CN110252374A - A kind of porous silica silica gel particle loading graphite phase carbon nitride and the paper and preparation method thereof with it - Google Patents
A kind of porous silica silica gel particle loading graphite phase carbon nitride and the paper and preparation method thereof with it Download PDFInfo
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- CN110252374A CN110252374A CN201910544137.6A CN201910544137A CN110252374A CN 110252374 A CN110252374 A CN 110252374A CN 201910544137 A CN201910544137 A CN 201910544137A CN 110252374 A CN110252374 A CN 110252374A
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- carbon nitride
- phase carbon
- graphite phase
- gel particle
- paper
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 332
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 135
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 87
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 82
- 239000010439 graphite Substances 0.000 title claims abstract description 82
- 239000002245 particle Substances 0.000 title claims abstract description 74
- 239000000741 silica gel Substances 0.000 title claims abstract description 66
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000011068 loading method Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 22
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000012071 phase Substances 0.000 claims description 85
- 229910052681 coesite Inorganic materials 0.000 claims description 32
- 229910052906 cristobalite Inorganic materials 0.000 claims description 32
- 229910052682 stishovite Inorganic materials 0.000 claims description 32
- 229910052905 tridymite Inorganic materials 0.000 claims description 32
- 239000000499 gel Substances 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- 239000000908 ammonium hydroxide Substances 0.000 claims description 14
- 238000004108 freeze drying Methods 0.000 claims description 14
- 239000007863 gel particle Substances 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 10
- 239000000017 hydrogel Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229960004756 ethanol Drugs 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 230000002045 lasting effect Effects 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 16
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 210000003850 cellular structure Anatomy 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 90
- 235000019256 formaldehyde Nutrition 0.000 description 29
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 239000000835 fiber Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229920001131 Pulp (paper) Polymers 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 238000005286 illumination Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241000115038 Chelura Species 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
-
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/18—Paper- or board-based structures for surface covering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
Abstract
The invention discloses a kind of porous silica silica gel particle for loading graphite phase carbon nitride and with its paper and preparation method thereof, belong to environmental catalysis technical field.Using sol-gel method by ethyl orthosilicate aqueous solution and g-C3N4The porous silica silica gel particle of load graphite phase carbon nitride is prepared in mixing, has biggish specific surface area, cellular structure size is controllable, and auxiliary agent particle size is controllable.Preparation condition is mild, simple process, raw material are cheap, reproducible, and the material being prepared has good photocatalysis performance.The catalytic efficiency that catalysis material can be improved when adding it in ornament materials has widened the research range of catalysis material.
Description
Technical field
The invention belongs to environmental catalysis technical fields, and in particular to a kind of porous silica for loading graphite phase carbon nitride
Gel particle and paper and preparation method thereof with it.
Background technique
The big outstanding problem that environmental pollution has become China and the whole world needs to face, formaldehyde are that one kind is colourless, are had
The gas of intense irritation smell, 37% aqueous solution are known as formalin, and medicine and scientific research department are usually used in the anti-of sample
Corruption saves.The corrosion of house decorative material and furniture in order to prevent, timber also commonly uses formalin immersion before processing prevents corruption
Erosion and chelura damage purpose.The boiling point of formaldehyde is 19.5 DEG C, highly volatile when room temperature, as the rising evaporation rate of temperature adds
Fastly.Column occupy second in China's toxic chemical priority acccess control list, are determined as carcinogenic and teratogenesis by the World Health Organization
Shape substance.Synthetic plate used in interior decoration, such as glued board, core-board, high-density plate, particieboard and wood furniture
Formaldehyde plays adhesive, preservative in equal materials, understands always to indoor slow release, burst size several years ago especially
It is prominent.Release how to effectively control formaldehyde is to solve the problems, such as this difficult point and research hotspot.
Graphite phase carbon nitride (g-C3N4) it is used as a kind of non-metal optical catalyst, because suitable forbidden bandwidth (2.7eV) makes it
It just can be carried out photolysis water hydrogen reaction under visible light illumination and attract attention.In addition, because of its thermal stability and chemical stability
Well, the features such as cost of material is cheap, is widely used in photocatalytic water photocatalysis field.g-C3N4Photochemical catalyst is a kind of two-dimensional layer
Block catalysis material made of material is piled up, since special two-dimensional layered structure leads to that electronics is excited to transmit resistance in layer
Small, interlayer resistance is big, so that the activity of marginal position ((100) crystal face) is significantly larger than on two-dimensional surface ((002) crystal face)
Activity.Traditional powder catalyst sufficiently with reactant (such as photolysis water hydrogen, CO2Reduction, NOxRemoval etc.) it is uniformly mixed i.e.
