CN106283923B - A kind of appendix has the mildew-proof wallpaper and preparation method thereof of load medicine chitosan - Google Patents

A kind of appendix has the mildew-proof wallpaper and preparation method thereof of load medicine chitosan Download PDF

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Publication number
CN106283923B
CN106283923B CN201610822670.0A CN201610822670A CN106283923B CN 106283923 B CN106283923 B CN 106283923B CN 201610822670 A CN201610822670 A CN 201610822670A CN 106283923 B CN106283923 B CN 106283923B
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chitosan
wallpaper
antimildew
mildew
antibacterial agent
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CN106283923A (en
Inventor
陈礼辉
林辉
黄六莲
曹石林
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Fujian Agriculture and Forestry University
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Fujian Agriculture and Forestry University
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/18—Paper- or board-based structures for surface covering
    • D21H27/20—Flexible structures being applied by the user, e.g. wallpaper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/10—Coatings without pigments
    • D21H19/12—Coatings without pigments applied as a solution using water as the only solvent, e.g. in the presence of acid or alkaline compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/64—Inorganic compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
    • D21H21/52—Additives of definite length or shape
    • D21H21/54—Additives of definite length or shape being spherical, e.g. microcapsules, beads

Abstract

The present invention, which discloses a kind of appendix, the mildew-proof wallpaper and preparation method thereof for carrying medicine chitosan, the mildew-proof wallpaper is using chitosan/glacial acetic acid mixed solution as carrier, using tripolyphosphate sodium water solution as crosslinking agent, it is mixed to prepare using ionic cross-linking and antimildew and antibacterial agent aqueous solution and carries medicine chitosan microball lotion, and it is sprayed on the base paper surface using plant fiber body paper as the PVC wallpaper of substrate, all kinds of load medicine chitosan/PVC mildew-proof wallpapers are prepared after dry.Mildew-proof wallpaper prepared by the present invention reaches 0 grade standard of national standard (GB/T 24346-2009), and anti-mold effect is splendid.The present invention is mixed to prepare using ionic cross-linking and carries medicine chitosan microball lotion, without introducing organic solvent, and then makes the mildew-proof wallpaper environmental protection of preparation, safety.

Description

A kind of appendix has the mildew-proof wallpaper and preparation method thereof of load medicine chitosan
Technical field
The present invention relates to wallpaper field, in particular to a kind of medicine chitosan and appendix of carrying has the mildew-proof wallpaper for carrying medicine chitosan And preparation method thereof.
Background technique
In use, wall easily gets damp common wallpaper, prevent wallpaper adhesive and plant fiber substrate are from keeping Dry, furthermore construction gluing is blocked up but also glue is not easy drying, and the moulds such as easy growth aspergillus niger cause wallpaper in use process Mouldy raw bacterium, endangers the health of occupant.After wallpaper is mouldy, fungal spore diffuses in air, and fungal spore passes through People breathe air and are directly entered human body, and when human contact's wallpaper, fungal spore also can enter body by the wound of skin surface In body, so that human health causes serious harm.Modern medicine study show the generation of many kinds of respiratory diseases be exactly because It is touched caused by fungal spore for human body, some moulds can also cause Fungal Skin Infection disease.Main Bacteria in air Category has Penicillium, cladosporium and aspergillus etc., they are to cause the anaphylactoid cause of disease of people's respiratory.Aspergillus is to cause spy The dangerous spores of different reaction, the respiratory symptom of child is such as：Asthma, the concentration wheezed etc. all with Aspergillus in room air manifest It writes and is positively correlated.
Mold proof product mainly includes at present：Textile is mould proof, wrapping paper is mould proof, wood mould, coating for wall surface are mould proof etc., by In wallpaper industry industrial production than later, wallpaper currently on the market also has mould proof in the case where being provided simultaneously with antibacterial and deodouring Performance it is seldom, it is therefore necessary to develop a kind of environment-friendly type antibiotic mildew-proof wallpaper.
Chitosan is the natural polymers that content is only second to cellulose in nature, is the production of chitin acetylation Object has many advantages, such as nontoxic, biocompatibility and biological degradability.There is also amino on chitosan surface, in acid medium Under, amino easily with free H+In conjunction with formation NH3 +, therefore chitosan is also the positively charged natural polymer of a few surface.
Chitosan is also a kind of natural antibacterial agent, all has good antibacterial to Gram-negative bacteria and gram-positive bacteria Performance.Currently, chitosan is applied in the mould proof processing of wallpaper by also non-someone.
Summary of the invention
To solve the problems, such as that above-mentioned existing wallpaper anti-mold effect is poor, the present invention proposes that a kind of load medicine chitosan and appendix have load The mildew-proof wallpaper and preparation method thereof of medicine chitosan.
For this purpose, inventor providing following technical solution：
A kind of preparation method carrying medicine chitosan, the preparation method comprises the following steps：
It is that 0.5~3g/L is mould proof that configuration concentration, which is 2~3g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Antibacterial agent aqueous solution；
Chitosan is added in 0.5~2% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 2~4, configuration Obtaining chitosan concentration is chitosan/glacial acetic acid mixed solution of 4~16g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1~2:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 2~4h is stirred at room temperature by liquid, until Mixed solution shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution with Chitosan/glacial acetic acid solution volume ratio is 1:1~1.5.
The present invention selects the carrier of chitosan (CS) as antimildew and antibacterial agent, is because its is nontoxic, and drugloading rate is high, stays Rate it is high, the load medicine chitosan antimildew and antibacterial prepared it is functional.Using tripolyphosphate sodium water solution as crosslinking agent, selection It is due to not being related to organic solvent in ionic cross-linking preparation process, to addition that ionic cross-linking preparation, which carries medicine chitosan, Pharmaceutical properties will not generate large effect to human body.
