CN109293807A - A kind of long acting antibiotic moldproof polyethylene alcohol and the preparation method and application thereof - Google Patents

A kind of long acting antibiotic moldproof polyethylene alcohol and the preparation method and application thereof Download PDF

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Publication number
CN109293807A
CN109293807A CN201810990869.3A CN201810990869A CN109293807A CN 109293807 A CN109293807 A CN 109293807A CN 201810990869 A CN201810990869 A CN 201810990869A CN 109293807 A CN109293807 A CN 109293807A
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long acting
acting antibiotic
alcohol
polyvinyl alcohol
polyethylene alcohol
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杨祺铖
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WEIXING TECHNOLOGICAL INDUSTRY Co Ltd SHANTOU
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WEIXING TECHNOLOGICAL INDUSTRY Co Ltd SHANTOU
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00Chemical modification by after-treatment
    • C08F8/34Introducing sulfur atoms or sulfur-containing groups
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J129/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
    • C09J129/02Homopolymers or copolymers of unsaturated alcohols
    • C09J129/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

A kind of long acting antibiotic moldproof polyethylene alcohol, it is characterised in that be mainly made of polyvinyl alcohol, bromine, organic antibacterial agent and sodium alkoxide;Organic antibacterial agent is one of 5-Chloro-2-methyl-4-isothiazolin-3-one, 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one, 2- octyl -4- isothiazoline -3- ketone, probenazole, 2-methyl-4-isothiazolin-3-one, Kathon and isothiazole -3- ketone or in which a variety of combinations.The present invention also provides a kind of preparation methods of above-mentioned long acting antibiotic moldproof polyethylene alcohol.Above-mentioned long acting antibiotic moldproof polyethylene alcohol can be used as antimicrobial additive matter and be added in substrate polyvinyl alcohol, prepares the polyvinyl alcohol product with antibacterial and mouldproof performance, also can be used as the component of adhesive.Long acting antibiotic moldproof polyethylene alcohol of the invention has excellent antimildew and antibacterial performance and excellent antimicrobial long-acting, and preparation cost is low, simple process.

Description

A kind of long acting antibiotic moldproof polyethylene alcohol and the preparation method and application thereof
Technical field
The present invention relates to anti-biotic material technical fields, and in particular to a kind of long acting antibiotic moldproof polyethylene alcohol and its preparation side Method and application.
Background technique
Polyvinyl alcohol (PVA) is a kind of very widely used soluble resin, has numerous excellent performances, such as water-soluble Property, film forming, cementability, thermal stability etc. are widely used in adhesive for building, spinning sizing agent, adhesive, fiber, papermaking and can The fields such as degradation biological film.But due to polyvinyl alcohol be can high molecular material and own by bacterium as utilization of carbon source The good aqueous solubility being had, not only leads to that polyvinyl alcohol product is easy to breed, spreads germs, and is easy mouldy rot.It is anti- The deficiency of bacterium performance limits the further genralrlization application of polyvinyl alcohol, therefore researches and develops antibacterial polyethylene alcohol with very big reality Application value.
By adding antibacterial agent in the polymer, antimicrobial macromolecule material can be prepared, to make it have anti-microbial property. According to chemical component, antibacterial agent can be divided into inorganic antibacterial agent, organic antibacterial agent, natural products class antibacterial agent.Inorganic antibacterial Agent has many advantages, such as safety, heat resistance, duration and broad spectrum antibacterial, is the life product optimum such as fiber, plastics, building materials Antibacterial agent kind be not suitable for preparing transparent article the disadvantage is that price is higher and the late effect property of antibacterial.Organic low molecular is anti- The advantages of microbial inoculum is from a wealth of sources, technology maturation, sterilizing power is strong, sterilization rate is fast, antibacterial range is wide, cheap etc., mostly Number antibacterial agent can be well dispersed in matrix, but its disadvantage is also significant, and predominantly toxicity is big, safety is poor, heat resistance Difference, chemical stability are poor, it is often more important that are easy that microorganism is made to generate drug resistance, service life is short.Organic polymer antibacterial The advantages of agent is that type is more, sterilizing power is strong, performance is stable, non-volatile, nontoxic, good anti-bacterial effect, antibiotic property are lasting, high-efficient, The disadvantage is that dosage is larger, it is incompatible with high molecular material.The advantages of natural antibacterial agent is broad-spectrum antiseptic, natural environmental-protective, nontoxic It is harmless, good biocompatibility, from a wealth of sources, the disadvantage is that it is thermo-labile, and drug effect is generally shorter.