Efficient photocatalysis performance, but pure g-C can be played3N4Due to the powder characteristics of itself, it is unable to control and degradable out of furniture
The formaldehyde that portion releases.Therefore, it is necessary to using certain carrier as skeleton structure by g-C3N4It is uniformly dispersed and carries out photocatalysis
Degradation of formaldehyde reaction.
Traditional wallpaper uses it to disperse g-C as skeleton carrier due to poor air permeability3N4The formaldehyde overflowed cannot not only be made
Molecule smoothly penetrates wallpaper and g-C3N4Reaction, can also make formaldehyde molecule for a long time by catalyst blockage because of cellular structure cannot dissipate
Hair falls, and in several years, still there was formaldehyde molecule spilling in the even longer time.Sponge, can due to good cellular structure and mechanical strength
Using as the evenly dispersed g-C of good carrier3N4Carry out Degradation Formaldehyde, but due to the cellular structure in sponge is too many and aperture too
Greatly, most of not by Catalyst Adsorption when causing formaldehyde molecule to overflow, it directly distributes to interior, goes effect of formaldehyde bad.
Therefore, a kind of carrying g-C is manufactured3N4Multi-pore channel material be current urgent problem to be solved.
Summary of the invention
In order to overcome the problems of the above-mentioned prior art, the invention discloses a kind of the porous of load graphite phase carbon nitride
Silica dioxide gel particle and paper and preparation method thereof with it, preparation condition is mild, simple process, raw material are cheap, repeats
Property it is good, the material being prepared have good photocatalysis performance.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of porous silica silica gel particle loading graphite phase carbon nitride disclosed by the invention, including
Following steps:
Step 1: weighing the g-C that solid-liquid ratio is (0.2~1.0) g:100mL respectively3N4It, will just with ethyl orthosilicate aqueous solution
Silester aqueous solution is placed in dispersing agent after stirring and g-C3N4Mixing, obtain reaction system A, in lasting whipping process to
Curing agent is added dropwise in reaction system A until sticky, standing obtains SiO after being aged2/g-C3N4Gel rubber system；
Step 2: by SiO2/g-C3N4Gel rubber system is freeze-dried, and obtaining load has porous the two of graphite phase carbon nitride
Silica gel；
Step 3: the load that step 2 is obtained has the porous silica Silica hydrogel of graphite phase carbon nitride at 450~650 DEG C
It is calcined, the porous silica silica gel particle of load graphite phase carbon nitride is obtained after cooled to room temperature.
Preferably, the specific steps of step 1 are as follows:
Step 1.1: by ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stir 30min after with g-C3N4It is mixed
It closes, stir evenly, obtain system A；
Step 1.2: concentration being added dropwise into system A in lasting whipping process and is less than 1mol L-1Ammonium hydroxide, when dropwise addition, on
Next drop ammonium hydroxide is added dropwise after being uniformly mixed in system A in one drop ammonium hydroxide, until thick, stood, be aged after obtain
SiO2/g-C3N4Gel rubber system.
It is further preferred that in step 2, before freeze-drying, type solvent is dissolved each other using deionized water, ethyl alcohol or ethyl alcohol makes
SiO2/g-C3N4Liquid phase unification in gel rubber system.
Preferably, in step 2, when freeze-drying, is frozen into the time < 1min, the time > 20h of freeze-drying of solid.
The invention also discloses the porous silica Silica hydrogels that graphite phase carbon nitride is loaded made from above-mentioned preparation method
Grain, aperture are 20~30nm.