Before making the present invention, after antimildew and antibacterial agent and chitosan are prepared by mixing into load medicine chitosan by also non-someone, then it is attached It is downloaded in PVC wallpaper.After the present invention will innovatively carry on medicine chitosan appendix to PVC wallpaper, antimildew and antibacterial agent and chitosan Synergy, so that the anti-mold effect of PVC wallpaper is not only substantially exceeded the effect of independent loading chitosan, but also substantially exceed The effect of independent appendix antimildew and antibacterial agent.
Preferably, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution is one of the following：Sodium fluoride, fluorination Copper, copper sulphate, Kocide SD, zinc chloride or sorbic acid.The present invention selects sodium fluoride (NaF), copper fluoride (CuF2), copper sulphate (CuSO4), Kocide SD (Cu (OH)2), zinc chloride (ZnCl2) or sorbic acid (SA) etc. be used as antimildew and antibacterial agent, be due to these The antimildew and antibacterial performance of antimildew and antibacterial agent is good, cheap, lower to the toxicity of human body.Wherein, the antimildew and antibacterial agent is preferred For sodium fluoride.
Since antimildew and antibacterial agent aqueous solution and chitosan/glacial acetic acid mixed solution concentration will affect antibacterial effect.So In the present invention, the concentration of the antimildew and antibacterial agent aqueous solution is preferably 3g/L, the chitosan/glacial acetic acid mixed solution it is dense Degree is preferably 16g/L.
The present invention also provides a kind of appendix have carry medicine chitosan mildew-proof wallpaper preparation method, the mildew-proof wallpaper be with Plant fiber body paper is the PVC wallpaper of substrate, and the preparation method comprises the following steps：
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 0.5~4mL/m2；
PVC wallpaper after spraying is dried into 45~60s at 150~180 DEG C, appendix is prepared and carries the anti-of medicine chitosan Mould wallpaper.
Preferably, the antimildew and antibacterial agent is one of the following：Sodium fluoride, copper fluoride, copper sulphate, Kocide SD, chlorine Change zinc or sorbic acid.
Preferably, the quantity for spray for carrying medicine chitosan microball lotion in PVC wallpaper is 2~3mL/m2。
Preferably, the preparation method of the mildew-proof wallpaper further includes step：100~120 before the PVC wallpaper spraying Dry 60~90s at DEG C.By the step, all kinds of bacteriums and mould of institute's band on wallpaper are removed in advance.
There is the mildew-proof wallpaper for carrying medicine chitosan the present invention also provides a kind of appendix comprising PVC wallpaper layer, the PVC wall Paper layer is using plant fiber body paper as the PVC wallpaper of substrate, and the mildew-proof wallpaper further includes the plant fiber coated in PVC wallpaper Load medicine chitosan layer on body paper substrate surface, the load medicine chitosan carried in medicine chitosan layer are prepared by the above method.
Preferably, the medicine chitosan layer that carries is by the plant fiber original of load medicine chitosan microball Emulsion Spraying to PVC wallpaper It is formed on paper base face, the quantity for spray for carrying medicine chitosan microball lotion in PVC wallpaper is 0.5~4mL/m2。
Beneficial effects of the present invention are：
1, it after the present invention is mixed by antimildew and antibacterial agent aqueous solution with chitosan/glacial acetic acid solution, is formed and carries medicine chitosan, then It will carry on medicine chitosan appendix to PVC wallpaper, so that PVC wallpaper has anti-mold effect.Meanwhile the cost of material that the present invention uses Cheap, simple production process is suitble to produce in enormous quantities.
2, load medicine chitosan of the invention is mixed using ionic cross-linking and is made using tripolyphosphate sodium water solution as crosslinking agent Medicine chitosan microball lotion must be carried, without introducing organic solvent, the PVC wallpaper of preparation is not only environmentally friendly, and has anti-mold effect.
3, show that the mould proof grade of mildew-proof wallpaper of appendix load medicine chitosan prepared by the present invention can reach according to detection data 《The evaluation of textile fungicidal properties》0 grade standard of national standard (GB/T 24346-2009), anti-mold effect are splendid.
4, the present invention carries out mould proof modification to PVC wallpaper, will not reduce the mechanical property of PVC wallpaper too much, horizontal, vertical The requirement of professional standard high-class product is still able to satisfy to wet tensile (strength).
Detailed description of the invention
Fig. 1 is mildew situation of the mildew-proof wallpaper containing different antimildew and antibacterial agents after inoculated aspergillus niger 20d；Wherein, (A) Without mould proof reagent；(B) chitosan/copper sulphate；(C) chitosan/zinc chloride；(D) chitosan/Kocide SD；(E) chitosan/fluorine Change copper；(F) chitosan/sorbic acid；(G) chitosan/sodium fluoride；
Fig. 2 is mildew situation of all kinds of wallpapers after inoculated aspergillus niger 20d；Wherein, (A) is without mould proof reagent；(B) shell is poly- Sugar；(C) sodium fluoride；(D) chitosan/sodium fluoride
Fig. 3 is chitosan/mildew of the sodium fluoride mildew-proof wallpaper after inoculated aspergillus niger 20d of different chitosan concentrations preparation Situation；Wherein, (a) is without mould proof reagent；(b) 4g/L chitosan；(c) 6g/L chitosan；(d) 8g/L chitosan；(e) 10g/L shell Glycan；(f) 12g/L chitosan；(g) 14g/L chitosan；(h) 16g/L chitosan
Fig. 4 is mildew situation of the chitosan/sodium fluoride/PVC mildew-proof wallpaper after inoculated aspergillus niger 20d；
Fig. 5 is chitosan/sodium fluoride microballoon projection electron microscope；
Fig. 6 is chitosan/sodium fluoride microballoon grain size distribution；
Fig. 7 is the infrared spectrogram of chitosan/sodium fluoride (CS/NaF) microballoon and chitosan (CS).
Specific embodiment
Technology contents, construction feature, the objects and the effects for detailed description technical solution, below in conjunction with specific reality It applies example and attached drawing is cooperated to be explained in detail.