Blending method adds antibacterial agent into high molecular material, is a kind of the simplest, convenient, economic raising material antibacterial The method of material property, but due to substrate macromolecule material without chemistry key connection, or with substrate macromolecule material not phase Hold, be easy to cause antibacterial agent in basis material be easy be precipitated, be lost the problems such as, cause the antimicrobial long-acting of anti-biotic material compared with Difference.It is substantially in the prior art and is directly added into antibacterial agent into polyvinyl alcohol, make polyvinyl alcohol that there is anti-microbial property, but still deposit The problems such as antibacterial agent is easy to be precipitated, be unevenly distributed, long-term effect is poor.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of long acting antibiotic moldproof polyethylene alcohol and this long-acting anti- The preparation method and application of bacterium moldproof polyethylene alcohol, this long acting antibiotic moldproof polyethylene alcohol have excellent antimildew and antibacterial performance With excellent antimicrobial long-acting.The technical solution adopted is as follows:
A kind of long acting antibiotic moldproof polyethylene alcohol, it is characterised in that mainly by polyvinyl alcohol, bromine, organic antibacterial agent and sodium alkoxide system At;The organic antibacterial agent is 5-Chloro-2-methyl-4-isothiazolin-3-one, the chloro- 2- n-octyl -4- isothiazoline-of 4,5- bis- 3- ketone, 2- octyl -4- isothiazoline -3- ketone, probenazole, 2-methyl-4-isothiazolin-3-one, the different thiophene of 2- n-octyl -4- One of oxazoline -3- ketone and isothiazole -3- ketone or in which a variety of combinations.
First by organic antibacterial agent bromo-reaction occurs in bromine for above-mentioned long acting antibiotic moldproof polyethylene alcohol, then by bromo after Organic antibacterial agent and polyvinyl alcohol sodium alkoxide be catalyzed under conditions of by etherification reaction be made.
In preferred embodiment, above-mentioned long acting antibiotic moldproof polyethylene alcohol is made of the raw material that following weight matches: polyvinyl alcohol 10~150 parts, 10~100 parts of bromine, 5~100 parts of organic antibacterial agent, 100~1000 parts of solvent, 0.1~5 part of sodium alkoxide.
In preferred embodiment, above-mentioned sodium alkoxide is sodium methoxide, sodium ethoxide, ethyl mercaptan sodium, sodium tert-butoxide, sodium tert-amyl alcohol, normal propyl alcohol One of sodium and sodium methyl mercaptide or in which a variety of combinations.
In preferred embodiment, above-mentioned solvent is methylene chloride, acetone, tetrahydrofuran, dimethylformamide, dimethylamine, petroleum One of ether, dimethyl sulfoxide and pentane or in which a variety of combinations.
The present invention also provides a kind of preparation methods of above-mentioned long acting antibiotic moldproof polyethylene alcohol, it is characterised in that including following Step:
(1) polyvinyl alcohol of 10~150 parts by weight is added in the solvent of 50~500 parts by weight, is heated to 60~130 DEG C simultaneously Stirring 2~5 hours, obtains poly-vinyl alcohol solution;
(2) organic antibacterial agent of the bromine of 10~100 parts by weight, 5~100 parts by weight is added to the molten of 50~500 parts by weight In agent, reacted 2~5 hours at 40~80 DEG C;Then purification (primarily discrete solvent out), obtains brominated organic antibacterial agent (brominated organic antibacterial agent is usually light yellow solid);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and The sodium alkoxide of 0.1~5 parts by weight is added, flows back 2~4 hours at 60~140 DEG C, carries out etherification reaction;After etherification reaction, Reaction solution is cooled to room temperature, then is poured into distilled water, drying after film forming is precipitated, obtains required long acting antibiotic moldproof polyethylene Alcohol.
