CN108906121A - A kind of C6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst - Google Patents
A kind of C6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst Download PDFInfo
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- CN108906121A CN108906121A CN201810737781.0A CN201810737781A CN108906121A CN 108906121 A CN108906121 A CN 108906121A CN 201810737781 A CN201810737781 A CN 201810737781A CN 108906121 A CN108906121 A CN 108906121A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 37
- 239000001257 hydrogen Substances 0.000 title claims abstract description 37
- 229920000642 polymer Polymers 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 241000219112 Cucumis Species 0.000 claims abstract description 11
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 claims abstract description 11
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 claims abstract description 11
- ALIFPGGMJDWMJH-UHFFFAOYSA-N n-phenyldiazenylaniline Chemical compound C=1C=CC=CC=1NN=NC1=CC=CC=C1 ALIFPGGMJDWMJH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- RNMCQEMQGJHTQF-UHFFFAOYSA-N 3,5,6,7-tetrahydrotetrazolo[1,5-b][1,2,4]triazine Chemical compound N1CCN=C2N=NNN21 RNMCQEMQGJHTQF-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- 239000003599 detergent Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 description 11
- 238000011161 development Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000006414 CCl Chemical group ClC* 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000000919 Fourier transform infrared map Methods 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005713 exacerbation Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- B01J35/39—Photocatalytic properties
-
- 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
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0254—Nitrogen containing compounds on mineral substrates
-
- 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
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of C6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst, using melamine as Material synthesis Melon, C is prepared in then Melon and KOH reaction6N7(OK)3, then with solid reaction process by C6N7(OK)3And PCl5Synthetic intermediate C6N7Cl3, finally by intermediate C6N7Cl3It is reacted in toluene with DAAB and obtains C6N7Cl3- DAAB polymer.Then to C6N7Cl3The research of-DAAB polymer progress photocatalysis hydrogen production performance.Result of study shows C6N7Cl3The hydrogen-producing speed of-DAAB polymer is 9.05 μm of ol g‑1 h‑1, it is 5.79 μm of ol g of Melon‑1 h‑11.5 times of hydrogen-producing speed.
Description
Technical field
The present invention relates to a kind of C6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst, is urged applied to light
Change hydrolytic hydrogen production field.
Background technique
The energy is the indispensable material base of human survival, while being also the important substance of Sustainable Socioeconomic Development
Guarantee.Into after 20th century, science and technology rapid development, economically developed, huge variation, the mankind are had occurred in people's lives
Society enters the unprecedented prosperity period.But while social fast-developing, consequent be shortage of resources,
The severe exacerbation of a series of problems, such as environmental pollution and disruption of ecological balance.Unquestionably, environmental pollution and lack of energy are that the mankind are raw
Deposit and develop two huge challenges to be faced.It has been observed that thoroughly to solve the above problems is the mankind without looking back
Sorrow, the most fundamental approach is to speed up the development of clean energy resource, realizes large-scale developing and utilizing for clean energy resource.Currently, can be again
The development and utilization of raw clean energy resource are widely recognized as by countries in the world.Energy density is high, can store, can transport because having for Hydrogen Energy
It is the features such as defeated, pollution-free, in recent years more and more to the developmental research of Hydrogen Energy as low-carbon and the zero carbon energy.Currently, photocatalysis system
Hydrogen technology has become one of the direction of the most researching value using solar energy and hydrogen production by water decomposition.On the one hand, water resource ten
Divide and enriches, it is widely distributed, it is low in cost, it is easy to get.On the other hand, hydrogen energy density is high, and calorific value is high, and only water is burning
Product, a point pressure will not be caused to environment, realizes the benign cycle of using energy source.The nitridation of polymer semiconductor's graphite-phase
Carbon（Melon）, because causing the great attention of people with excellent chemical stability and unique semiconductor energy band structure.Though
So it has been widely studied, but still has smaller sun light utilization efficiency deficiency, specific surface area, light induced electron and hole
The shortcomings such as recombination rate height limit the development of Melon material.
Summary of the invention
The object of the present invention is to provide a kind of C with new construction6N7Cl3- DAAB polymer light catalyzing manufacturing of hydrogen catalyst
Preparation method.A kind of C of the invention6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst is according to the following steps
It completes：
Step 1: by melamine (C3H6N6) it is put into porcelain crucible, with 520 DEG C of calcining 8h in Muffle furnace, it is naturally cooling to room
Temperature obtains Melon after grinding（C6N7(NH2)3）, appropriate Melon is claimed to be placed in KOH solution heating stirring back flow reaction 4h then
Crystallisation by cooling obtains white needle-like crystals C6N7(OK)3, weighed appropriate C6N7(OK)3Excess PCl is added5It is sufficiently ground in mortar
It is fitted into after mill in water heating kettle and is placed in 220 DEG C of heating in baking oven and obtains intermediate C afterwards for 24 hours6N7Cl3；
Step 2: the intermediate C that step 1 is obtained6N7Cl3With 4,4- azoic diphenylamine（DAAB）It respectively weighs and sequentially adds in right amount
Into toluene, first shading is stirred at room temperature, and a period of time is then reacted under oil bath heating counterflow condition.After the reaction was completed, normal pressure
Solid is obtained by filtration, and successively uses toluene, acetone, acetone-water mixture (v:v = 1:1) it respectively washs 3 ~ 5 times, after 80 DEG C of dryings
Obtain C6N7Cl3- DAAB polymer；
C described in step 26N7Cl3It is 1g with toluene quality and volume ratio:15~20mL；
C described in step 26N7Cl3Mass ratio with DAAB dosage is 1g：1~2g；
Reaction condition described in step 2 is that 12 ~ 36h is stirred in shading at room temperature, is then flowed back in 100 ~ 135 DEG C of oil bath heatings
Under the conditions of react 1 ~ 3h.
