CN115613361A - Preparation method of nano-silver microcapsule and application of nano-silver microcapsule in protective cloth cover - Google Patents
Preparation method of nano-silver microcapsule and application of nano-silver microcapsule in protective cloth cover Download PDFInfo
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- CN115613361A CN115613361A CN202211078584.5A CN202211078584A CN115613361A CN 115613361 A CN115613361 A CN 115613361A CN 202211078584 A CN202211078584 A CN 202211078584A CN 115613361 A CN115613361 A CN 115613361A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 239000003094 microcapsule Substances 0.000 title claims abstract description 81
- 239000004744 fabric Substances 0.000 title claims abstract description 42
- 230000001681 protective effect Effects 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000003756 stirring Methods 0.000 claims description 105
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 72
- 239000000463 material Substances 0.000 claims description 62
- 238000005488 sandblasting Methods 0.000 claims description 60
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 57
- 239000000661 sodium alginate Substances 0.000 claims description 57
- 235000010413 sodium alginate Nutrition 0.000 claims description 57
- 229940005550 sodium alginate Drugs 0.000 claims description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 55
- 239000008367 deionised water Substances 0.000 claims description 50
- 229910021641 deionized water Inorganic materials 0.000 claims description 50
- 239000007788 liquid Substances 0.000 claims description 47
- 238000002156 mixing Methods 0.000 claims description 41
- 238000001035 drying Methods 0.000 claims description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 30
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000010306 acid treatment Methods 0.000 claims description 23
- 239000011162 core material Substances 0.000 claims description 23
- 239000002202 Polyethylene glycol Substances 0.000 claims description 22
- 229920001223 polyethylene glycol Polymers 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 21
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 20
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 239000000194 fatty acid Substances 0.000 claims description 20
- 229930195729 fatty acid Natural products 0.000 claims description 20
- 239000004745 nonwoven fabric Substances 0.000 claims description 20
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 20
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 19
- 239000004576 sand Substances 0.000 claims description 18
- 230000000844 anti-bacterial effect Effects 0.000 claims description 17
- 238000001694 spray drying Methods 0.000 claims description 17
- 238000004381 surface treatment Methods 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 12
- -1 sorbitan fatty acid ester Chemical class 0.000 claims description 11
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 10
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 10
- 150000004665 fatty acids Chemical class 0.000 claims description 10
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 10
- 239000000347 magnesium hydroxide Substances 0.000 claims description 10
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 239000011775 sodium fluoride Substances 0.000 claims description 10
- 235000013024 sodium fluoride Nutrition 0.000 claims description 10
- 239000000600 sorbitol Substances 0.000 claims description 10
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 5
- 239000006004 Quartz sand Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- KVRITRBZWNXTTC-UHFFFAOYSA-N (1,2,2,3,3-pentaphosphonooxycyclohexyl) dihydrogen phosphate Chemical compound P(=O)(O)(O)OC1(C(C(CCC1)(OP(=O)(O)O)OP(=O)(O)O)(OP(=O)(O)O)OP(=O)(O)O)OP(=O)(O)O KVRITRBZWNXTTC-UHFFFAOYSA-N 0.000 claims description 4
- 230000035699 permeability Effects 0.000 abstract description 12
- 238000012360 testing method Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 5
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229940068041 phytic acid Drugs 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 241000222122 Candida albicans Species 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 229940095731 candida albicans Drugs 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 206010011409 Cross infection Diseases 0.000 description 2
- 206010029803 Nosocomial infection Diseases 0.000 description 2
- 229940072056 alginate Drugs 0.000 description 2
- 235000010443 alginic acid Nutrition 0.000 description 2
- 229920000615 alginic acid Polymers 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000005541 medical transmission Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a preparation method of a nano-silver microcapsule and application of the nano-silver microcapsule in a protective cloth cover, belonging to the field of medical preparation. After the nano-silver microcapsule prepared by the invention is used for treating the protective cloth cover, the air permeability of the protective cloth cover cannot be reduced, and the initial air permeability of the protective cloth cover is 295.2L/(cm) 2 S) and the air permeability after padding is 288.8-296.8L/(cm) 2 ·s）。
Description
Technical Field
The invention relates to a preparation method of a nano-silver microcapsule and application of the nano-silver microcapsule in a protective cloth cover, belonging to the field of medical preparations.
Background
In daily medical care work, microorganisms such as bacteria can be rapidly transmitted through droplets, contact, aerosol and other ways, so that medical care personnel who often directly or indirectly contact patients have a great infection risk, the bacteria are easy to propagate on various fabrics, most used fabrics can provide conditions for disease transmission and cross infection caused by pathogenic bacteria, in addition, the warm environment is more favorable for microorganism propagation, and the fabrics are good residences of the microorganisms.
