CN108479707A - A kind of preparation method of material for air purification - Google Patents
A kind of preparation method of material for air purification Download PDFInfo
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- CN108479707A CN108479707A CN201810515508.3A CN201810515508A CN108479707A CN 108479707 A CN108479707 A CN 108479707A CN 201810515508 A CN201810515508 A CN 201810515508A CN 108479707 A CN108479707 A CN 108479707A
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- air purification
- cellulose
- halloysite nanotubes
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000004887 air purification Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920002678 cellulose Polymers 0.000 claims abstract description 48
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000001913 cellulose Substances 0.000 claims abstract description 42
- 239000002071 nanotube Substances 0.000 claims abstract description 35
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 claims abstract description 34
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052621 halloysite Inorganic materials 0.000 claims abstract description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229960000583 acetic acid Drugs 0.000 claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 11
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 10
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims abstract description 10
- 229960002218 sodium chlorite Drugs 0.000 claims abstract description 10
- 241000183024 Populus tremula Species 0.000 claims abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000706 filtrate Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 230000003197 catalytic effect Effects 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 229920000297 Rayon Polymers 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 229910021556 Chromium(III) chloride Inorganic materials 0.000 claims description 9
- 229960000359 chromic chloride Drugs 0.000 claims description 9
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 229920005610 lignin Polymers 0.000 claims description 7
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 7
- 241000196324 Embryophyta Species 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 238000000527 sonication Methods 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 8
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000809 air pollutant Substances 0.000 abstract description 3
- 231100001243 air pollutant Toxicity 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000011068 loading method Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 14
- 239000007789 gas Substances 0.000 description 11
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 230000000505 pernicious effect Effects 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 235000019256 formaldehyde Nutrition 0.000 description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 229960004279 formaldehyde Drugs 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 206010025482 malaise Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01D53/8678—Removing components of undefined structure
- B01D53/8687—Organic components
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B01J35/39—
Abstract
The present invention relates to technical field of air purification, and in particular to a kind of preparation method of material for air purification.The present invention by halloysite nanotubes, toluene,(3 mercaptopropyis)Trimethoxy silane hybrid reaction obtains dredging base halloysite nanotubes, it recycles hydrogen peroxide and methanol oxidation to dredge base halloysite nanotubes and obtains sulfonated halloysite nanotubes, aspen fibers by using silicon powder is handled using sodium chlorite solution and glacial acetic acid solution to obtain wooden nano-cellulose, absolute ethyl alcohol is mixed with nano-cellulose, nano-cellulose suspension is obtained through ultrasonic disperse, tetraethyl titanate etc. is added in nano-cellulose suspension and obtains material for air purification, nano-cellulose charing back loading can effectively inhibit the compound of light induced electron and hole in halloysite nanotubes in the present invention, improve the efficiency of photocatalytic degradation air pollutants, halloysite nanotubes can make the volatile organic contaminant fast enriching of low concentration, it improves to indoor photocatalytic oxidation efficiency, it has a extensive future.
Description
Technical field
The present invention relates to technical field of air purification, and in particular to a kind of preparation method of material for air purification.
Background technology
In recent years, with the fast development of China's city industrialization, atmosphere pollution getting worse, air quality is further disliked
Change, not only jeopardizes the normal life of people, but also cause damages to the physical and mental health of people.The closely bound up interior with people
Air quality also makes people worried, and especially various new decorative material for building especially chemical composite materials carry greatly in recent years
The toxic gases such as formaldehyde, benzene homologues, the ammonia of amount cause serious pollution to room air, eyes are dry, skin itches, has a headache,
The malaise symptoms such as failure of memory frequently occur.How such as formaldehyde, toluene, benzene volatile organic compound are efficiently removed
As researcher's focus of attention.
Absorption method is because its method is simple and the pollution-free absorption for being widely used in pernicious gas.But most adsorbents exist
The shortcomings of adsorption efficiency is low, saturated velocity is fast or cost is higher or even some can bring secondary pollution, therefore cost effective
The research and development of scavenging material easy to use are very urgent.
