CN107474779A - A kind of antibacterial resistant modified adhesive and preparation method thereof - Google Patents
A kind of antibacterial resistant modified adhesive and preparation method thereof Download PDFInfo
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- CN107474779A CN107474779A CN201710630123.7A CN201710630123A CN107474779A CN 107474779 A CN107474779 A CN 107474779A CN 201710630123 A CN201710630123 A CN 201710630123A CN 107474779 A CN107474779 A CN 107474779A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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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
- 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
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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
- 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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of antibacterial resistant modified adhesive, its raw material includes polyurethane, methyl methacrylate, butyl acrylate, methacrylic acid, benzoyl peroxide, potassium peroxydisulfate, polyvinyl alcohol, DAAM, AH, neck dibatyl phithalate, ATBC, tartaric acid, sodium acid carbonate, antibacterial modified dose, resistant reinforcing agent and deionized water.The present invention also proposes a kind of preparation method of above-mentioned antibacterial resistant modified adhesive.The modified adhesive that the present invention is prepared is applied to textile process, has excellent antibacterial anti-pollution characteristic.
Description
Technical field
The present invention relates to the technical field of adhesive, more particularly to a kind of antibacterial resistant modified adhesive and its preparation side
Method.
Background technology
Existing adhesive generally existing adhesive strength is poor, water resistance, cold-proof are undesirable, is used in textile process
Adhesive, its antibacterial anti-pollution characteristic can not meet the needs of in actual production, so continuing to design a kind of antibacterial resistant modified adhesive
Stick solves the problems of the prior art.
The content of the invention
To solve technical problem present in background technology, the present invention proposes a kind of antibacterial resistant modified adhesive and its system
Preparation Method, the adhesive applications being prepared are in preventing in processing thering is excellent antibacterial anti-pollution characteristic.
A kind of antibacterial resistant modified adhesive proposed by the present invention, its raw material include by weight：Polyurethane 40-60 parts,
Methyl methacrylate 3-9 parts, butyl acrylate 2-5 parts, methacrylic acid 1-4 parts, benzoyl peroxide 1-3 parts, persulfuric acid
Potassium 5-15 parts, polyvinyl alcohol 3-9 parts, DAAM 2-5 parts, AH 1-5 parts, neck dibatyl phithalate 3-5
Part, ATBC 2-4 parts, tartaric acid 1-5 parts, sodium acid carbonate 3-6 parts, antibacterial modified dose of 2-5 part, resistant reinforcing agent 1-4
Part, deionized water 10-20 parts.
Preferably, antibacterial modified dose of raw material includes by weight：3,4- and 4-dihydroxy benzaldehyde 3-6 parts, chitosan 2-5
Part, distilled water 4-9 parts, acetic acid 3-5 parts, methanol 2-4 parts, sodium borohydride 3-5 parts, hydrochloric acid solution 1-5 parts, acetic acid solution 2-6 parts,
Silane coupling reagent KH-570 4-8 parts, ethanol 4-9 parts.
Preferably, antibacterial modified dose is prepared by following technique：4-dihydroxy benzaldehyde, chitosan, distillation by 3,4-
Water, acetic acid and methanol are well mixed, and normal temperature is stood, and are then added sodium borohydride and are well mixed, stir, the precipitation obtained after suction filtration
Thing is dialysed in hydrochloric acid solution, is dialysed in acetic acid solution, and material a is obtained after freeze-dried；By silane coupler KH-
570 and ethanol be well mixed, then add material a be well mixed, heat up, insulation, be followed by stirring for, be cooled to room temperature and obtain antibacterial
Modifying agent.
Preferably, antibacterial modified dose is prepared by following technique：4-dihydroxy benzaldehyde, chitosan, distillation by 3,4-
Water, acetic acid and methanol are well mixed, and normal temperature stands 3-5h, are then added sodium borohydride and are well mixed, turn in 650-850r/min
Speed stirring 20-40min, the sediment obtained after suction filtration are dialysed 5-8h in hydrochloric acid solution, and dialyse 1-3h in acetic acid solution,
Material a is obtained after freeze-dried；Silane coupling reagent KH-570 and ethanol are well mixed, material a is then added and is well mixed,
110-130 DEG C is warming up to, is incubated 20-40min, then 20-40min is stirred in 250-350r/min, is cooled to room temperature and is resisted
Bacterium modifying agent.
Preferably, in antibacterial modified dose of preparation technology, the mass fraction of hydrochloric acid solution is 0.5-1.5mol/L；Acetic acid is molten
The mass fraction of liquid is 0.3-0.6%.
Preferably, the raw material of resistant reinforcing agent includes by weight：Concentrated sulfuric acid 5-15 parts, phosphorus pentoxide 3-6 parts, over cure
Sour potassium 2-4 parts, sodium nitrate 1-3 parts, potassium permanganate 1-4 parts, mass fraction are 25-35% hydrogenperoxide steam generator 2-5 parts, dichloro
Methane 1-4 parts, DMAP 3-6 parts, dicyclohexylcarbodiimide 2-5 parts, acyl in 1- methylol -5,5- dimethyl second
Urea 1-5 parts.