The excellent protective material can generate a germ barrier layer, prevent germ migration and reduce cross infection, so that various medical protective materials are particularly important for guaranteeing the health of medical workers, and the nano-silver has higher thermal stability, surface activity and catalytic performance, is a nano-material with lasting antibacterial activity on pathogenic bacteria, is widely applied to textiles as an antibacterial finishing agent and further endows the textiles with antibacterial efficacy.
The method for processing the fabric by the antibacterial finishing agent comprises a surface coating method, a dipping method and the like, and the antibacterial finishing agent is further adsorbed and fixed on the surface of a fiber product, in order to ensure the continuity of the antibacterial performance, the microcapsule containing nano silver is prepared, and then the microcapsule is coated or dipped to be attached to the fabric, so that the long-time antibacterial performance is provided, and a common capsule wall material is alginate. CN102251408A discloses a nano silver antibacterial fabric based on microcapsule fabric finishing technology and a preparation method thereof, wherein alginate is used to wrap nano silver and prepare microcapsules are prepared, so that the fabric has long-term antibacterial performance, but when the prepared microcapsules are applied to antibacterial finishing of SMS nonwoven fabric materials, the air permeability of the nonwoven fabric can be reduced.
In summary, in the prior art, the antibacterial finishing agent containing nano-silver prepared by the microcapsule method can reduce the air permeability of the non-woven fabric after the SMS non-woven fabric material is subjected to antibacterial finishing.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and the nano-silver microcapsule is further prepared by processing the nano-silver and the wall material, so that the prepared nano-silver microcapsule can not reduce the air permeability of the non-woven fabric after the SMS non-woven fabric material is subjected to antibacterial finishing.
In order to solve the technical problem, the invention adopts the following technical scheme:
a preparation method of nano-silver microcapsules comprises the steps of nano-silver surface treatment, microcapsule wall material preparation and microcapsule preparation.
The following is a further improvement of the above technical solution:
the step of nano silver surface treatment comprises sand blasting treatment and acid treatment liquid treatment;
the sand blasting method comprises the steps of controlling the sand blasting pressure to be 0.45-0.55MPa and the sand blasting distance to be 140-160mm, carrying out sand blasting treatment on the nano-silver by using sand grains for sand blasting, wherein the sand blasting time is 4.5-5.5min, filtering the nano-silver by a filter screen after the sand blasting treatment, and removing the sand grains for sand blasting to obtain the nano-silver subjected to sand blasting treatment;
the grain size of the nano silver is 25-35nm;
mixing and stirring a phosphoric acid solution, inositol hexaphosphate, a hydrochloric acid solution and deionized water, completely dissolving all the components, adding ammonium persulfate and sodium fluoride, controlling the temperature to be 75-85 ℃, controlling the stirring speed to be 300-400r/min, stirring for 20-40min to obtain a mixed acid treatment solution, adding the sandblasted nano-silver into the mixed acid treatment solution, keeping the temperature unchanged, controlling the stirring speed to be 2800-3500r/min, stirring for 150-200min, filtering, washing and drying after stirring to obtain the surface-treated nano-silver;
the mass ratio of the phosphoric acid solution to the inositol hexaphosphate, the hydrochloric acid solution to the deionized water to the ammonium persulfate to the sodium fluoride is 14-16;
the mass ratio of the mixed acid treatment solution to the sandblasted nano-silver is 6.5-7.5.
The step of preparing the microcapsule wall material comprises cationization and post-treatment;
mixing and stirring sodium alginate and deionized water to completely dissolve the sodium alginate, adding a certain amount of potassium hydroxide, controlling the temperature to be 65-75 ℃, controlling the stirring speed to be 220-250r/min, stirring for 40-60min, then adding lauryl trimethyl ammonium bromide, keeping the temperature unchanged, controlling the stirring speed to be 250-350r/min, stirring for 85-110min, adding ethanol after stirring to separate out the sodium alginate, and then washing with alcohol and drying to obtain the cationized sodium alginate;
the mass ratio of the sodium alginate to the deionized water to the potassium hydroxide to the lauryl trimethyl ammonium bromide is (18-22);
mixing cationized sodium alginate with absolute ethyl alcohol, stirring to uniformly disperse the cationized sodium alginate, adding magnesium hydroxide, polyethylene glycol and sorbitol, controlling the stirring speed to be 1150-1450r/min, stirring for 85-115min, evaporating the ethanol after stirring to obtain a mixture, mixing the mixture with deionized water, filtering, adding ethanol into the filtrate to obtain a precipitate, and washing and drying the precipitate to obtain the posttreated sodium alginate;
the mass ratio of the cationized sodium alginate to the absolute ethyl alcohol to the magnesium hydroxide to the polyethylene glycol to the sorbitol is (45-55);
the mass ratio of the mixture to the deionized water is 1.