The present invention provides a kind of preparation method for carrying medicine chitosan, and the preparation method comprises the following steps：
It is that 0.5~3g/L is mould proof that configuration concentration, which is 2~3g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Antibacterial agent aqueous solution；
Chitosan is added in 0.5~2% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 2~4, configuration Obtaining chitosan concentration is chitosan/glacial acetic acid mixed solution of 4~16g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1~2:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 2~4h is stirred at room temperature by liquid, until Mixed solution shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution with Chitosan/glacial acetic acid solution volume ratio is 1:1~1.5.
The present invention selects the carrier of chitosan (CS) as antimildew and antibacterial agent, is because its is nontoxic, and drugloading rate is high, stays Rate it is high, the load medicine chitosan antimildew and antibacterial prepared it is functional.Selection ionic cross-linking preparation carry medicine chitosan be by It is not related to organic solvent in ionic cross-linking preparation process, therefore the pharmaceutical properties of addition will not generates human body biggish It influences.
In some embodiments, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution is one of the following：Fluorination Sodium, copper fluoride, copper sulphate, Kocide SD, zinc chloride or sorbic acid.The present invention selects sodium fluoride (NaF), copper fluoride (CuF2)、 Copper sulphate (CuSO4), Kocide SD (Cu (OH)2), zinc chloride (ZnCl2) or sorbic acid (SA) etc. be used as antimildew and antibacterial agent, be by It is good, cheap, lower to the toxicity of human body in the antimildew and antibacterial performance of these antimildew and antibacterial agents.Wherein, the antimildew and antibacterial Agent is preferably sodium fluoride.
Since antimildew and antibacterial agent aqueous solution and chitosan/glacial acetic acid mixed solution concentration will affect antibacterial effect.So In the present invention, the concentration of the antimildew and antibacterial agent aqueous solution is preferably 3g/L, the chitosan/glacial acetic acid mixed solution it is dense Degree is preferably 16g/L.
The present invention also provides a kind of appendix have carry medicine chitosan mildew-proof wallpaper preparation method, the mildew-proof wallpaper be with Plant fiber body paper is the PVC wallpaper of substrate, and the preparation method comprises the following steps：
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 0.5~4mL/m2；
PVC wallpaper after spraying is dried into 45~60s at 150~180 DEG C, appendix is prepared and carries the anti-of medicine chitosan Mould wallpaper.
In some embodiments, the antimildew and antibacterial agent is one of the following：Sodium fluoride, copper fluoride, copper sulphate, hydrogen-oxygen Change copper, zinc chloride or sorbic acid.
In some embodiments, the quantity for spray for carrying medicine chitosan microball lotion in PVC wallpaper is 2~3mL/m2。
In some embodiments, the preparation method of the mildew-proof wallpaper further includes step to Astir：Before the PVC wallpaper spraying Dry 60~90s at 100~120 DEG C.By the step, all kinds of bacteriums and mould of institute's band on wallpaper are removed in advance.
There is the mildew-proof wallpaper for carrying medicine chitosan the present invention also provides a kind of appendix comprising PVC wallpaper layer, the PVC wall Paper layer is using plant fiber body paper as the PVC wallpaper of substrate, and the mildew-proof wallpaper further includes the plant fiber coated in PVC wallpaper Load medicine chitosan layer on body paper substrate surface, the load medicine chitosan carried in medicine chitosan layer are prepared by the above method.
In some embodiments, the medicine chitosan layer that carries is by the plant of load medicine chitosan microball Emulsion Spraying to PVC wallpaper It is formed on fibres body paper substrate surface, the quantity for spray for carrying medicine chitosan microball lotion in PVC wallpaper is 0.5~4mL/ m2。
The specific embodiment of mildew-proof wallpaper preparation
Embodiment 1
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution；Antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution is sodium fluoride.
Chitosan is added in 0.5% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 2, configuration obtains shell Glycan concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 2h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 90s at 100 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould；
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 0.5mL/m2；
PVC wallpaper after spraying is dried into 60s at 150 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 2
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are copper fluoride.
Chitosan is added in 0.5% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 2, configuration obtains shell Glycan concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 2h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 90s at 100 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 4mL/m2；
PVC wallpaper after spraying is dried into 60s at 150 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 3
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are copper sulphate.
Chitosan is added in 0.1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, configuration obtains shell Glycan concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 90s at 100 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 4mL/m2；
PVC wallpaper after spraying is dried into 45s at 180 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 4
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are Kocide SD.
Chitosan is added in 0.1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, configuration obtains shell Glycan concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 60s at 120 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 3mL/m2；
PVC wallpaper after spraying is dried into 45s at 180 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 5
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are zinc chloride.
Chitosan is added in 2% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 4, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 4h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 60s at 120 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 3mL/m2；
PVC wallpaper after spraying is dried into 55s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 6
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sorbic acid.
Chitosan is added in 2% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 4, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 4h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 60s at 120 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 170 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 7
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 3g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 4g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1.5:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature by liquid, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 60s at 120 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 8
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 6g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1.5:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature by liquid, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 60s at 120 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 9
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 8g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 2:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature, until mixing molten Liquid shows shallow white, stops stirring, obtains carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell are poly- Sugar/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 10
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 10g/L as appendix agent；
Antimildew and antibacterial agent aqueous solution and crosslinking agent are pressed into volume 2:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, so Antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution afterwards, 3h is stirred at room temperature, until mixed solution Shallow white is showed, stirring is stopped, obtaining carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and chitosan/ The volume ratio of glacial acetic acid solution is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 70s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 11
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 12g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1.5:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature by liquid, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 12
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 14g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1.5:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature by liquid, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 13
1, it first prepares and carries medicine chitosan comprising following steps：
It is 0.5g/L antimildew and antibacterial agent that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Aqueous solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 16g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1.5:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature by liquid, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 14 (referring to embodiment)
Mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
Chitosan microball lotion (chitosan concentration 16g/L) not containing antimildew and antibacterial agent is sprayed into PVC wallpaper In the one side of plant fiber body paper substrate, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 45~60s at 150~180 DEG C, appendix is prepared and carries the anti-of medicine chitosan Mould wallpaper.
