CN105647453B - Anti-corrosive antibacterial epoxy sealing glue and preparation method thereof - Google Patents
Anti-corrosive antibacterial epoxy sealing glue and preparation method thereof Download PDFInfo
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- CN105647453B CN105647453B CN201610031328.9A CN201610031328A CN105647453B CN 105647453 B CN105647453 B CN 105647453B CN 201610031328 A CN201610031328 A CN 201610031328A CN 105647453 B CN105647453 B CN 105647453B
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- 239000003292 glue Substances 0.000 title claims abstract description 62
- 239000004593 Epoxy Substances 0.000 title claims abstract description 27
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 16
- 238000007789 sealing Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 14
- -1 morpholine quaternary ammonium salt Chemical class 0.000 claims abstract description 14
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Natural products C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 150000001805 chlorine compounds Chemical class 0.000 claims abstract description 4
- 239000003822 epoxy resin Substances 0.000 claims abstract description 4
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- UJMDYLWCYJJYMO-UHFFFAOYSA-N benzene-1,2,3-tricarboxylic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1C(O)=O UJMDYLWCYJJYMO-UHFFFAOYSA-N 0.000 claims description 8
- HSTOKWSFWGCZMH-UHFFFAOYSA-N 3,3'-diaminobenzidine Chemical class C1=C(N)C(N)=CC=C1C1=CC=C(N)C(N)=C1 HSTOKWSFWGCZMH-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920002480 polybenzimidazole Polymers 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- YTVNOVQHSGMMOV-UHFFFAOYSA-N naphthalenetetracarboxylic dianhydride Chemical compound C1=CC(C(=O)OC2=O)=C3C2=CC=C2C(=O)OC(=O)C1=C32 YTVNOVQHSGMMOV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000004693 Polybenzimidazole Substances 0.000 claims 1
- 229920000137 polyphosphoric acid Polymers 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 239000007822 coupling agent Substances 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000000565 sealant Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 229940106691 bisphenol a Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 2
- 229940100630 metacresol Drugs 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 229920006389 polyphenyl polymer Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- 229910001335 Galvanized steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000006159 dianhydride group Chemical group 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008397 galvanized steel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000004173 sunset yellow FCF Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/56—Amines together with other curing agents
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/35—Heterocyclic compounds having nitrogen in the ring having also oxygen in the ring
- C08K5/357—Six-membered rings
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
Abstract
The invention discloses a kind of anti-corrosive antibacterial epoxy sealing glues, including component A glue and B component glue, wherein component A glue includes：Bisphenol A type epoxy resin, epoxy silane coupling agent KH 560, dry vapor silica, 2,3 epoxypropyltrimethylchloride chlorides and epoxy morpholine quaternary ammonium salt；B component glue includes：Amino-terminated poly- pyrrole throat prepolymer, phenolic aldehyde amine and amino silicane coupling agent KH 550.The invention also discloses the preparation methods of the anti-corrosive antibacterial epoxy sealing glue.
Description
Technical field
The invention belongs to high molecule sealing materials technical fields, more particularly it relates to a kind of anti-corrosive antibacterial epoxy
Fluid sealant and preparation method thereof.
Background technology
Epoxy sealing glue use scope is wide, has a very reliable and easy to use advantage of sealing effect, but due to
Raw material are inflammable, cause some potential safety problems, although can be made moderate progress by the way that inorganic combustion inhibitor is added, often exist
The problem of compatibility, and reduce the intensity of fluid sealant.It is also uncommon and in order to adapt to different use environments and reduce difficulty of construction
Epoxy sealing glue is hoped to have the ability of preferable acid/alkali-corrosion-resistant and the ability of room temperature curing.Further, since fluid sealant is usually
Applied in home life, such as kitchen, it is also desirable to which it has certain anti-microbial property, more safety and environmental protection.
Hence it is highly desirable to by the improvement of formula and production technology, to obtain a kind of ambient temperature curable, and has height
The epoxy sealing glue of intensity, high fire-retardance, high antibacterial and high antiseptic property.