Preferably, resistant reinforcing agent is prepared by following technique：The concentrated sulfuric acid is warming up to 80-100 DEG C, is incubated 5-
15min, 20-40min then is stirred in 650-850r/min rotating speeds, then add phosphorus pentoxide and potassium peroxydisulfate mixing is equal
It is even, 70-80 DEG C is cooled to, 3-5h is incubated, is cooled to room temperature, then sodium nitrate is added and potassium permanganate is well mixed, in 350-
550r/min rotating speeds stir 20-40min, are then warming up to 30-50 DEG C, are incubated 80-100min, then continue to be warming up to 90-100
DEG C, 10-30min is incubated, the hydrogenperoxide steam generator that mass fraction is 25-35% is then added and is well mixed, filter, washing, from
The heart, freeze-drying, then add dichloromethane be well mixed, sonic oscillation 30-50min, then add DMAP,
Dicyclohexylcarbodiimide is well mixed with 1- methylol -5,5- dimethyl hydantoins, is warming up to 50-70 DEG C, nitrogen protection
Under in 650-850r/min rotating speeds stir 10-14h, remove supernatant liquor, wash, filter, freeze-drying obtain resistant reinforcing agent.
A kind of preparation method of antibacterial resistant modified adhesive of the present invention, including：Polyvinyl alcohol and deionized water are mixed
Close uniformly, warming-in-water is incubated 1-3h to 80-100 DEG C, is subsequently added into tartaric acid, sodium acid carbonate, antibacterial modified dose and resistant increasing
Strong agent is well mixed, and is cooled to 60-80 DEG C, then adds benzoyl peroxide and potassium peroxydisulfate is well mixed, in 650-850r/
Min rotating speeds stir 20-50min, then add methyl methacrylate, butyl acrylate, methacrylic acid, diacetone acrylamide acyl
Amine and polyurethane are well mixed, and are warming up to 93-95 DEG C, are incubated 5-15min, then add AH, the neck fourth of phthalic acid two
Ester and ATBC are well mixed, and are warming up to 45-55 DEG C, are incubated 10-30min, are then stirred in 650-850r/min rotating speeds
20-40min is mixed, room temperature is cooled to and obtains antibacterial resistant modified adhesive.
A kind of antibacterial resistant modified adhesive of the present invention, its raw material include polyurethane, methyl methacrylate, acrylic acid
Butyl ester, methacrylic acid, benzoyl peroxide, potassium peroxydisulfate, polyvinyl alcohol, DAAM, AH, neck benzene two
Formic acid dibutyl ester, ATBC, tartaric acid, sodium acid carbonate, antibacterial modified dose, resistant reinforcing agent and deionized water.Wherein,
Antibacterial modified dose by by 3,4- and 4-dihydroxy benzaldehyde, chitosan, distilled water, acetic acid and methanol are well mixed, normal temperature stand,
Then add sodium borohydride to be well mixed, stir, the sediment obtained after suction filtration is dialysed in hydrochloric acid solution, then at acetic acid solution
Middle dialysis, material a is obtained after freeze-dried；Silane coupling reagent KH-570 and ethanol are well mixed, material a is then added and mixes
Close uniformly, heat up, insulation, be followed by stirring for, be cooled to room temperature and obtain antibacterial modified dose, in the adhesive with the present invention, assign
Invention adhesive excellent anti-microbial property.Wherein, resistant reinforcing agent is incubated, is followed by stirring for, so by the way that the concentrated sulfuric acid is heated up
Add phosphorus pentoxide afterwards and potassium peroxydisulfate is well mixed, cool, insulation, be cooled to room temperature, then add sodium nitrate and Gao Meng
Sour potassium is well mixed, and stirring, is then heated up, and is incubated, is then continued to heat up, and is incubated, and it is equal then to add hydrogenperoxide steam generator mixing
It is even, filter, wash, centrifuge, freeze-drying, then add dichloromethane and be well mixed, sonic oscillation, then add 4- diformazan ammonia
Yl pyridines, dicyclohexylcarbodiimide and 1- methylol -5,5- dimethyl hydantoins are well mixed, heating, under nitrogen protection
Stirring, supernatant liquor is removed, washed, filtered, freeze-drying obtains resistant reinforcing agent, applies in the adhesive of the present invention, assigns
The anti-pollution characteristic that invention adhesive is excellent is given.The modified adhesive that the present invention is prepared is applied to textile process, has
Excellent antibacterial anti-pollution characteristic.
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
It is bright, rather than for limiting the invention, any modification made on the basis of the present invention, equivalent substitution etc. are in this hair
In bright protection domain.