Embodiment 15 (referring to embodiment)
Mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
The sodium fluoride aqueous solution that concentration is 3g/L is sprayed in the one side of plant fiber body paper substrate of PVC wallpaper, is sprayed The lotion amount of painting is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
Embodiment 16
1, it first prepares and carries medicine chitosan comprising following steps：
It is 3g/L antimildew and antibacterial agent water that configuration concentration, which is 2g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Solution, the antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution are sodium fluoride.
Chitosan is added in 1% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 3, it is poly- that configuration obtains shell Sugared concentration is chitosan/glacial acetic acid mixed solution of 16g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1.5:1 is uniformly mixed, and it is molten to obtain antimildew and antibacterial agent mixing Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 3h is stirred at room temperature by liquid, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1.5.
2, mildew-proof wallpaper is prepared, is included the following steps：
It selects using plant fiber body paper as the PVC wallpaper of substrate, the dry 80s at 110 DEG C, removes in PVC wallpaper in advance Various bacteriums and mould.
By the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On on one side, the lotion amount of spraying is 2mL/m2；
PVC wallpaper after spraying is dried into 50s at 160 DEG C, the mildew-proof wallpaper that appendix carries medicine chitosan is prepared.
The various performance detections of the mildew-proof wallpaper of each embodiment preparation.
First carry out the culture of aspergillus niger strain and its preparation of spore liquid.Specific method is：By peeling potatoes, stripping and slicing, It is put into deionized water, boils 30min at 121 DEG C, be cooked into after pureed and go out potato starch filtrate with filtered through gauze；In filtrate Middle addition glucose is packed into triangular flask after mixing evenly, potato culture solution is prepared after cooling gel.
Oese and potato culture are sterilized by pressure cooker, are placed in bio-safety aseptic superclean bench, The aspergillus niger spore purchased is seeded in potato culture inclined-plane, is put into biochemical cultivation case, at 28 DEG C cultivate 7d~ 14d, until covering with mycotic spore on potato culture inclined-plane.
It measures 10mL to pour into the potato culture inclined-plane for covering with mycotic spore by autoclaved deionized water, use The oese that high pressure sterilization is crossed lightly wipes the surface of aspergillus niger strain, is dispersed in aspergillus niger spore in sterile ionized water, As the aqueous solution containing spore；The aqueous solution containing spore of wash-off is poured into the triangular flask containing bead, constant temperature is used Oscillator vibrates triangular flask at 28 DEG C, is mixed spore liquid sufficiently；Spore liquid after mixing is filtered with qualitative filter paper, is removed The impurity such as mycelia fragment, agar and spore ball, filtered solution are the aspergillus niger spore liquid prepared.
Inoculation and cultural method of the aspergillus niger on mildew-proof wallpaper be：Pass through high pressure in potato culture, oese etc. After steam sterilizing, potato culture solution is uniformly introduced in culture dish on a sterile work bench, it is cooling solidifying to culture medium After Gu, 1mL spore liquid is drawn with the rubber head suction pipe that sterilized, evenly distributes the surface for being inoculated into entire culture medium, with sterilizing Glass spreading rod smear it is uniform；The a piece of PVC wallpaper sample by sterilization processing is put into inoculated media surface, PVC wallpaper sample is the square of side length 40mm or the circle of diameter 40mm.After media surface moisture slightly evaporates, lid Ware lid is cultivated well, and is sealed with sealed membrane and preservative film；Every kind of PVC wallpaper sample does 3 parallel tests；It is vaccinated and add The culture dish for entering mould proof PVC wallpaper sample is put into THE CONSTANT TEMPERATURE AND HUMIDITY BIOLOGICAL CABINET, in 28 DEG C ± 2 DEG C of temperature and relative humidity 20d is cultivated under conditions of 90% ± 5%；After the culture of 20d, pass through the length of culture medium and PVC wallpaper in observation culture dish Mould situation picks out the optimal load medicine chitosan of anti-mold effect/PVC mildew-proof wallpaper sample.
1, the different anti-mold effects for carrying medicine chitosan are investigated
The first step of embodiment 1 to embodiment 6 prepares 6 kinds of load medicine chitosans for containing different antimildew and antibacterial agents respectively. Wherein, the concentration of the antimildew and antibacterial agent aqueous solution is 3g/L.The antimildew and antibacterial agent is respectively sodium fluoride (NaF), fluorination Copper (CuF2), copper sulphate (CuSO4), Kocide SD (Cu (OH)2), zinc chloride (ZnCl2) and sorbic acid (sorbic acid, letter Claim SA).Sodium tripolyphosphate (STPP) aqueous solution that the antimildew and antibacterial agent aqueous solution that concentration is 3g/L is 2g/L with concentration is mixed Afterwards, cross-linking reaction is carried out with chitosan (CS)/glacial acetic acid (AC) solution that concentration is 6g/L respectively, prepare 6 kinds are different Medicine chitosan microball lotion is carried, specially：Chitosan/sodium fluoride (CS/NaF), chitosan/copper fluoride (CS/CuF2), shell it is poly- Sugar/copper sulphate (CS/CuSO4), chitosan/Kocide SD (CS/Cu (OH)2), chitosan/zinc chloride (CS/ZnCl2) and shell it is poly- Sugar/sorbic acid (CS/SA).
The second step spray treatment that embodiment 6 is arrived through embodiment 1, obtains 6 kinds of mildew-proof wallpapers.Above-described embodiment 1 is in fact 6 kinds of mildew-proof wallpapers for applying the preparation of example 6, are put into togerther aspergillus niger spore with control sample (PVC wallpaper of non-appendix antimildew and antibacterial agent) Sub- liquid is sprawled in uniform potato culture, is cultivated under conditions of 28 DEG C ± 2 DEG C of temperature and relative humidity 90% ± 5% After 20d, mildew situation is observed.Every kind of wallpaper is divided into 3 groups, as parallel test to exclude error, the test of wallpaper mildew situation As a result as shown in Figure 1.