Material for air purification be by the harmful substance in the modes adsorption-decomposition function air such as physics, chemistry, it is net using air
It is a kind of mode of effective control air pollution source to change material.Currently, air filting material on the market is mainly with activated carbon
It is main, but normal activated carbon, based on micropore, Surface chemical functional group of wood content is few, and polarity is small, can only carry out simple physics suction
It is attached, poor selectivity, in high temperature small to nitrogen oxides, oxysulfide, heavy metal ion isopolarity pollutant adsorption capacity in air
Pernicious gas can also be discharged, can not be locked under environment.Also, it is full that activated carbon can reach absorption after adsorbing a period of time
With also pernicious gas can be released to form secondary pollution again.Therefore, the effective storage life of activated carbon is very short, and
In many cases, the release of pernicious gas is long-term, such as the complete Form aldehyde release of interior decoration at least needs several years, even
More than ten years.
It is therefore desirable to provide a kind of novel material for air purification that there is efficient removal rate, do not cause secondary pollution, with
Solve the air quality problems increasingly paid attention to.
Invention content
Present invention mainly solves the technical issues of, be with activated carbon mainly for material for air purification at present on the market
It is main, but normal activated carbon, based on micropore, Surface chemical functional group of wood content is few, and polarity is small, can only carry out simple physics suction
It is attached, poor selectivity, in high temperature small to nitrogen oxides, oxysulfide, heavy metal ion isopolarity pollutant adsorption capacity in air
Pernicious gas can also be released under environment, can not be locked or decompose, and activated carbon meeting after adsorbing a period of time
Reach adsorption saturation, pernicious gas can again be released to the defect to form secondary pollution, provides a kind of air purification material
The preparation method of material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of material for air purification, it is characterised in that specifically preparation process is:
(1)Count in parts by weight, by 20~30 parts of halloysite nanotubes, 40~50 parts of toluene, 20~25 parts(3- mercaptopropyis)
Trimethoxy silane is placed in three-necked flask, and heat temperature raising is heated to reflux, and obtained reflux is filtered removal filtrate, separation
Solid is obtained, is dried in vacuo, obtains sulfhydrylation halloysite nanotubes;
(2)Sulfhydrylation halloysite nanotubes, hydrogen peroxide, distilled water, methanol are mixed and is placed in single port bottle, mixed liquor, room are obtained
Under temperature under conditions of magnetic agitation rotating speed is 300~400r/min oxidation reaction, then chromium trichloride is added into single port bottle, chromium
Change reaction, filtering removal filtrate obtains filter residue, is placed in vacuum drying chamber, dry, obtains catalytic nanometer tube material;
(3)Aspen fibers by using silicon powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, obtain mixed liquor, and
The pH of mixed liquor is adjusted with glacial acetic acid solution, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains comprehensive fiber
Element;
(4)With 120~150mL sodium hydroxide solutions, holocellulose is impregnated, filtering removal filtrate obtains purifying cellulose, will be pure
Cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, and wooden nano-cellulose is made;
(5)40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and the wooden nano-celluloses of 2~3g, ultrasonic disperse obtain
Cellulose suspension is placed in the conical flask with blender by cellulose suspension, is added into conical flask with dropping funel
18~20mL butyl titanates, while starting blender, start to stir, obtains mixed liquor;
(6)4~5mL acetic acid solutions, 20~30mL Ludox are added into above-mentioned mixed liquor, stirring obtains mixed sols, by 40
~45g catalytic nanometer tube materials are impregnated in mixed sols, and ageing obtains dry colloidal sol, dry colloidal sol is placed in electric furnace, micro- charcoal
Change, obtain charing blob of viscose, charing blob of viscose is put into mortar and is ground, sieving obtains material for air purification.
Step(1)Temperature is 100~110 DEG C after the heat temperature raising, be heated to reflux the time be 20~for 24 hours, vacuum is dry
Dry temperature is 70~80 DEG C.
Step(2)The sulfhydrylation halloysite nanotubes, hydrogen peroxide, distilled water, methanol mixing quality ratio are 7 ︰, 4 ︰, 5 ︰
3, hydrogen peroxide mass fraction is 30%, and oxidation time is 12~13h, and the chromium trichloride of addition is residual mixed liquor quality
10%, chromaking reacts 10~12h, and drying temperature is 70~90 DEG C, and drying time is 4~5h.
Step(3)Sodium chlorite solution's mass fraction is 20%, and the mass fraction of glacial acetic acid solution is 98%, is adjusted
The pH of mixed liquor is 4~5, and isothermal holding temperature is 75~80 DEG C, and the isothermal holding time is 5~7h.
