CN106381017B - A kind of low-temperature setting antimicrobial form epoxy coating and preparation method thereof - Google Patents
A kind of low-temperature setting antimicrobial form epoxy coating and preparation method thereof Download PDFInfo
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a kind of low-temperature setting antimicrobial form epoxy coatings, it is by component A system and B component system with 1：（0.5~1）Parts by weight proportioning be mixed to prepare, steps are as follows：(1) ratio weighs epoxy resin in parts by weight：80~100 parts, epoxy resin diluent：5~20 parts, antifoaming agent：5~3 parts, filler：0~30 part is mixed, and is stirred 10min, is obtained component A mixture, that is, obtains component A system；(2) ratio weighs antimicrobial form curing agent in parts by weight：30~70 parts, coloring pigment：1~10 part, accelerating agent 0：1~20 part is mixed, and is stirred 5min, is obtained B component mixture, that is, obtains B component system；(3) component A system and B component system are matched into uniform mixing in parts by weight, obtains antimicrobial form epoxy coating.The coating contains the low molecular chitosan and phenolic hydroxyl group, parahelium base class low temperature active group of antibacterial, and bactericidal properties are lasting, can rapid curing at low ambient temperatures, it is good with substrate bonding.
Description
Technical field
The present invention relates to a kind of coating composite material and preparation methods, more particularly to a kind of low-temperature setting antibacterial type ring
Oxygen cold coating and preparation method thereof is applied to coating new material technology field.
Background technology
Epoxy coating is because it is with excellent low cure shrinkage, caking property, wearability, electrical insulating property, chemically-resistant
Drug and be widely used.But epoxy coating is in the prevalence of solidification（Hardening, crosslinking）Temperature is high, in low temperature ring
Difficult solidification under border, it is big not have antibiotic property, inflammable, solidfied material poor toughness, brittleness, limits it and is more widely used.In order to drop
The solidification temperature of low powder coating improves solidification effect and endowing antibacterial energy of the epoxy coating in low temperature environment,
Meet the requirement of some certain applications, develop the epoxide resin paint solidifying agent with antibiotic property is very significant
's.
Make curing agent, still, epoxy resin using polyamines or low molecule mercaptan compound mostly in epoxy coating
Polyamines in curing agent is readily volatilized, has larger damage to human respiratory, and low molecule mercaptan compound smell is big, and cures
Object brittleness is larger, and bad adhesion does not have antibiotic property.
Invention content
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
Low-temperature setting antimicrobial form epoxy coating and preparation method thereof, the epoxy coating contain the low molecular chitosan of antibacterial with
And phenolic hydroxyl group, thiocarbonyl, parahelium base class low temperature active group, bactericidal properties are lasting, can rapid curing at low ambient temperatures, with base
Material cementability is good.
In order to achieve the above objectives, using following technical proposals：
A kind of low-temperature setting antimicrobial form epoxy coating, it is made of component A system and B component system, component A system
With B component system with 1：（0.5~1）Parts by weight proportioning be mixed to prepare：
Wherein component A system is based in parts by weight, including raw material is as follows：
80~100 parts of epoxy resin；
5~20 parts of epoxy resin diluent；
0.5~3 part of antifoaming agent；
0~30 part of filler；
Wherein B component system is based in parts by weight, including raw material is as follows：
30~70 parts of antimicrobial form curing agent；
1~10 part of coloring pigment；
1~20 part of accelerating agent.
Further, the epoxy resin is E-44 bisphenol A-type liquid epoxies resin, E-51 bisphenol A-type liquid epoxy trees
In fat and E-20 bisphenol A-type liquid epoxy resins any one or it is arbitrary several.
Further, the epoxy resin diluent be allyl glycidyl ether, n-butyl glycidyl ether, phenyl
In glycidol ether and furfuryl alcohol glycidol ether any one or it is arbitrary several.
Further, the antifoaming agent is any one in hydroxyl dimethyl silicone polymer and organic modified polyorganosiloxane
Or it is arbitrary several.