In embodiment, the parts by weight of polyurethane can be 40 parts, 45 parts, 50 parts, 55 parts, 60 parts；Metering system
The parts by weight of sour methyl esters can be 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts；The parts by weight of butyl acrylate can be 2 parts,
2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts；The parts by weight of methacrylic acid can be 1 part, 1.5 parts, 2 parts, 2.5 parts, 3
Part, 3.5 parts, 4 parts；The parts by weight of benzoyl peroxide can be 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts；The weight of potassium peroxydisulfate
Part can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts；The parts by weight of polyvinyl alcohol can
Think 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts；The parts by weight of DAAM can be 2 parts, 2.5 parts, 3 parts, 3.5
Part, 4 parts, 4.5 parts, 5 parts；The parts by weight of AH can be 1 part, 2 parts, 3 parts, 4 parts, 5 parts；Lead dibatyl phithalate
Parts by weight can be 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts；The parts by weight of ATBC can be 2 parts, 2.5 parts, 3 parts,
3.5 parts, 4 parts；The parts by weight of tartaric acid can be 1 part, 2 parts, 3 parts, 4 parts, 5 parts；The parts by weight of sodium acid carbonate can be 3 parts,
3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts；Antibacterial modified dose of parts by weight can be 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4
Part, 4.5 parts, 5 parts；The parts by weight of resistant reinforcing agent can be 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts；Deionization
The parts by weight of water can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts.
Embodiment 1
A kind of antibacterial resistant modified adhesive proposed by the present invention, its raw material include by weight：50 parts of polyurethane, methyl
It is 6 parts of methyl acrylate, 3.5 parts of butyl acrylate, 2.5 parts of methacrylic acid, 2 parts of benzoyl peroxide, 10 parts of potassium peroxydisulfate, poly-
6 parts of vinyl alcohol, 3.5 parts of DAAM, 3 parts of AH, 4 parts of dibatyl phithalate of neck, ATBC 3
Part, 3 parts of tartaric acid, 4.5 parts of sodium acid carbonate, antibacterial modified dose 3.5 parts, 2.5 parts of resistant reinforcing agent, 15 parts of deionized water.
Antibacterial modified dose is prepared by following technique：By weight by 4.5 parts of 3,4- 4-dihydroxy benzaldehyde, 3.5 parts
Chitosan, 6.5 parts of distilled water, 4 parts of acetic acid and 3 parts of methanol are well mixed, and normal temperature stands 4h, are then added 4 parts of sodium borohydrides and are mixed
Close uniform, hydrochloric acid of the sediment obtained after 750r/min rotating speeds stirring 30min, suction filtration in 3 parts of mass fractions for 1mol/L
Dialysed 6.5h in solution, and dialysed 2h in the acetic acid solution that 4 parts of mass fractions are 0.45%, and material is obtained after freeze-dried
a；6 parts of Silane coupling reagent KH-570s and 6.5 parts of ethanol are well mixed, material a is then added and is well mixed, be warming up to 120 DEG C,
30min is incubated, then 30min is stirred in 300r/min, is cooled to room temperature and obtains antibacterial modified dose.
Resistant reinforcing agent is prepared by following technique：10 parts of concentrated sulfuric acids are warming up to 90 DEG C by weight, insulation
10min, 30min then is stirred in 750r/min rotating speeds, then add 4.5 parts of phosphorus pentoxides and 3 parts of potassium peroxydisulfate mixing are equal
It is even, 75 DEG C are cooled to, 4h is incubated, is cooled to room temperature, then 2 parts of sodium nitrate is added and 2.5 parts of potassium permanganate is well mixed, in
450r/min rotating speeds stir 30min, are then warming up to 40 DEG C, are incubated 90min, then continue to be warming up to 95 DEG C, are incubated 20min,
Then add the hydrogenperoxide steam generator that 3.5 parts of mass fractions are 30% to be well mixed, filter, wash, centrifuge, freeze-drying, so
Afterwards add 2.5 parts of dichloromethane be well mixed, sonic oscillation 40min, then add 4.5 parts of DMAPs, 3.5 part two
Carbodicyclo hexylimide and 3 parts of 1- methylol -5,5- dimethyl hydantoins are well mixed, and are warming up to 60 DEG C, under nitrogen protection
12h is stirred in 750r/min rotating speeds, removes supernatant liquor, is washed, is filtered, freeze-drying obtains resistant reinforcing agent.
A kind of preparation method of antibacterial resistant modified adhesive of the present invention, including：Polyvinyl alcohol and deionized water are mixed
Close uniform, warming-in-water is incubated 2h to 90 DEG C, is subsequently added into tartaric acid, sodium acid carbonate, antibacterial modified dose and resistant reinforcing agent mix
Close uniformly, be cooled to 70 DEG C, then add benzoyl peroxide and potassium peroxydisulfate is well mixed, stirred in 750r/min rotating speeds
35min, then add methyl methacrylate, butyl acrylate, methacrylic acid, DAAM and polyurethane mixing
Uniformly, 94 DEG C are warming up to, is incubated 10min, then adds AH, neck dibatyl phithalate and ATBC mixing
Uniformly, 50 DEG C are warming up to, is incubated 20min, then 30min is stirred in 750r/min rotating speeds, is cooled to room temperature and obtains antibacterial resistant
Modified adhesive.