Step(4)The sodium hydroxide solution mass fraction is 20%, and soaking temperature is 90~100 DEG C, and soaking time is
2~3h, the mass fraction of water slurry are 10~20%, and ultrasonic power is 1200~1500W, sonication treatment time is 30~
45min, control supersonic frequency are 30~35kHz.
Step(5)The supersonic frequency is 30~33kHz, and the ultrasonic disperse time is 4~6min, and speed is added dropwise in dropping funel
Rate is 2~3mL/min.
Step(6)The mass fraction of the acetic acid solution is 20%, and Ludox mass fraction is 10%, mixing time 1
~2h, digestion time are 2~3 days, and electric furnace set temperature is 200~220 DEG C, and micro- carbonization time is 2~3h, and be sieved specification is
400 mesh.
The beneficial effects of the invention are as follows:
(1)The present invention by halloysite nanotubes, toluene,(3- mercaptopropyis)Trimethoxy silane Hybrid Heating is reacted, and is dredged
Base halloysite nanotubes recycle hydrogen peroxide and methanol oxidation to dredge base halloysite nanotubes, and vacuum drying obtains sulfonated
Halloysite nanotubes add chromium trichloride chromaking and obtain catalytic nanometer tube material, and aspen fibers by using silicon powder is molten using sodium chlorite
Liquid and glacial acetic acid solution are handled, and are removed lignin under heating condition, are obtained holocellulose, by holocellulose sodium hydroxide
Solution heat-insulation soaking is separated by filtration to obtain purifying cellulose, and purifying cellulose is configured to water slurry, is ultrasonically treated, and is made
Ethyl orthosilicate is mixed with absolute ethyl alcohol, dilute hydrochloric acid acidification hydrolization is added to obtain silicon dioxide gel by wooden nano-cellulose, will
Absolute ethyl alcohol is mixed with nano-cellulose, obtains nano-cellulose suspension through ultrasonic disperse, nano-cellulose suspension is added
Enter in tetraethyl titanate, be stirred to obtain mixed liquor, acetic acid, Ludox are added dropwise into mixed liquor, stirs to get mixed sols, passes through
Cross still aging, micro- charing, grinding obtains material for air purification, nano-cellulose charing back loading is received in galapectite in the present invention
Mitron has high-specific surface area, has very strong adsorption capacity to gas trace heavy metal element and certain gas organic matters, will
After it and the nano-titanium dioxide mixing with optics catalysis characteristics, generation synergistic effect and photosensitive between meeting and titania molecule
Effect, can improve the photocatalytic activity of nano-titanium dioxide, and receptor of the nano-cellulose as electronics is easy to receive titanium dioxide
The light induced electron that titanium generates, to effectively inhibit compound, the raising photocatalytic degradation air pollutants of light induced electron and hole
Efficiency;
(2)Nano-titanium dioxide can form film in halloysite nanotubes hole in the present invention, and halloysite nanotubes can
The volatile organic contaminant fast enriching of low concentration, the organic pollution concentration on degradation nano-titanium dioxide surface is set to improve
To indoor photocatalytic oxidation efficiency, hydrogen peroxide and methanol oxidation dredge base halloysite nanotubes and keep its sulfonated, sulfonic group pair
Polar contaminants suction-operated is apparent, while halloysite nanotubes can be with the hydration of nitrogen oxides, oxysulfide using chromaking
Object is complexed, to make chromium ion in halloysite nanotubes that can improve adsorption rate in low concentration air pollutants, in addition, galapectite
Nanotube is doped in titanium dioxide forbidden band energy gap in mixed sols and narrows, and generates red shift, nano-titanium dioxide is allow to absorb wave
The light of long bigger, titanium dioxide show stronger catalytic activity under visible light, more sensitive to organic gas volatile matter, energy
Enough reduce organic pollution catalytic degradation concentration, it is often more important that the cleaning principle of material for air purification of the present invention is after first adsorbing
Degradation has the difference of essence with common active carbon purifying material, has a extensive future.
