CN107980772A - A kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent - Google Patents
A kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent Download PDFInfo
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- CN107980772A CN107980772A CN201711083317.6A CN201711083317A CN107980772A CN 107980772 A CN107980772 A CN 107980772A CN 201711083317 A CN201711083317 A CN 201711083317A CN 107980772 A CN107980772 A CN 107980772A
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- smell agent
- eliminating smell
- diatomite
- time
- bacteriostatic
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- 238000001816 cooling Methods 0.000 title claims abstract description 25
- 230000003385 bacteriostatic effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 51
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002893 slag Substances 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 14
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 14
- 241000894006 Bacteria Species 0.000 claims abstract description 11
- 230000007062 hydrolysis Effects 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 10
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 239000012065 filter cake Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000005554 pickling Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 235000010215 titanium dioxide Nutrition 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003837 high-temperature calcination Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 5
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000002950 deficient Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 230000001408 fungistatic effect Effects 0.000 abstract description 2
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 229910052720 vanadium Inorganic materials 0.000 abstract description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008676 import Effects 0.000 abstract 1
- 230000000505 pernicious effect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 14
- 235000019256 formaldehyde Nutrition 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 230000003466 anti-cipated effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 102000016938 Catalase Human genes 0.000 description 1
- 108010053835 Catalase Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010276 construction Methods 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
- 238000001514 detection method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000001257 hydrogen Chemical group 0.000 description 1
- 229910052739 hydrogen Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003641 microbiacidal effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Environmental Sciences (AREA)
- Zoology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Biomedical Technology (AREA)
- Toxicology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent, belong to eliminating smell agent preparing technical field.The present invention is acidified to obtain titanium tetrachloride solution with high titanium slag, crystal seed is used as by the use of a small amount of rutile titanium dioxide, hydrolysis generation nano-titanium dioxide, nano-titanium dioxide mixes scattered with diatomite suspension after modified, be made gel, calcining obtain it is antibacterial with de-tasting permanent seal cooling eliminating smell agent, when bacterium and pernicious gas Molecular Adsorption are on its surface, chain type degradation reaction will occur, play fungistatic effect；Nano-titanium dioxide with photocatalysis is the key component of bacteriostasis, the doping of vanadium can import defective locations in nano-titanium dioxide lattice or change crystal structure degree in ammonium vanadate, effectively nano-titanium dioxide can be modified, make nano-titanium dioxide existence time in diatomite lasting, so as to which that improves eliminating smell agent de-tastes durability, have a extensive future.
Description
Technical field
The invention discloses a kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent, belongs to eliminating smell agent technology of preparing neck
Domain.
Background technology
The taste removal principle of eliminating smell agent is to be present in high humility（95-100%）Stench particle in air or water is by hydrone quilt
Film is surrounded, and deodorization at this time must destroy the envelope of hydrone, be caught by its stench particle, and the oiliness grain particle of dry and wet
Then ineffective for this, deodorization liquid is natural botanical extraction liquid, and the complex of peptide and ferment component, is biological catalase system
System.
Eliminating smell agent is a kind of cleaning products for being used for removing peculiar smell in local space.For the water-based system containing hydrogen sulfide
In, main component is low polymer, it with hydrogen sulfide, mercaptan by chemically reacting.Eliminating smell agent mainly has following several
Type：Physics eliminating smell agent, chemistry eliminating smell agent, microbiocidal eliminating smell agent, plant type eliminating smell agent and compound eliminating smell agent etc..Physics
Eliminating smell agent is eliminated the unusual smell by physical method, using the physical property of eliminating smell agent or gas with foreign flavor, does not change gas group
Point as a result, only change its local concentration, or perhaps relative concentration.It common are absorption eliminating smell agent, cover eliminating smell agent etc..Change
Eliminating smell agent is learned using oxidation, reduction decomposition, neutralization reaction, addition reaction, condensation reaction, ion-exchange reactions etc. by generation
Smell substance is changed into free from extraneous odour material so as to eliminate peculiar smell.