Embodiment 2
A kind of antibacterial resistant modified adhesive proposed by the present invention, its raw material include by weight：40 parts of polyurethane, methyl
9 parts of methyl acrylate, 2 parts of butyl acrylate, 4 parts of methacrylic acid, 1 part of benzoyl peroxide, 15 parts of potassium peroxydisulfate, polyethylene
3 parts of alcohol, 5 parts of DAAM, 1 part of AH, 5 parts of dibatyl phithalate of neck, 2 parts of ATBC, winestone
Acid 5 parts, 3 parts of sodium acid carbonate, antibacterial modified dose 5 parts, 1 part of resistant reinforcing agent, 20 parts of deionized water.
Antibacterial modified dose is prepared by following technique：By weight by 3 parts of 3,4-, 4-dihydroxy benzaldehyde, 5 parts of shells gather
Sugar, 4 parts of distilled water, 5 parts of acetic acid and 2 parts of methanol are well mixed, and normal temperature stands 5h, are then added 3 parts of sodium borohydrides and are well mixed,
20min is stirred in 850r/min rotating speeds, the sediment obtained after suction filtration is in the hydrochloric acid solution that 5 parts of mass fractions are 0.5mol/L
Dialysed 8h, and dialysed 1h in the acetic acid solution that 2 parts of mass fractions are 0.6%, and material a is obtained after freeze-dried；By 8 parts of silicon
Alkane coupling agent kh-570 and 4 parts of ethanol are well mixed, and are then added material a and are well mixed, be warming up to 130 DEG C, are incubated 20min,
Then 20min is stirred in 350r/min, is cooled to room temperature and obtains antibacterial modified dose.
Resistant reinforcing agent is prepared by following technique：5 parts of concentrated sulfuric acids are warming up to 100 DEG C by weight, are incubated 5min,
Then 20min is stirred in 850r/min rotating speeds, then adds 6 parts of phosphorus pentoxides and 2 parts of potassium peroxydisulfates are well mixed, be cooled to
80 DEG C, 3h is incubated, is cooled to room temperature, then added 3 parts of sodium nitrate and 1 part of potassium permanganate is well mixed, in 550r/min rotating speeds
20min is stirred, is then warming up to 50 DEG C, is incubated 80min, then continues to be warming up to 100 DEG C, is incubated 10min, then add 5 parts
The hydrogenperoxide steam generator that mass fraction is 25% is well mixed, and is filtered, and is washed, and is centrifuged, and freeze-drying, then adds 4 parts of dichloros
Methane blended is uniform, sonic oscillation 30min, then 6 parts of DMAPs of addition, 2 parts of dicyclohexylcarbodiimides and 5 parts
1- methylol -5,5- dimethyl hydantoins are well mixed, and are warming up to 50 DEG C, are stirred under nitrogen protection in 850r/min rotating speeds
10h, supernatant liquor is removed, washed, filtered, freeze-drying obtains resistant reinforcing agent.
A kind of preparation method of antibacterial resistant modified adhesive of the present invention, including：Polyvinyl alcohol and deionized water are mixed
Close uniform, warming-in-water is incubated 3h to 80 DEG C, is subsequently added into tartaric acid, sodium acid carbonate, antibacterial modified dose and resistant reinforcing agent mix
Close uniformly, be cooled to 60 DEG C, then add benzoyl peroxide and potassium peroxydisulfate is well mixed, stirred in 850r/min rotating speeds
20min, then add methyl methacrylate, butyl acrylate, methacrylic acid, DAAM and polyurethane mixing
Uniformly, 95 DEG C are warming up to, is incubated 5min, then adds AH, neck dibatyl phithalate and ATBC mixing
Uniformly, 55 DEG C are warming up to, is incubated 10min, then 20min is stirred in 850r/min rotating speeds, is cooled to room temperature and obtains antibacterial resistant
Modified adhesive.
Embodiment 3
A kind of antibacterial resistant modified adhesive proposed by the present invention, its raw material include by weight：60 parts of polyurethane, methyl
3 parts of methyl acrylate, 5 parts of butyl acrylate, 1 part of methacrylic acid, 3 parts of benzoyl peroxide, 5 parts of potassium peroxydisulfate, polyethylene
9 parts of alcohol, 2 parts of DAAM, 5 parts of AH, 3 parts of dibatyl phithalate of neck, 4 parts of ATBC, winestone
Acid 1 part, 6 parts of sodium acid carbonate, antibacterial modified dose 2 parts, 4 parts of resistant reinforcing agent, 10 parts of deionized water.
