohydride to produce hydrogen according to claim 12A method for producing particles, characterized by: step S1, the SiO2The mass ratio of the particles to the (amino) alkylalkoxysilane is 1 (0.1-10).
4. The polyacrylic acid-modified SiO for catalyzing sodium borohydride to hydrolyze hydrogen production according to claim 12A method for producing particles, characterized by: step S2, the SiO with the surface containing amino2The mass ratio of the particles to the polyacrylic acid is 1 (0.1-10), and the surface of the particles contains amino SiO2The mass ratio of the particles to the coupling agent is 1 (0.01-10).
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