Further, the filler be in titanium dioxide, calcium carbonate, mica powder and silica flour any one or it is arbitrary several
Kind.
Further, the coloring pigment is in pigment, phthalein blueness red pigment, phthalocyanine blue pigment and dark green pigment
Any one is arbitrary several.
Further, the accelerating agent be phenol, salicylic acid and 2,4,6 ,-three（Dimethylamino methyl）Phenol（DMP-30）
In any one or it is arbitrary several.
A kind of preparation method of low-temperature setting antimicrobial form epoxy coating, includes the following steps：
(1) prepares component A system：Ratio weighs epoxy resin in parts by weight：80~100 parts, epoxy resin dilution
Agent：5~20 parts, antifoaming agent：0.5~3 part, filler：0~30 part is mixed, and is stirred 10min, is obtained component A mixture, i.e.,
Obtain component A system；
(2) prepares B component system：Ratio weighs antimicrobial form curing agent in parts by weight：30~70 parts, coloring pigment：1
~10 parts, accelerating agent：1~20 part is mixed, and is stirred 5min, is obtained B component mixture, that is, obtains B component system；
(3) by the B component system obtained in the component A system obtained in above-mentioned steps (1) and above-mentioned steps (2) according to
1：（0.5~1）Parts by weight proportioning uniformly mixing to get to antimicrobial form epoxy coating.
Antimicrobial form curing agent its preparation process described in above-mentioned steps (2) is：
A certain amount of chitosan is dissolved in a concentration of 10% acetic acid solution of 200ml by (2-1), obtained mixing
Solution carries out being heated to 50~70 DEG C, and ultrasonic degradation is used in combination, and degrade 25~35h, and the sodium hydroxide of dropwise addition a concentration of 10% is molten
Liquid, it is 6~7 to adjust pH value, is filtered to remove precipitation, clear liquid is concentrated, and ethyl alcohol is added, precipitation, separation is precipitated, and be dried in vacuo
Heat up drying in case, and drying temperature is 50~60 DEG C, obtains low molecular chitosan；
Low molecular chitosan and the thiocarbamide mixing that (2-2) obtains above-mentioned steps, obtain mixed reactant, are passed through nitrogen,
Mixed reactant is heated under stiring, is dissolved into liquid in 50~60 DEG C of oil bath heatings, then be warming up to 125~135 DEG C of progress
Reaction is stirred with 200~400r/min rotating speeds, after 2~3h of isothermal reaction, is cooled to 55 DEG C and constant temperature 2h, is stopped heating, is stirred
Mix, be cooled to room temperature discharging, obtain thiocarbamide modified amine, wherein low molecular chitosan in the hybrid reaction objects system with
The mass ratio of thiocarbamide is 1:（0.5~1）；
(2-3) mixes the thiocarbamide modified amine obtained in above-mentioned steps b and 30.4g anacardols, heats under stiring, then
Paraformaldehyde is added, mixed reactant is passed through nitrogen, 45~55 DEG C is heated under stirring, thiocarbamide modified amine and anacardol mix
Reactant is dissolved into liquid reactant, and most 90~110 DEG C of heating is reacted, and is stirred with 300~500r/min rotating speeds, constant temperature
React 2.5h, slow cooling to 55 DEG C and constant temperature 2h stops heating, stirring, is cooled to room temperature discharging, then at 105 DEG C into
Row vacuum distillation, distillation air pressure are 0.13~0.26kPa, remove moisture, obtain antimicrobial form curing agent after cooling, wherein described
Mixed reactant in long alkyl chain phenol and the mass ratio of thiocarbamide modified amine be（0.5~1.1）:1, the mixed reactant
In paraformaldehyde and the mass ratio of thiocarbamide modified amine be（0.5~0.9）:1 .
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage：
1. the low-temperature setting antimicrobial form epoxy coating of the present invention uses low molecular chitosan and phenol containing antibiotic property
Hydroxyl, thiocarbonyl, parahelium base class low temperature active group, can realize sterilization, moreover it is possible in rapid curing at low temperature, preparation method
Simply, environmentally protective；
It, can be extensively 2. the antimicrobial form epoxy coating easy construction and substrate bonding of the present invention are good, and good flame resistance
Applied to interior decoration.
