CN103999880B - A kind of fragrance leather fungicide and its preparation method and application - Google Patents
A kind of fragrance leather fungicide and its preparation method and application Download PDFInfo
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- 239000010985 leather Substances 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000417 fungicide Substances 0.000 title claims description 50
- 230000000855 fungicidal effect Effects 0.000 title claims description 48
- 239000003205 fragrance Substances 0.000 title claims description 41
- 239000000341 volatile oil Substances 0.000 claims abstract description 46
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 14
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 14
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 241000196324 Embryophyta Species 0.000 claims description 43
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 26
- 239000000839 emulsion Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- 238000010792 warming Methods 0.000 claims description 18
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000003643 water by type Substances 0.000 claims description 12
- 230000001276 controlling effect Effects 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 239000010634 clove oil Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 239000010678 thyme oil Substances 0.000 claims description 5
- 239000003429 antifungal agent Substances 0.000 abstract description 20
- 241000228245 Aspergillus niger Species 0.000 abstract description 6
- 125000003118 aryl group Chemical group 0.000 abstract description 3
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract description 2
- 241000228150 Penicillium chrysogenum Species 0.000 abstract 2
- HBXWUCXDUUJDRB-UHFFFAOYSA-N 1-octadecoxyoctadecane Chemical compound CCCCCCCCCCCCCCCCCCOCCCCCCCCCCCCCCCCCC HBXWUCXDUUJDRB-UHFFFAOYSA-N 0.000 abstract 1
- 229920001213 Polysorbate 20 Polymers 0.000 abstract 1
- 229940121375 antifungal agent Drugs 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 150000002191 fatty alcohols Chemical class 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229920000058 polyacrylate Polymers 0.000 abstract 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 abstract 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 230000000694 effects Effects 0.000 description 11
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 10
- 241000465255 Penicillium citreoviride Species 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 238000002356 laser light scattering Methods 0.000 description 4
- 239000002775 capsule Substances 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- -1 acrylic ester Chemical class 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- 229940123208 Biguanide Drugs 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 239000001888 Peptone Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004283 biguanides Chemical class 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000001408 fungistatic effect Effects 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
本发明公开了一种芳香皮革防霉剂及制备方法和其在皮革防霉处理中的应用，所述的芳香皮革防霉剂按质量份数计算，由0.300～0.900份植物精油、0.176～0.930份吐温20、0.075～0.160份脂肪醇聚氧乙烯醚、0.075～0.160份聚氧乙烯-2(21)硬脂醇醚、2.835～3.743份丙烯酸乙酯、5.275～6.165份甲基丙烯酸甲酯、0.216～0.242份过硫酸铵和89.404～89.471份去离子水组成。其制备方法是以聚丙烯酸酯为壁材通过乳液聚合法对植物精油进行包覆，制备出的芳香皮革防霉剂能有效防止皮革上霉菌，特别是黑曲霉、黄绿青霉和产黄青霉的滋长，并能同时实现皮革的加香。The invention discloses an aromatic leather anti-mold agent, a preparation method and its application in leather anti-mold treatment. Parts of Tween 20, 0.075-0.160 parts of fatty alcohol polyoxyethylene ether, 0.075-0.160 parts of polyoxyethylene-2(21) stearyl ether, 2.835-3.743 parts of ethyl acrylate, 5.275-6.165 parts of methyl methacrylate , 0.216-0.242 parts of ammonium persulfate and 89.404-89.471 parts of deionized water. The preparation method uses polyacrylate as the wall material to coat the plant essential oil by emulsion polymerization, and the prepared aromatic leather antifungal agent can effectively prevent mold on the leather, especially Aspergillus niger, Penicillium chrysogenum and Penicillium chrysogenum. It grows and at the same time achieves the perfuming of the leather.
Description
Technical field
The present invention relates to a kind of fragrance leather fungicide and its preparation method and application.
