CN115430371A - Meyer sedge essential oil microcapsule, preparation method and application - Google Patents
Meyer sedge essential oil microcapsule, preparation method and application Download PDFInfo
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- CN115430371A CN115430371A CN202210764624.5A CN202210764624A CN115430371A CN 115430371 A CN115430371 A CN 115430371A CN 202210764624 A CN202210764624 A CN 202210764624A CN 115430371 A CN115430371 A CN 115430371A
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- essential oil
- sedge
- oil microcapsule
- fabric
- emulsifier
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 124
- 239000003094 microcapsule Substances 0.000 title claims abstract description 85
- 241001290610 Abildgaardia Species 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000004744 fabric Substances 0.000 claims abstract description 61
- 239000000463 material Substances 0.000 claims abstract description 54
- 241000045459 Carex meyeriana Species 0.000 claims abstract description 36
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 23
- 239000011162 core material Substances 0.000 claims abstract description 23
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229920002396 Polyurea Polymers 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 19
- 239000004814 polyurethane Substances 0.000 claims description 18
- 239000000839 emulsion Substances 0.000 claims description 15
- 229920002635 polyurethane Polymers 0.000 claims description 14
- 230000001804 emulsifying effect Effects 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims description 6
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 230000002688 persistence Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 34
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 30
- 239000007788 liquid Substances 0.000 description 20
- 239000007864 aqueous solution Substances 0.000 description 17
- 229920000742 Cotton Polymers 0.000 description 16
- 239000004753 textile Substances 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 15
- 239000000853 adhesive Substances 0.000 description 12
- 230000001070 adhesive effect Effects 0.000 description 12
- USDJGQLNFPZEON-UHFFFAOYSA-N [[4,6-bis(hydroxymethylamino)-1,3,5-triazin-2-yl]amino]methanol Chemical compound OCNC1=NC(NCO)=NC(NCO)=N1 USDJGQLNFPZEON-UHFFFAOYSA-N 0.000 description 11
- 238000004132 cross linking Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 239000004721 Polyphenylene oxide Substances 0.000 description 9
- 229920000570 polyether Polymers 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 229940052016 turmeric extract Drugs 0.000 description 7
- 235000020240 turmeric extract Nutrition 0.000 description 7
- 239000008513 turmeric extract Substances 0.000 description 7
- 230000000844 anti-bacterial effect Effects 0.000 description 6
- 241000722731 Carex Species 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 244000025254 Cannabis sativa Species 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000222122 Candida albicans Species 0.000 description 1
- FZPYMZUVXJUAQA-ZDUSSCGKSA-N Turmerone Chemical compound CC(C)=CC(=O)C[C@H](C)C1=CCC(C)=CC1 FZPYMZUVXJUAQA-ZDUSSCGKSA-N 0.000 description 1
- FZPYMZUVXJUAQA-UHFFFAOYSA-N Turmerone Natural products CC(C)=CC(=O)CC(C)C1=CCC(C)=CC1 FZPYMZUVXJUAQA-UHFFFAOYSA-N 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- XOCANRBEOZQNAQ-KBPBESRZSA-N alpha-turmerone Natural products O=C(/C=C(\C)/C)C[C@H](C)[C@H]1C=CC(C)=CC1 XOCANRBEOZQNAQ-KBPBESRZSA-N 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 235000012754 curcumin Nutrition 0.000 description 1
- 229940109262 curcumin Drugs 0.000 description 1
- 239000004148 curcumin Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/005—Compositions containing perfumes; Compositions containing deodorants
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
- D06M15/233—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated aromatic, e.g. styrene
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/423—Amino-aldehyde resins
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
- D06M15/568—Reaction products of isocyanates with polyethers
-
- 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
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of B01J13/00, and particularly relates to a carex meyeriana essential oil microcapsule, a preparation method and application thereof. A carex meyeriana essential oil microcapsule is prepared from the following raw materials: wall material and core material; the wall material is a polyurea type coating base material and/or a melamine type coating base material; the core material comprises an emulsifier and essential oil; the essential oil is Meyer sedge essential oil. The Wula sedge essential oil microcapsule prepared by the invention has excellent persistence on fabrics and better water washing resistance. According to the invention, the binder is added and mixed with the carex meyeriana essential oil microcapsule to be used as a finishing agent, so that the durability and hydrolysis resistance of the carex meyeriana essential oil microcapsule in the fabric are improved.