Specific implementation mode
Details are as follows for the preferred embodiment of the present invention：
Embodiment 1：
A kind of low-temperature setting antimicrobial form epoxy coating, it is made of component A system and B component system, component A system
With B component system with 1：（0.5~1）Parts by weight proportioning be mixed to prepare：
Wherein component A system composition proportion is as follows：
6002 100 parts of epoxy resin；
5746 10 parts of epoxy resin diluents；
1 part of organic modified polyorganosiloxane；
5 parts of silica flour；
Wherein B component system composition proportion is as follows：
50 parts of antimicrobial form curing agent；
5 parts of phthalein blueness red pigment；
5 parts of altax P-30.
The preparation method of the low-temperature setting antimicrobial form epoxy coating of the present embodiment 1, includes the following steps：
(1) prepares component A system：Ratio weighs 6002 epoxy resin in parts by weight：100 parts, 5746 epoxy resin
Diluent：20 parts, organic modified polyorganosiloxane：1 part, silica flour：5 parts are mixed, and 10 min are stirred, and obtain component A mixing
Material obtains component A system；
(2) prepares B component system：Ratio weighs antimicrobial form curing agent in parts by weight：50 parts, coloring pigment：5 parts,
Altax P-30：10 parts are mixed, and are stirred 5min, are obtained B component mixture, that is, obtain B component system；
Described its preparation process of antimicrobial form curing agent is：
The chitosan of 5g is dissolved in a concentration of 10% acetic acid solution of 200ml by (2-1), and mixed solution is added
Heat is used in combination the wave cell disruptor that power is 100w to pop one's head in and is placed in beaker to 60 DEG C, and regulation and control ultrasonic frequency is 30Hz, degradation
A concentration of 10% sodium hydroxide solution is added dropwise in 30h, and it is 7 to adjust pH value, is filtered to remove precipitation, clear liquid is concentrated, and ethyl alcohol is added
Precipitation, separation, and the drying that heats up in vacuum drying oven is precipitated, drying temperature is 50 DEG C, obtains low molecular chitosan, yield is
85%；
The thiocarbamide for the low molecular chitosan and 7.6g that (2-2) obtains above-mentioned steps mixes, and obtains mixed reactant, leads to
Enter nitrogen, mixed reactant is heated under stiring, is dissolved in 50 DEG C of oil bath heatings, mixed reactant is made to be dissolved into liquid, then
It is warming up to 130 DEG C to be reacted, be stirred with 250r/min rotating speeds, after isothermal reaction 2.5h, be cooled to 55 DEG C and constant temperature 2h, stop
Heating, stirring, are cooled to room temperature discharging, obtain thiocarbamide modified amine, wherein the low molecule shell in the hybrid reaction objects system
The mass ratio of glycan and thiocarbamide is 1:0.5；
(2-3) mixes the 38.8g thiocarbamides modified amine obtained in above-mentioned steps b and 30.4g anacardols to be added under stiring
Heat adds paraformaldehyde, and mixed reactant is passed through nitrogen, 45 DEG C are heated under stirring, is dissolved into liquid reactant, heating
Most 105 DEG C are reacted, and are stirred with 350r/min rotating speeds, isothermal reaction 2.5h, and slow cooling stops to 55 DEG C and constant temperature 2h
Heating, stirring, are cooled to room temperature discharging, are then evaporated under reduced pressure at 105 DEG C, and distillation air pressure is 80kPa, removes moisture,
Antimicrobial form curing agent is obtained after cooling, wherein the quality of long alkyl chain phenol and thiocarbamide modified amine in the mixed reactant
Than being 0.7:1, the mass ratio of paraformaldehyde and thiocarbamide modified amine in the mixed reactant is 0.8:1 ；
(3) by the B component system obtained in the component A system obtained in above-mentioned steps (1) and above-mentioned steps (2) according to
1：1 parts by weight proportioning uniformly mixing to get to antimicrobial form epoxy coating.