Solvent used in above-mentioned steps (1), step (2) may be the same or different.In step (2), bromine is logical Often slightly excessively, remaining bromine is separated with solvent when purification.
Above-mentioned preparation method technique is relatively simple, excellent antibacterial performance, nontoxic, persistence is good.Due to having and matrix material Expect the identical main chain of polyvinyl alcohol, do not influence the performance of basis material polyvinyl alcohol, and it is anti-to improve polyvinyl alcohol material antibacterial Mould ability.
Above-mentioned preparation method is made former with bromine on organic antibacterial agent molecular structure by the bromination using organic antibacterial agent Son;With polyvinyl alcohol etherification reaction is occurred into for the organic antibacterial agent with bromine atom under the catalytic condition of sodium alkoxide again, makes poly- second The side chain of enol chains the substance containing antibacterial group, so that polyvinyl alcohol itself be made to have the performance of antibacterial and mouldproof, and resists Bacterium fungicidal properties has long-term effect.This method can be well solved in the prior art Blending Processes antibacterial agent in polyvinyl alcohol It is unevenly distributed and is easy precipitation problem, effectively solves the problems, such as that antimicrobial long-acting is poor;Meanwhile it is long-acting anti-prepared by this method Bacterium moldproof polyethylene alcohol can be dispersed in substrate polyvinyl alcohol as antibacterial additives, and additive amount is few, will not influence substrate The mechanical property of polyvinyl alcohol.
In a kind of scheme, the application of above-mentioned long acting antibiotic moldproof polyethylene alcohol, it is characterised in that the long acting antibiotic is mould proof Polyvinyl alcohol is added in substrate polyvinyl alcohol as antimicrobial additive matter, prepares the polyvinyl alcohol system with antibacterial and mouldproof performance Product (such as antibacterial moldproof polyethylene alcohol film).Above-mentioned long acting antibiotic moldproof polyethylene alcohol has good phase with substrate polyvinyl alcohol Capacitive is not easy to release.It is preferred that the weight percent content of long acting antibiotic moldproof polyethylene alcohol is in above-mentioned polyvinyl alcohol product 0.01~10%;The weight percent content of long acting antibiotic moldproof polyethylene alcohol is 0.02 in more preferable above-mentioned polyvinyl alcohol product ~5%.
In another scheme, the application of above-mentioned long acting antibiotic moldproof polyethylene alcohol, it is characterised in that the long acting antibiotic is anti- Component of the mould polyvinyl alcohol as adhesive.Adhesive is used in paper base gift box for packing, improves the fungicidal properties of paper base gift box for packing.
The present invention first passes through bromo-reaction, by organic antibacterial agent bromination, then by etherification reaction, will contain antibacterial group Organic antibacterial agent be grafted on the side chain of polyvinyl alcohol and (antibacterial group be introduced into polyvinyl alcohol in a manner of chemical bond), from And the polyvinyl alcohol of preparation is made to have excellent antibacterial and mouldproof performance (when the bacterial adsorption in environment is to its surface, in material Antibacterial functions group chemical action will occur with bacterium, and can be by killing bacteria), while can guarantee the anti-of polyvinyl alcohol Bacterium long-term effect.Compared with prior art, long acting antibiotic moldproof polyethylene alcohol provided by the invention has excellent antimildew and antibacterial Can, it is blended, can be well dispersed in polyvinyl alcohol matrix material with polyvinyl alcohol matrix material, greatly improved poly- The antibacterial and mouldproof performance of vinyl alcohol product, and since additive amount is few, the gluing performance of polyvinyl alcohol gluing agent is not influenced, is solved Polyvinyl alcohol product existing in the prior art is easy the problems such as mouldy, anti-microbial property is poor, the antibacterial period is short.In short, of the invention Long acting antibiotic moldproof polyethylene alcohol preparation cost it is low, simple process, anti-microbial property is excellent, and due to the effect of grafting, modified Polyvinyl alcohol anti-microbial property persistence is good, gluing performance does not have impacted, there is huge market application prospect and market Value.