Description
Technical Field
The invention relates to the technical field of B01J13/00, and particularly relates to a carex meyeriana essential oil microcapsule, a preparation method and application.
Background
Chinese patent No. CN201910110751.1 discloses a preparation method of a carex volatile oil microcapsule, which adopts carex volatile oil microcapsule for inhibiting staphylococcus aureus and escherichia coli, but does not disclose the application scene of the carex volatile oil microcapsule, and does not disclose and solve whether the carex volatile oil microcapsule has a lasting antibacterial property, therefore, providing a carex volatile oil microcapsule which can have excellent stability and maintain durability, has better water washing resistance, and has a long-term effective antibacterial property is a main technical problem to be solved at present.
Disclosure of Invention
In order to solve the above problems, the present invention provides a wula sedge essential oil microcapsule, which is prepared from the following raw materials: wall material and core material;
the wall material is a polyurea type coating base material and/or a melamine type coating base material;
the core material comprises an emulsifier and essential oil;
the essential oil is Meyer sedge essential oil.
Preferably, the weight ratio of the wall material to the core material is 1: (2-3).
The preparation method of the melamine-type coated substrate comprises the following steps:
and (3) regulating the pH value of melamine and formaldehyde in the aqueous solution to 8-9 by using a NaOH aqueous solution with the mass concentration of 20%, stirring the aqueous solution, heating to 40-50 ℃, and preserving heat for 1-2 hours to obtain the melamine-type coated base material.
Preferably, the molar ratio of melamine to formaldehyde is 1: (1-6).
The inventor finds in experiments that by setting the molar ratio of 1: the melamine and the formaldehyde in the (1-6) are stirred in the aqueous solution to be heated to 40-50 ℃, and heat preservation is carried out for 1-2h, the melamine and the formaldehyde can be fully contacted in the aqueous solution to form a melamine-formaldehyde prepolymer, the temperature for heating and heat preservation is lower, and compared with the conventional processing method of repeatedly adding materials and heating at a higher temperature, the method has the advantages of simple preparation method and operation.
Preferably, the weight ratio of the emulsifier to the essential oil is 1: (0.55-0.75).
Preferably, the raw material for preparing the emulsifier comprises styrene-maleic anhydride copolymer.
Preferably, the preparation method of the emulsifier comprises the following steps:
according to parts by weight, 12-22 parts of styrene-maleic anhydride copolymer, 1.5-2.5 parts of sodium hydroxide and 72-82 parts of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid to obtain the emulsifier.
The second aspect of the invention provides a preparation method of a carex meyeriana essential oil microcapsule, which comprises the following steps:
s1, adding essential oil and an emulsifier into a stirrer, and stirring and emulsifying to obtain an emulsion;
s2, slowly adding the wall material into the emulsion, adding water, mixing and stirring to obtain the wula sedge essential oil microcapsule.
Preferably, naOH water solution with the mass concentration of 20% is used for adjusting the pH value of the solution in S2 to 7-8.
Preferably, the rotation speed of stirring in the S1 is 4000-6000r/min, and the emulsifying time is 10-25min.
Preferably, the speed of adding the wall material into the emulsion in the S2 is 10-20g/min.
Preferably, the S2 is added with trimethylolmelamine, and the weight ratio of the trimethylolmelamine to the wall material, the core material and the water is 0.5:1: (2-3): (0.8-1.2).
The inventor finds that the trimethylolmelamine is added into a material system to be matched with the melamine-formaldehyde prepolymer, the emulsifier, the essential oil and the water, and particularly, the weight ratio of the hydroxymethylmelamine to the wall material, the core material and the water is 0.5:1: (2-3): (0.8-1.2), the pH value of the solution is adjusted to 7-8, the amount of the polymer with the three-dimensional network structure formed by the methylol melamine and the melamine-formaldehyde prepolymer in the mixed solution through further dehydration condensation is increased, and the more the amount of the polymer with the three-dimensional network structure is, so that the more the number of networks which can be wrapped by the emulsifier and the carex meyeriana essential oil is, the more the wrapping rate of the emulsifier and the carex meyeriana essential oil can be increased after emulsification, and the stability of the carex meyeriana essential oil microcapsule can be improved.
The third aspect of the invention provides application of a carex meyeriana essential oil microcapsule in fabric treatment.