Eliminating smell agent can be used for the exceeded plate of artificial liner enterprise processing burst size of methanal；Handled available for carpet weaving mill containing formaldehyde
Gum；The wood-based plate produced with three-aldehyde glue is anticipated available for Furniture Factory；Anticipated available for house ornamentation engineering poisonous artificial
Plate, implements green home decoration engineering；Furniture for sale is handled available for furniture shop, is allowed to innoxious；Contain formaldehyde available for processing
Adhesive；Available for eliminate new purchase furniture, family, office and public place because finishing and caused by formaldehyde pollution, remove
Formaldehyde peculiar smell.
Though eliminating smell agent can remove peculiar smell, bactericidal effect is preferable not enough, can not maintain much time using, because
This, invent a kind of bacteriostatic and odour removing permanent seal cooling eliminating smell agent has positive effect to eliminating smell agent preparing technical field.
The content of the invention
Present invention mainly solves technical problem, poor for eliminating smell agent biocidal property, the unendurable defect of taste removal effect, carries
A kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent is supplied.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent, it is characterised in that specifically preparation process is：
（1）100~120g high titanium slags and 30~40g sodium acid carbonates are weighed, is placed in resistance furnace, power-up procedure heating, high temperature is forged
Burn, after cooled to room temperature, obtain light-burned high titanium slag, light-burned high titanium slag is placed in the three-necked flask with blender, to
Three-necked flask adds 200~220mL hydrochloric acid, starts blender, is stirred, and stands, and filters, removal residue, and isolated four
Titanium chloride solution；
（2）The above-mentioned titanium tetrachloride solutions of 100~120mL are added to the three-necked flask with reflux and blender, startup is stirred
Mix device to stir, after heat temperature raising, add 5~8g rutile titanium dioxides to three-necked flask, continue to heat up, hydrolysis, goes out
Material, obtains nano-titanium dioxide；
（3）Weigh 40~50g diatomite and add in ball mill and wash mill, wash after the completion of mill, powder in ball mill is outwelled, then to ball
100~110g diatomite is added in grinding machine, grinding, sieving obtains diatomite powder, by diatomite powder and 200~250mL sulphur
Acid solution mixes, and is stirred under room temperature, and filtering removes filtrate, obtains filter cake, filter cake is washed with deionized, by the filter after washing
Cake is placed in baking oven, heat temperature raising, obtains the diatomite of pickling drying；
（4）The diatomite that 50~70g pickling is dried is placed in beaker, 90~100mL absolute ethyl alcohols is added to beaker, is stirred
Afterwards, after adding 10~15g butyl titanates into beaker, with magnetic stirrer, diatomite suspension is obtained；
（5）8~10g ammonium vanadate is added in 100~110mL hydrochloric acid, mixed liquor is obtained, mixed liquor is ultrasonically treated, by weight
70~80 parts of diatomite suspension, 20~25 nano-titanium dioxides, 30~40 portions of mixed liquors are placed in high speed dispersor by number meter
In, high speed dispersion, obtains pre-dispersed material；
（6）Gel is formed after pre-dispersed material is stood, then gel ageing is placed in drying baker, heat temperature raising is dry, obtains
Gel solids, gel solids are placed in Muffle furnace, heat temperature raising, and calcining, cooled to room temperature, discharging, is pressed down
Bacterium de-tastes permanent seal cooling eliminating smell agent.
Step（1）Temperature is 1200~1250 DEG C after described power-up procedure heating, and the high-temperature calcination time is 2~3h, salt
The mass fraction of acid is 20%, and speed of agitator is 400~420r/min, and it is 1.0~1.5h to be stirred the time, and quiescent time is
10~12h.
Step（2）The speed of agitator is 250~270r/min, and temperature is 70~80 DEG C after heat temperature raising, continue plus
Temperature is 110~120 DEG C after heat heating, and hydrolysis time is 1.5~2.0h.
Step（3）Described to wash time consuming be 2.5~3.0h, and drum's speed of rotation is 50~60r/min, milling time 3
~4h, specification of sieving are 200 mesh, and the mass fraction of sulfuric acid solution is 40%, and mixing time is 6~7h, and deionized water washing is secondary
Number is 3~5 times, and temperature is 80~85 DEG C after heat temperature raising.