A kind of porous silica silica gel particle using above-mentioned load graphite phase carbon nitride disclosed by the invention prepares paper
Method, comprising the following steps:
Step 1: the porous silica silica gel particle for loading graphite phase carbon nitride being sieved, and screens mass point
The uniform particle of cloth is stand-by；
Step 2: body paper being starched and is discongested by 0.5~5.0% mass concentration, the more of load graphite phase carbon nitride are added
Hole silica dioxide gel particle, the porous silica silica gel particle stable suspersion of stirring to load graphite phase carbon nitride is in solution
In, obtain system B；
Step 3: system B is subjected to page of manufacturing paper with pulp, gained page is dry under ventilation condition, obtain that there is load graphite
The paper of the porous silica silica gel particle of phase carbon nitride.
Preferably, in step 1, the thickness of paper for grain diameter=1~1.5 times being sieved.
Preferably, in step 2, the porous silica silica gel particle of graphite phase carbon nitride and the mass ratio of body paper slurry are loaded
For (0.1~10): 100.
Preferably, in step 3, dry temperature is 50~80 DEG C, and the dry time is greater than for 24 hours, and the air quantity of ventilation is greater than
2.0m3/min。
The invention also discloses have porous the two of load graphite phase carbon nitride made from the method for paper using above-mentioned prepare
The paper of silica gel particle.
Compared with prior art, the invention has the following beneficial technical effects:
The preparation method of the porous silica silica gel particle of load graphite phase carbon nitride disclosed by the invention, use are molten
Glue-gel method is by ethyl orthosilicate aqueous solution and g-C3N4The porous silica of load graphite phase carbon nitride is prepared in mixing
Gel particle.High-temperature calcination can guarantee g-C3N4In SiO2Stability in duct removes the object for easily decomposing and blocking duct
Matter, it is ensured that SiO2Cellular structure be not blocked.SiO2Aeroge is that a kind of porosity constituted that mutually coalesced by nanoparticle is consolidated
State material has many advantages, such as that density is low, porosity is high, the uniform light transmission of pore size distribution is good, is capable of providing specific duct knot
Structure realizes the control of formaldehyde diffusion rate in duct, makes the photochemical catalyst g-C carried3N4It can effectively oxidize the formaldehyde into nontoxic
Harmless formic acid is reduced into the lesser methanol of harm, and its energy source is that diffusing reflection enters indoor sunlight, is not necessarily to
It is additionally provided the energy.In addition, g-C3N4With nitrogen active site abundant, photochemical catalyst itself will not be by during removing formaldehyde
Consumption, it is ensured that nitrogen active site continues high efficiency utilization, continuously disposes the formaldehyde molecule of spilling.Theoretically,
As long as the cellular structure of silica is not blocked, photocatalysis goes formaldehyde performance to may insure in 5 years (burst size of methanal is maximum)
Still effectively.This method preparation condition is mild, simple process, raw material are cheap, reproducible.
Further, 1mol L is less than using concentration-1Ammonium hydroxide as curing agent, be swift in response, reaction rate controllability
It is good；And to guarantee that next drop ammonium hydroxide is added dropwise after upper drop ammonium hydroxide is thoroughly mixed uniformly in reaction system A when being added dropwise, it can
Ensure that ammonium hydroxide is uniformly dispersed in the solution, keep the cross-linked speed of ethyl orthosilicate identical, guarantees the duct of silica after crosslinking
Structure is uniform.
Further, the time > 20h of freeze-drying, it can be ensured that the moisture in duct all volatilizees, and will not block
SiO2Cellular structure.
Further, before freeze-drying, the liquid phase in system reacts remaining water, unreacted molten at this time before including
Agent ethyl alcohol dissolves each other type solvent using deionized water, ethyl alcohol or ethyl alcohol makes SiO2/g-C3N4Liquid phase unification in gel rubber system, really
The pore size of silica obtained by protecting is possessed otherwise comprising dispersing agent and polymeric reaction product in system than more uniform
Surface can be different, and pore size and particle diameter distribution are with regard to uneven.
The present invention discloses the porous silica Silica hydrogel of the load graphite phase carbon nitride obtained using above-mentioned preparation method
Grain has biggish specific surface area, and cellular structure size is controllable, and auxiliary agent particle size is controllable.It adds it in ornament materials
When the catalytic efficiency of catalysis material can be improved, widened the research range of catalysis material.