Background technology
Leatherware commonly uses in daily life. Leather is a kind of natural polymer converted products, and it is mainly composed of collagen protein and fat, additionally adds a large amount of animal oil, inorganic salt and casein etc. in the course of processing, and these all become the nutrient source of fungus growth; Meanwhile to have loose structure and hygroscopicity relatively strong for leather, and water content is higher, environment sultry in storage and transport process, and these are all that mycete grows and provides suitable temperature and moisture environment. Mouldy leatherware there will be bacterium colony or the mottle of white, blueness, yellow and black, and the mycete on surface is to leather fiber in-house development so that the wearability of leatherware, intensity and elasticity are all affected, and therefore mildew-resistant is to leatherware particular importance.
Common leather fungicide according to chemical composition can be divided into organic and inorganic and natural fungicidal agent. Organic antifungus agent is quaternary ammonium salt, biguanides, pyridines, imidazoles, thiophene-based etc. such as, and such antifungus agent has quick-acting anti-mold effect, but toxicity is big.
The metal class of mineral-type antifungus agent and photocatalysis class, such as silver system antifungus agent, anti-mold effect secure persistent, but expensive, speed of action is slow, easy to change.
Natural fungicidal agent rests in Conventional wisdom level more.
Though common antifungus agent can play certain anti-mold effect above, but all not mentioned improve leather fatty odor.
Plants essential oil is a kind of natural antibacterial agent, is made up of multiple aromatic, but it is volatile, oxidizable under the conditions such as photo-thermal. Adopt emulsion polymerization that plants essential oil is coated with, the stability of quintessence oil can be effectively improved, there is stronger slow-release capability. Applied Leather mildew-proof to process, not only there is good anti-mold effect, and the fragrance of plants essential oil can be effectively improved the oils and fats gas of leather. This preparation technology is simple, has good application prospect.
Summary of the invention
An object of the present invention is to provide a kind of fragrance leather fungicide, and this fragrance leather fungicide is possible not only to play anti-mold effect, but also can be effectively improved the oils and fats gas of leather.
The preparation method that the two of the purpose of the present invention are to provide above-mentioned a kind of fragrance leather fungicide.
The three of the purpose of the present invention are to provide above-mentioned a kind of fragrance leather fungicide using method in Leather mildew-proof processes.
Technical scheme
A kind of fragrance leather fungicide, calculates according to the mass fraction, and composition and the content of its raw material are as follows:
Plants essential oil 0.300��0.900 part
Polysorbas20 0.176��0.930 part
Fatty alcohol-polyoxyethylene ether 0.075��0.160 part
The stearic alcohol ether 0.075��0.160 part of polyoxyethylene-2 (21)
Ethyl acrylate 2.835��3.743 parts
Methyl methacrylate 5.275��6.165 parts
Ammonium persulfate. 0.216��0.242 part
Deionized water 89.404��89.471 parts
Described plants essential oil is clove oil, Herba Lysimachiae foenum-graeci quintessence oil or thyme oil.
The preparation method of above-mentioned fragrant leather fungicide, specifically includes following steps:
(1), by 0.300��0.900 part of plants essential oil, 0.176��0.930 part of polysorbas20,0.075��0.160 part of fatty alcohol-polyoxyethylene ether and 0.075��0.160 part of stearic alcohol ether of polyoxyethylene-2 (21) join in 79.404��79.471 parts of deionized waters, it is stirring 30min under 300-450r/min at rotating speed, homogenizing 10min, obtains plants essential oil emulsion;
(2), 2.835��3.743 parts of ethyl acrylate and 5.275��6.165 parts of methyl methacrylate Homogeneous phase mixing are obtained solution A;
Being dissolved in 10 parts of deionized waters by 0.216��0.242 part of Ammonium persulfate. Homogeneous phase mixing obtains solution B;
(3), step (1) gained plants essential oil emulsion is added in 250ml there-necked flask, being stir under 250-350r/min at rotating speed, be warming up to 60 DEG C and keep 10min, the solution B of the solution A and 1/5 volume that take 1/5 volume respectively joins there-necked flask, continue reaction 30min, obtain emulsion;
(4) after, step (3) gained emulsion being warming up to 70 DEG C, drip the solution A of remaining 4/5 volume and the solution B of remaining 4/5 volume successively respectively, controlling total time for adding is 50��90min, 80 DEG C it are warming up to after dropwising, it is reaction 5��7h under 250-350r/min at rotating speed, finally regulating pH with the strong aqua ammonia of mass fraction 25% is 6��7, obtains fragrant leather fungicide.
