CN106883707A - A kind of galapectite antibiotic water paint and preparation method and application - Google Patents
A kind of galapectite antibiotic water paint and preparation method and application Download PDFInfo
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- CN106883707A CN106883707A CN201710167817.1A CN201710167817A CN106883707A CN 106883707 A CN106883707 A CN 106883707A CN 201710167817 A CN201710167817 A CN 201710167817A CN 106883707 A CN106883707 A CN 106883707A
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- galapectite
- antiseptic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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Abstract
The invention belongs to technical field of coatings, a kind of galapectite antibiotic water paint and preparation method and application is disclosed.Preparation method of the present invention is comprised the following steps：The mixed aqueous solution of galapectite, shitosan class antiseptic is carried out into negative pressure of vacuum treatment, is separated, dried, obtain loading the galapectite powder of antiseptic；Mix with water-based acrylic resin coating again, obtain galapectite antibiotic water paint.Galapectite antibiotic water paint of the present invention utilizes the cavity structure of halloysite nanotubes, by Molecular Adsorption and negative pressure of vacuum process, antibacterial moleucles are made to load on galapectite, and then mix with acrylic resin paint, obtain with long acting antibiotic function, and the acrylic resin paint that mechanical performance is improved.The inventive method is loaded and is sustained using halloysite nanotubes to antiseptic, is realized compatible in acrylic resin paint of the antiseptics such as shitosan and is shown excellent antibacterial effect, and system is aqueous, environmental protection, can be widely applied to each field.
Description
Technical field
The invention belongs to technical field of coatings, more particularly to a kind of galapectite antibiotic water paint and preparation method thereof with should
With.
Background technology
High performance antibiotic paint can not only play a part of the protection base material of conventional coating, can also prevent substrate surface
Upper bacterium generates and mouldy, therefore is widely used on marine antifouling, building decoration, furniture and electronic product and toy,
Paid attention to by every country research and development.Antiseptic can be divided into according to composition and source：Natural antibacterial agent, inorganic antiseptic, have
Machine antiseptic and complex antimicrobials.The special requirement of antibiotic paint are with long-acting, wide spectrum, safety non-toxic, colour stability, valency
Lattice are cheap etc..But existing antibiotic paint cannot also very well meet these requirements, such as nano-TiO2Although photocatalitic germicide
Anti-microbial property in coating is excellent, but to film forming matter acrylate copolymer has destruction in use.Will
Coating is assigned with antibiotic property, it is also contemplated that how antiseptic is incorporated into the middle of material.Common physics blending method can be in film
Under the influence of use environment, volatilization and migration is caused to cause the decrease of protection.And there is complex process, cost in chemical bonding
Higher the shortcomings of.If antiseptic can be anchored on the filler used by coating by absorption carriage, protection can be played
And the purpose of slow delivery of antimicrobials, will be the effective ways for preparing antibiotic paint.
Halloysite nanotubes (HNTs) belong to clay minerals material, with unique hollow tubular structure.Its pipe range is
200nm~1.5 μm, pipe external diameter is 50~100nm, and internal diameter is 10~30nm, and specific surface area is about 56m2/g.Because it easily divides
The features such as scattered, high length-diameter ratio and strong interface are acted on, galapectite can be used for the reinforcing agent of multiple polymers.The adsorptivity of galapectite
Can be high, can be used to remove the dyestuff and metal ion in waste water.Using its high adsorption and the pipe cavity structure of uniqueness, also may be used
For as the carrier of chemicals and genomic medicine, realizing the purpose of the gentle On The Drug Release of protection of medicine.Because its is good
Environmental compatibility, its be considered as it is a kind of green material.Its tubular structure causes it to have in polymer solution and melt
There is the ability to form network structure, the thixotropic agent for coating can be developed using this characteristic of its shear shinning, with generation
For common lithium diatomaceous earth.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of galapectite to resist
Bacterium water paint.Coating of the present invention using galapectite as carrier load shitosan class antiseptic, with long acting antibiotic function.
Another object of the present invention is to provide a kind of preparation method of above-mentioned galapectite antibiotic water paint.
