CN108192357A - A kind of antibacterial unsaturated polyester resin and preparation method thereof - Google Patents
A kind of antibacterial unsaturated polyester resin and preparation method thereof Download PDFInfo
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- CN108192357A CN108192357A CN201711486216.3A CN201711486216A CN108192357A CN 108192357 A CN108192357 A CN 108192357A CN 201711486216 A CN201711486216 A CN 201711486216A CN 108192357 A CN108192357 A CN 108192357A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C08L87/005—Block or graft polymers not provided for in groups C08L1/00 - C08L85/04
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of antibacterial unsaturated polyester resins, belong to resin making technique field, the antibacterial unsaturated polyester resin, including following raw material：Unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol, hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine, ethylene glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, N dimethylanilines, nano zinc powder, kaolin, calcium sulfate crystal whiskers, nano imvite, nano-titanium dioxide, silane coupling agent KH 560, antibacterial modified auxiliary agent, the antibacterial unsaturated polyester resin be through preparation base-material, prepare modified materials, and will the materials such as base-material, modified materials mix and etc. made of.The unsaturated polyester resin that the present invention is prepared has excellent anti-microbial property.
Description
Technical field
The present invention relates to the technical field of resin preparation process more particularly to a kind of antibacterial unsaturated polyester resin and its systems
Preparation Method.
Background technology
Unsaturated polyester (UP) is a kind of mature, industrialized thermosetting resin, and corresponding product is in laminate, Building wood
Material, adhesive, coating, construction industry and power industry are used widely.Unsaturated polyester (UP) raw material sources are wide, of low cost；
Normal temperature solidified molding, hardening time is controllable, and moulding process is simple；Product surface light is plentiful after curing, hardness is high, wearability
Good, electrical property and against weather are excellent.Although unsaturated polyester (UP) possesses many advantages, there is also some defects.Such as tradition not
Saturated polyester material is usually all more crisp, poor toughness, inflammable and not acidproof, caustic corrosion.
A kind of Chinese patent application document " unsaturated polyester resin and preparation method thereof (application publication number：
CN102532424A a kind of unsaturated polyester resin and preparation method thereof) " is disclosed, raw material components mass percent is benzene second
Alkene is 10-35%, and polymerization inhibitor 0.001-0.01%, auxiliary agent 0.01-0.05%, polyester is surplus：By dihydric alcohol and binary acid
Through 210-220 DEG C of pyroreaction, esterification dehydration, the polyester of generation mixes again with styrene, add auxiliary agent and polymerization inhibitor to get
Unsaturated polyester resin, the unsaturated polyester resin can provide the brightness of resin surface, abrasion and impact strength, can
Applied in a variety of chemical fields.But the anti-microbial property of unsaturated polyester resin the needs of can not meeting in actual use.
Invention content
To solve technical problem present in background technology, the present invention proposes a kind of antibacterial unsaturated polyester resin and its system
Preparation Method, to solve in a kind of Chinese patent application document " unsaturated polyester resin and preparation method thereof (application publication number：
CN102532424A the problem of unsaturated polyester resin anti-microbial property is insufficient disclosed in) ".
A kind of antibacterial unsaturated polyester resin proposed by the present invention, including following raw material：Unsaturated polyester resin, isophthalic two
Formic anhydride, phthalic anhydride, benzenetriol, hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine
Amine, ethylene glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate crystal whiskers,
Nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent；
The nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent weight ratio be
(4-8)：(6-9)：(1-3)：(15-25).
Further, the nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent
Weight ratio is 6：7.5：2：20.
Further, as unit of parts by weight, including following raw material：80-120 parts of unsaturated polyester resin, isophthalic diformazan
15-25 parts of acid anhydrides, 4-9 parts of phthalic anhydride, 3-6 parts of benzenetriol, 2-5 parts of hydroquinone, 1-4 parts of cobalt naphthenate, styrene
3-5 parts, 2-6 parts of methyl ethyl ketone peroxide, 4-8 parts of phosphate melamine, 2-6 parts of ethylene glycol, 1-5 parts of organosilicon, aluminium hydroxide
3-9 parts, 2-5 parts of carbon nanotubes, N, 1-4 parts of accelerine, 2-5 parts of nano zinc powder, 3-6 parts of kaolin, calcium sulfate crystal whiskers
2-8 parts, 4-8 parts of nano imvite, 6-9 parts of nano-titanium dioxide, 1-3 parts of silane coupling agent KH-560, antibacterial modified auxiliary agent
15-25 parts.