The antimicrobial form epoxy coating of the present embodiment 1 is fully cured in 3~6 days at 5 DEG C, shear strength 2.1Mpa,
Tensile strength 2.5Mpa.
Embodiment 2：
The present embodiment 2 is substantially the same manner as Example 1, is particular in that：
In the present embodiment 2, wherein component A system composition proportion is as follows：
6350 100 parts of epoxy resin；
5746 5 parts of epoxy resin diluents；
2 parts of organic modified polyorganosiloxane；
10 parts of silica flour；
Wherein B component system composition proportion is as follows：
40 parts of antimicrobial form curing agent prepared by embodiment 1；
The performance measurement of the present embodiment antimicrobial form epoxy coating：
The low-temperature setting antimicrobial form epoxy coating of the present embodiment 2 can be fully cured in 3~6 days at 5 DEG C, shearing
Intensity 2.1Mpa, tensile strength 2.5Mpa.
Embodiment 3：
The present embodiment 3 and previous embodiment 1 are essentially identical, are particular in that：
In the present embodiment 3, wherein component A system composition proportion is as follows：
6350 100 parts of epoxy resin；
502 5 parts of epoxy resin diluents；
15 parts of silica flour；
Wherein B component system composition proportion is as follows：
30 parts of antimicrobial form curing agent prepared by embodiment 1；
5 parts of phthalocyanine blue pigment；
10 parts of altax P-30.
The performance measurement of the present embodiment low-temperature setting antimicrobial form epoxy coating：
The low-temperature setting antimicrobial form epoxy coating of the present embodiment 3 can be fully cured in 3~6 days at 5 DEG C, shearing
Intensity 1.9Mpa, tensile strength 2.4Mpa.
Embodiment 4：
The present embodiment 4 and previous embodiment 1 are essentially identical, are particular in that：
In the present embodiment, wherein component A system composition proportion is as follows：
618 100 parts of epoxy resin；
502 10 parts of epoxy resin diluents；
3 parts of organic modified polyorganosiloxane；
15 parts of silica flour；
Wherein B component system composition proportion is as follows：
60 parts of antimicrobial form curing agent prepared by embodiment 1；
10 parts of phthalocyanine blue pigment；
15 parts of altax P-30.
The performance measurement of the present embodiment low-temperature setting antimicrobial form epoxy coating：
The epoxy coating of the present embodiment 4 can be fully cured in 3~6 days at 5 DEG C, shear strength 1.8Mpa, draw
Stretch intensity 2.2Mpa.
Embodiment 5：
The present embodiment 5 and previous embodiment 1 are essentially identical, are particular in that：
In the present embodiment, wherein component A system composition proportion is as follows：
6002 50 parts of epoxy resin；
618 10 parts of epoxy resin；
3 parts of organic modified polyorganosiloxane；
Wherein B component system composition proportion is as follows：
70 parts of the antimicrobial form curing agent of the preparation of embodiment 1；
10 parts of dark green pigment；
20 parts of altax P-30.
The performance measurement of the present embodiment low-temperature setting antimicrobial form epoxy coating：
The evil low-temperature setting antimicrobial form epoxy coating of the present embodiment 5 can be fully cured in 3~6 days at 5 DEG C, cut
Shearing stress 2.6Mpa, tensile strength 3.2Mpa.