The inventive method uses negative pressure of vacuum physical adsorption process, using the space structure of nanotube, antiseptic is loaded
To in galapectite pipe, antiseptic is nontoxic and can slowly be discharged from galapectite.The method has load capacity big, mutual
The characteristics of acting on strong, and simple to operate, low cost, load capacity it is high, can be to antiseptic sustained release, water-based system, environment-protecting asepsis.
Still a further object of the present invention be provide above-mentioned galapectite antibiotic water paint marine antifouling, building decoration, furniture,
Application in coil painting, electronic product and toy.
The purpose of the present invention is realized by following proposal：
A kind of preparation method of galapectite antibiotic water paint, comprises the following steps：By galapectite (HNTs), shitosan class
The mixed aqueous solution of antiseptic carries out negative pressure of vacuum treatment, separates, and dries, and obtains loading the galapectite powder of antiseptic；Again with
Water-based acrylic resin coating mixes, and obtains galapectite antibiotic water paint.
The shitosan class antiseptic includes shitosan, chitosan oligosaccharide, chitosan quaternary ammonium salt, chitosan hydrochloride, shitosan
Sulfate, carboxymethyl chitosan, sulfated chitosan, etherificate shitosan etc..
The HNTs is 100 with the mass ratio of shitosan class antiseptic:0.01~100:100.
In the mixed aqueous solution, the concentration of shitosan class antiseptic is 0.01~30wt%.
In the mixed aqueous solution, the concentration of HNTs is 0.01~50wt%.
Preferably use the aqueous solution of concentration of the present invention, it is ensured that appropriate liquid viscosity, be conducive to galapectite therein
Dispersed and realization antiseptic load capacity higher.
The length of HNTs used is 200~1000nm, a diameter of 50~100nm.
In order to the present invention is better achieved, HNTs used is preferably the HNTs after purification.
Described negative pressure of vacuum treatment refers to takes out solution connection vacuum tube using vacuum pump or oil pump or membrane pump repeatedly
Vacuum 3~10 times.
The mass ratio 100 of the galapectite powder of water-based acrylic resin coating used and load antiseptic:0.2~100:
60。
Preferably, the galapectite, the mixed aqueous solution of shitosan class antiseptic are prepared by including following methods：First
Shitosan class antiseptic is soluble in water, add galapectite and be uniformly dispersed and obtain.
Described being uniformly dispersed can be realized by mechanical agitation or ultrasonic disperse, more preferably first be stirred in 50~1000 turns of lower machineries
5~60min is mixed, then 30~60min of ultrasonic disperse is realized under 60~1000W power.
Described separation preferably realized by being centrifuged, it is centrifuged under 2000~20000 turns 3 more preferably by mixed aqueous solution~
20min, removes supernatant.
Described drying can dry 1~24h by drying or freeze-drying realization more preferably at 40~100 DEG C, or
12~24h of freeze-drying at -50~-80 DEG C.
It is described to mix with water-based acrylic resin coating preferably in 50~1000 turns of lower 5~60min of mechanical agitation.
Described water-based acrylic resin coating can be the cold coating of this area any conventional.
Galapectite antibiotic water paint of the invention has long acting antibiotic function, can be applied to marine antifouling, building decoration,
In the fields such as furniture, coil painting, electronic product and toy.
Specially：By galapectite antibiotic water paint of the present invention spraying or roller coating on base material, dry, obtain galapectite and resist
Bacterium coating.
The base material is including aluminium flake, timber, sheet glass, stainless steel, plastic sheet etc..
The drying is preferably and 0.5~48h is dried at 25~150 DEG C.
The present invention, by Molecular Adsorption and negative pressure of vacuum process, makes antiseptic using the cavity structure of halloysite nanotubes
Molecule is loaded on galapectite, and then is mixed with coating.Coating is sprayed to by techniques such as sprayings turn on base material protection painting
Layer.In use, antiseptic is gradually discharged from galapectite, and then realizes permanent antibacterial effect.Meanwhile, add
Galapectite the mechanical performance of coating can also be improved.It is a kind of not only with higher-strength but also with long-acting anti-so as to prepare
The nano paint of bacterium performance.