Step（4）The time that is stirred is 10~15min, and magnetic stirring apparatus rotating speed is 700~800r/min, is stirred
It is 30~35min to mix the time.
Step（5）The mass fraction of the hydrochloric acid is 15%, and sonication treatment time is 20~30min, controls supersonic frequency
For 30~32KHz, high speed dispersor rotating speed is 4500~4800r/min, and the high speed dispersion time is 18~20min.
Step（6）The time of repose is 3~4h, and gel digestion time is 10~12h, temperature after baking oven heat temperature raising
For 80~90 DEG C, drying time is 5~7h, and temperature is 540~560 DEG C after Muffle furnace heat temperature raising, and calcination time is 3~4h.
The beneficial effects of the invention are as follows：
（1）The present invention is acidified to obtain titanium tetrachloride solution with high titanium slag, and crystal seed, hydrolysis are used as by the use of a small amount of rutile titanium dioxide
Nano-titanium dioxide is generated, nano-titanium dioxide is mixed with diatomite suspension after modified to be disperseed, and gel is made, calcining obtains
Bacteriostatic and odour removing permanent seal cooling eliminating smell agent, under the conditions of light irradiation, electronics will be excited and enter and lead in nano-titanium dioxide valence band
Band, and form the electronics of electronegativity and high activity, meanwhile, the hole of positively charged is formd in valence band because losing electronics,
Form electron-hole pair, this electron-hole pair is otherwise known as photo-generated carrier, and carrier can be with quickly after producing
Speed is moved to its surface, and the oxygen and hydrone of activated surface absorption, produces living radical and active oxygen, when bacterium and has
Evil gas molecule absorption will occur chain type degradation reaction, play fungistatic effect at its surface；
（2）The present invention has the key component that the nano-titanium dioxide of photocatalysis is bacteriostasis, and vanadium mixes in ammonium vanadate
It is miscellaneous that defective locations can be imported in nano-titanium dioxide lattice or change crystal structure degree, can be effectively to nano-titanium dioxide
It is modified, under the action of illumination, it is larger to adulterate the concentration of electronics, its spectral response can be made to visible ray by reducing band gap
Direction is moved, and efficiently separates photo-generate electron-hole pair, therefore doped metal ion improves the catalytic activity of titanium dioxide
With the utilization rate of light, make the taste removal time more longlasting, diatomite is the carrier of nano-titanium dioxide, has special porosity construction,
Specific surface area is big, and there are many silicone hydroxyls and hydrogen bond in surface, it can form powerful combination between titania nanoparticles
Can, it can suppress gathering and protecting titanium dioxide to make it be not flushed away in running system for titanium dioxide, make nanometer two
Titanium oxide existence time in diatomite is lasting, and diatomite is the good prize body of photohole, to the invalid of electron-hole pair
It is compound to play inhibitory action, so that improves eliminating smell agent de-tastes durability, have a extensive future.