Antibacterial modified dose is prepared by following technique：By weight by 6 parts of 3,4-, 4-dihydroxy benzaldehyde, 2 parts of shells gather
Sugar, 9 parts of distilled water, 3 parts of acetic acid and 4 parts of methanol are well mixed, and normal temperature stands 3h, are then added 5 parts of sodium borohydrides and are well mixed,
40min is stirred in 650r/min rotating speeds, the sediment obtained after suction filtration is in the hydrochloric acid solution that 1 part of mass fraction is 1.5mol/L
Dialysed 5h, and dialysed 3h in the acetic acid solution that 6 parts of mass fractions are 0.3%, and material a is obtained after freeze-dried；By 4 parts of silicon
Alkane coupling agent kh-570 and 9 parts of ethanol are well mixed, and are then added material a and are well mixed, be warming up to 110 DEG C, are incubated 40min,
Then 40min is stirred in 250r/min, is cooled to room temperature and obtains antibacterial modified dose.
Resistant reinforcing agent is prepared by following technique：15 parts of concentrated sulfuric acids are warming up to 80 DEG C by weight, insulation
15min, 40min then is stirred in 650r/min rotating speeds, then adds 3 parts of phosphorus pentoxides and 4 parts of potassium peroxydisulfates are well mixed,
70 DEG C are cooled to, 5h is incubated, is cooled to room temperature, then 1 part of sodium nitrate is added and 4 parts of potassium permanganate is well mixed, in 350r/
Min rotating speeds stir 40min, are then warming up to 30 DEG C, are incubated 100min, then continue to be warming up to 90 DEG C, are incubated 30min, then
Add the hydrogenperoxide steam generator that 2 parts of mass fractions are 35% to be well mixed, filter, wash, centrifuge, freeze-drying, then add 1
Part dichloromethane is well mixed, sonic oscillation 50min, and it is sub- then to add 3 parts of DMAPs, 5 parts of dicyclohexyl carbon two
Amine and 1 part of 1- methylol -5,5- dimethyl hydantoin are well mixed, and are warming up to 70 DEG C, are turned under nitrogen protection in 650r/min
Speed stirring 14h, removes supernatant liquor, washs, filter, freeze-drying obtains resistant reinforcing agent.
A kind of preparation method of antibacterial resistant modified adhesive of the present invention, including：Polyvinyl alcohol and deionized water are mixed
Close uniformly, warming-in-water is incubated 1h, is subsequently added into tartaric acid, sodium acid carbonate, antibacterial modified dose and resistant reinforcing agent to 100 DEG C
It is well mixed, 80 DEG C are cooled to, then benzoyl peroxide is added and potassium peroxydisulfate is well mixed, is stirred in 650r/min rotating speeds
50min, then add methyl methacrylate, butyl acrylate, methacrylic acid, DAAM and polyurethane mixing
Uniformly, 93 DEG C are warming up to, is incubated 15min, then adds AH, neck dibatyl phithalate and ATBC mixing
Uniformly, 45 DEG C are warming up to, is incubated 30min, then 40min is stirred in 650r/min rotating speeds, is cooled to room temperature and obtains antibacterial resistant
Modified adhesive.
Embodiment 4
A kind of antibacterial resistant modified adhesive proposed by the present invention, its raw material include by weight：45 parts of polyurethane, methyl
8 parts of methyl acrylate, 3 parts of butyl acrylate, 3 parts of methacrylic acid, 1.5 parts of benzoyl peroxide, 12 parts of potassium peroxydisulfate, poly- second
4 parts of enol, 4 parts of DAAM, 2 parts of AH, 4.5 parts of dibatyl phithalate of neck, ATBC 2.5
Part, 4 parts of tartaric acid, 4 parts of sodium acid carbonate, antibacterial modified dose 4 parts, 2 parts of resistant reinforcing agent, 18 parts of deionized water.
Antibacterial modified dose is prepared by following technique：By weight by 4 parts of 3,4-, 4-dihydroxy benzaldehyde, 4 parts of shells gather
Sugar, 5 parts of distilled water, 4.5 parts of acetic acid and 2.5 parts of methanol are well mixed, and normal temperature stands 4.5h, then add 3.5 parts of sodium borohydrides
It is well mixed, 25min is stirred in 820r/min rotating speeds, the sediment obtained after suction filtration is 0.8mol/L's in 4 parts of mass fractions
Dialyse 7h in hydrochloric acid solution, and dialyse 1.5h in the acetic acid solution that 3 parts of mass fractions are 0.5%, is obtained after freeze-dried
Material a；7 parts of Silane coupling reagent KH-570s and 5 parts of ethanol are well mixed, material a is then added and is well mixed, be warming up to 125
DEG C, 25min is incubated, then 25min is stirred in 320r/min, is cooled to room temperature and obtains antibacterial modified dose.