Natural antibacterial agent with Chitosan-phospholipid complex as representative, its Antibacterial Mechanism is the-NH on strand2Group with
The anion binding that silicic acid, phosphate ester contained by bacteria cell wall etc. are dissociateed, makes the free activity of bacterium be obstructed, and hinders its big
Amount breeding；Then, shitosan is further degraded, by cell membrane enter bacterium it is intracellular, make gene from DNA to
The transition process of RNA is obstructed, and causes bacterium to breed.But, because the antiseptics such as shitosan need to be showed in acid condition
Be antibiotic property, and with the poor compatibility of acrylic resin, therefore both systems for being mixed to get in, show as without antibacterial activity.
The present invention is loaded and is sustained using halloysite nanotubes to it, efficiently solves above-mentioned technical problem, the performance of gained coating
Go out excellent antibacterial effect, can be widely applied to each field.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) preparation method of present invention load antiseptic using water as decentralized medium, non-environmental-pollution, antiseptic can be
Load Balanced on clay, and with good load effect, further promote the raising of anti-microbial property.
(2) interaction that the present invention passes through the load factor and galapectite of vacuum suction method raising antiseptic, it is to avoid general
The shortcoming that adsorbance is small, suction-operated is weak that logical mechanical agitation absorption is caused.
(3) application of the inventive method to galapectite, shitosan etc. in antibiotic paint provides solution, solves
Prior art causes coating antibiosis to be deteriorated due to there may be microorganism in natural clay, and shitosan shows as in coating
Problem without antibiotic property.
(4) preparation method of the present invention is simple to operate, favorable repeatability, cost are relatively low, using water as dispersant, without poisonous
Material is remained, and may be implemented in the preparation of antibiotic paint on various substrate materials.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
The reagent used in the following example can be obtained from commercial channel.
Embodiment 1
(1) aqueous solution that 1g shitosans are configured to 1% concentration is weighed, 20g galapectite powder, 500 turns of mechanical agitations is added
60min；
(2) mixture solution in step (1) is carried out, by negative pressure of vacuum 5 times, antiseptic being adsorbed onto into galapectite pipe
Inside and outside wall；
10min is centrifuged under (3) 5000 turns, supernatant is outwelled, after being centrifuged for 3 times with pure water, lower sediment is taken out, 50
DEG C drying 12h, loaded the galapectite powder of shitosan；
(4) by water-based acrylic resin coating (DSM NeoCryl XK-258) and the galapectite powder of shitosan has been loaded
According to 100:5 mass ratioes are in 300 turns of lower mechanical agitation mixing 30min.
(5) 24h is dried by 25 DEG C on above-mentioned coating spraying to aluminium flake, to antibiotic paint coating.
(6) above-mentioned sample is embedded in the culture medium of Escherichia coli bacteria liquid, is placed in 54~57 DEG C of incubators 14 days, with micro-
Its long-term antimicrobial efficiency of bio-detector is 0 grade.
Embodiment 2
(1) aqueous solution that 0.5g chitosan quaternary ammonium salts are configured to 5% concentration is weighed, 20g galapectite powder, 800 turns is added
Mechanical agitation 30min；
(2) mixture solution in step (1) is carried out, by negative pressure of vacuum 6 times, antiseptic being adsorbed onto into galapectite pipe
Inside and outside wall；
5min is centrifuged under (3) 8000 turns, supernatant is outwelled, after being centrifuged for 3 times with pure water, lower sediment is taken out, 40
DEG C drying 16h, loaded the galapectite powder of antiseptic；
(4) by water-borne acrylic coatings cold coating (Nuplex Setaque 6716) and the Ai Luo of antiseptic has been loaded
Stone powder is according to 100:10 mass ratioes are in 500 turns of lower mechanical agitation mixing 20min.
(5) 40h is dried by 50 DEG C on above-mentioned coating spraying to timber, to antibiotic paint coating.
(6) above-mentioned sample is embedded in the culture medium of Escherichia coli bacteria liquid, is placed in 54~57 DEG C of incubators 14 days, with micro-
Its long-term antimicrobial efficiency of bio-detector is 1 grade.