The step of preparing the microcapsule comprises preparing a wall material solution, preparing a core material solution, mixing, stirring and drying;
the method for preparing the wall material solution comprises the steps of mixing the post-treatment sodium alginate with deionized water, and completely dissolving the mixture to obtain the wall material solution;
the mass ratio of the post-treatment sodium alginate to the deionized water is 20-110;
the method for preparing the core material solution comprises the steps of mixing the surface-treated nano silver, deionized water and glyceryl tristearate, and uniformly stirring to obtain a core material dispersion liquid;
the mass ratio of the surface treatment nano silver to the deionized water to the tristearin is (30-50);
adding the core material dispersion liquid into the wall material solution, adding lauryl alcohol, sorbitan fatty acid ester and fatty acid diethanolamide, controlling the stirring speed to be 850-1100r/min, stirring for 40-50min, and stirring to obtain a microcapsule liquid;
the mass ratio of the core material dispersion liquid to the wall material solution to the lauryl alcohol to the sorbitan fatty acid ester to the fatty acid diethanolamide is 140-160;
the drying method comprises the step of carrying out spray drying on the microcapsule liquid to obtain the nano-silver microcapsule.
In the sand blasting step, the filter screen is a 300-mesh filter screen, and the sand grains for sand blasting are 0.1mm quartz sand.
In the step of treating the acid treatment solution, the mass concentration of the phosphoric acid solution is 80-87%, and the mass concentration of the hydrochloric acid solution is 32-36%.
In the step of preparing the microcapsule, the drying pressure of spray drying is 11.5-12.5MPa, the air inlet temperature of the spray drying is 115-125 ℃, and the air outlet temperature of the spray drying is 85-95 ℃.
The application method of the nano-silver microcapsule in the protective cloth cover comprises the steps of mixing the nano-silver microcapsule with absolute ethyl alcohol, acrylic acid and polyethylene glycol to obtain padding liquid, padding the protective cloth cover material, wherein the padder speed is 30m/min, the padder pressure is 1.5kg, 150kg of the protective cloth cover material is processed by every 100kg of the padding liquid, and drying the protective cloth cover material at 80 ℃ after padding to obtain the antibacterial protective cloth cover material;
the padding liquid comprises the following components in parts by mass: 7 parts of nano-silver microcapsules, 100 parts of absolute ethyl alcohol, 5 parts of acrylic acid and 3 parts of polyethylene glycol;
the protective cloth cover is made of SMS non-woven fabric.
Compared with the prior art, the invention has the following beneficial effects:
after the nano-silver microcapsule prepared by the invention is used for treating the protective cloth cover, the high bacteriostasis rate can be maintained for a long time, the initial bacteriostasis rate after finishing is high, the bacteriostasis rate to staphylococcus aureus is 99.6-99.8%, the bacteriostasis rate to escherichia coli is 96.8-97.9%, the bacteriostasis rate to candida albicans is 98.1-99.2%, after washing resistance test (washing in clean water for 50 times), the bacteriostasis rate to staphylococcus aureus is 99.3-99.4%, the bacteriostasis rate to escherichia coli is 96.5-97.2%, the bacteriostasis rate to candida albicans is 98.0-98.7%, after washing resistance test (washing in acid, alkaline and inorganic salt artificial sweat for 30 times), the bacteriostasis rate to staphylococcus aureus is 99.1-99.3%, the bacteriostasis rate to escherichia coli is 95.8-96.9%, and the bacteriostasis rate to candida albicans is 97.3-98.2%;
after the nano-silver microcapsule prepared by the invention is used for treating the protective cloth cover, the air permeability of the protective cloth cover cannot be reduced, and the initial air permeability of the protective cloth cover is 295.2L/(cm) 2 S) and the air permeability after padding is 288.8-296.8L/(cm) 2 ·s）；
After the nano-silver microcapsule prepared by the invention is used for treating the protective cloth cover, the water impermeability of the protective cloth cover can be improved, and the initial water impermeability of the protective cloth cover is 65cmH 2 O, the water permeability resistance after padding is 92-99cmH 2 O。
Detailed Description
Example 1 preparation method of nano silver microcapsule
(1) Surface treatment of nano silver