As shown in Figure 1, embodiment 2 uses chitosan/copper fluoride (CS/CuF to embodiment 6 respectively2), chitosan/sulfuric acid Copper (CS/CuSO4), chitosan/Kocide SD (CS/Cu (OH)2), chitosan/zinc chloride (CS/ZnCl2) and chitosan/sorb Sour (CS/SA) preparation goes out mildew-proof wallpaper sample B, sample C, sample D, sample E and sample F, cultivates in aspergillus niger spore liquid Mildew situation after 20d, it is similar with the PVC wallpaper control sample A of no mould inhibitor, illustrate that embodiment 2 is prepared to embodiment 6 Load medicine chitosan it is poor to the anti-mold effect of aspergillus niger；Chitosan/sodium fluoride (the CS/ prepared using 1 first step of embodiment NaF the mould proof PVC wallpaper that appendix obtains) is carried out, aspergillus niger mildew area is minimum, illustrates chitosan/sodium fluoride in PVC wallpaper After upper appendix, there is preferable anti-mold effect to aspergillus niger.
Since the mould proof grade of wall paper products not yet has any country, place or professional standard, therefore pushed away according to country Recommend standard《The evaluation of textile fungicidal properties》Anti-mold effect evaluation criterion in (GB/T 24346-2009) in relation to textile is right Self-control mildew-proof wallpaper evaluates the anti-mold effect of aspergillus niger.The evaluation of standard GB/T/T 24346-2009 anti-mold effect Grade is as shown in table 1,
The evaluation of 1 textile anti-mold effect of table
According to the evaluation criterion in relation to textile anti-mold effect in table 1, to above 7 groups of loads medicine chitosan/PVC wallpaper to black The anti-mold effect of aspergillus carries out mould proof grade evaluation, and the result is shown in tables 2.
Table 2 carries the mould proof grade evaluation of medicine chitosan
As shown in table 2, the mould proof PVC wallpaper that embodiment 1 is prepared using chitosan/sodium fluoride (CS/NaF), to black The average mould proof grade of aspergillus reaches national 2 grade standards, and anti-mold effect is preferable；The average mould proof grade and blank of other drugs are tried The average mould proof grade for testing group is identical, and for national 4 grade standards, mould proof area is almost nil, and anti-mold effect is very poor.So of the invention It is preferred that chitosan/sodium fluoride (CS/NaF) microballoon lotion carries out mould proof modification to PVC wallpaper as mould inhibitor.
In embodiment 1 into embodiment 6, chitosan concentration is 6g/L in chitosan/glacial acetic acid mixed solution, if by mentioning High chitosan concentration, then after copper fluoride, copper sulphate, Kocide SD, zinc chloride or sorbic acid are mixed with chitosan/glacial acetic acid solution The load medicine chitosan of preparation can also carry out mould proof modification to PVC wallpaper.
2, chitosan/sodium fluoride system mould proof test
Specific method is：There is the PVC wallpaper of chitosan for control with one group of non-appendix, embodiment 14 is that antibacterial agent is not added And the PVC wallpaper that concentration sprays for the chitosan solution of 6g/L, embodiment 15 are sodium fluoride (NaF) solution for individually using 3g/L The PVC wallpaper of spraying, by above-mentioned three groups of PVC wallpapers and embodiment 13 with chitosan/sodium fluoride (CS/NaF) microballoon Emulsion Spraying PVC wallpaper synchronize the mould proof test carried out to aspergillus niger.Every kind of wallpaper is divided into 2 groups, as parallel test to exclude error, wall The test result of paper mildew situation is as shown in Figure 2.
As seen from Figure 2, embodiment 14 goes out PVC wallpaper sample B using chitosan (CS) spraying preparation, in aspergillus niger The mildew situation after 20d is cultivated in spore liquid, it is similar with the PVC wallpaper control sample A of no mould inhibitor, illustrate chitosan to black The anti-mold effect of aspergillus is poor；Embodiment 15 is used alone sodium fluoride (NaF) and sprays the PVC wallpaper sample C prepared, to black song It is mould that there is certain anti-mold effect, substantially no discovery mildew on sample, but sample surrounding media blank space is mould proof Effect is poor, and mildew area is larger；The mould proof PVC wallpaper sample that embodiment 13 is prepared using chitosan/sodium fluoride (CS/NaF) Product D, without discovery mildew on sample, the aspergillus niger mildew area of sample surrounding media blank space is minimum.This illustrates to implement The independent chitosan appendix wallpaper of example 14 does not play anti-mold effect to aspergillus niger, the wallpaper of the independent sodium fluoride appendix of embodiment 15, Poor to the anti-mold effect of aspergillus niger, embodiment 13 mixes chitosan and sodium fluoride, prepares attached after chitosan/sodium fluoride microballoon It is loaded in PVC wallpaper, there is preferable anti-mold effect to aspergillus niger.
According to the evaluation criterion in relation to textile anti-mold effect in table 1, to above 4 groups of PVC wallpapers to the mould proof of aspergillus niger Effect carries out mould proof grade evaluation, and the result is shown in tables 3.
The mould proof grade evaluation of 3 PVC wallpaper of table
As shown in table 3, the mould proof PVC wallpaper of 13 appendix chitosan of embodiment/sodium fluoride (CS/NaF), to aspergillus niger Average mould proof grade reaches national 2 grade standards, and mould proof area has reached 70%, and anti-mold effect is preferable；The independent appendix of embodiment 15 The PVC wallpaper of sodium fluoride (NaF) reaches national 3 grade standards to the average mould proof grade of aspergillus niger, and anti-mold effect is general；It is real The PVC wallpaper of the independent appendix chitosan (CS) of example 14 is applied, the average mould proof grade phase of average mould proof grade and blank test group It together, is national 4 grade standards, mould proof area is almost nil, and anti-mold effect is very poor.Chitosan is illustrated in above-mentioned analytical table and sodium fluoride is total Same-action improves sodium fluoride to the anti-mold effect of aspergillus niger.