Preferably, the mulleria sedge essential oil microcapsule is mixed with a polyurethane type adhesive and then is applied to the fabric as a finishing agent.
Preferably, the application of the wula sedge essential oil microcapsule in fabric treatment comprises the following steps:
(1) Mixing the Meyer sedge essential oil microcapsules with a binder to serve as a finishing agent;
(2) Adding a finishing agent into a liquid tank of a setting machine, and enabling the fabric to pass through the liquid tank and a roller;
(3) And heating and drying the fabric.
Preferably, the polyurethane-type adhesive has a viscosity of 30 to 70mpa.s.
The polyurethane type adhesive is self-crosslinking polyether polyurethane.
The invention is not limited to the vendors of self-crosslinking polyether polyurethanes, and examples include: the purchase manufacturer is Tuonan chemical, the model is
NANO PU, viscosity 50mPa.s.
Preferably, the weight ratio of the Meyer sedge essential oil microcapsules to the binder is 1 (0.5-1).
Preferably, the mass concentration of the finishing agent in the finishing liquid is 3-6%.
Preferably, the weight ratio of the finishing liquid to the fabric is (45-55): 1.
preferably, the fabric is a cotton fiber textile fabric.
Furthermore, the fabric is a cotton fiber textile fabric printed and dyed by a turmeric extract.
Preferably, the temperature for heating and drying the fabric is 145-165 ℃, and the fabric is dried for 40-60s.
The inventor uses self-crosslinking polyether polyurethane with the viscosity of 30-70mPa.s as a binder to be matched with the carex meyeriana essential oil microcapsule, wherein the weight ratio of the carex meyeriana essential oil microcapsule to the binder is 1: (0.5-1), the water washing resistance and the retention durability of the carex meyeriana essential oil microcapsules in the cotton fiber textile fabric can be improved, particularly the water washing resistance and the retention durability of the carex meyeriana essential oil microcapsules in the cotton fiber textile fabric printed by natural plant dyes are improved, particularly the cotton fiber textile fabric printed by a turmeric extract is improved, the possible reasons are that the self-crosslinking polyether polyurethane can generate certain interaction with curcumin and turmerone contained in the turmeric extract, the self-crosslinking polyether polyurethane forms a certain film layer on the surface of the carex meyeriana essential oil microcapsules, the self-crosslinking polyether polyurethane can permeate into the cotton fiber textile fabric printed by the turmeric extract and generate a mutual entangled structure with cotton fibers, the firmness of the microcapsules and the natural plant dyes in the cotton fiber textile fabric is improved, the carex meyeriana essential oil can be slowly released during application, the lasting and long-term action of the carex meyeriana essential oil on the surface of the fabric is improved, and the problem that the antibacterial and acaricidal properties cannot be maintained for a long time is solved.
Advantageous effects
Compared with the conventional processing method of repeatedly feeding and heating at a higher temperature, the melamine type coated base material obtained by the invention has the advantages of simple preparation method and operation.
According to the invention, the trihydroxymethyl melamine is added, so that the coating rate of the emulsifier and the carex meyeriana essential oil is improved, and the stability of the carex meyeriana essential oil microcapsule is also improved.
According to the invention, the firmness of the prepared Wula grass essential oil microcapsule in the cotton fiber textile fabric is improved by adopting the adhesive with the viscosity of 30-70mPa.s and limiting the adhesive to be a polyurethane adhesive, the Wula grass essential oil encapsulated in the Wula grass essential oil microcapsule can be slowly released in application, the Wula grass essential oil can be continuously and permanently acted in the fabric, and the problem that the antibacterial property and the mite removing property can not be maintained for a long time is solved.
The mulleria sedge essential oil microcapsule prepared by the invention has excellent retention durability on fabrics and better water washing resistance. According to the invention, the binder is added and mixed with the carex meyeriana essential oil microcapsules to serve as a finishing agent, so that the durability and hydrolysis resistance of the carex meyeriana essential oil microcapsules in the fabric are improved.
Drawings
Fig. 1 is a photograph of the wula sedge essential oil microcapsule prepared in example 1 taken by a microscope.
Detailed Description
Example 1
A carex meyeriana essential oil microcapsule is prepared from the following raw materials: wall material and core material;
the wall material is a melamine type coating base material;
the core material comprises an emulsifier and essential oil;
the essential oil is Meyer sedge essential oil.
The purchase of the Meyer sedge essential oil is Shanghai Bingyou New Material science and technology Limited.