a. Sand blasting treatment
Controlling the sand blasting pressure of a sand blasting machine to be 0.5MPa, controlling the sand blasting distance to be 150mm, carrying out sand blasting treatment on the nano silver by using sand grains for sand blasting, wherein the sand blasting time is 5min, filtering the sand grains for sand blasting by using a 300-mesh filter screen after the sand blasting treatment, and removing the sand grains for sand blasting to obtain the sand blasting nano silver;
the sand particles for sand blasting are 0.1mm quartz sand;
the grain size of the nano silver is 30nm;
b. acid treatment fluid treatment
Mixing and stirring a phosphoric acid solution, a cyclohexanehexol hexaphosphate, a hydrochloric acid solution and deionized water, completely dissolving all the components, then adding ammonium persulfate and sodium fluoride, controlling the temperature to be 80 ℃, controlling the stirring speed to be 350r/min, stirring for 25min to obtain a mixed acid treatment solution, then adding sandblasting nano-silver into the mixed acid treatment solution, keeping the temperature unchanged, controlling the stirring speed to be 3000r/min, stirring for 180min, filtering, washing and drying after stirring to obtain surface treatment nano-silver;
the mass ratio of the phosphoric acid solution to the inositol hexaphosphate, the hydrochloric acid solution to the deionized water to the ammonium persulfate to the sodium fluoride is 15;
the mass concentration of the phosphoric acid solution is 85 percent;
the mass concentration of the hydrochloric acid solution is 35%;
the mass ratio of the mixed acid treatment solution to the sandblasted nano-silver is 7.
(2) Preparation of microcapsule wall material
a. Cationization
Mixing and stirring sodium alginate and deionized water to completely dissolve the sodium alginate, adding a certain amount of potassium hydroxide, controlling the temperature to be 70 ℃ and the stirring speed to be 230r/min, stirring for 45min, then adding lauryl trimethyl ammonium bromide, keeping the temperature constant, controlling the stirring speed to be 300r/min, stirring for 90min, adding ethanol after stirring to separate out the sodium alginate, and then washing with alcohol and drying to obtain cationized sodium alginate;
the mass ratio of the sodium alginate to the deionized water to the potassium hydroxide to the lauryl trimethyl ammonium bromide is 20;
b. post-treatment
Mixing cationized sodium alginate with absolute ethyl alcohol, stirring to uniformly disperse the cationized sodium alginate, adding magnesium hydroxide, polyethylene glycol and sorbitol, controlling the stirring speed to be 1300r/min, stirring for 90min, evaporating the ethanol after stirring to obtain a mixture, mixing the mixture with deionized water, filtering, adding the ethanol into the filtrate to obtain a precipitate, and washing and drying the precipitate to obtain the post-treatment sodium alginate;
the mass ratio of the cationized sodium alginate to the absolute ethyl alcohol to the magnesium hydroxide to the polyethylene glycol to the sorbitol is 50;
the mass ratio of the mixture to the deionized water is 1.
(3) Preparation of microcapsules
a. Preparation of wall Material solution
Mixing the post-treated sodium alginate with deionized water, and completely dissolving the mixture to obtain a wall material solution;
the mass ratio of the post-treatment sodium alginate to the deionized water is 20;
b. preparation of core Material solution
Mixing the surface-treated nano silver, deionized water and glyceryl tristearate, and uniformly stirring to obtain a core material dispersion liquid;
the mass ratio of the surface treatment nano silver to the deionized water to the tristearin is (40);
c. mixing and stirring
Adding the core material dispersion liquid into the wall material solution, adding lauryl alcohol, sorbitan fatty acid ester and fatty acid diethanolamide, controlling the temperature to be 70 ℃ and the stirring speed to be 900r/min, stirring for 45min, and stirring to obtain microcapsule liquid;
the mass ratio of the core material dispersion liquid to the wall material solution to the lauryl alcohol to the sorbitan fatty acid ester to the fatty acid diethanolamide is 150;
d. drying
And (3) passing the microcapsule liquid through a spray dryer, controlling the spray drying pressure to be 12MPa, controlling the air inlet temperature of spray drying to be 120 ℃, controlling the air outlet temperature of spray drying to be 90 ℃, and drying to obtain the nano-silver microcapsule.