Detailed description of the invention
Fig. 1 is to add adhesive prepared by long acting antibiotic moldproof polyethylene alcohol prepared by embodiment 1 by being pressed down with Oxford cup (two curves are respectively long acting antibiotic moldproof polyethylene alcohol to Escherichia coli to the antibacterial circle diameter curve graph that bacterium circle method is obtained Antibacterial circle diameter, the antibacterial circle diameter to staphylococcus aureus);
Fig. 2 is that (Far Left is without the addition mould proof poly- second of long acting antibiotic to 6 months polyvinyl alcohol anti-mold effect figures of standing in Fig. 2 The pure PVA adhesive of enol;A is the PVA adhesive added with 1 long acting antibiotic moldproof polyethylene alcohol of embodiment;B is added with reality Apply the PVA adhesive of 2 long acting antibiotic moldproof polyethylene alcohol of example).
Specific embodiment
Embodiment 1
In the present embodiment, the preparation method of long acting antibiotic moldproof polyethylene alcohol the following steps are included:
(1) 10g polyvinyl alcohol is added in 100g methylene chloride (can all be added to 250mL for polyvinyl alcohol and methylene chloride In there-necked flask), it is heated to 70 DEG C and stirs 2 hours, obtain poly-vinyl alcohol solution;
(2) 25g bromine, 20g organic antibacterial agent (being 5-Chloro-2-methyl-4-isothiazolin-3-one) are added to 120g acetone In (bromine, organic antibacterial agent and acetone can be all added in 250mL there-necked flask), reacted 3 hours at 50 DEG C;Then it purifies (primarily discrete solvent out), obtains brominated organic antibacterial agent (brominated organic antibacterial agent is usually light yellow solid);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and It is added 0.2g sodium alkoxide (being sodium methoxide), flows back 2 hours at 80 DEG C, carry out etherification reaction;After etherification reaction, it will react Liquid is cooled to room temperature, then is poured into distilled water and (can be poured into the 1L beaker equipped with 500mL distilled water), and drying after film forming is precipitated, Obtain required long acting antibiotic moldproof polyethylene alcohol.
Various raw materials are equipped in the above ratio when batch production.
Embodiment 2
In the present embodiment, the preparation method of long acting antibiotic moldproof polyethylene alcohol the following steps are included:
(1) 12g polyvinyl alcohol is added in 100g dimethyl sulfoxide (can all be added to 250mL for polyvinyl alcohol and dimethyl sulfoxide In there-necked flask), it is heated to 90 DEG C and stirs 3 hours, obtain poly-vinyl alcohol solution;
(2) 18g bromine, 15g organic antibacterial agent (being 2- octyl -4- isothiazoline -3- ketone) are added to 100g methylene chloride In (bromine, organic antibacterial agent and methylene chloride can be all added in 250mL there-necked flask), reacted 2 hours at 65 DEG C;Then Purification (primarily discrete solvent out), obtaining brominated organic antibacterial agent, (brominated organic antibacterial agent is usually light yellow solid Body);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and It is added 0.1g sodium alkoxide (being sodium methoxide), flows back 3 hours at 100 DEG C, carry out etherification reaction;It, will be anti-after etherification reaction It answers liquid to be cooled to room temperature, then pours into distilled water and (can pour into the 1L beaker equipped with 400mL distilled water), done after film forming is precipitated It is dry, obtain required long acting antibiotic moldproof polyethylene alcohol.
Various raw materials are equipped in the above ratio when batch production.