The preparation method of the paper of the porous silica silica gel particle of load graphite phase carbon nitride disclosed by the invention, to negative
The porous silica silica gel particle for carrying graphite phase carbon nitride carried out filtering out the close particle of partial size, using air blast screening method
Remove the too small or excessive sample in duct, it is ensured that the overall air permeability of subsequent gained paper.Then it is made as paper aid
Paper, porous silica silica gel particle of the manufactured paper inside containing load graphite phase carbon nitride, can make formaldehyde pass through duct
By graphite phase carbon nitride photocatalysis when structure, this method preparation condition is mild, simple process, raw material are cheap, reproducible.
Further, the thickness of paper for grain diameter=1~1.5 times being sieved makes to load the porous of graphite phase carbon nitride
Silica dioxide gel particle can run through paper, reach good air permeability effect.Partial size is too big, then will affect the smooth of paper
Degree；Partial size is too small, then can block the cellular structure of porous silica, influence reaction rate.
Further, the mass ratio of the porous silica silica gel particle and body paper slurry that load graphite phase carbon nitride is (0.1
~10): 100, best catalytic performance is not achieved in the porous silica silica gel particle additional amount for loading graphite phase carbon nitride very little,
Additional amount will affect greatly very much paper strength.
Further, dry temperature is 50~80 DEG C, and the dry time is greater than for 24 hours, and the air quantity of ventilation is greater than 2.0m3/
Min, it is ensured that can dry thoroughly, and the cellular structure of silica dioxide gel will not be blocked by paper fibre, be avoided because of technique
Reason influences formaldehyde passage capacity.
It is disclosed by the invention load graphite phase carbon nitride porous silica silica gel particle paper, can be used as wallpaper,
The ornament materials such as Decorative paster use, using diffusing reflection to indoor light as the energy, passing through the formaldehyde molecule overflowed in furniture
Load g-C3N4Fallen when porous silica duct by photocatalyst treatment, the source excessive from formaldehyde solves indoor air quality.
The program is not necessarily to external energy and used catalyst and carrier are nontoxic, will not lead to air quality because of the introducing of catalyst
Decline.
Detailed description of the invention
A~e is respectively the porous silica Silica hydrogel that Examples 1 to 5 load obtained has graphite phase carbon nitride in Fig. 1
Pictorial diagram；F is pure SiO2The pictorial diagram of gel；
A~e is respectively the Examples 1 to 5 porous silica Silica hydrogel with load graphite phase carbon nitride obtained in Fig. 2
The pictorial diagram of the paper of particle；F is pure SiO2Pictorial diagram of the gel as the papermaking of auxiliary agent institute；
Fig. 3 is the SEM of the porous silica silica gel particle of the load graphite phase carbon nitride obtained of the embodiment of the present invention 1
Scheme (200nm)；
Fig. 4 is the SEM of the porous silica silica gel particle of the load graphite phase carbon nitride obtained of the embodiment of the present invention 1
Scheme (2 μm)；
Fig. 5 is the SEM of the porous silica silica gel particle of the load graphite phase carbon nitride obtained of the embodiment of the present invention 1
Scheme (10 μm)；
Fig. 6 be the Examples 1 to 5 porous silica silica gel particle with load graphite phase carbon nitride obtained paper and
Formaldehyde performance curve is removed in the photocatalysis of paper made from pure silicon dioxide gel particle.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Load the preparation method of the porous silica silica gel particle of graphite phase carbon nitride:
Embodiment 1
Under room temperature, take 100mL ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stirring 30min is fully hydrolyzed
The g-C of 0.2g is added afterwards3N4, instill concentration dropwise after mixing evenly and be less than 1mol L-1Ammonium hydroxide persistently stir 1h to solution become
It is stood after thick, ageing, after the dehydrated alcohol in system is repeatedly displaced using deionized water, outwells deionized water, obtain
SiO2/g-C3N4Gel rubber system.By SiO2/g-C3N4Gel rubber system is frozen into solid in 1min, the freeze-drying through 20h, so
It calcines 2h at 550 DEG C in Muffle furnace afterwards, the porous silica of load graphite phase carbon nitride is obtained after cooled to room temperature
Gel particle.