Embodiment
100~120g high titanium slags and 30~40g sodium acid carbonates are weighed, is placed in resistance furnace, power-up procedure is warming up to 1200
~1250 DEG C, 2~3h of high-temperature calcination, after cooled to room temperature, light-burned high titanium slag is obtained, light-burned high titanium slag is placed in stirring
In the three-necked flask for mixing device, the hydrochloric acid that 200~220mL mass fractions are 20% is added to three-necked flask, starts blender, with 400
The rotating speed of~420r/min is stirred 1.0~1.5h, stands 10~12h, filters, and removes residue, isolated titanium tetrachloride
Solution；The above-mentioned titanium tetrachloride solutions of 100~120mL are added to the three-necked flask with reflux and blender, start stirring
Device, is stirred with the rotating speed of 250~270r/min, and after being heated to 70~80 DEG C, 5~8g rutile-types are added to three-necked flask
Titanium dioxide, is continuously heating to 110~120 DEG C, 1.5~2.0h of hydrolysis, discharging, obtains nano-titanium dioxide；Weigh 40
~50g diatomite adds in ball mill and washes 2.5~3.0h of mill, washes after the completion of mill, powder in ball mill is outwelled, then to ball mill
Middle addition 100~110g diatomite, 3~4h is ground with the rotating speed of 50~60r/min, is crossed 200 mesh sieves and is obtained diatomite powder, will
Diatomite powder is mixed with 200~250mL mass fractions for 40% sulfuric acid solution, and 6~7h is stirred under room temperature, and filtering removes filtrate,
Filter cake is obtained, filter cake is washed with deionized 3~5 times, the filter cake after washing is placed in baking oven, is heated to 80~85
DEG C, obtain the diatomite of pickling drying；The diatomite that 50~70g pickling is dried is placed in beaker, 90~100mL is added to beaker
Absolute ethyl alcohol, after being stirred 10~15min, after adding 10~15g butyl titanates into beaker, with magnetic stirring apparatus with 700
The rotating speed of~800r/min stirs 30~35min, obtains diatomite suspension；8~10g ammonium vanadate is added into 100~110mL matter
Measure fraction be 15% hydrochloric acid in, obtain mixed liquor, by mixed liquor be ultrasonically treated 20~30min, control supersonic frequency be 30~
32KHz, counts put 70~80 parts of diatomite suspension, 20~25 nano-titanium dioxides, 30~40 portions of mixed liquors in parts by weight
In high speed dispersor, with the rotating speed of 4500~4800r/min, 18~20min of high speed dispersion, obtains pre-dispersed material；It will divide in advance
Bulk cargo forms gel after standing 3~4h, then gel is aged 10~12h and is placed in drying baker, is heated to 80~90 DEG C,
Dry 5~7h, obtains gel solids, gel solids is placed in Muffle furnace, is heated to 540~560 DEG C, calcining 3
~4h, cooled to room temperature, discharging, obtains bacteriostatic and odour removing permanent seal cooling eliminating smell agent.
Example 1
100g high titanium slags and 30g sodium acid carbonates are weighed, is placed in resistance furnace, power-up procedure is warming up to 1200 DEG C, high-temperature calcination 2h,
After cooled to room temperature, light-burned high titanium slag is obtained, light-burned high titanium slag is placed in the three-necked flask with blender, Xiang Sankou
Flask adds the hydrochloric acid that 200mL mass fractions are 20%, starts blender, 1.0h is stirred with the rotating speed of 400r/min, stands
10h, filters, and removes residue, isolated titanium tetrachloride solution；Added to the three-necked flask with reflux and blender
The above-mentioned titanium tetrachloride solutions of 100mL, start blender, are stirred with the rotating speed of 250r/min, after being heated to 70 DEG C, Xiang Sankou
Flask adds 5g rutile titanium dioxides, is continuously heating to 110 DEG C, hydrolysis 1.5h, discharging, obtains nanometer titanium dioxide
Titanium；Weigh 40g diatomite and add in ball mill and wash mill 2.5h, wash after the completion of mill, powder in ball mill is outwelled, then to ball mill
Middle addition 100g diatomite, 3h is ground with the rotating speed of 50r/min, is crossed 200 mesh sieves and is obtained diatomite powder, by diatomite powder with
200mL mass fractions mix for 40% sulfuric acid solution, and 6h is stirred under room temperature, and filtering removes filtrate, obtains filter cake, filter cake is spent
Ion water washing 3 times, the filter cake after washing is placed in baking oven, is heated to 80 DEG C, obtains the diatomite of pickling drying；Will
The diatomite of 50g pickling drying is placed in beaker, and 90mL absolute ethyl alcohols are added to beaker, after being stirred 10min, adds into beaker
After entering 10g butyl titanates, 30min is stirred with the rotating speed of 700min with magnetic stirring apparatus, obtains diatomite suspension；By 8g vanadic acid
Ammonium is added in the hydrochloric acid that 100mL mass fractions are 15%, obtains mixed liquor, and mixed liquor is ultrasonically treated 20min, controls supersonic frequency
Rate is 30KHz, counts 70 parts of diatomite suspension, 20 nano-titanium dioxides, 30 portions of mixed liquors being placed in parts by weight and divides at a high speed
Dissipate in machine, with the rotating speed of 4500r/min, high speed dispersion 18min, obtains pre-dispersed material；Formation is solidifying after pre-dispersed material is stood 3h
Glue, then gel ageing 10h is placed in drying baker, 80 DEG C are heated to, dry 5h, obtains gel solids, gel is consolidated
Body is placed in Muffle furnace, is heated to 540 DEG C, calcines 3h, cooled to room temperature, discharging, it is resistance to obtain bacteriostatic and odour removing
Long type eliminating smell agent.
