CN106519846B - A kind of preparation method of antibacterial interior wall nano-latex - Google Patents
A kind of preparation method of antibacterial interior wall nano-latex Download PDFInfo
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Abstract
This patent belongs to paint field, specifically discloses a kind of preparation method of antibacterial interior wall nano-latex, prepares the precursor colloids solution of silver/titanium dioxide nanotube first；After electrostatic spinning, the precursor product that spinning obtains is cooled down immediately, is subsequently placed in Muffle furnace, heat preservation sintering obtains silver/titanium dioxide nanotube；It takes above-mentioned silver/titanium dioxide nanotube to be dispersed in water under agitation, propylene glycol, coalescing agent, wetting agent, preservative, hydroxyethyl cellulose, dispersing agent is added, is uniformly mixed in grinder；Then titanium dioxide, coarse whiting, kaolin, talcum powder is added, after sufficiently grinding in high-speed grinder, acrylic emulsion, defoaming agent, thickener is added；Mixing is finally stirred evenly in grinder, finally filters barrelling, obtains antibacterial interior wall nano-latex finished product.Purpose is to solve the problem of room inner wall surface bacteria breed and wet weather is long that interior wall is caused to mildew.
Description
Technical field
The present invention relates to paint fields, and in particular to a kind of preparation method of antibacterial interior wall nano-latex.
Background technique
Chinese paint industry grows stronger day by day under the promotion of building trade.Statistical data shows that Chinese architecture applied in 2011
Material amounts to about 351.82 ten thousand tons of yield, increases by 30% or more on a year-on-year basis.It follows that although Chinese architecture paint industry experienced
The influence of global financial crisis in 2008, prices of raw materials rise bring pressure, but its growth momentum does not subtract still, and also
Remain higher growth rate.
Interior wall coating is the indispensable material of house decoration, now with the enhancing of people's environmental consciousness, to for decoration interior
The requirement of wall latex paint is higher and higher, and the relatively high polyvinyl formal class coating of Form aldehyde release is gradually eliminated, respectively
Kind of release anion, low VOC Environment-friendlyinternal internal wall paint using more and more, into major step in terms of health type and environmental protection,
The problem of how to develop the coating of health environment-friendly becomes people's growing interest.Especially in recent years, with people's living standard
Continuous improvement, the continuous improvement of living conditions, requirement to coating is also not only to achieve the effect that beautiful decoration, it is also necessary to
It is special to have the function of, to improve itself living environment quality.
One investigation of living environment microbes contamination shows that cities and towns total number of bacteria is 72.10cfu/cm2.It can be seen that
Pollution caused by microorganism is very important in living environment, and in moist south, and it is also very urgently that interior wall, which mildews,
The technical issues of solution.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of antibacterial interior wall nano-latex, and its object is to solve to occupy
The problem of the problem of indoor wall bacteria breed and wet weather are long, and interior wall is caused to mildew.
In order to achieve the above objectives, basic technology scheme of the invention is a kind of preparation side of antibacterial interior wall nano-latex
Method, the coating match in parts by weight, and specific step is as follows,
Step 1,10 parts of butyl titanate dissolutions solution A: are dissolved in 5~10 parts of ethyl alcohol and 5~8 parts under agitation
In the mixed solution of acetic acid, 0.8~2.16 part of polyvinylpyrrolidone is then added, is sufficiently stirred 12 hours；
B solution: 2~6 parts of acetylacetone,2,4-pentanediones, 5~10 parts of ethyl alcohol and 5~7 parts of acetic acid are mixed under agitation, and will
2.4~6.48 parts of mineral oil and 0.1~1 part of silver nitrate are added in above-mentioned mixed solution, are sufficiently stirred 12 hours；
Step 2, solution A and B solution are mixed according to the ratio of 1:1, is sufficiently stirred 12 hours and obtains preparing silver/titanium dioxide
The precursor colloids solution of nanotube；