The test of photocatalysis Decomposition aquatic products hydrogen
To investigate C6N7Cl3- DAAB polymer light catalyzing manufacturing of hydrogen catalyst decomposes aquatic products hydrogen effect, by the following method to it
Photocatalyzed Hydrogen Production performance is tested.Test process is as follows：Photocatalyzed Hydrogen Production is tested in photocatalytic activity evaluation on-line analysis system
System carries out, and before reaction starts, opens condenser system, passes through air in vacuum pump exclusion system.The xenon lamp of 300W is as light source（≥
320nm）.
It is as follows that photocatalysis hydrogen production tests process：By C6N7Cl3- DAAB polymer hydrogen production photocatalyst material assay balance
30mg is weighed to be added in the mixed solution of 90mL distilled water and 10mL triethanolamine.To keep photochemical catalyst uniform in reaction process
Ultrasound 30min before reactor is added in dispersion, solution, and 1wt%Pt is added and does co-catalyst, mixed solution is then transferred to hydrogen
It persistently stirs in generating device and during the reaction, 40min vacuum pumping is carried out to system before reaction, after opening light source,
It is sampled under illumination condition every 1h, is analyzed using gas chromatograph, reaction duration amounts to 5h.
Beneficial effects of the present invention
Using melamine as Material synthesis Melon, C is prepared in then Melon and KOH reaction6N7(OK)3, then use solid phase reaction
Method is by C6N7(OK)3And PCl5Synthetic intermediate C6N7Cl3, finally by intermediate C6N7Cl3With DAAB in toluene first stirring at normal temperature
For 24 hours, then 125 ~ 135 DEG C of oil bath heating reflux 2h obtain C6N7Cl3Then-DAAB polymer is carried out photocatalysis hydrogen production
The research of energy.Result of study proves C6N7Cl3The hydrogen-producing speed of-DAAB polymer is 9.05 μm of olg-1h-1, it is Melon5.79 μ
mol g-1 h-11.5 times of hydrogen-producing speed.
Detailed description of the invention
Fig. 1 is C6N7Cl3And C6N7Cl3- DAAB polymer FT-IR map；
Fig. 2 is C6N7Cl3- DAAB polymer SEM figure；
Fig. 3 is Melon and C6N7Cl3Aquatic products hydrogen rate comparison figure is catalytically decomposed in-DAAB polymer light.
Specific embodiment
Embodiment 1：A kind of C of present embodiment6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst is
It completes according to the following steps：
Step 1: 30g melamine is put into porcelain crucible, it is placed in Muffle furnace with 520 DEG C of calcining 8h, is naturally cooling to room
Temperature obtains Melon after grinding；It weighs 10gMelon and is placed in 200mL, heating stirring back flow reaction 4h is right in the KOH solution of 2.5M
After stand a night crystallisation by cooling and obtain white needle-like crystals, crystal is obtained by filtration and it is washed into 2 ~ 3 postpositions with dehydrated alcohol
70 DEG C of dry 8h in a vacuum drying oven, obtain C6N7(OK)3；Weighed appropriate 2.5gC6N7(OK)3, 8gPCl is added5In mortar
In be fully ground after be fitted into water heating kettle and be placed in baking oven 220 DEG C of heating for 24 hours, be then naturally cooling to consolidating in kettle after room temperature
Body is transferred under the conditions of ice salt bath lower than being dispersed with stirring in 4 DEG C of cold distilled waters, and it is dry that the solid obtained after suction filtration is put into discoloration silica gel
C is obtained after drying in dry device6N7Cl3It seals and is put into refrigerator preservation；
Step 2: the C that step 1 is obtained6N7Cl3It respectively weighs 2g and 2.303g with DAAB to be added in 30mL toluene, at room temperature
Then 125 ~ 135 DEG C of oil bath heatings reflux 2h are stirred for 24 hours in shading.After the reaction was completed, natural filtration and successively with toluene, acetone,
Acetone-water mixture (v:v= 1:1) each 20mL is washed 3 ~ 5 times, obtains C after 80 DEG C of dryings6N7Cl3- DAAB polymer.