Embodiment 3
In the present embodiment, the preparation method of long acting antibiotic moldproof polyethylene alcohol the following steps are included:
(1) 14g polyvinyl alcohol is added in 130g tetrahydrofuran (can all be added to 250mL for polyvinyl alcohol and tetrahydrofuran In there-necked flask), it is heated to 120 DEG C and stirs 2 hours, obtain poly-vinyl alcohol solution;
(2) 20g bromine, 18g organic antibacterial agent (being probenazole) are added in 100g tetrahydrofuran (can by bromine, Organic antibacterial agent and tetrahydrofuran are all added in 250mL there-necked flask), it is reacted 3 hours at 80 DEG C;Then it purifies (mainly Isolate solvent), obtain brominated organic antibacterial agent (brominated organic antibacterial agent is usually light yellow solid);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and It is added 0.3g sodium alkoxide (being sodium ethoxide), flows back 2 hours at 120 DEG C, carry out etherification reaction;It, will be anti-after etherification reaction It answers liquid to be cooled to room temperature, then pours into distilled water and (can pour into the 1L beaker equipped with 450mL distilled water), done after film forming is precipitated It is dry, obtain required long acting antibiotic moldproof polyethylene alcohol.
Various raw materials are equipped in the above ratio when batch production.
Embodiment 4
In the present embodiment, the preparation method of long acting antibiotic moldproof polyethylene alcohol the following steps are included:
(1) 12g polyvinyl alcohol is added in 120g solvent (can all be added to 250mL there-necked flask for polyethylene alcohol and solvent In), it is heated to 110 DEG C and stirs 4 hours, obtain poly-vinyl alcohol solution;
(2) 18g bromine, 15g organic antibacterial agent (being Kathon) are added in 130g solvent (bromine, organic antibacterial agent and solvent all can be added in 250mL there-necked flask) reacts 3 hours at 70 DEG C;Then it purifies (primarily discrete solvent out), obtains brominated organic antibacterial agent (brominated organic antibacterial agent is usually light yellow solid);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and It is added 0.2g sodium alkoxide (being sodium tert-butoxide), flows back 3 hours at 60~140 DEG C, carry out etherification reaction;Etherification reaction finishes Afterwards, reaction solution is cooled to room temperature, then pours into distilled water and (can pour into the 1L beaker equipped with 500mL distilled water), be precipitated at It is dry after film, obtain required long acting antibiotic moldproof polyethylene alcohol.
Various raw materials are equipped in the above ratio when batch production.
Embodiment 5
In the present embodiment, the preparation method of long acting antibiotic moldproof polyethylene alcohol the following steps are included:
(1) 120g polyvinyl alcohol is added in 100g dimethyl sulfoxide (can all be added to 250mL for polyvinyl alcohol and dimethyl sulfoxide In there-necked flask), it is heated to 90 DEG C and stirs 3 hours, obtain poly-vinyl alcohol solution;
(2) by 10g bromine, 8g organic antibacterial agent (being 2-methyl-4-isothiazolin-3-one) is added to (can in 180g solvent Bromine, organic antibacterial agent and solvent are all added in 250mL there-necked flask), it is reacted 4 hours at 80 DEG C;Then purification is (main It is to isolate solvent), obtain brominated organic antibacterial agent (brominated organic antibacterial agent is usually light yellow solid);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and It is added 0.4g sodium alkoxide (being normal propyl alcohol sodium), flows back 3 hours at 100 DEG C, carry out etherification reaction;It, will after etherification reaction Reaction solution is cooled to room temperature, then is poured into distilled water and (can be poured into the 1L beaker equipped with 400mL distilled water), is done after film forming is precipitated It is dry, obtain required long acting antibiotic moldproof polyethylene alcohol.
Various raw materials are equipped in the above ratio when batch production.