Step 3, precursor solution made from step 2 is put into the spinning head that internal diameter is 1~1.2mm, reception device is to connect
Ground rotates the aluminium roller that diameter is 100mm, and receiving distance is 18~20cm, and spinning voltage is 15~20kV, carries out electrostatic spinning；
Step 4, the precursor product that step 3 processing obtains is cooled down immediately, is subsequently placed in Muffle furnace, with 1~5
DEG C heating rate per minute rises to 450~550 DEG C and heat preservation sintering 1~3 hour, obtains silver/titanium dioxide nanotube；
Step 5, take made from step 4 10~15 parts of silver/titanium dioxide nanotube be scattered in 200 under agitation~
In 300 parts of water, 8~15 parts of propylene glycol of addition, 10~20 parts of coalescing agent, 1~3 part of wetting agent, 1~3 part of preservative, ethoxy
It 1~3 part of cellulose, 4~8 parts of dispersing agent, is stirred 3 hours and is uniformly mixed with 400~600 revs/min in grinder；
Step 6,150~300 parts of titanium dioxide of addition in the mixture made from step 5,80~120 parts of coarse whiting, kaolin
60~100 parts, 40~60 parts of talcum powder, it is small that 3 are fully ground under 2000~4000 revs/min of revolving speed in high-speed grinder
When；
Step 7,200~400 parts of acrylic emulsion are added in the mixture made from step 6,1~3 part of defoaming agent, thickens
10~15 parts of agent；Finally finally filtered in grinder with stirring uniformly mixing in 3 hours under 400~600 revs/min of revolving speed
Barrelling obtains antibacterial interior wall nano-latex finished product.
The working principle and advantage of this programme are: nano-Ag particles and the intracorporal oxo of bacterium in interior wall nano paint
The sulfydryl (- SH) for thanking to enzyme combines, and inactivates enzyme, blocks respiratory metabolism that it is made to be choked to death.And under the irradiation of light, coating
The screw type titania nanotube of middle addition absorbs the energy of photon, sends out with vapor a small amount of on interior wall coating is adhered to
It is raw, it is formed on its surface free radical (- OH), this free radical has extremely strong bactericidal property, further improves interior wall nanometer
The bactericidal property of coating.And silver has splendid electric conductivity, can promote the biography of carrier in screw type titania nanotube
It is defeated, improve its bactericidal property.And screw type titania nanotube is not susceptible to reunite, meanwhile, the microcosmic nanometer of screw type
Structure not only increases specific surface area, and is pinned at it in coating particles, compared to common titania nanotube with
The combination of coating particles is even closer.
Preferred embodiment one: as the preferred embodiment of basic scheme, the wetting agent is alkyl phenol polyoxyethylene ether；It is described at
Film auxiliary agent is polyaminoester emulsion；The foaming agent is polysiloxane defoamer；The preservative is Dao Weixier -75；Dispersion
Agent is neopelex；The thickener is polyurethane high molecule compound water solution.
Preferred embodiment two: preferably one preferred embodiment: the formula of step 1 titania nanotube, A are molten
Liquid: 6 parts of polyvinylpyrrolidones, 6.5 parts of dehydrated alcohols, 1.7 parts of chlorine silver acid；B solution: 12.5 parts of bismuth nitrates, 7.5 parts of levulinics
Ketone vanadyl, 25 parts of N-N dimethylformamides, 20 parts of acetic acid, 8.5 parts of dehydrated alcohols, 18 parts of mineral oil；Inventor passes through experiment hair
Interior wall nano paint anti-microbial property now using said ratio preparation is good.
Preferred embodiment three: preferably two preferred embodiment: the additional amount of step 5 titania nanotube
Mass fraction is 13 parts, and inventor is had found through a large number of experiments using interior wall nano paint anti-microbial property made from said ratio
It is good.
Preferred embodiment four: preferably three preferred embodiment: the heating rate of step 4 Muffle furnace is 2.5 DEG C/
Min, inventor are had found to be saved completely using above-mentioned parameter silver/titanium dioxide nanocrystailine microstructures through a large number of experiments, be obtained
Interior wall nano paint anti-microbial property it is good.
Preferred embodiment five: preferably four preferred embodiment: the step 4 Muffle furnace soaking time is 1.5 hours,
Inventor has found to save completely using the silver/titanium dioxide nanocrystailine microstructures of above-mentioned parameter preparation through a large number of experiments, obtains
The interior wall nano paint anti-microbial property arrived is good.