Resistant reinforcing agent is prepared by following technique：8 parts of concentrated sulfuric acids are warming up to 95 DEG C by weight, are incubated 8min,
Then 25min is stirred in 820r/min rotating speeds, then adds 5 parts of phosphorus pentoxides and 2.5 parts of potassium peroxydisulfates are well mixed, cooled
To 78 DEG C, 3.5h is incubated, is cooled to room temperature, then added 2.5 parts of sodium nitrate and 2 parts of potassium permanganate are well mixed, in 520r/
Min rotating speeds stir 25min, are then warming up to 45 DEG C, are incubated 85min, then continue to be warming up to 98 DEG C, are incubated 15min, Ran Houjia
Enter the hydrogenperoxide steam generator that 4 parts of mass fractions are 28% to be well mixed, filter, wash, centrifuge, freeze-drying, then add 3 parts
Dichloromethane is well mixed, sonic oscillation 35min, then adds 5 parts of DMAPs, 3 parts of dicyclohexylcarbodiimides
It is well mixed with 4 parts of 1- methylol -5,5- dimethyl hydantoins, 55 DEG C is warming up to, in 820r/min rotating speeds under nitrogen protection
11h is stirred, removes supernatant liquor, is washed, is filtered, freeze-drying obtains resistant reinforcing agent.
A kind of preparation method of antibacterial resistant modified adhesive of the present invention, including：Polyvinyl alcohol and deionized water are mixed
Close uniformly, warming-in-water is incubated 2.5h, is subsequently added into tartaric acid, sodium acid carbonate, antibacterial modified dose and resistant reinforcing agent to 85 DEG C
It is well mixed, 65 DEG C are cooled to, then benzoyl peroxide is added and potassium peroxydisulfate is well mixed, is stirred in 820r/min rotating speeds
25min, then add methyl methacrylate, butyl acrylate, methacrylic acid, DAAM and polyurethane mixing
Uniformly, 94.5 DEG C are warming up to, is incubated 8min, AH, neck dibatyl phithalate and ATBC is then added and mixes
Close uniform, be warming up to 52 DEG C, be incubated 15min, then stir 25min in 820r/min rotating speeds, being cooled to room temperature, to obtain antibacterial resistance to
Dirty modified adhesive.
Embodiment 5
A kind of antibacterial resistant modified adhesive proposed by the present invention, its raw material include by weight：55 parts of polyurethane, methyl
4 parts of methyl acrylate, 4 parts of butyl acrylate, 2 parts of methacrylic acid, 2.5 parts of benzoyl peroxide, 8 parts of potassium peroxydisulfate, poly- second
8 parts of enol, 3 parts of DAAM, 4 parts of AH, 3.5 parts of dibatyl phithalate of neck, ATBC 3.5
Part, 2 parts of tartaric acid, 5 parts of sodium acid carbonate, antibacterial modified dose 3 parts, 3 parts of resistant reinforcing agent, 12 parts of deionized water.
Antibacterial modified dose is prepared by following technique：By weight by 5 parts of 3,4-, 4-dihydroxy benzaldehyde, 3 parts of shells gather
Sugar, 8 parts of distilled water, 3.5 parts of acetic acid and 3.5 parts of methanol are well mixed, and normal temperature stands 3.5h, then add 4.5 parts of sodium borohydrides
It is well mixed, 35min is stirred in 680r/min rotating speeds, the sediment obtained after suction filtration is 1.2mol/L's in 2 parts of mass fractions
Dialyse 6h in hydrochloric acid solution, and dialyse 2.5h in the acetic acid solution that 5 parts of mass fractions are 0.4%, is obtained after freeze-dried
Material a；5 parts of Silane coupling reagent KH-570s and 8 parts of ethanol are well mixed, material a is then added and is well mixed, be warming up to 115
DEG C, 35min is incubated, then 35min is stirred in 280r/min, is cooled to room temperature and obtains antibacterial modified dose.
Resistant reinforcing agent is prepared by following technique：12 parts of concentrated sulfuric acids are warming up to 85 DEG C by weight, insulation
12min, 35min then is stirred in 680r/min rotating speeds, then add 4 parts of phosphorus pentoxides and 3.5 parts of potassium peroxydisulfate mixing are equal
It is even, 72 DEG C are cooled to, 4.5h is incubated, is cooled to room temperature, then 1.5 parts of sodium nitrate is added and 3 parts of potassium permanganate is well mixed, in
380r/min rotating speeds stir 35min, are then warming up to 35 DEG C, are incubated 95min, then continue to be warming up to 92 DEG C, are incubated 25min,
Then add the hydrogenperoxide steam generator that 3 parts of mass fractions are 32% to be well mixed, filter, wash, centrifuge, freeze-drying, then
Add 2 parts of dichloromethane to be well mixed, sonic oscillation 45min, then add 4 parts of DMAPs, 4 parts of dicyclohexyl carbon
Diimine and 2 parts of 1- methylol -5,5- dimethyl hydantoins are well mixed, and 65 DEG C are warming up to, in 680r/ under nitrogen protection
Min rotating speeds stir 13h, remove supernatant liquor, wash, and filter, and freeze-drying obtains resistant reinforcing agent.