Further, the raw material of the antibacterial modified auxiliary agent includes by weight：15-25 parts of diatomite, titanium dioxide 4-8
Part, 3-9 parts of neopelex, 4-6 parts of urea, 2-8 parts of polyvinylpyrrolidone, 10-20 parts of deionized water, sodium chloride
4-8 parts, 3-6 parts of aluminum nitrate, 2-5 parts of chitosan, 1-4 parts of sodium tripolyphosphate, 3-5 parts of potassium peroxydisulfate, 2-5 parts of natural zeolite, sulphur
Sour zirconium 1-4 parts, 3-6 parts of disodium hydrogen phosphate.
Further, the antibacterial modified auxiliary agent is prepared by following technique：By diatomite, titanium dioxide and dodecyl
Benzene sulfonic acid sodium salt is uniformly mixed, and is stirred 20-40min in 650-850r/min rotating speeds, is then adjusted pH to 0.5-1.5, staticly settle,
Supernatant is removed, washs after 20-30h dry in 50-70 DEG C of baking oven, is cooled to room temperature to obtain material a；By urea, polyethylene
Pyrrolidones and deionized water are uniformly mixed, then add in sodium chloride stirring 10-30min, then add in aluminum nitrate, chitosan,
Sodium tripolyphosphate, potassium peroxydisulfate, natural zeolite and zirconium sulfate are uniformly mixed, and then heating water bath is cooled to room temperature to 70-90 DEG C
Disodium hydrogen phosphate is added in afterwards to be uniformly mixed, and is stirred 10-30min in 650-850r/min rotating speeds, is then aged, filtration washing, does
Dry, calcining postcooling to room temperature obtains antibacterial modified auxiliary agent.
The present invention also provides a kind of preparation methods of antibacterial unsaturated polyester resin, include the following steps：
S1, unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol are uniformly mixed, are warming up to
70-80 DEG C, 20-30min is kept the temperature, is subsequently added into hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate trimerization
Cyanamide, ethylene glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate are brilliant
It must be uniformly mixed, be continuously heating to 70-80 DEG C, keep the temperature 30-50min, then stir 10-20min in 350-450r/min rotating speeds,
It is cooled to room temperature to obtain base-material；
S2, nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent are uniformly mixed, risen
Temperature keeps the temperature 20-40min to 80-90 DEG C, then stirs 5-15min in 1500-2500r/min rotating speeds, is cooled to room temperature and is changed
Property material；
S3, base-material is warming up to 60-80 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, in 1200-
1400r/min rotating speeds stir 2-4h, are cooled to room temperature to obtain antibacterial unsaturated polyester resin.
The invention has the advantages that：
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that using the anti-of embodiment 1-3 antibacterial unsaturated polyester resins
Bacterium performance significantly improves；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that nano imvite, nano-titanium dioxide, silane coupling agent
KH-560, antibacterial modified auxiliary agent add play synergistic effect in antibacterial unsaturated polyester resin is prepared simultaneously, significantly improve
The anti-microbial property of antibacterial unsaturated polyester resin, this may be：Nano imvite, nano-titanium dioxide, silane coupling agent KH-
560th, antibacterial modified auxiliary agent is applied to as modified system in the preparation of unsaturated polyester resin, and silane coupling agent KH- is utilized
560 graft modification effect, realizes nano imvite, the hydroxyl of nano-titanium dioxide and antibacterial modified auxiliary agent surface and insatiable hunger
Grafting is realized with the base-material of polyester resin, imparts the excellent anti-microbial property of unsaturated polyester resin, while antibacterial is utilized and changes
The antibacterial humidification of property auxiliary agent, wherein antibacterial modified auxiliary agent is by the way that diatomite, titanium dioxide and neopelex are mixed
It closes uniformly, then stirring adjusts pH, staticly settles, remove supernatant, washs after drying in baking oven, is cooled to room temperature to obtain
Material a；Urea, polyvinylpyrrolidone and deionized water are uniformly mixed, sodium chloride stirring is then added in, then adds in nitric acid
Aluminium, chitosan, sodium tripolyphosphate, potassium peroxydisulfate, natural zeolite and zirconium sulfate are uniformly mixed, then heating water bath, are cooled to room
Disodium hydrogen phosphate is added in after temperature to be uniformly mixed, stirs, is then aged, filtration washing, and dry, calcining postcooling to room temperature is resisted
Bacterium modified additive is applied in the preparation of unsaturated polyester resin of the present invention, under the action of silane coupling agent KH-560, is realized
With the major ingredient of unsaturated polyester resin carrying out grafting is combined, and effectively increases the anti-microbial property of unsaturated polyester resin.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this hair
Bright rather than for limiting the invention, any modification made on the basis of the present invention, equivalent replacement etc. are in this hair
In bright protection domain.