Specific implementation mode
Count in parts by weight, by 20~30 parts of halloysite nanotubes, 40~50 parts of toluene, 20~25 parts(3- mercaptopropyis)
Trimethoxy silane is placed in three-necked flask, is heated to 100~110 DEG C, it is heated to reflux 20~for 24 hours, the reflux that will be obtained
Object filtering removal filtrate, isolated solid are dried in vacuo under the conditions of being placed in 70~80 DEG C, obtain sulfhydrylation galapectite nanometer
Pipe;By sulfhydrylation halloysite nanotubes, mass fraction be 30% hydrogen peroxide, distilled water, methanol it is that 7 ︰, 4 ︰, 5 ︰ 3 are mixed in mass ratio
It is placed in single port bottle, obtains mixed liquor, at room temperature the oxidation reaction 12 under conditions of magnetic agitation rotating speed is 300~400r/min
~13h, then the chromium trichloride of residual mixed liquor quality 10% is added into single port bottle, chromaking reacts 10~12h, filtering removal filter
Liquid obtains filter residue, is placed in vacuum drying chamber, and dry 4~5h, obtains catalytic nanometer tube material under the conditions of 70~90 DEG C;It will
Aspen fibers by using silicon powder is put into beaker, and the sodium chlorite solution that 50~60mL mass fractions are 20% is added into beaker, is mixed
Liquid is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust the pH to 4~5 of mixed liquor, isothermal holding under the conditions of 75~80 DEG C
5~7h, repeats aforesaid operations 3~5 times, removes lignin, obtains holocellulose;It is 20% with 120~150mL mass fractions
Sodium hydroxide solution impregnates 2~3h of holocellulose under the conditions of 90~100 DEG C, and filtering removal filtrate obtains purifying cellulose, will
Purifying cellulose is made into the water slurry that mass fraction is 10~20%, be placed in ultrasonic wave plant cell pulverizer with 1200~
The power ultrasonic of 1500W handles 30~45min, and control supersonic frequency is 30~35kHz, and wooden nano-cellulose is made;Xiang Chao
40~50mL absolute ethyl alcohols and the wooden nano-celluloses of 2~3g are added in sound separating apparatus, is disperseed with the frequency ultrasound of 30~33kHz
4~6min obtains cellulose suspension, and cellulose suspension is placed in the conical flask with blender, with dropping funel with 2
18~20mL butyl titanates are added into conical flask for the drop rate of~3mL/min, while starting blender, with 200~
The rotating speed of 300r/min starts 10~15min of stirring, obtains mixed liquor;4~5mL mass fractions are added into above-mentioned mixed liquor is
20% acetic acid solution, the Ludox that 20~30mL mass fractions are 10%, stir 1~2h, mixed sols are obtained, by 40~45g
Catalytic nanometer tube material is impregnated in mixed sols, is aged 2~3 days, is obtained dry colloidal sol, dry colloidal sol, which is placed in set temperature, is
In 200~220 DEG C of electric furnace, 2~3h of micro- charing obtains charing blob of viscose, will charing blob of viscose be put into mortar grinding 30~
35min crosses 400 mesh and sieves to obtain material for air purification.
Example 1
Count in parts by weight, by 20 parts of halloysite nanotubes, 40 parts of toluene, 20 parts(3- mercaptopropyis)Trimethoxy silane is placed in
In three-necked flask, 100 DEG C are heated to, 20h is heated to reflux, obtained reflux is filtered into removal filtrate, it is isolated solid
Body is dried in vacuo under the conditions of being placed in 70 DEG C, obtains sulfhydrylation halloysite nanotubes;By sulfhydrylation halloysite nanotubes, quality point
Number is 30% hydrogen peroxide, distilled water, methanol are that 7 ︰, 4 ︰, 5 ︰ 3 mixing is placed in single port bottle in mass ratio, obtains mixed liquor, at room temperature
Oxidation reaction 12h under conditions of magnetic agitation rotating speed is 300r/min, then residual mixed liquor quality 10% is added into single port bottle
Chromium trichloride, chromaking react 10h, filtering removal filtrate obtain filter residue, be placed in vacuum drying chamber, in 70~90 DEG C of conditions
Lower dry 4h, obtains catalytic nanometer tube material;Aspen fibers by using silicon powder is put into beaker, 50mL mass fractions are added into beaker is
20% sodium chlorite solution, obtains mixed liquor, and the glacial acetic acid solution that mass fraction is 98% is used in combination to adjust the pH to 4 of mixed liquor,
Isothermal holding 5h under the conditions of 75 DEG C, repeats aforesaid operations 3 times, removes lignin, obtains holocellulose;With 120mL mass point