The mean diameter of above-mentioned obtained fragrant leather fungicide is 188.400nm��267.500nm, the load factor of plants essential oil is 15.581%��32.435%, fragrance leather fungicide is applied to leather and can effectively suppress the growth of aspergillus niger, Penicillium citreo-viride and Penicllium chrysogenum.
The mildew-resistant that above-mentioned fragrant leather fungicide is used for leather processes, and it specifically comprises the following steps that
Under 25��38 DEG C of conditions, leather is calculated in mass ratio with fragrance antifungus agent, i.e. leather: the ratio that fragrance antifungus agent is 1:5��8 mixes, then regulating pH with the sodium bicarbonate aqueous solution of mass fraction 10% is 5.6-7, controlling rotating speed is that 500-600r/min processes 3��6h, subsequently leather is taken out dewatering naturally to dry, namely obtain the leather processed with fragrance leather fungicide.
Beneficial effects of the present invention
A kind of fragrance leather fungicide of the present invention, i.e. plant essential oil capsules, owing to adopting low-cost acrylic ester monomer to be raw material, with plants essential oil drop for template, making acrylic ester monomer cladding plants essential oil drop be polymerized, obtain monodispersity better, particle size distribution is at the nano-essential oil capsule of 188.400nm��267.500nm, to the load factor of plants essential oil up to 15.581%��32.435%, it is effectively increased the utilization rate of plants essential oil.
A kind of fragrance leather fungicide of the present invention and plant essential oil capsules are directly used in Leather mildew-proof process, aspergillus niger, Penicillium citreo-viride and Penicllium chrysogenum are had good inhibitory action;And plants essential oil is as a kind of volatile oil, can effectively cover the distinctive fatty odor of leather, plays and composes fragrant effect. Therefore, a kind of fragrance leather fungicide of the present invention is applied to Leather mildew-proof, can effectively suppress common mycete and give leather fragrance.
Detailed description of the invention
By the examples below the present invention is described in further detail, but be not limiting as the present invention.
In various embodiments of the present invention, methyl methacrylate used, ethyl acrylate, polysorbas20, fatty alcohol-polyoxyethylene ether, the stearic alcohol ether of polyoxyethylene-2 (21) and Ammonium persulfate. are analytical pure, purchased from traditional Chinese medicines group chemical reagent Shanghai company limited, clove oil, Herba Lysimachiae foenum-graeci quintessence oil and thyme oil are purchased from Shanghai Jing Chun biochemical technology limited company, and deionized water is made by oneself. Aspergillus niger used in embodiments of the invention, Penicllium chrysogenum and Penicillium citreo-viride are all purchased from Shanghai City DSMZ of institute of microbiology.
Embodiment 1
A kind of fragrance leather fungicide, calculates according to the mass fraction, and composition and the content of its raw material are as follows:
Plants essential oil 0.300 part
Polysorbas20 0.930 part
Fatty alcohol-polyoxyethylene ether 0.075 part
The stearic alcohol ether 0.075 part of polyoxyethylene-2 (21)
Ethyl acrylate 2.835 parts
Methyl methacrylate 6.165 parts
Ammonium persulfate. 0.216 part
Deionized water 89.404 parts
Described plants essential oil is clove oil.