In embodiment, the antibacterial unsaturated polyester resin, as unit of parts by weight, including following raw material：It is unsaturated
80-120 parts of polyester resin, 15-25 parts of isophthalic anhydride, 4-9 parts of phthalic anhydride, 3-6 parts of benzenetriol, hydroquinone 2-
5 parts, 1-4 parts of cobalt naphthenate, 3-5 parts of styrene, 2-6 parts of methyl ethyl ketone peroxide, 4-8 parts of phosphate melamine, ethylene glycol 2-6
Part, 1-5 parts of organosilicon, 3-9 parts of aluminium hydroxide, 2-5 parts of carbon nanotubes, N, 1-4 parts of accelerine, 2-5 parts of nano zinc powder,
3-6 parts of kaolin, 2-8 parts of calcium sulfate crystal whiskers, 4-8 parts of nano imvite, 6-9 parts of nano-titanium dioxide, silane coupling agent KH-
560 1-3 parts, it is auxiliary agent 15-25 parts antibacterial modified.
The antibacterial modified auxiliary agent is prepared by following technique：By weight by 15-25 parts of diatomite, 4-8 parts of titanium whites
Powder and 3-9 parts of neopelexes are uniformly mixed, in 650-850r/min rotating speeds stir 20-40min, then adjust pH to
0.5-1.5 is staticly settled, and removes supernatant, is washed after 20-30h dry in 50-70 DEG C of baking oven, is cooled to room temperature to obtain object
Expect a；4-6 parts of urea, 2-8 parts of polyvinylpyrrolidones and 10-20 parts of deionized waters are uniformly mixed, then add in 4-8 parts of chlorine
Change sodium stirring 10-30min, then add in 3-6 parts of aluminum nitrates, 2-5 parts of chitosans, 1-4 parts of sodium tripolyphosphates, 3-5 parts of persulfuric acid
Potassium, 2-5 part natural zeolite and 1-4 parts of zirconium sulfates are uniformly mixed, and then heating water bath is added in 70-90 DEG C after being cooled to room temperature
3-6 parts of disodium hydrogen phosphates are uniformly mixed, and are stirred 10-30min in 650-850r/min rotating speeds, are then aged, filtration washing, do
Dry, calcining postcooling to room temperature obtains antibacterial modified auxiliary agent.
The preparation method of the antibacterial unsaturated polyester resin, includes the following steps：
S1, unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol are uniformly mixed, are warming up to
70-80 DEG C, 20-30min is kept the temperature, is subsequently added into hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate trimerization
Cyanamide, ethylene glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate are brilliant
It must be uniformly mixed, be continuously heating to 70-80 DEG C, keep the temperature 30-50min, then stir 10-20min in 350-450r/min rotating speeds,
It is cooled to room temperature to obtain base-material；
S2, nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent are uniformly mixed, risen
Temperature keeps the temperature 20-40min to 80-90 DEG C, then stirs 5-15min in 1500-2500r/min rotating speeds, is cooled to room temperature and is changed
Property material；
S3, base-material is warming up to 60-80 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, in 1200-
1400r/min rotating speeds stir 2-4h, are cooled to room temperature to obtain antibacterial unsaturated polyester resin.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of antibacterial unsaturated polyester resin, as unit of parts by weight, including following raw material：Unsaturated polyester resin 100
Part, 20 parts of isophthalic anhydride, 6.5 parts of phthalic anhydride, 4.5 parts of benzenetriol, 3.5 parts of hydroquinone, 3 parts of cobalt naphthenate,
4 parts of styrene, 4 parts of methyl ethyl ketone peroxide, 6 parts of phosphate melamine, 4 parts of ethylene glycol, 3 parts of organosilicon, 6 parts of aluminium hydroxide,
3.5 parts of carbon nanotubes, N, 3 parts of accelerine, 3.5 parts of nano zinc powder, 4.5 parts of kaolin, calcium sulfate crystal whiskers 5 part, nanometer
6 parts of montmorillonite, 7.5 parts of nano-titanium dioxide, 2 parts of silane coupling agent KH-560,20 parts of antibacterial modified auxiliary agent.