C6N7Cl3The characterization and performance detection of-DAAB polymer hydrogen production photocatalyst material：
The C that Fig. 1 obtains embodiment 16N7Cl3And C6N7Cl3- DAAB polymer carries out FT-IR detection, obtains as shown in Figure 1：1
For C6N7Cl3, 2 be C6N7Cl3- DAAB polymer.3200 cm are analyzed to obtain to 1-1The absorption peak at place is the asymmetric stretch of-C=N key
Vibration peak, 1637 cm-1、1500 cm-1With 1400 cm-1Left and right absorption peak be N-C=N skeletal vibration absorption peak, 1350
cm-1It is then the stretching vibration absorption of C-N, 850 cm-1Absorption peak be C-Cl stretching vibration generate deduction synthesis product
For C6N7Cl3.3500 cm can be speculated to 2 analyses-1The absorption peak at place is generated by the asymmetric stretching vibration of the N-H of secondary amine
, 3200 cm-1Absorption peak be C-H on phenyl ring asymmetric stretching vibration absorption peak, 1600 cm-1With 1500 cm-1Near
Four absorption peaks be then-C-N caused by the skeletal vibration as phenyl ring, the stretching vibration of-N=N- key and-C=N stretching vibration
Stretching vibration peak appear in 1300 cm-1Place, the bending vibration of-C-H is in 1250 cm-1、1150 cm-1With 1100 cm-1Is produced from place
Raw absorption peak, 850 cm-1It is that contraposition two replaces that the absorption peak at place, which demonstrates,.It can be inferred that C from figure6N7Cl3Pass through with DAAB
C is generated after reaction6N7Cl3- DAAB polymer.
The C that Fig. 2 obtains embodiment 16N7Cl3- DAAB polymer carries out sem analysis, obtains as shown in Figure 2：
Relatively regular round granular is presented in product appearance, and partial size is in 200 ~ 400nm.
The C that Fig. 3 obtains embodiment 16N7Cl3- DAAB polymer carries out progress photochemical catalyzing hydrogen-producing speed and compares
To as shown in Figure 3；1 is Melon, and 2 be C6N7Cl3-DAAB.From C known to figure6N7Cl3The hydrogen-producing speed of-DAAB polymer is 9.05
μmol g-1 h-1, it is 5.79 μm of ol g of Melon-1 h-11.5 times of hydrogen-producing speed.
Claims (4)
1. a kind of C6N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst, it is characterised in that C6N7Cl3- DAAB is poly-
The preparation method for closing object light catalyzing manufacturing of hydrogen catalyst is completed by the following steps：
Step 1: by melamine (C3H6N6) it is put into porcelain crucible, with 520 DEG C of calcining 8h in Muffle furnace, it is naturally cooling to room
Temperature obtains Melon after grinding（C6N7(NH2)3）, appropriate Melon is claimed to be placed in KOH solution heating stirring back flow reaction 4h then
Crystallisation by cooling obtains white needle-like crystals C6N7(OK)3, weighed appropriate C6N7(OK)3Excess PCl is added5It is sufficiently ground in mortar
It is fitted into after mill in water heating kettle and is placed in 220 DEG C of heating in baking oven and obtains intermediate C afterwards for 24 hours6N7Cl3；
Step 2: the intermediate C that step 1 is obtained6N7Cl3With 4,4- azoic diphenylamine（DAAB）It respectively weighs and sequentially adds in right amount
Into toluene, first shading is stirred at room temperature, and a period of time is then reacted under oil bath heating counterflow condition；
After the reaction was completed, natural filtration obtains solid, and successively uses toluene, acetone, acetone-water mixture (v:v = 1:1) each
Washing 3 ~ 5 times, obtains C after 80 DEG C of dryings6N7Cl3- DAAB polymer；
C described in step 26N7Cl3It is 1g with toluene quality and volume ratio:15~20mL；
C described in step 26N7Cl3Mass ratio with DAAB dosage is 1g：1~2g；
Reaction condition described in step 2 is that 12 ~ 36h is stirred in shading at room temperature, is then flowed back in 100 ~ 135 DEG C of oil bath heatings
Under the conditions of react 1 ~ 3h.
2. a kind of C according to claim 16N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst, it is special
Sign is：C described in step 26N7Cl3Mass ratio with azoic diphenylamine dosage can be preferably 1g：1~1.5g.
3. a kind of C according to claim 16N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst, it is special
Sign is：Reaction condition described in step 2 be can be preferably first at room temperature shading stirring 20 ~ for 24 hours, then at 125 ~ 135 DEG C
2h is reacted under oil bath heating counterflow condition.
4. a kind of C according to claim 16N7Cl3The preparation method of-DAAB polymer light catalyzing manufacturing of hydrogen catalyst, it is special
Sign is：C described in step 26N7Cl3With toluene used when washing, acetone, acetone-water mixture (v:v=1:1) every kind
The quality and volume ratio of each dosage of detergent are 1g:10~20mL.
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| CN109337068A (en) * | 2018-09-03 | 2019-02-15 | 哈尔滨理工大学 | A kind of polymer and its preparation method and application with photocatalytic activity |
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| CN105772056A (en) * | 2016-04-28 | 2016-07-20 | 成都理工大学 | Preparation method and application of graphite-phase carbon nitride photocatalysis material |
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2018
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