Example 2
110g high titanium slags and 35g sodium acid carbonates are weighed, is placed in resistance furnace, power-up procedure is warming up to 1220, high-temperature calcination 2.5h,
After cooled to room temperature, light-burned high titanium slag is obtained, light-burned high titanium slag is placed in the three-necked flask with blender, Xiang Sankou
Flask adds the hydrochloric acid that 210mL mass fractions are 20%, starts blender, 1.2h is stirred with the rotating speed of 410r/min, stands
11h, filters, and removes residue, isolated titanium tetrachloride solution；Added to the three-necked flask with reflux and blender
The above-mentioned titanium tetrachloride solutions of 110mL, start blender, are stirred with the rotating speed of 260r/min, after being heated to 75 DEG C, Xiang Sankou
Flask adds 6g rutile titanium dioxides, is continuously heating to 115 DEG C, hydrolysis 1.7h, discharging, obtains nanometer titanium dioxide
Titanium；Weigh 45g diatomite and add in ball mill and wash mill 2.7, wash after the completion of mill, powder in ball mill is outwelled, then to ball mill
Middle addition 105g diatomite, 3.5h is ground with the rotating speed of 55r/min, is crossed 200 mesh sieves and is obtained diatomite powder, by diatomite powder
Mixed with 225mL mass fractions for 40% sulfuric acid solution, 6.5h is stirred under room temperature, filtering removes filtrate, filter cake obtained, by filter cake
It is washed with deionized 4 times, the filter cake after washing is placed in baking oven, be heated to 82 DEG C, obtains the diatom of pickling drying
Soil；The diatomite that 60g pickling is dried is placed in beaker, 95mL absolute ethyl alcohols are added to beaker, after being stirred 12min, to burning
After adding 12g butyl titanates in cup, 32min is stirred with the rotating speed of 750r/min with magnetic stirring apparatus, obtains diatomite suspension；
9g ammonium vanadate is added in the hydrochloric acid that 105mL mass fractions are 15%, obtain mixed liquor, mixed liquor is ultrasonically treated 25min, controlled
Supersonic frequency processed is 31KHz, counts put 75 parts of diatomite suspension, 22 nano-titanium dioxides, 35 portions of mixed liquors in parts by weight
In high speed dispersor, with the rotating speed of 4600r/min, high speed dispersion 19min, obtains pre-dispersed material；Pre-dispersed material is stood
Gel is formed after 3.5h, then gel ageing 11h is placed in drying baker, is heated to 85 DEG C, dry 6h, obtains gel and consolidate
Body, gel solids are placed in Muffle furnace, are heated to 550 DEG C, calcine 3.5h, cooled to room temperature, discharging, obtains
To bacteriostatic and odour removing permanent seal cooling eliminating smell agent.