Example 2 preparation method of nano silver microcapsule
(1) Surface treatment of nano silver
a. Blasting treatment
Controlling the sand blasting pressure of a sand blasting machine to be 0.45MPa, controlling the sand blasting distance to be 140mm, carrying out sand blasting treatment on the nano-silver by using sand grains for sand blasting, wherein the sand blasting time is 5.5min, filtering the sand grains by using a 300-mesh filter screen after the sand blasting treatment, and removing the sand grains for sand blasting to obtain the sand blasting nano-silver;
the sand particles for sand blasting are 0.1mm quartz sand;
the particle size of the nano silver is 25nm;
b. acid treatment fluid treatment
Mixing and stirring a phosphoric acid solution, a hexachlorocyclohexane hexaphosphate, a hydrochloric acid solution and deionized water, completely dissolving all the components, then adding ammonium persulfate and sodium fluoride, controlling the temperature to be 75 ℃ and the stirring speed to be 300r/min, stirring for 40min to obtain a mixed acid treatment solution, then adding sandblasting nano-silver into the mixed acid treatment solution, keeping the temperature unchanged, controlling the stirring speed to be 2800r/min, stirring for 200min, filtering, washing and drying after stirring to obtain surface treatment nano-silver;
the mass ratio of the phosphoric acid solution to the inositol hexaphosphate, the hydrochloric acid solution to the deionized water to the ammonium persulfate to the sodium fluoride is 14;
the mass concentration of the phosphoric acid solution is 80%;
the mass concentration of the hydrochloric acid solution is 32%;
the mass ratio of the mixed acid treatment solution to the sandblasted nano-silver is 6.5.
(2) Preparation of microcapsule wall material
a. Cationization
Mixing and stirring sodium alginate and deionized water to completely dissolve the sodium alginate, adding a certain amount of potassium hydroxide, controlling the temperature to be 65 ℃ and the stirring speed to be 220r/min, stirring for 60min, then adding lauryl trimethyl ammonium bromide, keeping the temperature constant, controlling the stirring speed to be 250r/min, stirring for 110min, adding ethanol after stirring to separate out the sodium alginate, and then washing with alcohol and drying to obtain cationized sodium alginate;
the mass ratio of the sodium alginate to the deionized water to the potassium hydroxide to the lauryl trimethyl ammonium bromide is 18.5;
b. post-treatment
Mixing cationized sodium alginate with absolute ethyl alcohol, stirring to uniformly disperse the cationized sodium alginate, adding magnesium hydroxide, polyethylene glycol and sorbitol, controlling the stirring speed to 1150r/min, stirring for 115min, evaporating the ethanol after stirring to obtain a mixture, mixing the mixture with deionized water, filtering, adding ethanol into the filtrate to obtain a precipitate, and washing and drying the precipitate to obtain the post-treated sodium alginate;
the mass ratio of the cationized sodium alginate to the absolute ethyl alcohol to the magnesium hydroxide to the polyethylene glycol to the sorbitol is 45;
the mass ratio of the mixture to the deionized water is 1.
(3) Preparation of microcapsules
a. Preparation of wall Material solution
Mixing the post-treated sodium alginate with deionized water, and completely dissolving the mixture to obtain a wall material solution;
the mass ratio of the post-treatment sodium alginate to the deionized water is 20;
b. preparation of core Material solution
Mixing the surface-treated nano silver, deionized water and tristearin, and uniformly stirring to obtain a core material dispersion liquid;
the mass ratio of the surface treatment nano silver to the deionized water to the tristearin is 30.5;
c. mixing and stirring
Adding the core material dispersion liquid into the wall material solution, adding lauryl alcohol, sorbitan fatty acid ester and fatty acid diethanolamide, controlling the temperature to be 65 ℃ and the stirring speed to be 1100r/min, stirring for 40min, and stirring to obtain microcapsule liquid;
the mass ratio of the core material dispersion liquid to the wall material solution to the lauryl alcohol to the sorbitan fatty acid ester to the fatty acid diethanolamide is (140);
d. drying the mixture
And (3) passing the microcapsule liquid through a spray dryer, controlling the spray drying pressure to be 11.5MPa, controlling the air inlet temperature of spray drying to be 115 ℃, controlling the air outlet temperature of spray drying to be 85 ℃, and drying to obtain the nano-silver microcapsule.