Number is 20% sodium hydroxide solution, and holocellulose 2h is impregnated under the conditions of 90 DEG C, and filtering removal filtrate obtains purifying cellulose,
Purifying cellulose is made into the water slurry that mass fraction is 10%, is placed in ultrasonic wave plant cell pulverizer with the work(of 1200W
Rate is ultrasonically treated 30min, and control supersonic frequency is 30kHz, and wooden nano-cellulose is made;40mL is added into ultrasonic disperse instrument
Absolute ethyl alcohol and the wooden nano-celluloses of 2g disperse 4min with the frequency ultrasound of 30kHz, cellulose suspension are obtained, by fiber
Plain suspension is placed in the conical flask with blender, is added into conical flask with the drop rate of 2mL/min with dropping funel
18mL butyl titanates, while starting blender, start to stir 10min with the rotating speed of 200r/min, obtains mixed liquor;To above-mentioned
The acetic acid solution that 4mL mass fractions are 20% is added in mixed liquor, the Ludox that 20mL mass fractions are 10%, stirs 1h, obtain
40g catalytic nanometer tube materials are impregnated in mixed sols by mixed sols, are aged 2 days, are obtained dry colloidal sol, dry colloidal sol is placed in
In the electric furnace that set temperature is 200 DEG C, micro- charing 2h obtains charing blob of viscose, and charing blob of viscose is put into mortar and grinds 30min,
400 mesh are crossed to sieve to obtain material for air purification.
Example 2
Count in parts by weight, by 25 parts of halloysite nanotubes, 45 parts of toluene, 23 parts(3- mercaptopropyis)Trimethoxy silane is placed in
In three-necked flask, 105 DEG C are heated to, 22h is heated to reflux, obtained reflux is filtered into removal filtrate, it is isolated solid
Body is dried in vacuo under the conditions of being placed in 75 DEG C, obtains sulfhydrylation halloysite nanotubes;By sulfhydrylation halloysite nanotubes, quality point
Number is 30% hydrogen peroxide, distilled water, methanol are that 7 ︰, 4 ︰, 5 ︰ 3 mixing is placed in single port bottle in mass ratio, obtains mixed liquor, at room temperature
Oxidation reaction 12h under conditions of magnetic agitation rotating speed is 350r/min, then residual mixed liquor quality 10% is added into single port bottle
Chromium trichloride, chromaking react 11h, filtering removal filtrate obtain filter residue, be placed in vacuum drying chamber, under the conditions of 80 DEG C do
Dry 4h obtains catalytic nanometer tube material;Aspen fibers by using silicon powder is put into beaker, it is 20% that 55mL mass fractions are added into beaker
Sodium chlorite solution, obtain mixed liquor, be used in combination mass fraction be 98% glacial acetic acid solution adjust mixed liquor pH to 4,78
Isothermal holding 6h under the conditions of DEG C, repeats aforesaid operations 4 times, removes lignin, obtains holocellulose;It is with 135mL mass fractions
20% sodium hydroxide solution impregnates holocellulose 2h under the conditions of 95 DEG C, and filtering removal filtrate obtains purifying cellulose, will be pure
Cellulose is made into the water slurry that mass fraction is 15%, is placed in ultrasonic wave plant cell pulverizer super with the power of 1350W
Sonication 37min, control supersonic frequency are 32kHz, and wooden nano-cellulose is made;It is anhydrous that 45mL is added into ultrasonic disperse instrument
Ethyl alcohol and the wooden nano-celluloses of 2g disperse 5min with the frequency ultrasound of 32kHz, obtain cellulose suspension, cellulose is hanged
Supernatant liquid is placed in the conical flask with blender, and 19mL is added into conical flask with the drop rate of 2mL/min with dropping funel
Butyl titanate, while starting blender, start to stir 13min with the rotating speed of 250r/min, obtains mixed liquor;To above-mentioned mixing
The acetic acid solution that 4mL mass fractions are 20% is added in liquid, the Ludox that 25mL mass fractions are 10%, stirs 1h, mixed
42g catalytic nanometer tube materials are impregnated in mixed sols by colloidal sol, are aged 2 days, are obtained dry colloidal sol, dry colloidal sol is placed in setting
In the electric furnace that temperature is 210 DEG C, micro- charing 2h obtains charing blob of viscose, and charing blob of viscose is put into mortar and grinds 33min, crosses 400
Mesh sieves to obtain material for air purification.