Example 3
120g high titanium slags and 40g sodium acid carbonates are weighed, is placed in resistance furnace, power-up procedure is warming up to 1250 DEG C, high-temperature calcination 3h,
After cooled to room temperature, light-burned high titanium slag is obtained, light-burned high titanium slag is placed in the three-necked flask with blender, Xiang Sankou
Flask adds the hydrochloric acid that 220mL mass fractions are 20%, starts blender, 1.2h is stirred with the rotating speed of 420r/min, stands
11h, filters, and removes residue, isolated titanium tetrachloride solution；Added to the three-necked flask with reflux and blender
The above-mentioned titanium tetrachloride solutions of 110mL, start blender, are stirred with the rotating speed of 260r/min, after being heated to 75 DEG C, Xiang Sankou
Flask adds 6g rutile titanium dioxides, is continuously heating to 115 DEG C, hydrolysis 1.7h, discharging, obtains nanometer titanium dioxide
Titanium；Weigh 45g diatomite and add in ball mill and wash mill 2.7h, wash after the completion of mill, powder in ball mill is outwelled, then to ball mill
Middle addition 110g diatomite, 4h is ground with the rotating speed of 60r/min, is crossed 200 mesh sieves and is obtained diatomite powder, by diatomite powder with
250mL mass fractions mix for 40% sulfuric acid solution, and 7h is stirred under room temperature, and filtering removes filtrate, obtains filter cake, filter cake is spent
Ion water washing 5 times, the filter cake after washing is placed in baking oven, is heated to 85 DEG C, obtains the diatomite of pickling drying；Will
The diatomite of 70g pickling drying is placed in beaker, 100mL absolute ethyl alcohols is added to beaker, after being stirred 15min, into beaker
After adding 15g butyl titanates, 35min is stirred with the rotating speed of 800r/min with magnetic stirring apparatus, obtains diatomite suspension；Will
10g ammonium vanadate is added in the hydrochloric acid that 110mL mass fractions are 15%, obtains mixed liquor, mixed liquor is ultrasonically treated 30min, is controlled
Supersonic frequency is 32KHz, counts be placed in 80 parts of diatomite suspension, 25 nano-titanium dioxides, 40 portions of mixed liquors in parts by weight
In high speed dispersor, with the rotating speed of 4800r/min, high speed dispersion 20min, obtains pre-dispersed material；After pre-dispersed material is stood 4h
Gel is formed, then gel ageing 12h is placed in drying baker, is heated to 90 DEG C, dry 7h, obtains gel solids, will
Gel solids are placed in Muffle furnace, are heated to 560 DEG C, calcine 4h, cooled to room temperature, discharging, obtains antibacterial
De-taste permanent seal cooling eliminating smell agent.
Comparative example
It is resistance to bacteriostatic and odour removing produced by the present invention as a comparison case with the bacteriostatic and odour removing permanent seal cooling eliminating smell agent that Shandong company produces
Bacteriostatic and odour removing permanent seal cooling eliminating smell agent in long type eliminating smell agent and comparative example carries out performance detection, and testing result is as shown in table 1：
1st, test method：
Removal of bacteria rate and de-taste endurance performance testing method：Eliminating smell agent in the example 1~3 and comparative example of equivalent is sprayed respectively
Spill into four identical rooms just fitted up, measure the bacterial concentration m in room when four rooms have just been fitted up first1,
Measured again every 1 month sprinkling eliminating smell agent back room between bacterial concentration m2；
Removal of bacteria rate computational methods：A=m2/m1×100%
Note：A is removal of bacteria rate；
m1Bacterial concentration during just to have fitted up in room；
m2To measure bacterial concentration between sprinkling eliminating smell agent back room every 1 month.
Table 1
According to above-mentioned middle data, the removal of bacteria rate of bacteriostatic and odour removing permanent seal cooling eliminating smell agent produced by the present invention is high, after 3 months
Removal of bacteria rate reach more than 96%, it is and in rising trend, there is no peculiar smell after 2 months, and do not have after 3 months yet, de-taste
Endurance quality is good, and the eliminating smell agent in comparative example will become apparent from carrying out removal of bacteria rate constantly declining, and value has reached 84% after 3 months,
Removal of bacteria rate is low, and still has peculiar smell generation after 3 months, and it is bad to de-taste durability, therefore, produced by the present invention antibacterial to go
Taste permanent seal cooling eliminating smell agent has broad application prospects.