Invention content
To solve the above-mentioned problems, one aspect of the present invention provides a kind of anti-corrosive antibacterial epoxy sealing glue, including component A
The weight ratio of glue and B component glue, component A glue and B component glue is A:B=4:1, wherein：
Component A glue includes：The bisphenol A type epoxy resin of 100 parts by weight, 5 parts by weight epoxy silane coupling agent KH-560,
The epoxy of the dry vapor silica of 10 parts by weight, 2, the 3- epoxypropyltrimethylchloride chlorides of 5 parts by weight and 5 parts by weight
The structural formula of morpholine quaternary ammonium salt, the epoxy morpholine quaternary ammonium salt is：
B component glue includes：The amino-terminated poly- pyrrole throat prepolymer of 50 parts by weight, the phenolic aldehyde amine and 5 parts by weight of 5 parts by weight
Amino silicane coupling agent KH-550；
The amino-terminated poly- pyrrole throat prepolymer is prepared by following methods：
The 1,4,5,8 naphthalenetetracarboxylic acid dianhydride and 1000mL of 0.95 mole of addition in the three-necked flask being completely dried
Metacresol stirs under nitrogen protection, after dianhydride is completely dissolved, 1 mole of 3,3 '-diaminobenzidines is added, in room temperature
After lower stirring 30min, 75 DEG C are heated to, reacts 3.5h, then at 185 DEG C, reacts 4.5h；After reaction, it is down to room temperature,
Solution pours into methanol, there is Precipitation；It is washed with methanol after being filtered after removing solvent, is dried at 50 DEG C in vacuum drying oven repeatedly
It is dry for 24 hours to get.
In one embodiment, the anti-corrosive antibacterial epoxy sealing glue, wherein the B component glue further includes 10 weights
Measure part amino-terminated hyperbranched polybenzimidazoles, the amino-terminated hyperbranched polybenzimidazoles by following methods prepare and
At：
By 0.2 mole 3,3 '-diaminobenzidines are first dissolved in 1000 grams of poly phosphorus containing 85wt% phosphorus pentoxides
In acid, then benzenetricarboxylic acid between the 1 of 0.07 mole, 3,5- is added in reaction solution, after being reacted 15 hours at 220 DEG C, is down to room
Temperature in precipitating to water, is then neutralized with ammonium hydroxide, is filtered, is dried in vacuo at 100 DEG C, obtains amino-terminated hyperbranched polyphenyl simultaneously
Imidazoles.
Another aspect of the present invention provides the preparation method of anti-corrosive antibacterial epoxy sealing glue, including：
The ingredient of the component A glue is mixed at 50 DEG C, 30 points are dispersed with stirring with 1000 revs/min of speed mechanical
Clock is to get component A glue；
The ingredient of the B component glue is mixed at 50 DEG C, 30 points are dispersed with stirring with 1000 revs/min of speed mechanical
Clock is to get B component glue.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to following detailed description.
Specific implementation mode
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used
In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of aforementioned present invention, still fall within protection scope of the present invention.
Raw material：
3,3 '-diaminobenzidines, Isosorbide-5-Nitrae, 5,8- naphthalenetetracarbacidic acidic dianhydrides and 1, benzenetricarboxylic acid is purchased from CTI between 3,5-, and
It directly uses, without being further purified.Dry vapor silica is purchased from Shenyang Chemical Co., Ltd..Bisphenol-A epoxy tree
Fat (E51), KH-560, phenolic aldehyde amine and KH-550 are purchased from Sinopharm Chemical Reagent Co., Ltd..Other raw materials be purchased from Ah
Latin reagent Co., Ltd.