The preparation method of above-mentioned fragrant leather fungicide, specifically includes following steps:
(1), by 0.300 part of plants essential oil, 0.930 part of polysorbas20,0.075 part of fatty alcohol-polyoxyethylene ether and 0.075 part of stearic alcohol ether of polyoxyethylene-2 (21) join in 79.404 parts of deionized waters, it is stirring 30min under 300r/min at rotating speed, homogenizing 10min, obtains plants essential oil emulsion;
(2), 2.835 parts of ethyl acrylate and 6.165 parts of methyl methacrylate Homogeneous phase mixing are obtained solution A;
Being dissolved in 10 parts of deionized waters by 0.216 part of Ammonium persulfate. Homogeneous phase mixing obtains solution B;
(3), step (1) gained plants essential oil emulsion is added in 250ml there-necked flask, being stir under 350r/min at rotating speed, be warming up to 60 DEG C and keep 10min, the solution B of the solution A and 1/5 volume that take 1/5 volume respectively joins there-necked flask, continue reaction 30min, obtain emulsion;
(4) after, step (3) gained emulsion being warming up to 70 DEG C, drip the solution A of remaining 4/5 volume and the solution B of remaining 4/5 volume successively, controlling total time for adding is 50min, 80 DEG C it are warming up to after dropwising, it is reaction 5h under 250r/min at rotating speed, finally regulating pH with the strong aqua ammonia of mass fraction 25% is 6, obtains fragrant leather fungicide.
Above-mentioned obtained fragrant leather fungicide passes through dynamic laser light scattering instrument (ZetasizerNanoZS, Malvern Instr Ltd. of Britain) mean diameter that records is 188.400nm, the load factor being measured clove oil by thermogravimetric analyzer (TGAQ5000IR, TA Instrument Ltd. of the U.S.) is 15.581%.
The mildew-resistant that above-mentioned fragrant leather fungicide is used for leather processes, and specifically comprises the following steps that
Under 25 DEG C of conditions, leather is calculated in mass ratio with fragrance antifungus agent, i.e. leather: the ratio that fragrance antifungus agent is 1:5 mixes, then regulating pH with the sodium bicarbonate aqueous solution of mass fraction 10% is 5.6, controlling rotating speed is that 500r/min processes 4h, subsequently leather is taken out dewatering naturally to dry, namely obtain the leather processed with fragrance leather fungicide.
Embodiment 2
A kind of fragrance leather fungicide, calculates according to the mass fraction, and composition and the content of its raw material are as follows:
Plants essential oil 0.500 part
Polysorbas20 0.560 part
Fatty alcohol-polyoxyethylene ether 0.125 part
The stearic alcohol ether 0.125 part of polyoxyethylene-2 (21)
Ethyl acrylate 3.215 parts
Methyl methacrylate 5.785 parts
Ammonium persulfate. 0.219 part
Deionized water 89.471 parts
Described plants essential oil is Herba Lysimachiae foenum-graeci quintessence oil.
The preparation method of above-mentioned fragrant leather fungicide, specifically includes following steps:
(1), by 0.500 part of plants essential oil, 0.560 part of polysorbas20,0.125 part of fatty alcohol-polyoxyethylene ether and 0.125 part of stearic alcohol ether of polyoxyethylene-2 (21) join in 79.471 parts of deionized waters, it is stirring 30min under 450r/min at rotating speed, homogenizing 10min, obtains plants essential oil emulsion;
(2), 3.215 parts of ethyl acrylate and 5.785 parts of methyl methacrylate Homogeneous phase mixing are obtained solution A;
Being dissolved in 10 parts of deionized waters by 0.219 part of Ammonium persulfate. Homogeneous phase mixing obtains solution B;
(3), step (1) gained plants essential oil emulsion is added in 250ml there-necked flask, being stir under 300r/min at rotating speed, be warming up to 60 DEG C and keep 10min, the solution B of the solution A and 1/5 volume that take 1/5 volume respectively joins there-necked flask, continue reaction 30min, obtain emulsion;
(4) after, step (3) gained emulsion being warming up to 70 DEG C, drip the solution A of remaining 4/5 volume and the solution B of remaining 4/5 volume successively, controlling total time for adding is 70min, 80 DEG C it are warming up to after dropwising, it is reaction 6h under 300r/min at rotating speed, finally regulating pH with the strong aqua ammonia of mass fraction 25% is 7, obtains fragrant leather fungicide.