Example 3
Count in parts by weight, by 30 parts of halloysite nanotubes, 50 parts of toluene, 25 parts(3- mercaptopropyis)Trimethoxy silane is placed in
In three-necked flask, 110 DEG C are heated to, is heated to reflux for 24 hours, obtained reflux is filtered into removal filtrate, it is isolated solid
Body is dried in vacuo under the conditions of being placed in 80 DEG C, obtains sulfhydrylation halloysite nanotubes;By sulfhydrylation halloysite nanotubes, quality point
Number is 30% hydrogen peroxide, distilled water, methanol are that 7 ︰, 4 ︰, 5 ︰ 3 mixing is placed in single port bottle in mass ratio, obtains mixed liquor, at room temperature
Oxidation reaction 13h under conditions of magnetic agitation rotating speed is 400r/min, then residual mixed liquor quality 10% is added into single port bottle
Chromium trichloride, chromaking react 12h, filtering removal filtrate obtain filter residue, be placed in vacuum drying chamber, under the conditions of 90 DEG C do
Dry 5h obtains catalytic nanometer tube material;Aspen fibers by using silicon powder is put into beaker, it is 20% that 60mL mass fractions are added into beaker
Sodium chlorite solution, obtain mixed liquor, be used in combination mass fraction be 98% glacial acetic acid solution adjust mixed liquor pH to 5,80
Isothermal holding 7h under the conditions of DEG C, repeats aforesaid operations 5 times, removes lignin, obtains holocellulose;It is with 150mL mass fractions
20% sodium hydroxide solution impregnates holocellulose 3h under the conditions of 100 DEG C, and filtering removal filtrate obtains purifying cellulose, will be pure
Cellulose is made into the water slurry that mass fraction is 20%, is placed in ultrasonic wave plant cell pulverizer super with the power of 1500W
Sonication 45min, control supersonic frequency are 35kHz, and wooden nano-cellulose is made;It is anhydrous that 50mL is added into ultrasonic disperse instrument
Ethyl alcohol and the wooden nano-celluloses of 3g disperse 6min with the frequency ultrasound of 33kHz, obtain cellulose suspension, cellulose is hanged
Supernatant liquid is placed in the conical flask with blender, and 20mL is added into conical flask with the drop rate of 3mL/min with dropping funel
Butyl titanate, while starting blender, start to stir 15min with the rotating speed of 300r/min, obtains mixed liquor;To above-mentioned mixing
The acetic acid solution that 5mL mass fractions are 20% is added in liquid, the Ludox that 30mL mass fractions are 10%, stirs 2h, mixed
45g catalytic nanometer tube materials are impregnated in mixed sols by colloidal sol, are aged 3 days, are obtained dry colloidal sol, dry colloidal sol is placed in setting
In the electric furnace that temperature is 220 DEG C, micro- charing 3h obtains charing blob of viscose, and charing blob of viscose is put into mortar and grinds 35min, crosses 400
Mesh sieves to obtain material for air purification.
Comparative example
With the material for air purification of company of Nanning City production as a comparison case to material for air purification produced by the present invention and right
Material for air purification in ratio is detected, and testing result is as shown in table 1:
The removal effect that reference standard QB/T2761-2006 carries out organic gas is detected.
Formaldehyde absorbing efficiency test
Static test is carried out by pollutant of formaldehyde.Experimental condition is:Initial concentration of formaldehyde is 1.5 ± 0.2ppm, and test specimens are
200g, glass test chamber volume are 1m3, tested using methylene oxide detecting instrument.
Antibiotic property is tested
Using the material for air purification in material for air purification produced by the present invention and comparative example, its dust mite inhibiting rate is tested respectively
And the antimicrobial efficiency to Escherichia coli and staphylococcus aureus.
1 performance measurement result of table
According to data in table 1 it is found that material for air purification produced by the present invention, has excellent air purification performance, to harmful
Gas absorption capacity is big, purifying rate is high, purification speed is fast, persistence is good, and does not generate secondary pollution, the scope of application to environment
Extensively, flexible and convenient to use, wide market.