A1：Bisphenol A epoxide resin (E51)；
B1：Epoxy silane coupling agent KH-560；
C1：Dry vapor silica；
D1：2,3- epoxypropyltrimethylchloride chlorides；
E1：The structural formula of epoxy morpholine quaternary ammonium salt, the epoxy morpholine quaternary ammonium salt is：
And preparation method is：In dry three-necked bottle, 100ml second cyanogen is first added, then sequentially adds the N- first of 0.1mol
The epoxychloropropane of base morpholine and 0.1mol；After being sufficiently stirred, logical inert gas is simultaneously warming up to 50 DEG C, and reaction stops after 48 hours
Heating filters and fully washs obtained epoxy morpholine quaternary ammonium salt with ether, then washed with acetone, in vacuum drying oven fully
Dried for standby；
F1：Amino-terminated poly- pyrrole throat prepolymer, is prepared by following methods：
The 1,4,5,8 naphthalenetetracarboxylic acid dianhydride and 1000mL of 0.95 mole of addition in the three-necked flask being completely dried
Metacresol stirs under nitrogen protection, after dianhydride is completely dissolved, 1 mole of 3,3 '-diaminobenzidines is added, in room temperature
After lower stirring 30min, 75 DEG C are heated to, reacts 3.5h, then at 185 DEG C, reacts 4.5h；After reaction, it is down to room temperature,
Solution pours into methanol, there is Precipitation；It is washed with methanol after being filtered after removing solvent, is dried at 50 DEG C in vacuum drying oven repeatedly
It is dry for 24 hours to get；
G1：Phenolic aldehyde amine；
H1：KH-550；
I1：Amino-terminated hyperbranched polybenzimidazoles, is prepared by following methods：
By 0.2 mole 3,3 '-diaminobenzidines are first dissolved in 1000 grams of poly phosphorus containing 85wt% phosphorus pentoxides
In acid, then benzenetricarboxylic acid between the 1 of 0.07 mole, 3,5- is added in reaction solution, after being reacted 15 hours at 220 DEG C, is down to room
Temperature in precipitating to water, is then neutralized with ammonium hydroxide, is filtered, is dried in vacuo at 100 DEG C, obtains amino-terminated hyperbranched polyphenyl simultaneously
Imidazoles.
Embodiment 1：
Component A：By A1100 parts by weight, B15 parts by weight, C110 parts by weight, D15 parts by weight and E15 parts by weight are at 50 DEG C
Lower mixing is dispersed with stirring 30 minutes to get component A glue with 1000 revs/min of speed mechanical；
B component：By F150 parts by weight, G15 parts by weight and H15 parts by weight mix at 50 DEG C, with 1000 revs/min
Speed mechanical is dispersed with stirring 30 minutes to get B component glue；
By component A glue and B component glue component A in proportion when use：B=4：1 is uniformly mixed, and constructs in 2 hours, room temperature
It is fully cured within lower 5 hours.
Embodiment 2：
Component A：By A1100 parts by weight, B15 parts by weight, C110 parts by weight, D15 parts by weight and E15 parts by weight are at 50 DEG C
Lower mixing is dispersed with stirring 30 minutes to get component A glue with 1000 revs/min of speed mechanical；
B component：By F150 parts by weight, G15 parts by weight, H15 parts by weight and I110 parts by weight mix at 50 DEG C, with
1000 revs/min of speed mechanical is dispersed with stirring 30 minutes to get B component glue；
By component A glue and B component glue component A in proportion when use：B=4：1 is uniformly mixed, and constructs in 2 hours, room temperature
It is fully cured within lower 5 hours.
Comparative example 1
Component A：By A1100 parts by weight, B15 parts by weight, C110 parts by weight and D110 parts by weight mix at 50 DEG C, with
1000 revs/min of speed mechanical is dispersed with stirring 30 minutes to get component A glue；
B component：By F150 parts by weight, G15 parts by weight, H15 parts by weight and I110 parts by weight mix at 50 DEG C, with
1000 revs/min of speed mechanical is dispersed with stirring 30 minutes to get B component glue；
By component A glue and B component glue component A in proportion when use：B=4：1 is uniformly mixed, and constructs in 2 hours, room temperature
It is fully cured within lower 5 hours.