Claims (9)
1. a kind of low-temperature setting antimicrobial form epoxy coating, which is characterized in that it is made of component A system and B component system,
Component A system is with B component system with 1：The parts by weight proportioning of (0.5~1) is mixed to prepare：
Wherein component A system is based in parts by weight, including raw material is as follows：
Wherein B component system is based in parts by weight, including raw material is as follows：
30~70 parts of antimicrobial form curing agent；
1~10 part of coloring pigment；
1~20 part of accelerating agent；
The preparation process of the antimicrobial form curing agent is：
A certain amount of chitosan is dissolved in a concentration of 10% acetic acid solution of 200mL by (2-1), obtained mixed solution
It carries out being heated to 50~70 DEG C, ultrasonic degradation is used in combination, degrade 25~35h, and a concentration of 10% sodium hydroxide solution is added dropwise, and adjusts
It is 6~7 to save pH value, is filtered to remove precipitation, clear liquid is concentrated, and ethyl alcohol is added, precipitation, separation is precipitated, and risen in vacuum drying chamber
Temperature is dry, and drying temperature is 50~60 DEG C, obtains low molecular chitosan；
Low molecular chitosan and the thiocarbamide mixing that (2-2) obtains above-mentioned steps, obtain mixed reactant, are passed through nitrogen, stirring
Mix it is lower to mixed reactant heat, be dissolved into liquid in 50~60 DEG C of oil bath heatings, then be warming up to 125~135 DEG C and reacted,
It is stirred with 200~400r/min rotating speeds, after 2~3h of isothermal reaction, is cooled to 55 DEG C and constant temperature 2h, stop heating, stirring, it is cooling
It discharges to room temperature, obtains thiocarbamide modified amine, wherein the matter of low molecular chitosan and thiocarbamide in the hybrid reaction objects system
Amount is than being 1:(0.5~1)；
(2-3) mixes the thiocarbamide modified amine and 30.4g anacardols that are obtained in above-mentioned steps (2-2), heats under stiring, then
Paraformaldehyde is added, mixed reactant is passed through nitrogen, 45~55 DEG C is heated under stirring, thiocarbamide modified amine and anacardol mix
Reactant is dissolved into liquid reactant, and most 90~110 DEG C of heating is reacted, and is stirred with 300~500r/min rotating speeds, constant temperature
React 2.5h, slow cooling to 55 DEG C and constant temperature 2h stops heating, stirring, is cooled to room temperature discharging, then at 105 DEG C into
Row vacuum distillation, distillation air pressure are 0.13~0.26kPa, remove moisture, antimicrobial form curing agent is obtained after cooling, wherein mixing
The mass ratio of anacardol and thiocarbamide modified amine in reactant is (0.5~1.1):1, the poly first in the mixed reactant
Aldehyde and the mass ratio of thiocarbamide modified amine are (0.5~0.9):1.
2. a kind of low-temperature setting antimicrobial form epoxy coating according to claim 1, which is characterized in that the asphalt mixtures modified by epoxy resin
Fat is E-44 bisphenol A-type liquid epoxies resin, E-51 bisphenol A-type liquid epoxies resin and E-20 bisphenol A-type liquid epoxy resins
In any one or it is arbitrary several.
3. a kind of low-temperature setting antimicrobial form epoxy coating according to claim 1, which is characterized in that the asphalt mixtures modified by epoxy resin
Fat diluent is in allyl glycidyl ether, n-butyl glycidyl ether, phenyl glycidyl ether and furfuryl alcohol glycidol ether
Any one or it is arbitrary several.
4. a kind of low-temperature setting antimicrobial form epoxy coating according to claim 1, which is characterized in that the antifoaming agent
For in hydroxyl dimethyl silicone polymer and organic modified polyorganosiloxane any one or it is arbitrary several.
5. a kind of low-temperature setting antimicrobial form epoxy coating according to claim 1, which is characterized in that the filler is
In titanium dioxide, calcium carbonate, mica powder and silica flour any one or it is arbitrary several.
6. a kind of low-temperature setting antimicrobial form epoxy coating according to claim 1, which is characterized in that the coloring face
Material be in pigment, phthalein blueness red pigment, phthalocyanine blue pigment and dark green pigment any one or it is arbitrary several.
7. a kind of low-temperature setting antimicrobial form epoxy coating according to claim 1, which is characterized in that the accelerating agent
For phenol, salicylic acid and 2,4,6, in-three (dimethylamino methyl) phenol (DMP-30) any one or it is arbitrary several.