Claims (7)
1. a kind of preparation method of material for air purification, it is characterised in that specifically preparation process is:
(1)Count in parts by weight, by 20~30 parts of halloysite nanotubes, 40~50 parts of toluene, 20~25 parts(3- mercaptopropyis)
Trimethoxy silane is placed in three-necked flask, and heat temperature raising is heated to reflux, and obtained reflux is filtered removal filtrate, separation
Solid is obtained, is dried in vacuo, obtains sulfhydrylation halloysite nanotubes;
(2)Sulfhydrylation halloysite nanotubes, hydrogen peroxide, distilled water, methanol are mixed and is placed in single port bottle, mixed liquor, room are obtained
Under temperature under conditions of magnetic agitation rotating speed is 300~400r/min oxidation reaction, then chromium trichloride is added into single port bottle, chromium
Change reaction, filtering removal filtrate obtains filter residue, is placed in vacuum drying chamber, dry, obtains catalytic nanometer tube material;
(3)Aspen fibers by using silicon powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, obtain mixed liquor, and
The pH of mixed liquor is adjusted with glacial acetic acid solution, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains comprehensive fiber
Element;
(4)With 120~150mL sodium hydroxide solutions, holocellulose is impregnated, filtering removal filtrate obtains purifying cellulose, will be pure
Cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer and is ultrasonically treated, and wooden nano-cellulose is made;
(5)40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and the wooden nano-celluloses of 2~3g, ultrasonic disperse obtain
Cellulose suspension is placed in the conical flask with blender by cellulose suspension, is added into conical flask with dropping funel
18~20mL butyl titanates, while starting blender, start to stir, obtains mixed liquor;
(6)4~5mL acetic acid solutions, 20~30mL Ludox are added into above-mentioned mixed liquor, stirring obtains mixed sols, by 40
~45g catalytic nanometer tube materials are impregnated in mixed sols, and ageing obtains dry colloidal sol, dry colloidal sol is placed in electric furnace, micro- charcoal
Change, obtain charing blob of viscose, charing blob of viscose is put into mortar and is ground, sieving obtains material for air purification.
2. a kind of preparation method of material for air purification according to claim 1, it is characterised in that:Step(1)Described
After heat temperature raising temperature be 100~110 DEG C, be heated to reflux the time be 20~for 24 hours, vacuum drying temperature be 70~80 DEG C.
3. a kind of preparation method of material for air purification according to claim 1, it is characterised in that:Step(2)Described
Sulfhydrylation halloysite nanotubes, hydrogen peroxide, distilled water, methanol mixing quality ratio are 7 ︰, 4 ︰, 5 ︰ 3, and hydrogen peroxide mass fraction is 30%,
Oxidation time is 12~13h, and the chromium trichloride of addition is residual mixed liquor quality 10%, and chromaking reacts 10~12h, dry
Temperature is 70~90 DEG C, and drying time is 4~5h.
4. a kind of preparation method of material for air purification according to claim 1, it is characterised in that:Step(3)Described
Sodium chlorite solution's mass fraction is 20%, and the mass fraction of glacial acetic acid solution is 98%, and the pH for adjusting mixed liquor is 4~5, heat preservation
Treatment temperature is 75~80 DEG C, and the isothermal holding time is 5~7h.
5. a kind of preparation method of material for air purification according to claim 1, it is characterised in that:Step(4)Described
Sodium hydroxide solution mass fraction is 20%, and soaking temperature is 90~100 DEG C, and soaking time is 2~3h, the quality of water slurry
Score is 10~20%, and ultrasonic power is 1200~1500W, and sonication treatment time is 30~45min, and control supersonic frequency is 30
~35kHz.
6. a kind of preparation method of material for air purification according to claim 1, it is characterised in that:Step(5)Described
Supersonic frequency is 30~33kHz, and the ultrasonic disperse time is 4~6min, and dropping funel drop rate is 2~3mL/min.
7. a kind of preparation method of material for air purification according to claim 1, it is characterised in that:Step(6)Described
The mass fraction of acetic acid solution is 20%, and Ludox mass fraction is 10%, and mixing time is 1~2h, and digestion time is 2~3 days,
Electric furnace set temperature is 200~220 DEG C, and micro- carbonization time is 2~3h, and be sieved specification is 400 mesh.
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