The antibacterial modified auxiliary agent is prepared by following technique：By weight by 20 parts of diatomite, 6 parts of titanium dioxides and 6
Part neopelex is uniformly mixed, and is stirred 30min in 750r/min rotating speeds, is then adjusted pH to 1, staticly settle, go
Except supernatant, wash after 25h dry in 60 DEG C of baking ovens, be cooled to room temperature to obtain material a；By 5 parts of urea, 5 parts of polyethylene pyrroles
Pyrrolidone and 15 parts of deionized waters are uniformly mixed, and then add in 6 parts of sodium chloride stirring 20min, then add in 4.5 parts of aluminum nitrates,
3.5 parts of chitosans, 3 parts of sodium tripolyphosphates, 4 parts of potassium peroxydisulfates, 3.5 parts of natural zeolites and 3 parts of zirconium sulfates are uniformly mixed, Ran Houshui
Bath is heated to 80 DEG C, and 4.5 parts of disodium hydrogen phosphates are added in after being cooled to room temperature and are uniformly mixed, and 20min is stirred in 750r/min rotating speeds,
Then it is aged, filtration washing, dry, calcining postcooling to room temperature obtains antibacterial modified auxiliary agent.
The preparation method of the antibacterial unsaturated polyester resin, includes the following steps：
S1, unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol are uniformly mixed, are warming up to 75
DEG C, 25min is kept the temperature, is subsequently added into hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine, second
Glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate crystal whiskers mixing are equal
It is even, 75 DEG C are continuously heating to, keeps the temperature 40min, then 15min is stirred in 400r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent are uniformly mixed, risen
Temperature keeps the temperature 30min to 85 DEG C, then stirs 10min in 2000r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 70 DEG C, keeps the temperature 25min, be subsequently added into modified materials and be uniformly mixed, in 1300r/min rotating speeds
3h is stirred, is cooled to room temperature to obtain antibacterial unsaturated polyester resin.
Embodiment 2
A kind of antibacterial unsaturated polyester resin, as unit of parts by weight, including following raw material：Unsaturated polyester resin 80
Part, 25 parts of isophthalic anhydride, 4 parts of phthalic anhydride, 6 parts of benzenetriol, 2 parts of hydroquinone, 4 parts of cobalt naphthenate, styrene 3
Part, 6 parts of methyl ethyl ketone peroxide, 4 parts of phosphate melamine, 6 parts of ethylene glycol, 1 part of organosilicon, 9 parts of aluminium hydroxide, carbon nanotubes
2 parts, N, 4 parts of accelerine, 2 parts of nano zinc powder, 6 parts of kaolin, 2 parts of calcium sulfate crystal whiskers, nano imvite 8 part, nanometer
6 parts of titanium dioxide, 3 parts of silane coupling agent KH-560,15 parts of antibacterial modified auxiliary agent.
The antibacterial modified auxiliary agent is prepared by following technique：By weight by 15 parts of diatomite, 8 parts of titanium dioxides and 3
Part neopelex is uniformly mixed, and is stirred 20min in 850r/min rotating speeds, is then adjusted pH to 1.5, staticly settle,
Supernatant is removed, washs after 30h dry in 50 DEG C of baking ovens, is cooled to room temperature to obtain material a；By 4 parts of urea, 8 parts of polyethylene
Pyrrolidones and 10 parts of deionized waters are uniformly mixed, and are then added in 8 parts of sodium chloride stirring 10min, are then added in 6 parts of aluminum nitrates, 2
Part chitosan, 4 parts of sodium tripolyphosphates, 3 parts of potassium peroxydisulfates, 5 parts of natural zeolites and 1 part of zirconium sulfate are uniformly mixed, and then water-bath adds
Heat adds in 3 parts of disodium hydrogen phosphates to 90 DEG C, after being cooled to room temperature and is uniformly mixed, and 10min is stirred in 850r/min rotating speeds, then old
Change, filtration washing, dry, calcining postcooling to room temperature obtains antibacterial modified auxiliary agent.