Comparative example 2
Component A：By A1100 parts by weight, B15 parts by weight, C110 parts by weight and E110 parts by weight mix at 50 DEG C, with
1000 revs/min of speed mechanical is dispersed with stirring 30 minutes to get component A glue；
B component：By F150 parts by weight, G15 parts by weight, H15 parts by weight and I110 parts by weight mix at 50 DEG C, with
1000 revs/min of speed mechanical is dispersed with stirring 30 minutes to get B component glue；
By component A glue and B component glue component A in proportion when use：B=4：1 is uniformly mixed, and constructs in 2 hours, room temperature
It is fully cured within lower 5 hours.
Comparative example 3
Component A：By A1100 parts by weight, B15 parts by weight, C110 parts by weight, D12 parts by weight and E18 parts by weight are at 50 DEG C
Lower mixing is dispersed with stirring 30 minutes to get component A glue with 1000 revs/min of speed mechanical；
B component：By F150 parts by weight, G15 parts by weight, H15 parts by weight and I110 parts by weight mix at 50 DEG C, with
1000 revs/min of speed mechanical is dispersed with stirring 30 minutes to get B component glue；
By component A glue and B component glue component A in proportion when use：B=4：1 is uniformly mixed, and constructs in 2 hours, room temperature
It is fully cured within lower 5 hours.
Comparative example 4
Component A：By A1100 parts by weight, B15 parts by weight, C110 parts by weight, D15 parts by weight and E15 parts by weight are at 50 DEG C
Lower mixing is dispersed with stirring 30 minutes to get component A glue with 1000 revs/min of speed mechanical；
B component：G15 parts by weight and H15 parts by weight are mixed at 50 DEG C, are stirred with 1000 revs/min of speed mechanical
Dispersion is mixed 30 minutes to get B component glue；
By component A glue and B component glue component A in proportion when use：B=4：1 is uniformly mixed, and constructs in 2 hours, room temperature
It is fully cured within lower 5 hours.
Test method
The fluid sealant obtained to above-described embodiment 1~2 and comparative example 1~4 is tested, and to test it to galvanized steel
Cementitiousness, test method is as follows：
Tensile strength：According to ISO527 standard tests.
Shear strength：According to ISO1465 standard tests.
T-type peel strength：According to GB-T2790 standard tests.
High temperature resistance：Shear strength at 200 DEG C of test.
Alkaline resistance properties：Gained fluid sealant is immersed in the sodium hydrate aqueous solution of 50 DEG C of 1mol/L, is surveyed after 24 hours
Try its loss of tensile strength rate.
Acid resistance：Gained fluid sealant is immersed in the aqueous sulfuric acid of 50 DEG C of 1mol/L, it is tested after 24 hours
Loss of tensile strength rate.
Anti-microbial property：It is measured according to Japanese Industrial Standards JISZ2801.
Antibacterial stability：Made sample is immersed in 80 DEG C of water, after a week, tests the loss of its antibacterial activity value
Amount, computational methods are：Activity value loss amount=(Escherichia coli antibacterial is lived after Escherichia coli antibacterial activity value-test before test
Property value) Escherichia coli antibacterial activity value before/test.
Flame retardant property：According to 2046 standard test oxygen index (OI)s of GB/T.
Test result is shown in Table 1 and table 2.
Table 1
Table 2
Data above can be seen that and not use mixed type epoxy quaternary ammonium salt, amino-terminated poly- pyrrole throat prepolymer and ammonia
The product of the terminated hyperbranched polybenzimidazoles of base is compared, and fluid sealant prepared by the present invention also has while having high intensity
Better flame resistance, anti-microbial property and antiseptic property thus provide the advantageous effects of the present invention.
Example above-mentioned is merely illustrative, some features of the feature for explaining the disclosure.The attached claims
It is intended to the range as wide as possible for requiring to be contemplated that, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation.Therefore, the purpose of applicant is that the attached claims are not illustrated the present invention
Feature exemplary selectional restriction.And the progress in science and technology will be formed language express inaccuracy due to and not
The possible equivalent or son being presently considered are replaced, and these variations also should in the conceived case be interpreted by appended
Claim covers.