Example 3A method for preparing a Nanosilver microcapsule
(1) Surface treatment of nano silver
a. Blasting treatment
Controlling the sand blasting pressure of a sand blasting machine to be 0.55MPa and the sand blasting distance to be 160mm, carrying out sand blasting treatment on the nano-silver by using sand particles for sand blasting, wherein the sand blasting time is 4.5min, filtering the sand particles for sand blasting by using a 300-mesh filter screen after the sand blasting treatment, and removing the sand particles for sand blasting to obtain the sand blasting nano-silver;
the sand particles for sand blasting are 0.1mm quartz sand;
the particle size of the nano silver is 35nm;
b. acid treatment fluid treatment
Mixing and stirring a phosphoric acid solution, a cyclohexanehexol hexaphosphate, a hydrochloric acid solution and deionized water, completely dissolving all the components, then adding ammonium persulfate and sodium fluoride, controlling the temperature to be 85 ℃ and the stirring speed to be 400r/min, stirring for 20min to obtain a mixed acid treatment solution, then adding sandblasted nano-silver into the mixed acid treatment solution, keeping the temperature unchanged, controlling the stirring speed to be 3500r/min, stirring for 150min, filtering, washing and drying after stirring to obtain surface-treated nano-silver;
the mass ratio of the phosphoric acid solution to the inositol hexaphosphate, the hydrochloric acid solution to the deionized water to the ammonium persulfate to the sodium fluoride is 16;
the mass concentration of the phosphoric acid solution is 87%;
the mass concentration of the hydrochloric acid solution is 36%;
the mass ratio of the mixed acid treatment solution to the sandblasted nano-silver is 7.5.
(2) Preparation of microcapsule wall material
a. Cationization
Mixing and stirring sodium alginate and deionized water to completely dissolve the sodium alginate, adding a certain amount of potassium hydroxide, controlling the temperature to be 75 ℃ and the stirring speed to be 250r/min, stirring for 40min, then adding lauryl trimethyl ammonium bromide, keeping the temperature constant, controlling the stirring speed to be 350r/min, stirring for 85min, adding ethanol after stirring to separate out the sodium alginate, and then washing with alcohol and drying to obtain cationized sodium alginate;
the mass ratio of the sodium alginate to the deionized water to the potassium hydroxide to the lauryl trimethyl ammonium bromide is 22;
b. post-treatment
Mixing cationized sodium alginate with absolute ethyl alcohol, stirring to uniformly disperse the cationized sodium alginate, adding magnesium hydroxide, polyethylene glycol and sorbitol, controlling the stirring speed to 1450r/min, stirring for 85min, evaporating the ethanol after stirring to obtain a mixture, mixing the mixture with deionized water, filtering, adding the ethanol into the filtrate to obtain a precipitate, and washing and drying the precipitate to obtain the post-treatment sodium alginate;
the mass ratio of the cationized sodium alginate to the absolute ethyl alcohol to the magnesium hydroxide to the polyethylene glycol to the sorbitol is 55;
the mass ratio of the mixture to the deionized water is 1.
(3) Preparation of microcapsules
a. Preparation of wall Material solution
Mixing the post-treated sodium alginate with deionized water, and completely dissolving the mixture to obtain a wall material solution;
the mass ratio of the post-treatment sodium alginate to the deionized water is 20;
b. preparation of core Material solution
Mixing the surface-treated nano silver, deionized water and tristearin, and uniformly stirring to obtain a core material dispersion liquid;
the mass ratio of the surface treatment nano silver to the deionized water to the tristearin is 50;
c. mixing and stirring
Adding the core material dispersion liquid into the wall material solution, adding lauryl alcohol, sorbitan fatty acid ester and fatty acid diethanolamide, controlling the temperature to be 75 ℃ and the stirring speed to be 850r/min, stirring for 50min, and stirring to obtain a microcapsule liquid;
the mass ratio of the core material dispersion liquid to the wall material solution to the lauryl alcohol to the sorbitan fatty acid ester to the fatty acid diethanolamide is 160.5;
d. drying
And (3) passing the microcapsule liquid through a spray dryer, controlling the spray drying pressure to be 12.5MPa, controlling the air inlet temperature of spray drying to be 125 ℃, controlling the air outlet temperature of spray drying to be 95 ℃, and drying to obtain the nano-silver microcapsule.
Comparative example 1
On the basis of the example 1, in the step of nano-silver surface treatment, the step of acid treatment liquid treatment is omitted, in the step of preparing the core material solution for preparing the microcapsule, the nano-silver is subjected to sand blasting treatment instead of surface treatment, and the rest steps are the same, so that the nano-silver microcapsule is prepared.
Comparative example 2
On the basis of the embodiment 1, in the step of preparing the microcapsule wall material, the post-treatment step is omitted, in the step of preparing the wall material solution of the microcapsule, cationized sodium alginate is used for replacing the post-treatment sodium alginate, and the other steps are the same, so that the nano-silver microcapsule is prepared.