The porous silica silica gel particle of obtained load graphite phase carbon nitride is sieved, filtering out partial size is 50 μm
Silicon dioxide microsphere simultaneously ensures that its Mass Distribution is uniform.Body paper slurry is discongested in device in standard fibre and is discongested by 1.5% concentration,
The porous silica silica gel particle that 5g load graphite phase carbon nitride is added in paper pulp after discongesting to 100g is stirred to load stone
The porous silica silica gel particle stable suspersion of black phase carbon nitride is copied on pattern former in the solution, by gained suspension
Papermaking is simultaneously arranged institute's copy paper with a thickness of 40 μm, gained page is dried at 50 DEG C and is greater than 2.0m in air blast condition air quantity3/
It is divulged information more than for 24 hours under min, obtains the paper of the porous silica silica gel particle with load graphite phase carbon nitride.
Embodiment 2
Under room temperature, take 100mL ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stirring 30min is fully hydrolyzed
The g-C of 0.4g is added afterwards3N4, instill concentration dropwise after mixing evenly and be less than 1mol L-1Ammonium hydroxide persistently stir 1h to solution become
It is stood after thick, ageing, after the dehydrated alcohol and water in system are repeatedly displaced using methanol, outwells methanol, obtain SiO2/
g-C3N4Gel rubber system.By SiO2/g-C3N4Gel rubber system is frozen into solid in 1min, the freeze-drying through 21h, then in horse
2h is not calcined in furnace at 550 DEG C, the porous silica Silica hydrogel of load graphite phase carbon nitride is obtained after cooled to room temperature
Grain.
The porous silica silica gel particle of obtained load graphite phase carbon nitride is sieved, filtering out partial size is 50 μm
Silicon dioxide microsphere simultaneously ensures that its Mass Distribution is uniform.Body paper slurry is discongested in device in standard fibre and is discongested by 1.5% concentration,
The porous silica silica gel particle that 5g load graphite phase carbon nitride is added in paper pulp after discongesting to 100g is stirred to load stone
The porous silica silica gel particle stable suspersion of black phase carbon nitride is copied on pattern former in the solution, by gained suspension
Papermaking is simultaneously arranged institute's copy paper with a thickness of 40 μm, gained page is dried at 60 DEG C and is greater than 2.0m in air blast condition air quantity3/
It is divulged information more than for 24 hours under min, obtains the paper of the porous silica silica gel particle with load graphite phase carbon nitride.
Embodiment 3
Under room temperature, take 100mL ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stirring 30min is fully hydrolyzed
The g-C of 0.6g is added afterwards3N4, instill concentration dropwise after mixing evenly and be less than 1mol L-1Ammonium hydroxide persistently stir 1h to solution become
It is stood after thick, ageing, after the dehydrated alcohol in system is repeatedly displaced using deionized water, outwells deionized water, obtain
SiO2/g-C3N4Gel rubber system.By SiO2/g-C3N4Gel rubber system is frozen into solid in 1min, the freeze-drying through 22h, so
It calcines 2h at 550 DEG C in Muffle furnace afterwards, the porous silica of load graphite phase carbon nitride is obtained after cooled to room temperature
Gel particle.
The porous silica silica gel particle of obtained load graphite phase carbon nitride is sieved, filtering out partial size is 50 μm
Silicon dioxide microsphere simultaneously ensures that its Mass Distribution is uniform.Body paper slurry is discongested in device in standard fibre and is discongested by 1.5% concentration,
The porous silica silica gel particle that 5g load graphite phase carbon nitride is added in paper pulp after discongesting to 100g is stirred to load stone
The porous silica silica gel particle stable suspersion of black phase carbon nitride is copied on pattern former in the solution, by gained suspension
Papermaking is simultaneously arranged institute's copy paper with a thickness of 40 μm, gained page is dried at 70 DEG C and is greater than 2.0m in air blast condition air quantity3/
It is divulged information more than for 24 hours under min, obtains the paper of the porous silica silica gel particle with load graphite phase carbon nitride.
Embodiment 4
Under room temperature, take 100mL ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stirring 30min is fully hydrolyzed
The g-C of 0.8g is added afterwards3N4, instill concentration dropwise after mixing evenly and be less than 1mol L-1Ammonium hydroxide persistently stir 1h to solution become
It is stood after thick, ageing, after the water in system is repeatedly displaced using ethyl alcohol, outwells ethyl alcohol, obtain SiO2/g-C3N4Gel
System.By SiO2/g-C3N4Gel rubber system is frozen into solid in 1min, the freeze-drying through 20h, then 450 in Muffle furnace
2h is calcined at DEG C, and the porous silica silica gel particle of load graphite phase carbon nitride is obtained after cooled to room temperature.