Preferred embodiment six: preferably five preferred embodiment: the step 4 silver/titanium dioxide nanotube is described
In the case where Muffle furnace roasting condition is inert gas atmosphere, inventor has found through a large number of experiments using upper titania nanotube
Parameter is stated, can produce Lacking oxygen, reduces the recombination rate in titanic oxide electronic hole, improves photocatalysis performance, and then in raising
The anti-microbial property of wall nano paint.
Preferred embodiment seven: preferably six preferred embodiment: the step 4 silver/titanium dioxide nanotube is in Muffle
The inert gas conditions of furnace roasting are argon atmosphere, and inventor has found the interior wall using above-mentioned parameter preparation through a large number of experiments
Nano paint anti-microbial property is good.
Detailed description of the invention
Fig. 1 is the Scanning Electron microscope figure of 5 screw type silver/titanium dioxide nanotube of the embodiment of the present invention；
Fig. 2 is the isothermal nitrogen adsorption desorption curve graph of 5 screw type silver/titanium dioxide nanotube of the embodiment of the present invention.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
" number " as described below is " mass fraction ".
Embodiment 1: a kind of preparation method of antibacterial interior wall nano-latex,
Step 1, solution A: 8 parts of butyl titanates are dissolved in the mixed solution of 5 parts of dehydrated alcohols and 5 parts of acetic acid, are filled
Divide stirring 20 minutes；
B solution: 2 parts of acetylacetone,2,4-pentanediones and 5 parts of dehydrated alcohol dissolutions and 5 parts of anhydrous acetic acids are mixed under agitation, are added
It is uniformly mixed to enter 2.4 parts of mineral oil, 0.1 part of silver nitrate, is sufficiently stirred 12 hours；
Step 2, solution A and B solution are mixed according to the ratio of 1:1, is sufficiently stirred 12 hours and obtains preparing silver/titanium dioxide
The precursor colloids solution of nanotube；
Step 3, precursor solution made from step 2 is put into the spinning head that internal diameter is 1mm, reception device is ground connection rotation
It is directly 100mm aluminium roller, receiving distance is 18cm, spinning voltage 15kV, carries out electrostatic spinning；
Step 4, the precursor product that step 3 processing obtains is cooled down immediately, is subsequently placed in Muffle furnace, with 1 DEG C
Heating rate per minute rises to 450 DEG C and heat preservation sintering 1 hour, obtains silver/titanium dioxide nanotube；
Step 5, it takes and is scattered in 200 parts of water under agitation for 10 parts of silver/titanium dioxide nanotube made from step 4,
8 parts of propylene glycol of addition, 10 parts of polyaminoester emulsion, 1 part of alkyl phenol polyoxyethylene ether, Dao Weixier -751 parts, hydroxyethyl cellulose 1
Part, it 4 parts of neopelex, is stirred 3 hours and is uniformly mixed with 400 revs/min in grinder；
Step 6,150 parts of titanium dioxide of addition in the mixture made from step 5,80 parts of coarse whiting, 60 parts of kaolin, talcum powder
40 parts, to be fully ground under 2000 revs/min of revolving speed 3 hours in high-speed grinder；
Step 7,200 parts of acrylic emulsion are added in the mixture made from step 6,1 part of polysiloxane defoamer, gathers
10 parts of urethane high-molecular compound aqueous solution；To stir uniformly mixing in 3 hours under 400 revs/min of revolving speed in grinder, finally
Barrelling is filtered, antibacterial interior wall nano-latex is obtained.