Embodiment 6
In the present embodiment, the preparation method of long acting antibiotic moldproof polyethylene alcohol the following steps are included:
(1) 15g polyvinyl alcohol is added in 130g pentane (can all be added to 250mL there-necked flask for polyvinyl alcohol and pentane In), it is heated to 100 DEG C and stirs 4 hours, obtain poly-vinyl alcohol solution;
(2) by 80g bromine, 80g organic antibacterial agent, (wherein 2-methyl-4-isothiazolin-3-one 40g, 5- chloro-2-methyl -4- are different Thiazoline -3- ketone 40, which g) is added in 200g dimethylamine, (can all be added to 500mL tri- for bromine, organic antibacterial agent and dimethylamine In mouth bottle), it is reacted 2 hours at 65 DEG C;Then purification (primarily discrete solvent out), obtains brominated organic antibacterial agent (bromine The organic antibacterial agent of change is usually light yellow solid);
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and It is added 0.5g sodium alkoxide (being sodium methyl mercaptide), flows back 3 hours at 90 DEG C, carry out etherification reaction;It, will be anti-after etherification reaction It answers liquid to be cooled to room temperature, then pours into distilled water and (can pour into the 1L beaker equipped with 500mL distilled water), done after film forming is precipitated It is dry, obtain required long acting antibiotic moldproof polyethylene alcohol.
Various raw materials are equipped in the above ratio when batch production.
Performance test
1, the long acting antibiotic moldproof polyethylene alcohol addition prepared embodiment 1-6 is a certain amount of into substrate polyvinyl alcohol, and preparation is anti- Bacterium polyvinyl alcohol material, and make weight percent content of the long acting antibiotic moldproof polyethylene alcohol in antibacterial polyethylene alcohol material It is 0.01%;According still further to same method prepare long acting antibiotic moldproof polyethylene alcohol weight percent content be respectively 0.02%, 0.04%, 0.06%, 0.08%, 0.1%/0.2%, 0.4% and 0.6% antibacterial polyethylene alcohol material.By it by being surveyed with inhibition zone method Its antibacterial effect is tried, as a result as shown in Figure 1 (by taking embodiment 1 as an example).According to Fig. 1, antibacterial polyethylene alcohol material is to Escherichia coli Excellent inhibitory effect is all had with staphylococcus aureus;When additive amount be 0.02% when, antibacterial polyethylene alcohol material it is antibacterial Loop diameter is more than 20 mm, and fungistatic effect is clearly;And with the increase of long acting antibiotic moldproof polyethylene alcohol, antibacterial is poly- Vinyl alcohol material is more and more obvious the inhibitory effect of Escherichia coli and staphylococcus aureus, illustrates prepared long acting antibiotic Moldproof polyethylene alcohol can greatly improve the anti-microbial property of substrate polyvinyl alcohol.
2, long acting antibiotic moldproof polyethylene alcohol is prepared into adhesive, stands 6 months, as a result as shown in Figure 2.Pass through observation It can be found that obvious mildew has occurred in pure PVA adhesive, and the PVA adhesive for being added to antibacterial polyethylene alcohol material is not bright Aobvious mildew, shows that the addition of long acting antibiotic moldproof polyethylene alcohol can also improve the mould proof ability of material.
3, the long acting antibiotic moldproof polyethylene alcohol for preparing embodiment 1-6 is added to substrate polyvinyl alcohol by calculating In, prepare a series of different material of long acting antibiotic moldproof polyethylene determining alcohols.Equal amount of distilled water is added, dissolution passes through two times Test tube method antibacterial experiment is diluted, the minimum Mlc of the antibacterial polyethylene alcohol of Different adding amount is probed into.Every test tube is added The bacterium solution culture of equivalent concentration 24 hours, to the long acting antibiotic moldproof polyethylene in the 1-10 test tube of Escherichia coli bacteriostasis Alcohol content is followed successively by 20,10,5,2.5,1.25,0.625,0.313,0.156,0.078,0.039ug/mL, to golden yellow grape Long acting antibiotic moldproof polyethylene alcohol content in the 1-10 test tube of the bacteriostasis of coccus is followed successively by 200,100,50,25, 12.5,6.25,3.125,1.563,0.781,0.390ug/mL, and take 100 μ L to be applied to plate, verifying observation knot from every test tube Fruit.The result shows that added long acting antibiotic moldproof polyethylene alcohol is in distilled water-PVA system adhesive to Escherichia coli Minimum inhibitory concentration is 0.625ug/mL, and the minimum inhibitory concentration to staphylococcus aureus is 0.781ug/mL, to golden yellow Staphylococcic Mlc will a slightly high gradient.