The porous silica silica gel particle of obtained load graphite phase carbon nitride is sieved, filtering out partial size is 40 μm
Silicon dioxide microsphere simultaneously ensures that its Mass Distribution is uniform.Body paper slurry is discongested in device in standard fibre and is discongested by 0.5% concentration,
The porous silica silica gel particle that 3g load graphite phase carbon nitride is added in paper pulp after discongesting to 100g is stirred to load stone
The porous silica silica gel particle stable suspersion of black phase carbon nitride is copied on pattern former in the solution, by gained suspension
Papermaking is simultaneously arranged institute's copy paper with a thickness of 40 μm, gained page is dried at 50 DEG C and is greater than 2.0m in air blast condition air quantity3/
It is divulged information more than for 24 hours under min, obtains the paper of the porous silica silica gel particle with load graphite phase carbon nitride.
Embodiment 5
Under room temperature, take 100mL ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stirring 30min is fully hydrolyzed
The g-C of 1.0g is added afterwards3N4, instill concentration dropwise after mixing evenly and be less than 1mol L-1Ammonium hydroxide persistently stir 1h to solution become
It is stood after thick, ageing, after the dehydrated alcohol in system is repeatedly displaced using deionized water, outwells deionized water, obtain
SiO2/g-C3N4Gel rubber system.By SiO2/g-C3N4Gel rubber system is frozen into solid in 1min, the freeze-drying through 20h, so
It calcines 2h at 650 DEG C in Muffle furnace afterwards, the porous silica of load graphite phase carbon nitride is obtained after cooled to room temperature
Gel particle.
The porous silica silica gel particle of obtained load graphite phase carbon nitride is sieved, filtering out partial size is 60 μm
Silicon dioxide microsphere simultaneously ensures that its Mass Distribution is uniform.Body paper slurry is discongested in device in standard fibre and is discongested by 5.0% concentration,
The porous silica silica gel particle that 10g load graphite phase carbon nitride is added in paper pulp after discongesting to 100g is stirred to load stone
The porous silica silica gel particle stable suspersion of black phase carbon nitride is copied on pattern former in the solution, by gained suspension
Papermaking is simultaneously arranged institute's copy paper with a thickness of 50 μm, gained page is dried at 80 DEG C and is greater than 2.0m in air blast condition air quantity3/
It is divulged information more than for 24 hours under min, obtains the paper of the porous silica silica gel particle with load graphite phase carbon nitride.
Embodiment 6
Under room temperature, take 100mL ethyl orthosilicate aqueous dispersion into acetone, stirring 30min adds after being fully hydrolyzed
Enter the g-C of 0.6g3N4, instill concentration dropwise after mixing evenly and be less than 1mol L-1Ethylenediamine persistently stir 1h and become sticky to solution
It stands, be aged after thick shape, displaced in system after unreacted water using acetone, outwell acetone, obtain SiO2/g-C3N4Gel
System.By SiO2/g-C3N4Gel rubber system is rapidly frozen, then the freeze-drying through 20h is calcined at 550 DEG C in Muffle furnace
2h obtains the porous silica silica gel particle of load graphite phase carbon nitride after cooled to room temperature.
The porous silica silica gel particle of obtained load graphite phase carbon nitride is sieved, filtering out partial size is 50 μm
Silicon dioxide microsphere simultaneously ensures that its Mass Distribution is uniform.Body paper slurry is discongested in device in standard fibre and is discongested by 1.5% concentration,
The porous silica silica gel particle that 0.1g load graphite phase carbon nitride is added in paper pulp after discongesting to 100g is stirred to load
The porous silica silica gel particle stable suspersion of graphite phase carbon nitride in the solution, by gained suspension on pattern former
It manufactures paper with pulp and paper and institute's copy paper is set with a thickness of 30 μm, gained page is dried at 50 DEG C and is greater than in air blast condition air quantity
2.0m3It is divulged information more than for 24 hours under/min, obtains the paper of the porous silica silica gel particle with load graphite phase carbon nitride.