Embodiment 2: a kind of preparation method of antibacterial interior wall nano-latex,
Step 1, solution A: 10 parts of butyl titanates being dissolved in the mixed solution of 10 parts of dehydrated alcohols and 8 parts of acetic acid,
It is sufficiently stirred 12 hours；
B solution: 6 parts of acetylacetone,2,4-pentanediones and 10 parts of dehydrated alcohol dissolutions and 7 parts of anhydrous acetic acids are mixed under agitation, are added
It is uniformly mixed to enter 2.4 parts of mineral oil, 0.1 part of silver nitrate, is sufficiently stirred 12 hours；
Step 2, solution A and B solution are mixed according to the ratio of 1:1, is sufficiently stirred 12 hours and obtains preparing silver/titanium dioxide
The precursor colloids solution of nanotube；
Step 3, precursor solution made from step 2 is put into the spinning head that internal diameter is 1.2mm, reception device is that ground connection turns
Dynamic is directly 100mm aluminium roller, and receiving distance is 20cm, spinning voltage 20kV, carries out electrostatic spinning；
Step 4, the precursor product that step 3 processing obtains is cooled down immediately, is subsequently placed in Muffle furnace, with 5 DEG C
Heating rate per minute rises to 550 DEG C and heat preservation sintering 3 hours, obtains silver/titanium dioxide nanotube；
Step 5, it takes and is scattered in 300 parts of water under agitation for 15 parts of silver/titanium dioxide nanotube made from step 4,
15 parts of propylene glycol of addition, 20 parts of polyaminoester emulsion, 3 parts of alkyl phenol polyoxyethylene ether, Dao Weixier -753 parts, hydroxyethyl cellulose
It 3 parts, 8 parts of neopelex, is stirred 3 hours and is uniformly mixed with 600 revs/min in grinder；
Step 6,300 parts of titanium dioxide of addition in the mixture made of step 5,120 parts of coarse whiting, 100 parts of kaolin, talcum
60 parts of powder, to be fully ground under 4000 revs/min of revolving speed 3 hours in high-speed grinder；
Step 7,200 parts of acrylic emulsion are added in the mixture made of step 6,1 part of polysiloxane defoamer, gathers
10 parts of urethane high-molecular compound aqueous solution；To stir uniformly mixing in 3 hours under 600 revs/min of revolving speed in grinder, finally
Barrelling is filtered, antibacterial interior wall nano-latex is obtained.
Embodiment 3: a kind of preparation method of antibacterial interior wall nano-latex,
Step 1,10 parts of butyl titanates solution A: are dissolved in the mixed solution of 7.5 parts of dehydrated alcohols and 6.5 parts of acetic acid
In, it is sufficiently stirred 12 hours；
B solution: under agitation mixing 4 parts of acetylacetone,2,4-pentanediones and 7.5 parts of dehydrated alcohol dissolutions and 6 parts of anhydrous acetic acids,
It is uniformly mixed that 4.44 parts of mineral oil, 0.5 part of silver nitrate is added, is sufficiently stirred 12 hours；
Step 2, solution A and B solution are mixed according to the ratio of 1:1, is sufficiently stirred 12 hours and obtains preparing silver/titanium dioxide
The precursor colloids solution of nanotube；
Step 3, precursor solution made from step 2 is put into the spinning head that internal diameter is 1.1mm, reception device is that ground connection turns
Dynamic is directly 100mm aluminium roller, and receiving distance is 19cm, spinning voltage 18kV, carries out electrostatic spinning；
Step 4, the precursor product that step 3 processing obtains is cooled down immediately, is subsequently placed in Muffle furnace, with 2.5
DEG C heating rate per minute rises to 500 DEG C and heat preservation sintering 3 hours, obtains silver/titanium dioxide nanotube；
Step 5, it takes and is scattered in 250 parts of water under agitation for 13 parts of silver/titanium dioxide nanotube made from step 4,
13 parts of propylene glycol of addition, 15 parts of polyaminoester emulsion, 2 parts of alkyl phenol polyoxyethylene ether, Dao Weixier -752 parts, hydroxyethyl cellulose
It 2 parts, 6 parts of neopelex, is stirred 3 hours and is uniformly mixed with 500 revs/min in grinder；
Step 6,225 parts of titanium dioxide of addition in the mixture made of step 5,100 parts of coarse whiting, 80 parts of kaolin, talcum
50 parts of powder, to be fully ground under 3000 revs/min of revolving speed 3 hours in high-speed grinder；
Step 7,300 parts of acrylic emulsion are added in the mixture made of step 6,2 parts of polysiloxane defoamer, gathers
13 parts of urethane high-molecular compound aqueous solution；To stir uniformly mixing in 3 hours under 500 revs/min of revolving speed in grinder, finally
Barrelling is filtered, antibacterial interior wall nano-latex is obtained.