Embodiment 3
(1) aqueous solution that 10g chitosan oligosaccharides are configured to 8% concentration is weighed, 20g galapectite powder, ultrasonic disperse is added
60min；
(2) mixture solution in step (1) is carried out, by negative pressure of vacuum 6 times, antiseptic being adsorbed onto into galapectite pipe
Inside and outside wall；
12min is centrifuged under (3) 6000 turns, supernatant is outwelled, after being centrifuged for 3 times with pure water, lower sediment is taken out, 80
DEG C drying 4h, loaded the galapectite powder of antiseptic；
(4) by water-borne acrylic coatings cold coating (4400, Wanhua Chemical Group Co., Ltd.) and
The galapectite powder of antiseptic has been loaded according to 100:8 mass ratioes are in 300 turns of lower mechanical agitation mixing 40min.
(5) 5h is dried by 40 DEG C on above-mentioned coating spraying to stainless steel, to antibiotic paint coating.
(6) above-mentioned sample is embedded in the culture medium of staphylococcus aureus bacterium solution, is placed in 54~57 DEG C of incubators 14
My god, with microorganism detector, its long-term antimicrobial efficiency is 1 grade.
Embodiment 4
(1) aqueous solution that 2g chitosan hydrochlorides are configured to 10% concentration is weighed, 20g galapectite powder, ultrasound point is added
Dissipate 30min；
(2) mixture solution in step (1) is carried out, by negative pressure of vacuum 5 times, antiseptic being adsorbed onto into galapectite pipe
Inside and outside wall；
5min is centrifuged under (3) 8000 turns, supernatant is outwelled, after being centrifuged for 3 times with pure water, lower sediment is taken out, 100
DEG C drying 1h, loaded the galapectite powder of antiseptic；
(4) by water-borne acrylic coatings cold coating (Pb-428, Beijing Dongfang Yakeli Chemical Science Co., Ltd) and
The galapectite powder of antiseptic has been loaded according to 100:2 mass ratioes are in 200 turns of lower mechanical agitation mixing 60min.
(5) 2h is dried by 120 DEG C on above-mentioned coating spraying to glass, to antibiotic paint coating.
(6) above-mentioned sample is embedded in the culture medium of staphylococcus aureus bacterium solution, is placed in 54~57 DEG C of incubators 14
My god, with microorganism detector, its long-term antimicrobial efficiency is 0 grade.
Embodiment 5
(1) aqueous solution that 15g O-CMCs are configured to 1% concentration is weighed, 20g galapectite powder, 1000 is added
Turn mechanical agitation 40min；
(2) mixture solution in step (1) is carried out, by negative pressure of vacuum 5 times, antiseptic being adsorbed onto into galapectite pipe
Inside and outside wall；
15min is centrifuged under (3) 7000 turns, supernatant is outwelled, after being centrifuged for 3 times with pure water, lower sediment is taken out, 45
DEG C drying 18h, loaded the galapectite powder of antiseptic；
(4) by water-based acrylic resin coating (Fuchem-361, Shandong future chemical company product) and antibacterial has been loaded
The galapectite powder of agent is according to 100:1 mass ratio is in 300 turns of lower mechanical agitation mixing 30min.
(5) 8h is dried by 80 DEG C on above-mentioned coating spraying to Polycarbonate plastic sheet, to antibiotic paint coating.
(6) above-mentioned sample is embedded in the culture medium of Escherichia coli bacteria liquid, is placed in 54~57 DEG C of incubators 14 days, with micro-
Its long-term antimicrobial efficiency of bio-detector is 0 grade.
Embodiment 6
(1) aqueous solution that 3g sulfated chitosans are configured to 3% concentration is weighed, 20g galapectite powder, 1200 favourable turn tools is added
Stirring 30min；
(2) mixture solution in step (1) is carried out, by negative pressure of vacuum 7 times, antiseptic being adsorbed onto into galapectite pipe
Inside and outside wall；
5min is centrifuged under (3) 10000 turns, supernatant is outwelled, after being centrifuged for 3 times with pure water, lower sediment is taken out, 60
DEG C drying 20h, loaded the galapectite powder of antiseptic；
(4) by water-based acrylic resin coating (2710, A Kema coating resins) and loaded antiseptic
Galapectite powder is according to 100:1 mass ratio is in 300 turns of lower mechanical agitation mixing 30min.