3, influence of the chitosan concentration to anti-mold effect
Carrier of the chitosan as antimildew and antibacterial agent, concentration variation have a very big impact anti-mold effect.So real It applies example 7 and prepares chitosan/sodium fluoride (CS/NaF) microballoon lotion appendix to PVC wallpaper with different chitosan concentrations to embodiment 13 On, and detect the anti-mold effect of the PVC mildew-proof wallpaper of each embodiment preparation.
Meanwhile with non-appendix chitosan/sodium fluoride (CS/NaF) microballoon lotion PVC wallpaper as control sample, together Carry out the mould proof test to aspergillus niger.The PVC mildew-proof wallpaper of the chitosan preparation of various concentration is shown in the anti-mold effect of aspergillus niger Fig. 3.
As seen from Figure 3, embodiment 7 prepares chitosan/fluorine using the chitosan (CS) of various concentration to embodiment 13 Change sodium (CS/NaF)/PVC mildew-proof wallpaper, after inoculated aspergillus niger 20d, the mildew area of aspergillus niger with chitosan concentration increasing Add and constantly reduces.When the chitosan for being followed successively by 4g/L, 6g/L, 8g/L and 10g/L to 10 concentration of embodiment using embodiment 7 is molten Chitosan/sodium fluoride that liquid is prepared/PVC mildew-proof wallpaper sample b, sample c, sample d and sample e, in aspergillus niger spore liquid Mildew situation after cultivating 20d, similar with sodium fluoride (NaF)/PVC wallpaper control sample a of no chitosan, this illustrates concentration The chitosan solution of≤10g/L prepares chitosan/sodium fluoride/PVC mildew-proof wallpaper, poor to the anti-mold effect of aspergillus niger；Work as reality Apply chitosan/fluorination that example 11 is prepared to the chitosan solution that 13 concentration of embodiment is followed successively by 12g/L, 14g/L and 16g/L Sodium/PVC mildew-proof wallpaper sample f, sample g and sample h, almost without discovery mildew, sample surrounding media blank on sample The aspergillus niger mildew area at place is continuously increased and is gradually reduced with chitosan solution concentration, this illustrates concentration >=12g/L Chitosan solution prepares chitosan/sodium fluoride/PVC mildew-proof wallpaper, preferable to the anti-mold effect of aspergillus niger.
According to the evaluation criterion in relation to textile anti-mold effect in table 1, to above 8 groups of PVC wallpapers to the mould proof of aspergillus niger Effect carries out mould proof grade evaluation, and the result is shown in tables 4.
The mould proof grade evaluation of 4 various concentration chitosan of table
From table 4, it can be seen that chitosan/sodium fluoride (CS/NaF)/PVC is mould proof with the increase of chitosan solution concentration The mould proof grade evaluation effect of wallpaper sample is better；As chitosan solution concentration≤8g/L, chitosan/sodium fluoride for preparing (CS/NaF)/PVC mildew-proof wallpaper sample, average mould proof grade is identical as the average mould proof grade of blank test group, for country 4 Grade standard, anti-mold effect are very poor；When embodiment 10 and 11 chitosan solution concentration of embodiment reach 10g/L~12g/L, sample Mould proof area reach 40% or so, national 3 grade standards are reached to the average mould proof grade of aspergillus niger；When embodiment 12 and implement When 13 chitosan solution concentration of example reaches 14g/L~16g/L, the mould proof area of sample has reached 80% or so, to aspergillus niger Average mould proof grade reaches national 2 grade standards, and anti-mold effect is preferable.
4, chitosan/concentration of sodium fluoride formula determination
Embodiment 16 using chitosan concentration for 16g/L chitosan/glacial acetic acid (CS/AC) mixed solution as carrier, with Concentration is sodium fluoride (NaF) solution of 3g/L as antimildew and antibacterial agent, water-soluble for the sodium tripolyphosphate (STPP) of 2g/L with concentration Liquid is mixed to prepare chitosan/sodium fluoride (CS/NaF) microballoon lotion as crosslinking agent；Chitosan/sodium fluoride (CS/NaF) is micro- Ball Emulsion Spraying on plant fiber paper base/PVC wallpaper base paper surface, prepared after dry chitosan/sodium fluoride (CS/NaF)/ PVC mildew-proof wallpaper；The mould proof test of aspergillus niger is finally carried out to it.Chitosan/sodium fluoride (CS/NaF)/PVC mildew-proof wallpaper pair The anti-mold effect of aspergillus niger is shown in Fig. 4.
As seen from Figure 4, according to the experiment condition of embodiment 16, chitosan (CS) solution concentration is 16g/L, sodium fluoride (NaF) concentration of aqueous solution is chitosan/sodium fluoride (CS/NaF)/PVC mildew-proof wallpaper sample that 3g/L is prepared, and is being inoculated with black song After mould 20d, on sample and sample surrounding media blank space is almost without discovery mildew, according to textile related in table 1 The evaluation criterion of anti-mold effect prevents aspergillus niger chitosan/sodium fluoride (CS/NaF)/PVC mildew-proof wallpaper of above-mentioned preparation Mould effect carries out mould proof grade evaluation, and for sample without obvious mildew under magnifying glass, mould proof area has nearly reached 100%, made Sample reaches national 0 grade standard to the average mould proof grade of aspergillus niger, and anti-mold effect is splendid.
5, the materialization of chitosan/sodium fluoride microballoon characterizes
5.1 chitosans/sodium fluoride microballoon morphology analysis
In order to confirm the morphological feature of chitosan/sodium fluoride (CS/NaF) microballoon, using Japanese JEOL transmission electron microscope to reality Chitosan/sodium fluoride microballoon the form for applying the preparation of 16 first step of example is observed, and the result is shown in Fig. 5.
From fig. 5, it can be seen that when the concentration ratio of chitosan (CS) and sodium fluoride (NaF) is 16:When 3, chitosan (CS) and Sodium fluoride (NaF) as the crosslinking of sodium tripolyphosphate (STPP) it is compound made from chitosan/sodium fluoride (CS/NaF) microballoon shape Size distribution is uniform, substantially shows spherical state.