The preparation method of the antibacterial unsaturated polyester resin, includes the following steps：
S1, unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol are uniformly mixed, are warming up to 70
DEG C, 30min is kept the temperature, is subsequently added into hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine, second
Glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate crystal whiskers mixing are equal
It is even, 70 DEG C are continuously heating to, keeps the temperature 50min, then 20min is stirred in 350r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent are uniformly mixed, risen
Temperature keeps the temperature 40min to 80 DEG C, then stirs 15min in 1500r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 60 DEG C, keeps the temperature 35min, be subsequently added into modified materials and be uniformly mixed, in 1200r/min rotating speeds
4h is stirred, is cooled to room temperature to obtain antibacterial unsaturated polyester resin.
Embodiment 3
A kind of antibacterial unsaturated polyester resin, as unit of parts by weight, including following raw material：Unsaturated polyester resin 120
Part, 15 parts of isophthalic anhydride, 9 parts of phthalic anhydride, 3 parts of benzenetriol, 5 parts of hydroquinone, 1 part of cobalt naphthenate, styrene 5
Part, 2 parts of methyl ethyl ketone peroxide, 8 parts of phosphate melamine, 2 parts of ethylene glycol, 5 parts of organosilicon, 3 parts of aluminium hydroxide, carbon nanotubes
5 parts, N, 1 part of accelerine, 5 parts of nano zinc powder, 3 parts of kaolin, 8 parts of calcium sulfate crystal whiskers, nano imvite 4 part, nanometer
9 parts of titanium dioxide, 1 part of silane coupling agent KH-560,25 parts of antibacterial modified auxiliary agent.
The antibacterial modified auxiliary agent is prepared by following technique：By weight by 25 parts of diatomite, 4 parts of titanium dioxides and 9
Part neopelex is uniformly mixed, and is stirred 40min in 650r/min rotating speeds, is then adjusted pH to 0.5, staticly settle,
Supernatant is removed, washs after 20h dry in 70 DEG C of baking ovens, is cooled to room temperature to obtain material a；By 6 parts of urea, 2 parts of polyethylene
Pyrrolidones and 20 parts of deionized waters are uniformly mixed, and are then added in 4 parts of sodium chloride stirring 30min, are then added in 3 parts of aluminum nitrates, 5
Part chitosan, 1 part of sodium tripolyphosphate, 5 parts of potassium peroxydisulfates, 2 parts of natural zeolites and 4 parts of zirconium sulfates are uniformly mixed, and then water-bath adds
Heat adds in 6 parts of disodium hydrogen phosphates to 70 DEG C, after being cooled to room temperature and is uniformly mixed, and 30min is stirred in 650r/min rotating speeds, then old
Change, filtration washing, dry, calcining postcooling to room temperature obtains antibacterial modified auxiliary agent.
The preparation method of the antibacterial unsaturated polyester resin, includes the following steps：
S1, unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol are uniformly mixed, are warming up to 80
DEG C, 20min is kept the temperature, is subsequently added into hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine, second
Glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate crystal whiskers mixing are equal
It is even, 80 DEG C are continuously heating to, keeps the temperature 30min, then 10min is stirred in 450r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent are uniformly mixed, risen
Temperature keeps the temperature 20min to 90 DEG C, then stirs 5min in 2500r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 80 DEG C, keeps the temperature 15min, be subsequently added into modified materials and be uniformly mixed, in 1400r/min rotating speeds
2h is stirred, is cooled to room temperature to obtain antibacterial unsaturated polyester resin.
Comparative example 1
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the raw material of antibacterial unsaturated polyester resin
In lack nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent.
Comparative example 2
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the raw material of antibacterial unsaturated polyester resin
In lack nano imvite.
Comparative example 3
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the raw material of antibacterial unsaturated polyester resin
In lack nano-titanium dioxide.
Comparative example 4
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the raw material of antibacterial unsaturated polyester resin
In lack silane coupling agent KH-560.
Comparative example 5
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the raw material of antibacterial unsaturated polyester resin
In lack antibacterial modified auxiliary agent.
Comparative example 6
Using a kind of Chinese patent application document " unsaturated polyester resin and preparation method thereof (application publication number：
CN102532424A) " technique of embodiment 1 prepares unsaturated polyester resin.