A~e is respectively the porous silica Silica hydrogel that Examples 1 to 5 load obtained has graphite phase carbon nitride in Fig. 1
Pictorial diagram, f are pure SiO2The pictorial diagram of gel, as seen from the figure: pure SiO2Gel is white.The g-C of yellow3N4Powder adds
It is evenly dispersed in the solution after adding, the phenomenon that forming stable suspension, and do not sink to the bottom after forming gel, show that light is urged
Agent g-C3N4It is dispersed in SiO2In gel.
A~e is respectively the Examples 1 to 5 porous silica Silica hydrogel with load graphite phase carbon nitride obtained in Fig. 2
The pictorial diagram of the paper of particle, f are pure SiO2Pictorial diagram of the gel as the papermaking of auxiliary agent institute, as seen from the figure: prepared
Load different quality g-C3N4Paper color gradually deepen, show SiO2/g-C3N4Even particulate dispersion is in paper.In addition,
With g-C3N4The increase of content, SiO2/g-C3N4Particle is more uniform in paper surface dispersion, is more conducive to formaldehyde molecule in duct
In diffusion, enhance the processing capacity of formaldehyde.
Fig. 3~Fig. 5 is respectively the porous silica silica gel particle of load graphite phase carbon nitride prepared by embodiment 1 10
μm, 2 μm, the SEM figure under 200nm, as seen from the figure: amplify 800 times, it can be seen that exist perhaps in silica dioxide granule
Multi-pore channel structure is continued to be amplified to 8000 times, can more clearly see g-C3N4It is crosslinked together by silica and
Cellular structure in silica is more obvious, continues 25000 times of amplification, can more obviously find out that the distribution of its pore size is equal
It is even, about in 20-30nm or so.
Fig. 6 be the Examples 1 to 5 porous silica silica gel particle with load graphite phase carbon nitride obtained paper and
Formaldehyde performance curve is removed in the photocatalysis of paper made from pure silicon dioxide gel particle, and the initial concentration of formaldehyde is 100ppm in figure,
Pure SiO2The concentration of formaldehyde variation before and after illumination of gel institute copy paper sample is little, negative photocatalyst-bearing g-C3N4Afterwards, formaldehyde after illumination
Concentration be greatly reduced to 10ppm hereinafter, show load have g-C3N4Wallpaper photocatalysis go formaldehyde to have excellent performance.
It should be noted that the porous silica silica gel particle for the load graphite phase carbon nitride that the present invention prepares can be with
It is added in any surface layer, including but not limited to: wallpaper, wall cloth, Decorative paster, carpenter's lagging, finishing coat etc., it is only necessary to according to this
Invent record load graphite phase carbon nitride porous silica silica gel particle paper preparation method do corresponding raw material,
Technique adjustment.
Claims (10)
1. it is a kind of load graphite phase carbon nitride porous silica silica gel particle preparation method, which is characterized in that including with
Lower step:
Step 1: weighing the g-C that solid-liquid ratio is (0.2~1.0) g:100mL respectively3N4With ethyl orthosilicate aqueous solution, by positive silicic acid
Ethyl ester aqueous solution is placed in dispersing agent after stirring and g-C3N4Mixing, obtains reaction system A, the Xiang Fanying in lasting whipping process
Curing agent is added dropwise in system A until sticky, standing obtains SiO after being aged2/g-C3N4Gel rubber system；
Step 2: by SiO2/g-C3N4Gel rubber system is freeze-dried, and the porous silica that load has graphite phase carbon nitride is obtained
Silica hydrogel；
Step 3: the load that step 2 is obtained has the porous silica Silica hydrogel of graphite phase carbon nitride to carry out at 450~650 DEG C
It calcines, the porous silica silica gel particle of load graphite phase carbon nitride is obtained after cooled to room temperature.