In order to measure the particle size of chitosan/sodium fluoride (CS/NaF) microballoon, using Malvern laser particle instrument to shell Glycan/sodium fluoride microballoon particle diameter distribution measures, and the result is shown in Fig. 6.
As shown in fig. 6, when the concentration ratio of chitosan (CS) and sodium fluoride (NaF) is 16:When 3, chitosan/sodium fluoride (CS/ NaF) particle diameter distribution of microballoon is between 400nm~700nm, average grain diameter 615nm, and chitosan/sodium fluoride (CS/NaF) is micro- Ball size distribution is uniform, and partial size is smaller, is sprayed on after plant fiber paper base/PVC wallpaper base paper surface, chitosan/fluorination Sodium (CS/NaF) microballoon is liable to stick on the fiber of plant fiber paper base, and PVC wallpaper is made to have the effect of antimildew and antibacterial.
The infrared spectrum analysis of 5.2 chitosans/sodium fluoride microballoon
In order to measure the chemical bond variation after ionic cross-linking prepares chitosan/sodium fluoride (CS/NaF) microballoon, Fu is used Sodium fluoride/chitosan (CS/NaF) microballoon that vertical leaf infrared spectrometer prepare 16 first step of embodiment and the shell before preparing Glycan (CS) is detected, and to observe chemical bond variation of the chitosan (CS) before and after preparation, the result is shown in Fig. 7.
As shown in fig. 7, the concentration ratio in embodiment 16 as chitosan (CS) and sodium fluoride (NaF) is 16:When 3, chitosan (CS)-OH, c h bond stretching vibration appear in 3387cm-1And 2876cm-1；At the same time, chitosan includes that there are two features Absorption peak is 1598cm respectively-1(amido bond I) and 1384cm-1(amido bond II).It is logical at sodium fluoride (NaF) and chitosan (CS) It crosses after sodium tripolyphosphate (TPP) crosslinking agent is combined with each other, the infrared spectrogram and chitosan of chitosan/sodium fluoride (CS/NaF) It compares, characteristic absorption peak has been transferred to 1576cm-1And 1412cm-1, while chitosan is in 1085cm-1- OH the key at place passes through friendship Connection recombination reaction is moved to 1079cm-1Place.Two infrared spectroscopy absorbance curves can be seen that chitosan/fluorination from Fig. 7 Sodium (CS/NaF) spectrogram does not occur new characteristic peak, feature only occurs compared with the spectrogram of chitosan (CS) The movement at peak.This illustrates that the crosslinking of sodium fluoride (NaF) and chitosan (CS) is the crosslinking method of physical change, does not generate new Substance；Sodium fluoride (NaF) and chitosan (CS) form chitosan/sodium fluoride (CS/ under the action of sodium tripolyphosphate (TPP) NaF) microballoon；Chitosan in acid condition ,-the NH on surface2Key decomposes, so that chitosan solution has positive charge, by quiet Electro ultrafiltration is combined together to form with the crosslinking agent with negative electrical charge and carries medicine chitosan.
6, the mechanical property of mildew-proof wallpaper
Mould proof modification is carried out to PVC wallpaper, it is necessary to premised on not reducing its mechanical property.The shell prepared with embodiment 16 Glycan/sodium fluoride (CS/NaF)/PVC mildew-proof wallpaper is sample；It is carried out after being cut to it with the horizontal tensile testing machine of computer observing and controlling Wet tensile (strength) must test.Using plant fiber body paper as the PVC wallpaper of substrate carry out it is mould proof before modified after cross, longitudinal wet anti-tensile Intensity contrast is shown in Table 5.
As can be seen from Table 5, PVC wall of the embodiment 16 using chitosan/sodium fluoride (CS/NaF) microballoon after emulsion modified Paper, horizontal, longitudinal wet tensile (strength) reduce 2.65% and 1.74% than mould proof respectively before modified.This is because the present invention uses PVC wallpaper base material be plant fiber body paper, the quilt after coating chitosan/sodium fluoride (CS/NaF) microballoon lotion Sufficiently wetting.In wet conditions, the fiber in plant fiber paper has occurred profit and rises, and many hydrogen bonds between fiber are destroyed, and causes It is greatly reduced the binding force of paper；After drying again to wallpaper, the hydrogen bond of original fracture during drying again It can not restore completely, its mechanical property is caused to be declined.Although PVC wallpaper progress of the invention is mould proof modified, horizontal, Longitudinal wet tensile (strength) is declined respectively, but because of range of decrease very little, meets light industry proposed standard《Wallpaper》(QB/T 4034- 2010) standard of high-class product (horizontal, longitudinal wetting tensile load >=0.33kN/m) in.
As can also be seen from Table 5, longitudinal wet tensile (strength) of PVC wallpaper is all larger than laterally wet anti-tensile mould proof afterwards before modified Intensity.This is because the base material of PVC mildew-proof wallpaper of the invention is plant fiber body paper, longitudinal wet tensile (strength) is big In lateral wet tensile (strength).Therefore the cross of plant fiber body paper, the difference of vertical mixing coefficient determine the horizontal, vertical of PVC wallpaper The difference of mechanical property.
5 PVC wallpaper of table it is mould proof before modified after wet tensile (strength)
In short, the mould proof modification of PVC wallpaper will not reduce the mechanical property of PVC wallpaper too much, meets light industry and push away Recommend standard《Wallpaper》The standard of high-class product (horizontal, longitudinal wetting tensile load >=0.33kN/m) in (QB/T 4034-2010).
In conclusion the present invention has the following advantages that：
(1) present invention is using chitosan/glacial acetic acid mixed solution as carrier, using tripolyphosphate sodium water solution as crosslinking Agent uses ion respectively using sodium fluoride, copper fluoride, copper sulphate, Kocide SD, zinc chloride and sorbic acid as antimildew and antibacterial agent Cross-linking method, which is mixed to prepare, carries medicine chitosan microball lotion, and is sprayed on using plant fiber body paper as the PVC wallpaper of substrate All kinds of load medicine chitosan/PVC mildew-proof wallpapers are prepared after dry in base paper surface.In chitosan solution, antimildew and antibacterial agent, trimerization The concentration ratio of sodium phosphate aqueous solution is 16:3:When 2, chitosan/sodium fluoride/PVC mildew-proof wallpaper to the anti-mold effect of aspergillus niger most It is good.