Above-mentioned obtained fragrant leather fungicide is 216.100nm by the mean diameter that dynamic laser light scattering instrument records, and the load factor being measured Herba Lysimachiae foenum-graeci quintessence oil by thermogravimetric analyzer is 23.467%.
The mildew-resistant that above-mentioned fragrant leather fungicide is used for leather processes, and specifically comprises the following steps that
Under 30 DEG C of conditions, leather is calculated in mass ratio with fragrance antifungus agent, i.e. leather: the ratio that fragrance antifungus agent is 1:7 mixes, then regulating pH with the sodium bicarbonate aqueous solution of mass fraction 10% is 6, controlling rotating speed is that 550r/min processes 5h, subsequently leather is taken out dewatering naturally to dry, namely obtain the leather processed with fragrance leather fungicide.
Embodiment 3
A kind of fragrance leather fungicide, calculates according to the mass fraction, and composition and the content of its raw material are as follows:
Plants essential oil 0.700 part
Polysorbas20 0.310 part
The stearic alcohol ether 0.160 part of polyoxyethylene-2 (21)
Fatty alcohol-polyoxyethylene ether 0.160 part
Ethyl acrylate 3.515 parts
Methyl methacrylate 5.485 parts
Ammonium persulfate. 0.231 part
Deionized water 89.439 parts
Described plants essential oil is thyme oil.
The preparation method of above-mentioned fragrant leather fungicide, specifically includes following steps:
(1), by 0.700 part of plants essential oil, 0.310 part of polysorbas20,0.160 part of fatty alcohol-polyoxyethylene ether and 0.160 part of stearic alcohol ether of polyoxyethylene-2 (21) join in 79.439 parts of deionized waters, it is stirring 30min under 400r/min at rotating speed, homogenizing 10min, obtains plants essential oil emulsion;
(2), 3.515 parts of ethyl acrylate and 5.485 parts of methyl methacrylate Homogeneous phase mixing are obtained solution A;
Being dissolved in 10 parts of deionized waters by 0.231 part of Ammonium persulfate. Homogeneous phase mixing obtains solution B;
(3), step (1) gained plants essential oil emulsion is added in 250ml there-necked flask, being stir under 350r/min at rotating speed, be warming up to 60 DEG C and keep 10min, the solution B of the solution A and 1/5 volume that take 1/5 volume respectively joins there-necked flask, continue reaction 30min, obtain emulsion;
(4) after, step (3) gained emulsion being warming up to 70 DEG C, drip the solution A of remaining 4/5 volume and the solution B of remaining 4/5 volume successively, controlling total time for adding is 90min, 80 DEG C it are warming up to after dropwising, it is reaction 6h under 300r/min at rotating speed, finally regulating pH with the strong aqua ammonia that mass fraction is 25% is 7, obtains fragrant leather fungicide.
Above-mentioned obtained fragrant leather fungicide is 267.500nm by the mean diameter that dynamic laser light scattering instrument records, and the load factor being measured thyme oil by thermogravimetric analyzer is 32.435%.
The mildew-resistant that above-mentioned fragrant leather fungicide is used for leather processes, and specifically comprises the following steps that
Under 38 DEG C of conditions, leather is calculated in mass ratio with fragrance antifungus agent, i.e. leather: the ratio that fragrance antifungus agent is 1:7 mixes, then regulating pH with the sodium bicarbonate aqueous solution of mass fraction 10% is 6, controlling rotating speed is that 550r/min processes 5h, subsequently leather is taken out dewatering naturally to dry, namely obtain the leather processed with fragrance leather fungicide.