Claims (9)

1. a kind of long acting antibiotic moldproof polyethylene alcohol, it is characterised in that mainly by polyvinyl alcohol, bromine, organic antibacterial agent and sodium alkoxide It is made;The organic antibacterial agent is 5-Chloro-2-methyl-4-isothiazolin-3-one, the chloro- 2- n-octyl -4- isothiazole of 4,5- bis- Quinoline -3- ketone, 2- octyl -4- isothiazoline -3- ketone, probenazole, 2-methyl-4-isothiazolin-3-one, 2- n-octyl -4- One of isothiazoline -3- ketone and isothiazole -3- ketone or in which a variety of combinations.
2. long acting antibiotic moldproof polyethylene alcohol according to claim 1, it is characterised in that long acting antibiotic moldproof polyethylene alcohol It is made of the raw material that following weight matches: 10~150 parts of polyvinyl alcohol, 10~100 parts of bromine, 5~100 parts of organic antibacterial agent, 100~1000 parts of solvent, 0.1~5 part of sodium alkoxide.
3. long acting antibiotic moldproof polyethylene alcohol according to claim 1 or 2, it is characterised in that: the sodium alkoxide be sodium methoxide, One of sodium ethoxide, ethyl mercaptan sodium, sodium tert-butoxide, sodium tert-amyl alcohol, normal propyl alcohol sodium and sodium methyl mercaptide or in which a variety of combinations.
4. long acting antibiotic moldproof polyethylene alcohol according to claim 1 or 2, it is characterised in that: the solvent is dichloromethane One of alkane, acetone, tetrahydrofuran, dimethylformamide, dimethylamine, petroleum ether, dimethyl sulfoxide and pentane or in which a variety of Combination.
5. the preparation method of long acting antibiotic moldproof polyethylene alcohol of any of claims 1 or 2, it is characterised in that including following step It is rapid:
(1) polyvinyl alcohol of 10~150 parts by weight is added in the solvent of 50~500 parts by weight, is heated to 60~130 DEG C simultaneously Stirring 2~5 hours, obtains poly-vinyl alcohol solution;
(2) organic antibacterial agent of the bromine of 10~100 parts by weight, 5~100 parts by weight is added to the molten of 50~500 parts by weight In agent, reacted 2~5 hours at 40~80 DEG C;Then it purifies, obtains brominated organic antibacterial agent;
(3) brominated organic antibacterial agent obtained in step (2) is added in the poly-vinyl alcohol solution that step (1) obtains, and The sodium alkoxide of 0.1~5 parts by weight is added, flows back 2~4 hours at 60~140 DEG C, carries out etherification reaction;After etherification reaction, Reaction solution is cooled to room temperature, then is poured into distilled water, drying after film forming is precipitated, obtains required long acting antibiotic moldproof polyethylene Alcohol.
6. the application of long acting antibiotic moldproof polyethylene alcohol of any of claims 1 or 2, it is characterised in that: the long acting antibiotic is anti- Mould polyvinyl alcohol is added in substrate polyvinyl alcohol as antimicrobial additive matter, prepares the polyvinyl alcohol with antibacterial and mouldproof performance Product.
7. the application of long acting antibiotic moldproof polyethylene alcohol according to claim 6, it is characterised in that: the polyvinyl alcohol system The weight percent content of long acting antibiotic moldproof polyethylene alcohol is 0.01~10% in product.
8. the application of long acting antibiotic moldproof polyethylene alcohol according to claim 7, it is characterised in that: the polyvinyl alcohol system The weight percent content of long acting antibiotic moldproof polyethylene alcohol is 0.02~5% in product.
9. the application of long acting antibiotic moldproof polyethylene alcohol of any of claims 1 or 2, it is characterised in that: the long acting antibiotic is anti- Component of the mould polyvinyl alcohol as adhesive.
CN201810990869.3A 2018-08-28 2018-08-28 A kind of long acting antibiotic moldproof polyethylene alcohol and the preparation method and application thereof Pending CN109293807A (en)

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