2. the preparation method of the porous silica silica gel particle of load graphite phase carbon nitride as described in claim 1, special
Sign is, the specific steps of step 1 are as follows:
Step 1.1: by ethyl orthosilicate aqueous dispersion into dehydrated alcohol, stir 30min after with g-C3N4It mixed, stirred
It mixes uniformly, obtains system A；
Step 1.2: concentration being added dropwise into system A in lasting whipping process and is less than 1molL-1Ammonium hydroxide, when dropwise addition, upper drop ammonia
Next drop ammonium hydroxide is added dropwise in water after being uniformly mixed in system A, until thick, stood, be aged after obtain SiO2/g-
C3N4Gel rubber system.
3. the preparation method of the porous silica silica gel particle of load graphite phase carbon nitride as claimed in claim 2, special
Sign is, in step 2, before freeze-drying, dissolves each other type solvent using deionized water, ethyl alcohol or ethyl alcohol makes SiO2/g-C3N4Gel
Liquid phase unification in system.
4. the preparation method of the porous silica silica gel particle of load graphite phase carbon nitride as described in claim 1, special
Sign is, in step 2, when freeze-drying is frozen into the time < 1min, the time > 20h of freeze-drying of solid.
5. using the porous silica of the load graphite phase carbon nitride obtained of preparation method described in Claims 1 to 4 any one
Silica gel particle, which is characterized in that aperture is 20~30nm.
6. the method that paper is prepared using the porous silica silica gel particle of load graphite phase carbon nitride described in claim 5,
Characterized by comprising the following steps:
Step 1: the porous silica silica gel particle for loading graphite phase carbon nitride being sieved, and it is equal to filter out Mass Distribution
Even particle is stand-by；
Step 2: body paper being starched and is discongested by 0.5~5.0% mass concentration, porous the two of load graphite phase carbon nitride are added
Silica gel particle, stirring extremely load the porous silica silica gel particle stable suspersion of graphite phase carbon nitride in the solution,
Obtain system B；
Step 3: system B is subjected to page of manufacturing paper with pulp, gained page is dry under ventilation condition, obtain that there is load graphite-phase nitrogen
Change the paper of the porous silica silica gel particle of carbon.
7. the method for preparing paper as claimed in claim 6, which is characterized in that in step 1, grain diameter=1 be sieved
~1.5 times of thickness of paper.
8. the method for preparing paper as claimed in claim 6, which is characterized in that in step 2, load the porous of graphite phase carbon nitride
The mass ratio of silica dioxide gel particle and body paper slurry is (0.1~10): 100.
9. the method for preparing paper as claimed in claim 6, which is characterized in that in step 3, dry temperature is 50~80 DEG C,
The dry time is greater than for 24 hours, and the air quantity of ventilation is greater than 2.0m3/min。
10. there are the more of load graphite phase carbon nitride using the method for preparing paper described in claim 6~9 any one is obtained
The paper of hole silica dioxide gel particle.
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| CN111944353A (en) * | 2020-08-25 | 2020-11-17 | 陕西科技大学 | Coating containing porous filler and preparation method and use method thereof |
| CN112237938A (en) * | 2020-09-15 | 2021-01-19 | 西安工程大学 | Composite photocatalyst for treating textile printing and dyeing wastewater, fiber thereof and preparation method thereof |
| CN113083343A (en) * | 2021-03-17 | 2021-07-09 | 江苏索普化工股份有限公司 | Graphite-phase carbon nitride modified silicon oxide porous microsphere rhodium-loaded heterogeneous catalyst and preparation method and application thereof |
| CN113083343B (en) * | 2021-03-17 | 2023-08-29 | 江苏索普化工股份有限公司 | Heterogeneous catalyst of rhodium supported by graphite-phase carbon nitride modified silicon oxide porous microspheres and preparation method and application thereof |
| CN113529492A (en) * | 2021-07-16 | 2021-10-22 | 东北电力大学 | Preparation method of hydrophobic wallpaper base paper based on diatomite |
| CN113529492B (en) * | 2021-07-16 | 2023-02-03 | 东北电力大学 | Preparation method of hydrophobic wallpaper base paper based on diatomite |
| CN114832803A (en) * | 2022-04-08 | 2022-08-02 | 重庆城市综合交通枢纽（集团）有限公司 | Film-forming composition, preparation method thereof and application of composite photocatalyst |
| CN115430414A (en) * | 2022-09-15 | 2022-12-06 | 浙江冰虫环保科技有限公司 | Environment-friendly degradation photocatalyst formaldehyde scavenger |
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