Embodiment 4
A kind of fragrance leather fungicide, calculates according to the mass fraction, and composition and the content of its raw material are as follows:
Plants essential oil 0.900 part
Polysorbas20 0.176 part
Fatty alcohol-polyoxyethylene ether 0.137 part
The stearic alcohol ether 0.137 part of polyoxyethylene-2 (21)
Ethyl acrylate 3.743 parts
Methyl methacrylate 5.257 parts
Ammonium persulfate. 0.242 part
Deionized water 89.408 parts
Described plants essential oil is clove oil.
The preparation method of above-mentioned fragrant leather fungicide, specifically includes following steps:
(1), by 0.900 part of plants essential oil, 0.176 part of polysorbas20,0.137 part of fatty alcohol-polyoxyethylene ether and 0.137 part of stearic alcohol ether of polyoxyethylene-2 (21) join in 89.408 parts of deionized waters, it is stirring 30min under 400r/min at rotating speed, homogenizing 10min, obtains plants essential oil emulsion;
(2), 3.743 parts of ethyl acrylate and 5.275 parts of methyl methacrylate Homogeneous phase mixing are obtained solution A;
Being dissolved in 10 parts of deionized waters by 0.242 part of Ammonium persulfate. Homogeneous phase mixing obtains solution B;
(3), step (1) gained plants essential oil emulsion is added in 250ml there-necked flask, being stir under 250r/min at rotating speed, be warming up to 60 DEG C and keep 10min, the solution B of the solution A and 1/5 volume that take 1/5 volume respectively joins there-necked flask, continue reaction 30min, obtain emulsion;
(4) after, step (3) gained emulsion being warming up to 70 DEG C, drip the solution A of remaining 4/5 volume and the solution B of remaining 4/5 volume successively, controlling total time for adding is 70min, 80 DEG C it are warming up to after dropwising, it is reaction 6h under 300r/min at rotating speed, finally regulating pH with the strong aqua ammonia of mass fraction 25% is 7, obtains fragrant leather fungicide.
Above-mentioned obtained fragrant leather fungicide is 236.5nm by the mean diameter that dynamic laser light scattering instrument records, and the load factor being measured clove oil by thermogravimetric is 28.225%.
The mildew-resistant that above-mentioned fragrant leather fungicide is used for leather processes, and specifically comprises the following steps that
Under 35 DEG C of conditions, leather is calculated in mass ratio with fragrance antifungus agent, i.e. leather: the ratio that fragrance antifungus agent is 1:7 mixes, then regulating pH with the sodium bicarbonate aqueous solution of mass fraction 10% is 6, controlling rotating speed is that 600r/min processes 6h, subsequently leather is taken out dewatering naturally to dry, namely obtain the leather processed with fragrance leather fungicide.
The above-mentioned leather processed through fragrance leather fungicide is carried out anti-mold effect test, below step:
(1), taking containing strain concentration is 107��108The bacteria suspension 0.5ml of the aspergillus niger of CFU/ml, Penicllium chrysogenum and Penicillium citreo-viride is uniformly coated on the solid medium of beef extract-peptone, makes containing bacterium flat board;
(2), by embodiment 4 through fragrance antifungus agent process after leather sampling (diameter is 25mm), cut-off footpath is that the untreated common leather of 25mm is as reference simultaneously, take three groups of Duplicate Samples respectively, all leather samples are carried out ultra-vioket radiation, sterilizing 20min in biological aseptic operating platform;
(3), sterilized fragrance leather and common leather in step (2) are respectively placed in cultivating in 28 DEG C of constant incubators containing on bacterium flat board in step (1);
(4), cultivate and the mildew-resistant loop diameter that fragrance leather produces is deducted the mildew-resistant loop diameter that common leather produces, parallel assay three times after different time, average and be the anti-mold effect data of this fragrance leather, every 24h observed and recorded data.