8. a kind of preparation method of low-temperature setting antimicrobial form epoxy coating a kind of according to claim 1, feature exist
In including the following steps：
(1) prepares component A system：Ratio weighs epoxy resin in parts by weight：80~100 parts, epoxy resin diluent：5~
20 parts, antifoaming agent：0.5~3 part, filler：0~30 part is mixed, and is stirred 10min, is obtained component A mixture, that is, obtains A groups
Fission system；
(2) prepares B component system：Ratio weighs antimicrobial form curing agent in parts by weight：30~70 parts, coloring pigment：1~10
Part, accelerating agent：1~20 part is mixed, and is stirred 5min, is obtained B component mixture, that is, obtains B component system；
(3) by the B component system obtained in the component A system obtained in above-mentioned steps (1) and above-mentioned steps (2) according to 1：
The parts by weight proportioning of (0.5~1) uniformly mixing to get to antimicrobial form epoxy coating.
9. a kind of preparation method of low-temperature setting antimicrobial form epoxy coating a kind of according to claim 8, feature exist
In, the antimicrobial form curing agent described in above-mentioned steps (2), preparation process is：
A certain amount of chitosan is dissolved in a concentration of 10% acetic acid solution of 200mL by (2-1), obtained mixed solution
It carries out being heated to 50~70 DEG C, ultrasonic degradation is used in combination, degrade 25~35h, and a concentration of 10% sodium hydroxide solution is added dropwise, and adjusts
It is 6~7 to save pH value, is filtered to remove precipitation, clear liquid is concentrated, and ethyl alcohol is added, precipitation, separation is precipitated, and risen in vacuum drying chamber
Temperature is dry, and drying temperature is 50~60 DEG C, obtains low molecular chitosan；
Low molecular chitosan and the thiocarbamide mixing that (2-2) obtains above-mentioned steps, obtain mixed reactant, are passed through nitrogen, stirring
Mix it is lower to mixed reactant heat, be dissolved into liquid in 50~60 DEG C of oil bath heatings, then be warming up to 125~135 DEG C and reacted,
It is stirred with 200~400r/min rotating speeds, after 2~3h of isothermal reaction, is cooled to 55 DEG C and constant temperature 2h, stop heating, stirring, it is cooling
It discharges to room temperature, obtains thiocarbamide modified amine, wherein the matter of low molecular chitosan and thiocarbamide in the hybrid reaction objects system
Amount is than being 1:(0.5~1)；
(2-3) mixes the thiocarbamide modified amine and 30.4g anacardols that are obtained in above-mentioned steps (2-2), heats under stiring, then
Paraformaldehyde is added, mixed reactant is passed through nitrogen, 45~55 DEG C is heated under stirring, thiocarbamide modified amine and anacardol mix
Reactant is dissolved into liquid reactant, and most 90~110 DEG C of heating is reacted, and is stirred with 300~500r/min rotating speeds, constant temperature
React 2.5h, slow cooling to 55 DEG C and constant temperature 2h stops heating, stirring, is cooled to room temperature discharging, then at 105 DEG C into
Row vacuum distillation, distillation air pressure are 0.13~0.26kPa, remove moisture, antimicrobial form curing agent is obtained after cooling, wherein mixing
The mass ratio of anacardol and thiocarbamide modified amine in reactant is (0.5~1.1):1, the poly first in the mixed reactant
Aldehyde and the mass ratio of thiocarbamide modified amine are (0.5~0.9):1.
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| CN102559009B (en) * | 2011-12-19 | 2014-03-26 | 西安信誉精细化工有限公司 | Low temperature antibacterial heavy-duty fusion-bonded epoxy powder coating and preparation method thereof |
| CN103468096B (en) * | 2013-08-08 | 2015-08-12 | 洛阳双瑞防腐工程技术有限公司 | A kind of preparation method of environment-friendly type long-acting mildew-resisting paint |
| CN103694848B (en) * | 2013-12-03 | 2016-04-20 | 常州市拉特涂料有限公司 | A kind of Water-borne epoxy anticorrosive paint for concrete surface |
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2016
- 2016-09-10 CN CN201610813328.4A patent/CN106381017B/en active Active
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