The unsaturated polyester resin for measuring embodiment 1-3 and comparative example 1-6 carries out indices detection, obtained detection knot
Fruit such as following table：
| Experimental project | Bacteriostasis rate/% (Escherichia coli) |
| Embodiment 1 | 99.64 |
| Embodiment 2 | 98.83 |
| Embodiment 3 | 98.41 |
| Comparative example 1 | 23.12 |
| Comparative example 2 | 94.23 |
| Comparative example 3 | 91.35 |
| Comparative example 4 | 87.63 |
| Comparative example 5 | 81.68 |
| Comparative example 6 | 2.45 |
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that using the anti-of embodiment 1-3 antibacterial unsaturated polyester resins
Bacterium performance significantly improves；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that nano imvite, nano-titanium dioxide, silane coupling agent
KH-560, antibacterial modified auxiliary agent add play synergistic effect in antibacterial unsaturated polyester resin is prepared simultaneously, significantly improve
The anti-microbial property of antibacterial unsaturated polyester resin, this may be：Nano imvite, nano-titanium dioxide, silane coupling agent KH-
560th, antibacterial modified auxiliary agent is applied to as modified system in the preparation of unsaturated polyester resin, and silane coupling agent KH- is utilized
560 graft modification effect, realizes nano imvite, the hydroxyl of nano-titanium dioxide and antibacterial modified auxiliary agent surface and insatiable hunger
Grafting is realized with the base-material of polyester resin, imparts the excellent anti-microbial property of unsaturated polyester resin, while antibacterial is utilized and changes
The antibacterial humidification of property auxiliary agent, wherein antibacterial modified auxiliary agent is by the way that diatomite, titanium dioxide and neopelex are mixed
It closes uniformly, then stirring adjusts pH, staticly settles, remove supernatant, washs after drying in baking oven, is cooled to room temperature to obtain
Material a；Urea, polyvinylpyrrolidone and deionized water are uniformly mixed, sodium chloride stirring is then added in, then adds in nitric acid
Aluminium, chitosan, sodium tripolyphosphate, potassium peroxydisulfate, natural zeolite and zirconium sulfate are uniformly mixed, then heating water bath, are cooled to room
Disodium hydrogen phosphate is added in after temperature to be uniformly mixed, stirs, is then aged, filtration washing, and dry, calcining postcooling to room temperature is resisted
Bacterium modified additive is applied in the preparation of unsaturated polyester resin of the present invention, under the action of silane coupling agent KH-560, is realized
With the major ingredient of unsaturated polyester resin carrying out grafting is combined, and effectively increases the anti-microbial property of unsaturated polyester resin.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of antibacterial unsaturated polyester resin, which is characterized in that including following raw material：Unsaturated polyester resin, isophthalic diformazan
Acid anhydrides, phthalic anhydride, benzenetriol, hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine
Amine, ethylene glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate crystal whiskers,
Nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent；
The nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent weight ratio be (4-8)：
(6-9)：(1-3)：(15-25).
2. antibacterial unsaturated polyester resin according to claim 1, which is characterized in that the nano imvite, nanometer two
Titanium oxide, silane coupling agent KH-560, antibacterial modified auxiliary agent weight ratio be 6：7.5：2：20.
3. antibacterial unsaturated polyester resin according to claim 1 or 2, which is characterized in that as unit of parts by weight, including
Following raw material：80-120 parts of unsaturated polyester resin, 15-25 parts of isophthalic anhydride, 4-9 parts of phthalic anhydride, benzenetriol
3-6 parts, 2-5 parts of hydroquinone, 1-4 parts of cobalt naphthenate, 3-5 parts of styrene, 2-6 parts of methyl ethyl ketone peroxide, phosphate melamine
4-8 parts of amine, 2-6 parts of ethylene glycol, 1-5 parts of organosilicon, 3-9 parts of aluminium hydroxide, 2-5 parts of carbon nanotubes, N, accelerine 1-4
Part, 2-5 parts of nano zinc powder, 3-6 parts of kaolin, 2-8 parts of calcium sulfate crystal whiskers, 4-8 parts of nano imvite, nano-titanium dioxide 6-9
It is part, 1-3 parts of silane coupling agent KH-560, auxiliary agent 15-25 parts antibacterial modified.