(2) present invention using the PVC wallpaper of chitosan/sodium fluoride microballoon lotion preparation to the anti-mold effect of aspergillus niger most It is good.
(3) chitosan/sodium fluoride/PVC mildew-proof wallpaper anti-mold effect is continuous with the increase of chitosan solution concentration It is promoted, when chitosan solution concentration reaches 14g/L or more, mildew-proof wallpaper sample reaches the mould proof area of aspergillus niger 80% or so, national 2 grade standards are reached to the average mould proof grade of aspergillus niger, anti-mold effect is preferable.
(4) chitosan/fluorination for preparing when chitosan solution concentration is 16g/L, and Fluorinse concentration is 3g/L Sodium/PVC mildew-proof wallpaper, mildew-proof wallpaper have nearly reached 100% to the mould proof area of aspergillus niger, mould proof etc. to being averaged for aspergillus niger Grade reaches national 0 grade standard, and anti-mold effect is splendid.
(5) when the concentration of chitosan and sodium fluoride ratio is 16:When 3, project Electronic Speculum observation indicate that, chitosan/fluorine It is uniform to change sodium microballoon shape size distribution, shows spherical state, substantially so as to more effectively play the mould proof of sodium fluoride Effect；
(6) mould proof modification is carried out to PVC wallpaper, the mechanical property of PVC wallpaper, horizontal, longitudinal wet will not be reduced too much Tensile strength is still able to satisfy the requirement of professional standard high-class product.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or the terminal device that include a series of elements not only include those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or end The intrinsic element of end equipment.In the absence of more restrictions, being limited by sentence " including ... " or " including ... " Element, it is not excluded that there is also other elements in process, method, article or the terminal device for including the element.This Outside, herein, " being greater than ", " being less than ", " being more than " etc. are interpreted as not including this number；" more than ", " following ", " within " etc. understand Being includes this number.
Although the various embodiments described above are described, once a person skilled in the art knows basic wounds The property made concept, then additional changes and modifications can be made to these embodiments, so the above description is only an embodiment of the present invention, It is not intended to limit scope of patent protection of the invention, it is all to utilize equivalent structure made by description of the invention and accompanying drawing content Or equivalent process transformation, being applied directly or indirectly in other relevant technical fields, similarly includes in patent of the invention Within protection scope.

Claims (7)

1. a kind of appendix has the preparation method for the mildew-proof wallpaper for carrying medicine chitosan, the mildew-proof wallpaper is to be with plant fiber body paper The PVC wallpaper of substrate, it is characterised in that：The preparation method comprises the following steps：
By the one side of the plant fiber body paper substrate of the load medicine chitosan microball Emulsion Spraying containing antimildew and antibacterial agent to PVC wallpaper On, the lotion amount of spraying is 0.5~4mL/m2；
PVC wallpaper after spraying is dried into 45~60s at 150~180 DEG C, appendix, which is prepared, the mould proof of load medicine chitosan Wallpaper；
The preparation method for carrying medicine chitosan microball lotion includes the following steps：
It is 0.5~3g/L antimildew and antibacterial that configuration concentration, which is 2~3g/L tripolyphosphate sodium water solution as crosslinking agent and configuration concentration, Agent aqueous solution；
Chitosan is added in 0.5~2% glacial acetic acid solution, is sufficiently dissolved, and adjusting solution ph is 2~4, configuration obtains Chitosan concentration is chitosan/glacial acetic acid mixed solution of 4~16g/L as appendix agent；
By antimildew and antibacterial agent aqueous solution and crosslinking agent by volume 1~2:1 is uniformly mixed, and obtains antimildew and antibacterial agent mixed solution, Then antimildew and antibacterial agent mixed solution is slowly dropped into chitosan/glacial acetic acid solution, 2~4h is stirred at room temperature, until mixed It closes solution and shows shallow white, stop stirring, obtain carrying medicine chitosan microball lotion；The antimildew and antibacterial agent mixed solution and shell Glycan/glacial acetic acid solution volume ratio is 1:1~1.5；Antimildew and antibacterial agent in the antimildew and antibacterial agent aqueous solution is in following One kind：Sodium fluoride, copper fluoride, copper sulphate, Kocide SD, zinc chloride or sorbic acid.
2. the preparation method of mildew-proof wallpaper according to claim 1, it is characterised in that：The antimildew and antibacterial agent is fluorination Sodium.
3. the preparation method of mildew-proof wallpaper according to claim 1, it is characterised in that：The antimildew and antibacterial agent aqueous solution Concentration is 3g/L, and the concentration of the chitosan/glacial acetic acid mixed solution is 16g/L.
4. the preparation method of mildew-proof wallpaper according to claim 1, it is characterised in that：The load medicine chitosan microball lotion Quantity for spray in PVC wallpaper is 2~3mL/m2。
5. the preparation method of mildew-proof wallpaper according to claim 1, it is characterised in that：It further include step：The PVC wallpaper Preceding 60~the 90s dry at 100~120 DEG C of spraying.
6. a kind of appendix has the mildew-proof wallpaper for carrying medicine chitosan, it is characterised in that：It includes PVC wallpaper layer, the PVC wallpaper layer For using plant fiber body paper as the PVC wallpaper of substrate, the mildew-proof wallpaper further includes the plant fiber body paper coated in PVC wallpaper Load medicine chitosan layer on substrate surface, the load medicine chitosan carried in medicine chitosan layer side as described in one of Claims 1 to 5 Method preparation.
7. mildew-proof wallpaper according to claim 6, it is characterised in that：The load medicine chitosan layer is by load medicine chitosan microball It is formed on Emulsion Spraying to the plant fiber body paper substrate surface of PVC wallpaper, the load medicine chitosan microball lotion is in PVC wallpaper Quantity for spray be 0.5~4mL/m2。
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