(5) 6h is dried by 90 DEG C on above-mentioned coating spraying to makrolon/ABS blend plastic sheet, is applied to antibiotic paint
Layer.
(6) above-mentioned sample is embedded in the culture medium of hay bacillus liquid, is placed in 54~57 DEG C of incubators 14 days, use micro- life
Its long-term antimicrobial efficiency of analyte detection instrument is 1 grade.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of galapectite antibiotic water paint, it is characterised in that comprise the following steps：By galapectite, shitosan
The mixed aqueous solution of class antiseptic carries out negative pressure of vacuum treatment, separates, and dries, and obtains loading the galapectite powder of antiseptic；Again
Mix with water-based acrylic resin coating, obtain galapectite antibiotic water paint.
2. the preparation method of galapectite antibiotic water paint according to claim 1, it is characterised in that：The shitosan class
Antiseptic include shitosan, chitosan oligosaccharide, chitosan quaternary ammonium salt, chitosan hydrochloride, Chitosan Sulfate, carboxymethyl chitosan,
At least one in sulfated chitosan and etherificate shitosan.
3. the preparation method of galapectite antibiotic water paint according to claim 1, it is characterised in that：The galapectite with
The mass ratio of shitosan class antiseptic is 100:0.01~100:100.
4. the preparation method of galapectite antibiotic water paint according to claim 1, it is characterised in that：The mixing is water-soluble
In liquid, the concentration of shitosan class antiseptic is 0.01~30wt%；The concentration of galapectite is 0.01~50wt%.
5. the preparation method of galapectite antibiotic water paint according to claim 1, it is characterised in that：Galapectite used
Length is 200~1000nm, a diameter of 50~100nm；Described negative pressure of vacuum treatment refers to solution connection vacuum tube using true
Empty water pump or oil pump or membrane pump are vacuumized 3~10 times repeatedly.
6. the preparation method of galapectite antibiotic water paint according to claim 1, it is characterised in that：Aqueous acrylamide used
The mass ratio 100 of the galapectite powder of acid resin coating and load antiseptic:0.2~100:60.
7. a kind of galapectite antibiotic water paint, it is characterised in that the galapectite antibacterial according to any one of claim 1~6
The preparation method of water paint is obtained.
8. the galapectite antibiotic water paint described in claim 7 is in marine antifouling, building decoration, furniture, coil painting, electronics
Application in product and toy art.
9. application according to claim 8, it is characterised in that specially that the galapectite described in claim 7 is antibacterial aqueous
Coating is sprayed or roller coating is on base material, is dried, and obtains galapectite antimicrobial coating.
10. application according to claim 9, it is characterised in that：The base material includes aluminium flake, timber, sheet glass, stainless steel
Or plastic sheet；The drying is that 0.5~48h is dried at 25~150 DEG C.
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| CN108659525A (en) * | 2018-06-04 | 2018-10-16 | 东华大学 | A method of PA6/ meso-porous nano material@Ag composite antibacterial fibres are prepared based on situ aggregation method |
| CN109012174A (en) * | 2018-07-18 | 2018-12-18 | 凤台精兴生物科技有限公司 | A kind of method that galapectite auxiliary prepares automobile-used antibacterial urea solution |
| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
| CN109619100A (en) * | 2018-12-07 | 2019-04-16 | 国际竹藤中心 | A kind of halloysite nanotubes/quaternary ammonium salt composite antibacterial particle and its preparation method and application |
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| CN114805865A (en) * | 2022-03-25 | 2022-07-29 | 深圳市骏鼎达新材料股份有限公司 | Mildew-proof reinforced nylon 6 master batch and preparation method thereof |
| CN114834108A (en) * | 2022-05-19 | 2022-08-02 | 东莞市科迪实业有限公司 | Composite non-woven fabric and preparation method thereof |
| CN117281954A (en) * | 2023-08-31 | 2023-12-26 | 广东暨纳新材料科技有限公司 | Preparation method and application of halloysite-based titanium alloy antibacterial coating |
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Application publication date: 20170623 |