Claims (7)
1. a kind of preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent, it is characterised in that specifically preparation process is：
（1）100~120g high titanium slags and 30~40g sodium acid carbonates are weighed, is placed in resistance furnace, power-up procedure heating, high temperature is forged
Burn, after cooled to room temperature, obtain light-burned high titanium slag, light-burned high titanium slag is placed in the three-necked flask with blender, to
Three-necked flask adds 200~220mL hydrochloric acid, starts blender, is stirred, and stands, and filters, removal residue, and isolated four
Titanium chloride solution；
（2）The above-mentioned titanium tetrachloride solutions of 100~120mL are added to the three-necked flask with reflux and blender, startup is stirred
Mix device to stir, after heat temperature raising, add 5~8g rutile titanium dioxides to three-necked flask, continue to heat up, hydrolysis, goes out
Material, obtains nano-titanium dioxide；
（3）Weigh 40~50g diatomite and add in ball mill and wash mill, wash after the completion of mill, powder in ball mill is outwelled, then to ball
100~110g diatomite is added in grinding machine, grinding, sieving obtains diatomite powder, by diatomite powder and 200~250mL sulphur
Acid solution mixes, and is stirred under room temperature, and filtering removes filtrate, obtains filter cake, filter cake is washed with deionized, by the filter after washing
Cake is placed in baking oven, heat temperature raising, obtains the diatomite of pickling drying；
（4）The diatomite that 50~70g pickling is dried is placed in beaker, 90~100mL absolute ethyl alcohols is added to beaker, is stirred
Afterwards, after adding 10~15g butyl titanates into beaker, with magnetic stirrer, diatomite suspension is obtained；
（5）8~10g ammonium vanadate is added in 100~110mL hydrochloric acid, mixed liquor is obtained, mixed liquor is ultrasonically treated, by weight
70~80 parts of diatomite suspension, 20~25 nano-titanium dioxides, 30~40 portions of mixed liquors are placed in high speed dispersor by number meter
In, high speed dispersion, obtains pre-dispersed material；
（6）Gel is formed after pre-dispersed material is stood, then gel ageing is placed in drying baker, heat temperature raising is dry, obtains
Gel solids, gel solids are placed in Muffle furnace, heat temperature raising, and calcining, cooled to room temperature, discharging, is pressed down
Bacterium de-tastes permanent seal cooling eliminating smell agent.
A kind of 2. preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent according to claim 1, it is characterised in that：Step
（1）Temperature is 1200~1250 DEG C after described power-up procedure heating, and the high-temperature calcination time is 2~3h, the mass fraction of hydrochloric acid
For 20%, speed of agitator is 400~420r/min, and it is 1.0~1.5h to be stirred the time, and quiescent time is 10~12h.
A kind of 3. preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent according to claim 1, it is characterised in that：Step
（2）The speed of agitator is 250~270r/min, and temperature is 70~80 DEG C after heat temperature raising, continues temperature after heat temperature raising
For 110~120 DEG C, hydrolysis time is 1.5~2.0h.
A kind of 4. preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent according to claim 1, it is characterised in that：Step
（3）The time consuming of washing is 2.5~3.0h, and drum's speed of rotation is 50~60r/min, and milling time is 3~4h, rule of sieving
Lattice are 200 mesh, and the mass fraction of sulfuric acid solution is 40%, and mixing time is 6~7h, and deionized water washing times are 3~5 times, are added
Temperature is 80~85 DEG C after heat heating.
A kind of 5. preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent according to claim 1, it is characterised in that：Step
（4）Described to be stirred the time be 10~15min, and magnetic stirring apparatus rotating speed is 700~800r/min, mixing time for 30~
35min。
A kind of 6. preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent according to claim 1, it is characterised in that：Step
（5）The mass fraction of the hydrochloric acid is 15%, and sonication treatment time is 20~30min, and it is 30~32KHz to control supersonic frequency,
High speed dispersor rotating speed is 4500~4800r/min, and the high speed dispersion time is 18~20min.
A kind of 7. preparation method of bacteriostatic and odour removing permanent seal cooling eliminating smell agent according to claim 1, it is characterised in that：Step
（6）The time of repose is 3~4h, and gel digestion time is 10~12h, and temperature is 80~90 DEG C after baking oven heat temperature raising,
Drying time is 5~7h, and temperature is 540~560 DEG C after Muffle furnace heat temperature raising, and calcination time is 3~4h.
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