The weight ratio of the wall material to the core material is 1:2.5.
the preparation method of the melamine-type coated substrate comprises the following steps:
and (3) regulating the pH value of melamine and formaldehyde in the aqueous solution to 8 by using a NaOH aqueous solution with the mass concentration of 20%, stirring the aqueous solution, heating to 48 ℃, and preserving heat for 2 hours to obtain the melamine-type coated base material.
The molar ratio of the melamine to the formaldehyde is 1:4.
the weight ratio of the melamine to the water is 1:10.
the weight ratio of the emulsifier to the Meyer sedge essential oil is 1:0.7.
the preparation method of the emulsifier comprises the following steps:
according to the weight portion, 18 portions of styrene-maleic anhydride copolymer, 2 portions of sodium hydroxide and 75 portions of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, and the emulsifier is obtained.
The second aspect of this embodiment provides a preparation method of a wula sedge essential oil microcapsule, including the following steps:
s1, adding essential oil and an emulsifier into a stirrer, and stirring and emulsifying to obtain an emulsion;
s2, slowly adding the wall material into the emulsion, adding water, mixing and stirring to obtain the wula sedge essential oil microcapsule.
And in the S2, a NaOH aqueous solution with the mass concentration of 20% is used for regulating the pH value of the solution to be 8.
The rotation speed of stirring in the S1 is 5500r/min, and the emulsifying time is 20min.
And the speed of adding the emulsion into the wall material in the S2 is 15g/min.
And (2) adding trimethylolmelamine into the S2, wherein the weight ratio of the trimethylolmelamine to the wall material, the core material and the water is 0.5:1:2.5:1.
in a third aspect of the present embodiment, an application of the wula sedge essential oil microcapsule in fabric treatment is provided.
The application of the Wula sedge essential oil microcapsule in fabric treatment comprises the following steps:
(1) Mixing the Meyer sedge essential oil microcapsules with a binder to serve as a finishing agent;
(2) Adding a finishing agent into a liquid tank of a setting machine, and passing the fabric through the liquid tank and a roller;
(3) And heating and drying the fabric.
The adhesive is self-crosslinking polyether polyurethane, the purchase manufacturer is Tunna chemical, and the model is
NANO PU。
The weight ratio of the Meyer sedge essential oil microcapsules to the adhesive is 1.
The mass concentration of the finishing agent in the finishing liquid is 4.5%.
The weight ratio of the finishing liquid to the fabric is 50:1.
the fabric is a cotton fiber textile fabric.
The fabric is a cotton fiber textile fabric printed and dyed by a turmeric extract.
The temperature for heating and drying the fabric is 160 ℃, and the fabric is dried for 50s.
The carex meyeriana essential oil microcapsules prepared in example 1 were placed at 60 ℃ for 72 hours, and after being taken out, the existence state of the carex meyeriana essential oil microcapsules was observed to be turbidity-free and delamination-free.
Example 2
A carex meyeriana essential oil microcapsule is prepared from the following raw materials: wall material and core material;
the wall material is a melamine type coating base material;
the core material comprises an emulsifier and essential oil;
the essential oil is Meyer sedge essential oil.
The weight ratio of the wall material to the core material is 1:3.
the purchase of the Meyer sedge essential oil is Shanghai Bingyou New Material science and technology Limited.
The preparation method of the melamine-type coated substrate comprises the following steps:
and (3) regulating the pH value of melamine and formaldehyde in the aqueous solution to 8 by using a NaOH aqueous solution with the mass concentration of 20%, stirring the aqueous solution, heating to 48 ℃, and preserving heat for 2 hours to obtain the melamine-type coated base material.
The mol ratio of the melamine to the formaldehyde is 1:6.
the weight ratio of the melamine to the water is 1:10.
the weight ratio of the emulsifier to the carex meyeriana essential oil is 1:0.75.
the preparation method of the emulsifier comprises the following steps:
according to the weight portion, 22 portions of styrene-maleic anhydride copolymer, 2.5 portions of sodium hydroxide and 82 portions of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, thus obtaining the emulsifier.
The second aspect of this embodiment provides a preparation method of a wula sedge essential oil microcapsule, including the following steps:
s1, adding essential oil and an emulsifier into a stirrer, and stirring and emulsifying to obtain an emulsion;
s2, slowly adding the wall material into the emulsion, adding water, mixing and stirring to obtain the wula sedge essential oil microcapsule.