4. according to claim 1-3 any one of them antibacterial unsaturated polyester resins, which is characterized in that described antibacterial modified to help
The raw material of agent includes by weight：15-25 parts of diatomite, 4-8 parts of titanium dioxide, 3-9 parts of neopelex, urea 4-6
Part, 2-8 parts of polyvinylpyrrolidone, 10-20 parts of deionized water, 4-8 parts of sodium chloride, 3-6 parts of aluminum nitrate, 2-5 parts of chitosan, three
1-4 parts of polyphosphate sodium, 3-5 parts of potassium peroxydisulfate, 2-5 parts of natural zeolite, 1-4 parts of zirconium sulfate, 3-6 parts of disodium hydrogen phosphate.
5. according to claim 1-4 any one of them antibacterial unsaturated polyester resins, which is characterized in that described antibacterial modified to help
Agent is prepared by following technique：Diatomite, titanium dioxide and neopelex are uniformly mixed, in 650-850r/min
Rotating speed stirs 20-40min, then adjusts pH to 0.5-1.5, staticly settles, and removes supernatant, washs after 50-70 DEG C of baking oven
Middle dry 20-30h is cooled to room temperature to obtain material a；Urea, polyvinylpyrrolidone and deionized water are uniformly mixed, then
Sodium chloride stirring 10-30min is added in, then adds in aluminum nitrate, chitosan, sodium tripolyphosphate, potassium peroxydisulfate, natural zeolite and sulphur
Sour zirconium is uniformly mixed, and then heating water bath adds in disodium hydrogen phosphate to 70-90 DEG C, after being cooled to room temperature and is uniformly mixed, in 650-
850r/min rotating speeds stir 10-30min, are then aged, filtration washing, dry, and calcining postcooling to room temperature obtains antibacterial modified
Auxiliary agent.
6. a kind of preparation method according to claim 1-5 any one of them antibacterial unsaturated polyester resins, which is characterized in that
Include the following steps：
S1, unsaturated polyester resin, isophthalic anhydride, phthalic anhydride, benzenetriol are uniformly mixed, are warming up to 70-80
DEG C, keep the temperature 20-30min, be subsequently added into hydroquinone, cobalt naphthenate, styrene, methyl ethyl ketone peroxide, phosphate melamine,
Ethylene glycol, organosilicon, aluminium hydroxide, carbon nanotubes, N, accelerine, nano zinc powder, kaolin, calcium sulfate crystal whiskers mixing
Uniformly, 70-80 DEG C is continuously heating to, keeps the temperature 30-50min, then 10-20min is stirred in 350-450r/min rotating speeds, is cooled to
Room temperature obtains base-material；
S2, nano imvite, nano-titanium dioxide, silane coupling agent KH-560, antibacterial modified auxiliary agent are uniformly mixed, are warming up to
80-90 DEG C, 20-40min is kept the temperature, then 5-15min is stirred in 1500-2500r/min rotating speeds, is cooled to room temperature and is modified
Material；
S3, base-material is warming up to 60-80 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, in 1200-1400r/
Min rotating speeds stir 2-4h, are cooled to room temperature to obtain antibacterial unsaturated polyester resin.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485149A (en) * | 2018-03-22 | 2018-09-04 | 长沙小新新能源科技有限公司 | A kind of high hydroscopic resin and preparation method thereof |
| CN110577790A (en) * | 2019-09-01 | 2019-12-17 | 合众（佛山）化工有限公司 | Premixed flame-retardant antibacterial radiation-proof multifunctional water-based paint |
| CN113101891A (en) * | 2021-04-16 | 2021-07-13 | 中北大学 | A kind of high nitrogen carbon-based zirconium phosphate broad-spectrum gas adsorbent and its preparation method and application |
| CN113693080A (en) * | 2021-07-27 | 2021-11-26 | 李艳红 | Graphene ion sterilizing and antibacterial liquid and preparation method thereof |
-
2017
- 2017-12-30 CN CN201711486216.3A patent/CN108192357A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485149A (en) * | 2018-03-22 | 2018-09-04 | 长沙小新新能源科技有限公司 | A kind of high hydroscopic resin and preparation method thereof |
| CN110577790A (en) * | 2019-09-01 | 2019-12-17 | 合众（佛山）化工有限公司 | Premixed flame-retardant antibacterial radiation-proof multifunctional water-based paint |
| CN113101891A (en) * | 2021-04-16 | 2021-07-13 | 中北大学 | A kind of high nitrogen carbon-based zirconium phosphate broad-spectrum gas adsorbent and its preparation method and application |
| CN113693080A (en) * | 2021-07-27 | 2021-11-26 | 李艳红 | Graphene ion sterilizing and antibacterial liquid and preparation method thereof |
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