Embodiment 4:
Experimental procedure same as Example 3, the difference is that Muffle furnace roasts part, the present embodiment is in helium gas
Lower 500 DEG C of atmosphere roast 1.5 hours.
Embodiment 5:
Experimental procedure same as Example 3, the difference is that Muffle furnace roasts part, the present embodiment is in argon gas gas
Lower 500 DEG C of atmosphere roast 1.5 hours.
Part of detecting:
Antifungi test: GB/T1741-2007 paint film fungus resistance measuring method according to national standards, above embodiments system
The nano-latex obtained is coated on 50mm × 50mm, and with a thickness of on the sheet glass of 3mm, drying is placed on the constant temperature and humidity of 2500ml
In incubator (25~30 DEG C, relative humidity h >=85%), by 9 kinds of mixing moulds (bright mould, withered blueness of black Sibutramine Hydrochloride, aspergillus flavus, ball hair
As if mould, Trichoderma viride, Aureobasidium pullulans, cladosporium herbarum, formula Paecilomyces varioti, rod method) strain is seeded on paint film, and yin is arranged
Property control board A and positive control plate B, by above one recycle (28 days) test, if not yet finding any variation, to reality
It applies example and is carrying out a test loop, recycled until 10 times.Finally, being detected to its surface of the paint film.
Antibacterial test: GB/T21866-2008 antibiotic paint (paint film) anti-microbial property measuring method and antibacterial according to national standards
Effect, nano-latex made from above embodiments require to make coated on the cement plate of 50mm × 50mm according to GB/T1727
Make film, the application of coating is to brush twice, is brushed second time after first pass surface drying, film overall thickness wet film is less than 100 μm.It applies
According to 7 days dry under the conditions of as defined in GB/T 9278 after brush.Before experiment, using ultraviolet sterilization lamp and medicinal alcohol to paint film table
Face carries out disinfection.And negative control template A and blank control template B are set.Using staphylococcus aureus and escherichia coli
Bacterium is seeded on paint film, is cultivated 24 hours under the conditions of 37 ± 1 DEG C, relative humidity > 90% as strain is examined.It takes out
The sample of culture is separately added into 20ml washing lotion, washes sample repeatedly, washing lotion is inoculated in nutrient agar, at 37 ± 1 DEG C
Count plate after culture 24 hours.
Antibacterial test: use 1 30W, wavelength be 253.7nm ultraviolet lamp, antibiotic paint test plate (panel) apart from ultraviolet lamp 0.8~
1m irradiates 100h, is tested later according to antibacterial test.
Antifungi and anti-bacteria test result such as the following table 3
Such as table 3 it is known that being added to the antibacterial and resistance of the antibacterial interior wall nano-latex of silver/titanium dioxide nanotube
Silver/titanium dioxide after the effect of mould has significant raising, especially embodiment 5 to be added to roasting under an argon atmosphere is received
Mitron bacteria resistance is significantly improved again.
Claims (4)
1. a kind of preparation method of antibacterial interior wall nano-latex, which is characterized in that
Step 1,10 parts of butyl titanates solution A: are dissolved in the mixed of 5~10 parts of ethyl alcohol and 5~8 parts of acetic acid under agitation
It closes in solution, 0.8~2.16 part of polyvinylpyrrolidone is then added, is sufficiently stirred 12 hours；
B solution: under agitation mixing 2~6 parts of acetylacetone,2,4-pentanediones, 5~10 parts of ethyl alcohol and 5~7 parts of acetic acid, and by 2.4~
6.48 parts of mineral oil and 0.1~1 part of silver nitrate are added in above-mentioned mixed solution, are sufficiently stirred 12 hours；
Step 2, solution A and B solution are mixed according to the ratio of 1:1, is sufficiently stirred and obtains within 12 hours preparing silver/titanium dioxide nanometer
The precursor colloids solution of pipe；
Step 3, precursor solution made from step 2 is put into the spinning head that internal diameter is 1~1.2mm, reception device is that ground connection turns
The aluminium roller that dynamic diameter is 100mm, receiving distance is 18~20cm, and spinning voltage is 15~20kV, carries out electrostatic spinning；
Step 4, the precursor product that step 3 processing obtains is cooled down immediately, is subsequently placed in Muffle furnace under argon atmosphere