A kind of preparation method of antibacterial resistant modified adhesive of the present invention, including：Polyvinyl alcohol and deionized water are mixed
Close uniformly, warming-in-water is incubated 1.5h, is subsequently added into tartaric acid, sodium acid carbonate, antibacterial modified dose and resistant reinforcing agent to 95 DEG C
It is well mixed, 75 DEG C are cooled to, then benzoyl peroxide is added and potassium peroxydisulfate is well mixed, is stirred in 680r/min rotating speeds
45min, then add methyl methacrylate, butyl acrylate, methacrylic acid, DAAM and polyurethane mixing
Uniformly, 93.5 DEG C are warming up to, is incubated 12min, AH, neck dibatyl phithalate and ATBC is then added and mixes
Close uniform, be warming up to 48 DEG C, be incubated 25min, then stir 35min in 680r/min rotating speeds, being cooled to room temperature, to obtain antibacterial resistance to
Dirty modified adhesive.
By GB11178-89 venamuls textile material adhesive standard to 1- of embodiment of the present invention embodiments 5
In antibacterial resistant modified adhesive and commercially available common adhesives detected, performance comparision such as table 1.
Table 1：
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 the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (8)
1. a kind of antibacterial resistant modified adhesive, it is characterised in that its raw material includes by weight：Polyurethane 40-60 parts, methyl
Methyl acrylate 3-9 parts, butyl acrylate 2-5 parts, methacrylic acid 1-4 parts, benzoyl peroxide 1-3 parts, potassium peroxydisulfate 5-
15 parts, polyvinyl alcohol 3-9 parts, DAAM 2-5 parts, AH 1-5 parts, neck dibatyl phithalate 3-5 parts, lemon
Lemon acid tributyl 2-4 parts, tartaric acid 1-5 parts, sodium acid carbonate 3-6 parts, antibacterial modified dose of 2-5 part, resistant reinforcing agent 1-4 parts, go
Ionized water 10-20 parts.
2. antibacterial resistant modified adhesive according to claim 1, it is characterised in that antibacterial modified dose of raw material is by weight
Part includes：3,4- and 4-dihydroxy benzaldehyde 3-6 parts, chitosan 2-5 parts, distilled water 4-9 parts, acetic acid 3-5 parts, methanol 2-4 parts, boron
Sodium hydride 3-5 parts, hydrochloric acid solution 1-5 parts, acetic acid solution 2-6 parts, Silane coupling reagent KH-570 4-8 parts, ethanol 4-9 parts.
3. antibacterial resistant modified adhesive according to claim 1 or 2, it is characterised in that antibacterial modified dose is pressed following work
It is prepared by skill：By 3,4-, 4-dihydroxy benzaldehyde, chitosan, distilled water, acetic acid and methanol are well mixed, and normal temperature is stood, so
Sodium borohydride is added afterwards to be well mixed, and is stirred, the sediment obtained after suction filtration is dialysed in hydrochloric acid solution, in acetic acid solution
Dialysis, obtains material a after freeze-dried；Silane coupling reagent KH-570 and ethanol are well mixed, then add material a mixing
Uniformly, heat up, insulation, be followed by stirring for, be cooled to room temperature and obtain antibacterial modified dose.
4. the antibacterial resistant modified adhesive according to claim any one of 1-3, it is characterised in that antibacterial modified dose by such as
It is prepared by lower technique：By 3,4-, 4-dihydroxy benzaldehyde, chitosan, distilled water, acetic acid and methanol are well mixed, and normal temperature is stood
3-5h, then adds sodium borohydride and is well mixed, and 20-40min, the precipitation obtained after suction filtration are stirred in 650-850r/min rotating speeds
Thing is dialysed 5-8h in hydrochloric acid solution, and dialysed 1-3h in acetic acid solution, and material a is obtained after freeze-dried；Silane is even
Connection agent KH-570 and ethanol are well mixed, and are then added material a and are well mixed, be warming up to 110-130 DEG C, are incubated 20-40min,
Then 20-40min is stirred in 250-350r/min, is cooled to room temperature and obtains antibacterial modified dose.
5. the antibacterial resistant modified adhesive according to claim any one of 1-4, it is characterised in that antibacterial modified dose of system
In standby technique, the mass fraction of hydrochloric acid solution is 0.5-1.5mol/L；The mass fraction of acetic acid solution is 0.3-0.6%.
6. the antibacterial resistant modified adhesive according to claim any one of 1-5, it is characterised in that the original of resistant reinforcing agent
Material includes by weight：Concentrated sulfuric acid 5-15 parts, phosphorus pentoxide 3-6 parts, potassium peroxydisulfate 2-4 parts, sodium nitrate 1-3 parts, permanganic acid
Hydrogenperoxide steam generator 2-5 part, dichloromethane 1-4 parts, DMAP 3-6 that potassium 1-4 parts, mass fraction are 25-35%
Part, dicyclohexylcarbodiimide 2-5 parts, 1- methylol -5,5- dimethyl hydantoin 1-5 parts.