Example 4 application of nano silver microcapsule prepared in example 1 in protective cloth cover
Mixing the nano-silver microcapsules with absolute ethyl alcohol, acrylic acid and polyethylene glycol to obtain padding liquid, padding the protective cloth cover material, wherein the padder speed is 30m/min, the padder pressure is 1.5kg, 150kg of protective cloth cover material is treated by every 100kg of padding liquid, and drying the protective cloth cover material at 80 ℃ after padding to obtain the antibacterial protective cloth cover material;
the padding liquid comprises the following components in parts by mass: 7 parts of nano-silver microcapsules, 100 parts of absolute ethyl alcohol, 5 parts of acrylic acid and 3 parts of polyethylene glycol;
the protective cloth cover is made of SMS non-woven fabric.
Example 5 durability test for bacteriostatic ability
Mixing the nano-silver microcapsules prepared in the examples 1-3 and the comparative examples 1-2 with absolute ethyl alcohol, acrylic acid and polyethylene glycol to obtain padding liquid, padding the SMS non-woven fabric material at a padder speed of 30m/min and a padder pressure of 1.5kg, treating 150kg of the SMS non-woven fabric material with each 100kg of the padding liquid, drying the SMS non-woven fabric material at 80 ℃ after padding to obtain a protective fabric cover material, and testing the antibacterial performance by using the method in FZ/T73023-2006, wherein the results are shown in Table 1;
the padding liquid comprises the following components in parts by mass: 7 parts of nano-silver microcapsules, 100 parts of absolute ethyl alcohol, 5 parts of acrylic acid and 3 parts of polyethylene glycol.
Example 6 test of air permeability of nano-silver microcapsules to SMS nonwoven Fabric
Mixing the nano-silver microcapsules prepared in the examples 1-3 and the comparative examples 1-2 with absolute ethyl alcohol, acrylic acid and polyethylene glycol to obtain a padding liquid, padding the SMS non-woven fabric material, wherein the padder speed is 30m/min, the padder pressure is 1.5kg, 150kg of the SMS non-woven fabric material is treated by every 100kg of the padding liquid, drying the SMS non-woven fabric material at 80 ℃ after padding to obtain a protective fabric cover material, and testing the air permeability by using the method in GB/T24218.15-2018, wherein the results are shown in Table 2;
the padding liquid comprises the following components in parts by mass: 7 parts of nano-silver microcapsules, 100 parts of absolute ethyl alcohol, 5 parts of acrylic acid and 3 parts of polyethylene glycol.
Example 7 nanosilver microcapsules test of Water repellency to SMS nonwoven Fabric
Mixing the nano-silver microcapsules prepared in examples 1-3 and comparative examples 1-2 with absolute ethyl alcohol, acrylic acid and polyethylene glycol to obtain a padding liquid, padding an SMS (short message service) non-woven fabric material, wherein the padder speed is 30m/min, the padder pressure is 1.5kg, 150kg of the SMS non-woven fabric material is treated by every 100kg of the padding liquid, drying the SMS non-woven fabric material at 80 ℃ after padding to obtain a protective fabric cover material, testing the anti-seepage performance by using the method in GB/T24218.16-2017, and testing the liquid penetration time by using the method in GB/T24218.13-2010, wherein the results are shown in Table 3;
the padding liquid comprises the following components in parts by mass: 7 parts of nano-silver microcapsules, 100 parts of absolute ethyl alcohol, 5 parts of acrylic acid and 3 parts of polyethylene glycol.