Roasting rises to 450~550 DEG C and heat preservation sintering 1~3 hour with 1~5 DEG C of heating rate per minute, obtains screw type silver/bis-
Titanium oxide nanotubes；
Step 5, take 10~15 parts of screw type silver/titanium dioxide nanotube made from step 4 be scattered in 200 under agitation~
In 300 parts of water, 8~15 parts of propylene glycol of addition, 10~20 parts of coalescing agent, 1~3 part of wetting agent, 1~3 part of preservative, ethoxy
It 1~3 part of cellulose, 4~8 parts of dispersing agent, is stirred 3 hours and is uniformly mixed with 400~600 revs/min in grinder；
Step 6,150~300 parts of titanium dioxide of addition in the mixture made from step 5,80~120 parts of coarse whiting, kaolin 60~
100 parts, 40~60 parts of talcum powder, to be fully ground under 2000~4000 revs/min of revolving speed 3 hours in high-speed grinder；
Step 7,200~400 parts of acrylic emulsion of addition in the mixture made from step 6,1~3 part of defoaming agent, thickener 10
~15 parts；Barrelling is finally finally filtered to stir uniformly mixing in 3 hours under 400~600 revs/min of revolving speed in grinder,
Obtain antibacterial interior wall nano-latex finished product；
The wetting agent is alkyl phenol polyoxyethylene ether, the coalescing agent is polyaminoester emulsion, the defoaming agent is poly- silicon oxygen
Alkanes defoaming agent, the preservative are Dao Weixier -75, dispersing agent is neopelex, the thickener is poly- ammonia
Ester high-molecular compound aqueous solution.
2. the preparation method of antibacterial interior wall nano-latex as described in claim 1, which is characterized in that spiral shell in the step 5
The mass fraction of the additional amount of rotation type silver/titanium dioxide nanotube is 13 parts.
3. the preparation method of antibacterial interior wall nano-latex as claimed in claim 2, which is characterized in that horse in the step 4
Not the heating rate of furnace is 2.5 DEG C/min.
4. the preparation method of antibacterial interior wall nano-latex as claimed in claim 3, which is characterized in that horse in the step 4
Not furnace soaking time is 1.5 hours.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910458247.0A CN110184681A (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of silver/titanium dioxide nanotube |
| CN201611012897.5A CN106519846B (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of antibacterial interior wall nano-latex |
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| CN201611012897.5A CN106519846B (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of antibacterial interior wall nano-latex |
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| CN201910458247.0A Division CN110184681A (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of silver/titanium dioxide nanotube |
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| CN106519846B true CN106519846B (en) | 2019-05-17 |
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| CN201910458247.0A Withdrawn CN110184681A (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of silver/titanium dioxide nanotube |
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| CN109921171B (en) * | 2019-04-03 | 2020-02-18 | 宁波智诚祥科技发展有限公司 | Miniature 5G communication base station antenna |
| CN110105839A (en) * | 2019-06-12 | 2019-08-09 | 上海班众数据科技有限公司 | A kind of environment-friendly type inner wall nano paint and preparation method thereof |
| CN113089134B (en) * | 2021-03-24 | 2022-02-15 | 北京化工大学 | Preparation method of rod-shaped silver-titanium nano-fiber and method for synthesizing ammonia by electrochemical nitrogen reduction |
| CN113512313A (en) * | 2021-08-04 | 2021-10-19 | 青岛金芳华新型建材科技有限公司 | Waterproof and mildewproof composite coating and preparation method thereof |
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| KR101037333B1 (en) * | 2011-03-15 | 2011-05-26 | 삼한건업(주) | Manufacturing method of multi-color paint composition having improved antibiosis, contamination resistance, scratch resistance and uv resistnace, multi-color paint composition manufactured by the same and coating method using the same |
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| CN1583901A (en) * | 2004-06-15 | 2005-02-23 | 深圳清华大学研究院 | Nanometer titanial/nanometer silver coating and preparing method thereof |
| CN101613556A (en) * | 2009-07-16 | 2009-12-30 | 浙江大学 | The preparation method of titanium silver-based antimildew and antibacterial emulsion paint interior wall paint |
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| CN110184681A (en) | 2019-08-30 |
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