And in the S2, the pH value of the solution is adjusted to 8 by using a NaOH aqueous solution with the mass concentration of 20%.
The rotation speed of stirring in the S1 is 6000r/min, and the emulsifying time is 10min.
The speed of adding the emulsion into the wall material in the S2 is 20g/min.
And (2) adding trimethylolmelamine into the S2, wherein the weight ratio of the trimethylolmelamine to the wall material, the core material and the water is 0.5:1:3:1.
in a third aspect of the embodiment, an application of the wula sedge essential oil microcapsule in fabric treatment is provided.
The application of the carex meyeriana essential oil microcapsule in fabric treatment comprises the following steps:
(1) Mixing the Meyer sedge essential oil microcapsules with a binder to serve as a finishing agent;
(2) Adding a finishing agent into a liquid tank of a setting machine, and passing the fabric through the liquid tank and a roller;
(3) And heating and drying the fabric.
The adhesive is self-crosslinking polyether polyurethane, the purchase manufacturer is Tuonan chemistry, and the model is
NANO PU。
The weight ratio of the wula sedge essential oil microcapsules to the binder is 1.
The mass concentration of the finishing agent in the finishing liquid is 4%.
The weight ratio of the finishing liquid to the fabric is 50:1.
the fabric is a cotton fiber textile fabric.
The fabric is a cotton fiber textile fabric printed and dyed by a turmeric extract.
The temperature for heating and drying the fabric is 160 ℃, and the fabric is dried for 50s.
The carex meyeriana essential oil microcapsule prepared in example 2 is placed at 60 ℃ for 72 hours, and after being taken out, the existence state of the carex meyeriana essential oil microcapsule is observed to be turbidity-free and delamination-free.
Example 3
A carex meyeriana essential oil microcapsule is prepared from the following raw materials: wall material and core material;
the wall material is a melamine type coating base material;
the core material comprises an emulsifier and essential oil;
the essential oil is Meyer sedge essential oil.
The weight ratio of the wall material to the core material is 1:2.
the purchase of the Meyer sedge essential oil is Shanghai Bingyou New Material science and technology Limited.
The preparation method of the melamine-type coated substrate comprises the following steps:
and (3) regulating the pH value of melamine and formaldehyde in the aqueous solution to 8 by using a NaOH aqueous solution with the mass concentration of 20%, stirring the aqueous solution, heating to 48 ℃, and preserving heat for 2 hours to obtain the melamine-type coated base material.
The molar ratio of the melamine to the formaldehyde is 1:4.
the weight ratio of the melamine to the water is 1:10.
the weight ratio of the emulsifier to the Meyer sedge essential oil is 1:0.55.
the preparation method of the emulsifier comprises the following steps:
according to the weight portion, 12 portions of styrene-maleic anhydride copolymer, 1.5 portions of sodium hydroxide and 72 portions of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, thus obtaining the emulsifier.
The second aspect of the present invention provides a preparation method of a wula sedge essential oil microcapsule, including the following steps:
s1, adding essential oil and an emulsifier into a stirrer, and stirring and emulsifying to obtain an emulsion;
s2, slowly adding the wall material into the emulsion, adding water, mixing and stirring to obtain the wula sedge essential oil microcapsule.
And in the S2, the pH value of the solution is adjusted to 7-8 by using a NaOH aqueous solution with the mass concentration of 20%.
The rotation speed of stirring in the S1 is 6000r/min, and the emulsifying time is 10min.
The speed of adding the emulsion into the wall material in the S2 is 20g/min.
And (2) adding trimethylolmelamine into the S2, wherein the weight ratio of the trimethylolmelamine to the wall material, the core material and the water is 0.5:1:2:1.
in a third aspect of the embodiment, an application of the wula sedge essential oil microcapsule in fabric treatment is provided.
The application of the carex meyeriana essential oil microcapsule in fabric treatment comprises the following steps:
(1) Mixing the Meyer sedge essential oil microcapsules with a binder to serve as a finishing agent;
(2) Adding a finishing agent into a liquid tank of a setting machine, and passing the fabric through the liquid tank and a roller;
(3) And heating and drying the fabric.
The adhesive is self-crosslinking polyether polyurethane, the purchase manufacturer is Tuonan chemistry, and the model is
NANO PU。
The weight ratio of the Meyer sedge essential oil microcapsules to the adhesive is 1.