Claims (5)
1. The preparation method of the nano-silver microcapsule is characterized by comprising the steps of nano-silver surface treatment, microcapsule wall material preparation and microcapsule preparation;
the step of nano silver surface treatment comprises sand blasting treatment and acid treatment liquid treatment;
the sand blasting method comprises the steps of controlling the sand blasting pressure to be 0.45-0.55MPa and the sand blasting distance to be 140-160mm, carrying out sand blasting treatment on the nano-silver by using sand grains for sand blasting, wherein the sand blasting time is 4.5-5.5min, filtering the nano-silver by a filter screen after the sand blasting treatment, and removing the sand grains for sand blasting to obtain the nano-silver subjected to sand blasting treatment;
the grain size of the nano silver is 25-35nm;
mixing and stirring a phosphoric acid solution, a cyclohexanehexol hexaphosphate, a hydrochloric acid solution and deionized water, completely dissolving all the components, then adding ammonium persulfate and sodium fluoride, controlling the temperature to be 75-85 ℃, controlling the stirring speed to be 300-400r/min, stirring for 20-40min to obtain a mixed acid treatment solution, then adding the sandblasted nano-silver into the mixed acid treatment solution, keeping the temperature unchanged, controlling the stirring speed to be 2800-3500r/min, stirring for 150-200min, filtering, washing and drying after stirring to obtain the surface-treated nano-silver;
the mass ratio of the phosphoric acid solution, the cyclohexanehexol hexaphosphate, the hydrochloric acid solution, the deionized water, the ammonium persulfate and the sodium fluoride is (14-16);
the mass ratio of the mixed acid treatment solution to the sandblasted nano-silver is 6.5-7.5;
the step of preparing the microcapsule wall material comprises cationization and post-treatment;
mixing and stirring sodium alginate and deionized water to completely dissolve the sodium alginate, adding a certain amount of potassium hydroxide, controlling the temperature to be 65-75 ℃, controlling the stirring speed to be 220-250r/min, stirring for 40-60min, then adding lauryl trimethyl ammonium bromide, keeping the temperature unchanged, controlling the stirring speed to be 250-350r/min, stirring for 85-110min, adding ethanol after stirring to separate out the sodium alginate, and then washing with alcohol and drying to obtain the cationized sodium alginate;
the mass ratio of the sodium alginate to the deionized water to the potassium hydroxide to the lauryl trimethyl ammonium bromide is (18-22);
mixing cationized sodium alginate with absolute ethyl alcohol, stirring to uniformly disperse the cationized sodium alginate, adding magnesium hydroxide, polyethylene glycol and sorbitol, controlling the stirring speed to be 1150-1450r/min, stirring for 85-115min, evaporating the ethanol after stirring to obtain a mixture, mixing the mixture with deionized water, filtering, adding ethanol into the filtrate to obtain a precipitate, and washing and drying the precipitate to obtain the post-treated sodium alginate;
the mass ratio of the cationized sodium alginate to the absolute ethyl alcohol to the magnesium hydroxide to the polyethylene glycol to the sorbitol is 45-55;
the mass ratio of the mixture to the deionized water is 1.5-3.5;
the step of preparing the microcapsule comprises preparing a wall material solution, preparing a core material solution, mixing, stirring and drying;
the method for preparing the wall material solution comprises the steps of mixing the post-treatment sodium alginate with deionized water, and completely dissolving the mixture to obtain the wall material solution;
the mass ratio of the post-treatment sodium alginate to the deionized water is 20-110;
the method for preparing the core material solution comprises the steps of mixing the surface-treated nano silver, deionized water and tristearin, and uniformly stirring to obtain a core material dispersion liquid;
the mass ratio of the surface treatment nano silver to the deionized water to the tristearin is 30-50;
adding the core material dispersion liquid into the wall material solution, adding lauryl alcohol, sorbitan fatty acid ester and fatty acid diethanolamide, controlling the stirring speed to be 850-1100r/min, stirring for 40-50min, and stirring to obtain a microcapsule liquid;
the mass ratio of the core material dispersion liquid to the wall material solution to the lauryl alcohol to the sorbitan fatty acid ester to the fatty acid diethanolamide is 140-160;
the drying method comprises the step of carrying out spray drying on the microcapsule liquid to obtain the nano-silver microcapsule.
2. The method for preparing nano-silver microcapsules according to claim 1, wherein the method comprises the following steps:
in the sand blasting step, the filter screen is a 300-mesh filter screen, and the sand grains for sand blasting are 0.1mm quartz sand.
3. The method for preparing nano-silver microcapsules according to claim 1, wherein the method comprises the following steps:
in the step of treating the acid treatment solution, the mass concentration of the phosphoric acid solution is 80-87%, and the mass concentration of the hydrochloric acid solution is 32-36%.
4. The method for preparing nano-silver microcapsules according to claim 1, wherein the method comprises the following steps:
in the step of preparing the microcapsule, the drying pressure of spray drying is 11.5-12.5MPa, the air inlet temperature of spray drying is 115-125 ℃, and the air outlet temperature of spray drying is 85-95 ℃.
5. The use of the nanosilver microcapsule of claim 1 in a protective cloth cover, wherein:
the application method comprises the steps of mixing the nano-silver microcapsules with absolute ethyl alcohol, acrylic acid and polyethylene glycol to obtain padding liquid, padding the protective cloth cover material, wherein the padder speed is 30m/min, the padder pressure is 1.5kg, 150kg of protective cloth cover material is processed by every 100kg of padding liquid, and drying the protective cloth cover material at 80 ℃ after padding to obtain the antibacterial protective cloth cover material;
the padding liquid comprises the following components in parts by mass: 7 parts of nano-silver microcapsules, 100 parts of absolute ethyl alcohol, 5 parts of acrylic acid and 3 parts of polyethylene glycol;
the protective cloth cover is made of SMS non-woven fabric.
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