Claims (2)
1. the weight ratio of anti-corrosive antibacterial epoxy sealing glue, including component A glue and B component glue, component A glue and B component glue is A:B=
4:1, wherein：
Component A glue includes：The bisphenol A type epoxy resin of 100 parts by weight, the epoxy silane coupling agent KH-560 of 5 parts by weight, 10 weights
Measure the dry vapor silica, 2, the 3- epoxypropyltrimethylchloride chlorides of 5 parts by weight and the epoxy morpholine of 5 parts by weight of part
The structural formula of quaternary ammonium salt, the epoxy morpholine quaternary ammonium salt is：
B component glue includes：Amino-terminated poly- pyrrole throat prepolymer, the phenolic aldehyde amine of 5 parts by weight and the ammonia of 5 parts by weight of 50 parts by weight
Base silane coupling agent KH-550；
The amino-terminated poly- pyrrole throat prepolymer is prepared by following methods：
First between 0.95 mole of 1,4,5,8 naphthalenetetracarboxylic acid dianhydride and 1000mL is added in the three-necked flask being completely dried
Phenol stirs under nitrogen protection, after dianhydride is completely dissolved, 1 mole of 3,3 '-diaminobenzidines is added, stir at room temperature
After mixing 30min, 75 DEG C are heated to, reacts 3.5h, then at 185 DEG C, reacts 4.5h；After reaction, it is down to room temperature, solution
It pours into methanol, there is Precipitation；It is washed with methanol after being filtered after removing solvent, is dried at 50 DEG C in vacuum drying oven repeatedly
For 24 hours to get,
The B component glue further includes the amino-terminated hyperbranched polybenzimidazoles of 10 parts by weight, described amino-terminated hyperbranched poly-
Benzimidazole is prepared by following methods：By 0.2 mole 3,3 '-diaminobenzidines are first dissolved in be aoxidized containing 85wt% five
In 1000 grams of polyphosphoric acids of two phosphorus, then benzenetricarboxylic acid between the 1 of 0.07 mole, 3,5- is added in reaction solution, it is anti-at 220 DEG C
After answering 15 hours, it is down to room temperature, in precipitating to water, is then neutralized with ammonium hydroxide, filters, be dried in vacuo at 100 DEG C, obtain amino
Terminated hyperbranched polybenzimidazoles.
2. the preparation method of anti-corrosive antibacterial epoxy sealing glue, including：By the ingredient of component A glue described in claim 1 at 50 DEG C
Lower mixing is dispersed with stirring 30 minutes to get component A glue with 1000 revs/min of speed mechanical；By B groups described in claim 1
Divide the ingredient of glue to be mixed at 50 DEG C, 30 minutes are dispersed with stirring to get B component glue with 1000 revs/min of speed mechanical.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120865A (en) * | 2010-12-30 | 2011-07-13 | 宏昌电子材料股份有限公司 | Epoxy-phenolic aldehyde amine composition and preparation method and application thereof |
| CN102139190A (en) * | 2011-01-07 | 2011-08-03 | 上海交通大学 | Method for preparing epoxy morpholine quaternary ammonium salt-modified polybenzimidazole anion exchange membrane |
| WO2014179975A1 (en) * | 2013-05-10 | 2014-11-13 | Dow Global Technologies Llc | Epoxy resin compositions |
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2016
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120865A (en) * | 2010-12-30 | 2011-07-13 | 宏昌电子材料股份有限公司 | Epoxy-phenolic aldehyde amine composition and preparation method and application thereof |
| CN102139190A (en) * | 2011-01-07 | 2011-08-03 | 上海交通大学 | Method for preparing epoxy morpholine quaternary ammonium salt-modified polybenzimidazole anion exchange membrane |
| WO2014179975A1 (en) * | 2013-05-10 | 2014-11-13 | Dow Global Technologies Llc | Epoxy resin compositions |
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