Test result shows, after placing 8 days, common leather sample has covered with mycete, and the inhibition zone of aspergillus niger is 30 �� 2cm by leather after fragrance antifungus agent processes, and the inhibition zone to Penicllium chrysogenum is 28 �� 2cm, inhibition zone to Penicillium citreo-viride is 29 �� 2cm, and its fungistatic effect is substantially better than common leather. It is indicated above the fragrant leather fungicide of the present invention, there is good anti-mold effect.
In sum, the fragrant leather fungicide mean diameter of the present invention is 188.400nm��267.500nm, and the load factor to plants essential oil is 15.581%��32.435%. Fungus-proof test result shows, contrasts common leather sample, the leather after this fragrance antifungus agent processes, and effectively extends the anti-mold effect to different mycetes. This antifungus agent preparation method is simple simultaneously, and size tunable is strong, and plants essential oil load factor is high, and anti-mold effect is obvious, and application is stronger.
Above said content is only the basic explanation under present inventive concept, and according to any equivalent transformation that technical scheme is done, all should belong to protection scope of the present invention.
Claims (1)
1. a preparation method for fragrant leather fungicide, described fragrance leather fungicide, to calculate according to the mass fraction, composition and the content of its raw material are as follows:
Plants essential oil 0.300��0.900 part
Polysorbas20 0.176��0.930 part
Fatty alcohol-polyoxyethylene ether 0.075��0.160 part
The stearic alcohol ether 0.075��0.160 part of polyoxyethylene-2 (21)
Ethyl acrylate 2.835��3.743 parts
Methyl methacrylate 5.275��6.165 parts
Ammonium persulfate. 0.216��0.242 part
Deionized water 89.404��89.471 parts
Described plants essential oil is clove oil, Herba Lysimachiae foenum-graeci quintessence oil or thyme oil;
It is characterized in that the method specifically includes following steps:
(1) by 0.300��0.900 part of plants essential oil, 0.176��0.930 part of polysorbas20,0.075��0.160 part of fatty alcohol-polyoxyethylene ether and 0.075��0.160 part of stearic alcohol ether of polyoxyethylene-2 (21) join in 79.404��79.471 parts of deionized waters, it is stirring 30min under 300-450r/min at rotating speed, homogenizing 10min, obtains plants essential oil emulsion;
(2) 2.835��3.743 parts of ethyl acrylate and 5.275��6.165 parts of methyl methacrylate Homogeneous phase mixing are obtained solution A; Being dissolved in 10 parts of deionized waters by 0.216��0.242 part of Ammonium persulfate. Homogeneous phase mixing obtains solution B;
(3) step (1) gained plants essential oil emulsion is added in 250ml there-necked flask, being stir under 250-350r/min at rotating speed, be warming up to 60 DEG C and keep 10min, the solution B of the solution A and 1/5 volume that take 1/5 volume respectively joins there-necked flask, continue reaction 30min, obtain emulsion;
(4) after step (3) gained emulsion being warming up to 70 DEG C, drip the solution A of remaining 4/5 volume and the solution B of remaining 4/5 volume successively respectively, controlling total time for adding is 50��90min, 80 DEG C it are warming up to after dropwising, it is reaction 5��7h under 250-350r/min at rotating speed, finally regulating pH with the strong aqua ammonia of mass fraction 25% is 6��7, obtains fragrant leather fungicide.
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| CN105532745B (en) * | 2015-12-24 | 2018-11-06 | 浙江竹之语生物科技股份有限公司 | A kind of leather fungicide and its preparation method and application |
| CN107460263A (en) * | 2017-08-29 | 2017-12-12 | 安徽乐踏鞋业有限公司 | A kind of Leather mildew-proof method |
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