The mass concentration of the finishing agent in the finishing liquid is 4%.
The weight ratio of the finishing liquid to the fabric is 50:1.
the fabric is a cotton fiber textile fabric.
The fabric is a cotton fiber textile fabric printed and dyed by a turmeric extract.
The temperature for heating and drying the fabric is 160 ℃, and the fabric is dried for 50s.
The wula sedge essential oil microcapsules prepared in example 3 were left at 60 ℃ for 72 hours and after being taken out, the existence state of the wula sedge essential oil microcapsules was observed to be turbidity-free and delamination-free.
Example 4
Embodiment 4 provides a technical scheme of a wula sedge essential oil microcapsule, a preparation method and an application thereof, and is different from embodiment 1 in that trimethylol melamine is not adopted in the preparation method of the wula sedge essential oil microcapsule.
The carex meyeriana essential oil microcapsule prepared in example 4 is placed at 60 ℃ for 72 hours, and after the carex meyeriana essential oil microcapsule is taken out, the existence state of the carex meyeriana essential oil microcapsule is observed, and the phenomena of turbidity and layering occur.
Example 5
Embodiment 5 provides a technical scheme of a carex meyeriana essential oil microcapsule, a preparation method and an application, and the difference from embodiment 1 is that the adhesive is self-crosslinking acrylic latex, the year of the self-crosslinking acrylic latex is 60mpa.s, and a purchasing manufacturer is glaide new material science and technology (zhongshan) limited company.
The wula sedge essential oil microcapsules prepared in example 5 were left at 60 ℃ for 72 hours and after being taken out, the existence state of the wula sedge essential oil microcapsules was observed to be turbidity-free and delamination-free.
Performance testing
1. Coating integrity test
The turfgrass essential oil microcapsule prepared in example 1 is photographed by a microscope, and the photographed image is shown in fig. 1.
As can be seen from fig. 1, the core material of the prepared wula sedge essential oil microcapsule can be completely wrapped by the wall material, and the emulsifier and the wula sedge essential oil have higher wrapping rate.
2. Antibacterial property test
The treated fabric obtained by applying the wula sedge essential oil microcapsules prepared in examples 1-3 and 5 to the cotton fiber textile fabric is washed for 30min once a week before and 10 times, and the test results of the test method for inhibiting the bacteriostatic rates of candida albicans, staphylococcus aureus and escherichia coli in AATCC 100-2019 textile material antibacterial finishing agent are shown in table 1.
TABLE 1
Claims (10)
1. The Meyer sedge essential oil microcapsule is characterized in that the preparation raw materials comprise: wall material and core material;
the wall material is a polyurea type coating base material and/or a melamine type coating base material;
the core material comprises an emulsifier and essential oil;
the essential oil is Meyer sedge essential oil.
2. The Meyer sedge essential oil microcapsule according to claim 1, wherein the weight ratio of the wall material to the core material is 1: (2-3).
3. The Meyer sedge essential oil microcapsule according to claim 1 or 2, wherein the weight ratio of the emulsifier to the essential oil is 1: (0.55-0.75).
4. The mullery essential oil microcapsule of claim 1, wherein the emulsifier is prepared from a raw material comprising a styrene-maleic anhydride copolymer.
5. A method for preparing the wula sedge essential oil microcapsule according to any one of claims 1 to 4, comprising the steps of:
s1, adding essential oil and an emulsifier into a stirrer, and stirring and emulsifying to obtain an emulsion;
s2, slowly adding the wall material into the emulsion, adding water, mixing and stirring to obtain the wula sedge essential oil microcapsule.
6. The preparation method of the carex meyeriana essential oil microcapsule according to claim 5, wherein the stirring speed in the S1 is 4000-6000r/min, and the emulsifying time is 10-25min.
7. The method for preparing a Meyer sedge essential oil microcapsule according to claim 5, wherein the speed of adding the emulsion into the wall material in the S2 is 10-20g/min.
8. Use of the wula sedge essential oil microcapsules of any one of claims 1 to 4 in fabric treatment.
9. The use of the wula sedge essential oil microcapsule according to claim 8, wherein the wula sedge essential oil microcapsule is mixed with a polyurethane type binder and then used as a finishing agent in a fabric.
10. Use of the wula sedge essential oil microcapsules according to claim 9, wherein the viscosity of the polyurethane type binder is 30 to 70mpa.s.
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