7. the antibacterial resistant modified adhesive according to claim any one of 1-6, it is characterised in that resistant reinforcing agent is by such as
It is prepared by lower technique：The concentrated sulfuric acid is warming up to 80-100 DEG C, is incubated 5-15min, is then stirred in 650-850r/min rotating speeds
20-40min, then add phosphorus pentoxide and potassium peroxydisulfate is well mixed, be cooled to 70-80 DEG C, be incubated 3-5h, be cooled to room
Temperature, then add sodium nitrate and potassium permanganate is well mixed, stir 20-40min in 350-550r/min rotating speeds, be then warming up to
30-50 DEG C, 80-100min is incubated, then continues to be warming up to 90-100 DEG C, is incubated 10-30min, then adding mass fraction is
25-35% hydrogenperoxide steam generator is well mixed, and is filtered, and is washed, and is centrifuged, freeze-drying, and it is equal then to add dichloromethane mixing
It is even, sonic oscillation 30-50min, then add DMAP, dicyclohexylcarbodiimide and 1- methylols -5,5- bis-
Methyl hydantoin is well mixed, and is warming up to 50-70 DEG C, is stirred 10-14h in 650-850r/min rotating speeds under nitrogen protection, remove
Supernatant liquor is removed, is washed, is filtered, freeze-drying obtains resistant reinforcing agent.
A kind of 8. preparation method of antibacterial resistant modified adhesive according to claim any one of 1-7, it is characterised in that
Including：Polyvinyl alcohol and deionized water are well mixed, warming-in-water to 80-100 DEG C, be incubated 1-3h, be subsequently added into tartaric acid,
Sodium acid carbonate, antibacterial modified dose and resistant reinforcing agent are well mixed, and are cooled to 60-80 DEG C, then add benzoyl peroxide and
Potassium peroxydisulfate is well mixed, and is stirred 20-50min in 650-850r/min rotating speeds, is then added methyl methacrylate, acrylic acid
Butyl ester, methacrylic acid, DAAM and polyurethane are well mixed, and are warming up to 93-95 DEG C, are incubated 5-15min, then
Add AH, neck dibatyl phithalate and ATBC to be well mixed, be warming up to 45-55 DEG C, be incubated 10-
30min, 20-40min then is stirred in 650-850r/min rotating speeds, room temperature is cooled to and obtains antibacterial resistant modified adhesive.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108641607A (en) * | 2018-05-07 | 2018-10-12 | 安吉祥力胶粘剂有限公司 | A kind of macromolecule composite adhesive and preparation method thereof |
| CN108686257A (en) * | 2018-06-21 | 2018-10-23 | 浙江派菲特新材料科技有限公司 | A kind of high anti-microbial property adhesive of medical |
| CN108815552A (en) * | 2018-07-05 | 2018-11-16 | 四川大学 | A kind of drug controllably loads and the bio-medical coating material of long-acting slow-release and preparation method thereof |
| CN110039613A (en) * | 2019-03-28 | 2019-07-23 | 融安县大森林木业有限公司 | A kind of production method of the vertical glued board of resist delamination water-impervious |
| CN110055029A (en) * | 2019-03-28 | 2019-07-26 | 融安县大森林木业有限公司 | A kind of environmental protection type veneer board production method |
| CN113563632A (en) * | 2021-09-22 | 2021-10-29 | 南京嘉曜生物科技有限公司 | Chitosan derivative and preparation method and application thereof |
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| CN105482761A (en) * | 2015-12-29 | 2016-04-13 | 安徽安大华泰新材料有限公司 | High-performance modified polyurethane adhesive |
| CN105802431A (en) * | 2016-04-18 | 2016-07-27 | 芜湖县双宝建材有限公司 | High/low-temperature-resistant environment-friendly water-based polyurethane coating |
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| CN105482761A (en) * | 2015-12-29 | 2016-04-13 | 安徽安大华泰新材料有限公司 | High-performance modified polyurethane adhesive |
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| CN108641607A (en) * | 2018-05-07 | 2018-10-12 | 安吉祥力胶粘剂有限公司 | A kind of macromolecule composite adhesive and preparation method thereof |
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| CN108815552A (en) * | 2018-07-05 | 2018-11-16 | 四川大学 | A kind of drug controllably loads and the bio-medical coating material of long-acting slow-release and preparation method thereof |
| CN110039613A (en) * | 2019-03-28 | 2019-07-23 | 融安县大森林木业有限公司 | A kind of production method of the vertical glued board of resist delamination water-impervious |
| CN110055029A (en) * | 2019-03-28 | 2019-07-26 | 融安县大森林木业有限公司 | A kind of environmental protection type veneer board production method |
| CN110039613B (en) * | 2019-03-28 | 2021-06-01 | 融安县大森林木业有限公司 | Production method of anti-delaminating and water seepage-proof vertical plywood |
| CN113563632A (en) * | 2021-09-22 | 2021-10-29 | 南京嘉曜生物科技有限公司 | Chitosan derivative and preparation method and application thereof |
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Application publication date: 20171215 |