CN115976845B - Skin care microcapsule, preparation method and application - Google Patents
Skin care microcapsule, preparation method and application Download PDFInfo
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- CN115976845B CN115976845B CN202210761492.0A CN202210761492A CN115976845B CN 115976845 B CN115976845 B CN 115976845B CN 202210761492 A CN202210761492 A CN 202210761492A CN 115976845 B CN115976845 B CN 115976845B
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000004744 fabric Substances 0.000 claims abstract description 57
- 239000003921 oil Substances 0.000 claims abstract description 51
- 235000019198 oils Nutrition 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 38
- 239000011162 core material Substances 0.000 claims abstract description 35
- 239000000341 volatile oil Substances 0.000 claims abstract description 35
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000018936 Vitellaria paradoxa Nutrition 0.000 claims abstract description 23
- 241001135917 Vitellaria paradoxa Species 0.000 claims abstract description 23
- 229940057910 shea butter Drugs 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- 239000008169 grapeseed oil Substances 0.000 claims abstract description 22
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 21
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 34
- 238000004132 cross linking Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 24
- 229920000570 polyether Polymers 0.000 claims description 19
- 239000004814 polyurethane Substances 0.000 claims description 19
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 229920002635 polyurethane Polymers 0.000 claims description 15
- 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 13
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 3
- 230000014759 maintenance of location Effects 0.000 abstract description 4
- 239000010495 camellia oil Substances 0.000 abstract description 2
- 239000003240 coconut oil Substances 0.000 abstract description 2
- 235000019864 coconut oil Nutrition 0.000 abstract description 2
- 229940119170 jojoba wax Drugs 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 21
- 238000012360 testing method Methods 0.000 description 16
- 229920000742 Cotton Polymers 0.000 description 14
- 239000004753 textile Substances 0.000 description 13
- 238000001035 drying Methods 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 12
- 238000005406 washing Methods 0.000 description 10
- 230000001105 regulatory effect Effects 0.000 description 9
- 230000001804 emulsifying effect Effects 0.000 description 7
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 150000002500 ions Chemical group 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 229920001807 Urea-formaldehyde Polymers 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- HANVTCGOAROXMV-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine;urea Chemical compound O=C.NC(N)=O.NC1=NC(N)=NC(N)=N1 HANVTCGOAROXMV-UHFFFAOYSA-N 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention relates to the technical field of B01J13/00, in particular to a skin care microcapsule, a preparation method and application. The skin care microcapsule comprises wall materials and core materials, wherein the wall materials comprise, by weight, 5-7.5 parts of melamine, 5-6.5 parts of urea, 20-30 parts of formaldehyde aqueous solution and 20-30 parts of water, the core materials comprise emulsifying agents and essential oils, and the essential oils are selected from horse oil, grape seed oil, coconut oil, alaglycerol, shea butter, jojoba oil and camellia oil. The skin care microcapsule prepared by the method can be provided with excellent retention durability on the fabric and has better water resistance.
Description
Technical Field
The invention relates to the technical field of B01J13/00, in particular to a skin care microcapsule, a preparation method and application.
Background
The in-situ polymerization method is one of the most important methods in the synthesis process for preparing the microcapsules, can be used for preparing a plurality of high-quality microcapsules with special functions, and the Chinese patent with the patent application number of CN202010710563.5 discloses a preparation method of melamine phase-change microcapsules with low formaldehyde content.
Therefore, it is a major technical problem to be solved at present to provide a microcapsule which is excellent in retention durability, has a good water-washing resistance, and exerts a long-term effective skin care effect on the skin.
Disclosure of Invention
In order to solve the above problems, the present invention provides a skin care microcapsule, which is prepared from the following raw materials;
The wall material is prepared from the following raw materials, by weight, 5-7.5 parts of melamine, 5-6.5 parts of urea, 20-30 parts of formaldehyde aqueous solution and 20-30 parts of water;
the preparation raw materials of the core material comprise an emulsifying agent and essential oil;
The essential oil is selected from horse oil, grape seed oil, coconut oil, alaglycerol, shea butter, jojoba oil, and camellia oil.
Preferably, the essential oil is composed of a combination of horse oil, grape seed oil, shea butter.
Further, the weight ratio of the horse oil to the grape seed oil to the shea butter is 1 (0.5-2) to 1-2.
The CAS number of the melamine is 108-78-1.
The CAS number of the urea is 57-13-6.
The mass concentration of formaldehyde in the formaldehyde aqueous solution is 37%.
Preferably, the preparation method of the wall material comprises the following steps:
and regulating the pH value of the aqueous solution of melamine, urea and formaldehyde in water to 7.5-9.0, stirring, heating, preserving heat for a certain time, cooling to 30-50 ℃ after the reaction, and ending stirring to obtain the wall material.
Preferably, the temperature rise rate is 0.5-3 ℃ per minute, and the heat preservation temperature is 65-75 ℃.
The inventor finds in experiments that melamine, urea and formaldehyde aqueous solution can be fully contacted by stirring and heating up the melamine, urea and formaldehyde aqueous solution for a certain period of time, a mode of adding the melamine, urea and formaldehyde aqueous solution for multiple times is not adopted, and compared with the heating temperature required by conventional heating, the temperature for heating up and heat preservation is lower, the temperature for heating up and heat preservation is 65-75 ℃, and the melamine, urea and formaldehyde aqueous solution can be fully contacted and reacted at the temperature to obtain the wall material capable of better wrapping the core material.
Preferably, the raw materials for preparing the emulsifier comprise, by weight, 10-25 parts of a styrene-maleic anhydride copolymer, 1-3 parts of sodium hydroxide and 70-85 parts of water.
Preferably, the preparation method of the emulsifier comprises the following steps:
10-25 parts of styrene-maleic anhydride copolymer, 1-3 parts of sodium hydroxide and 70-85 parts of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, so as to obtain the emulsifier.
Preferably, the weight ratio of the emulsifier to the horse oil is 1 (0.5-0.8).
The inventor finds that the weight ratio of the emulsifying agent to the essential oil is 1 (0.5-0.8), the prepared skin care type microcapsule has better stability, particularly the essential oil is composed of a composition of the horse oil, the grape seed oil and the shea butter, the weight ratio of the horse oil, the grape seed oil and the shea butter is 1 (0.5-2), the skin care type microcapsule with excellent stability can be formed by being more easily wrapped by wall materials after being matched with the wall materials for use when the weight ratio of the horse oil, the grape seed oil and the shea butter is 1 (0.5-0.8), the stability of the skin care type microcapsule can be influenced when the content of the essential oil is high, the possible reason is that the linolenic acid and the unsaturated fatty acid contained in the horse oil can generate higher permeability at high temperature, and the core material formed by the emulsifying agent and the essential oil is influenced by the wall materials, but the styrene-maleic anhydride copolymer and the essential oil can generate co-acting force with the styrene-maleic anhydride in the presence of sodium hydroxide and the water, so that the styrene-maleic anhydride copolymer can be better interacted with the functional groups to keep the stable state and can be wrapped by the wall materials.
The second aspect of the invention provides a method for preparing skin care microcapsules, comprising the following steps:
s1, adding essential oil and an emulsifying agent into a stirrer, stirring and emulsifying to obtain a core material;
S2, slowly adding the wall material into the core material, and adding water to mix to obtain a mixed solution;
And S3, adding the citric acid solution into the mixed solution, regulating the pH value, stirring, heating and preserving heat for a certain time to obtain the skin care microcapsule.
Preferably, the weight ratio of the wall material to the core material to the water is 1 (2.6-3): 1-1.5.
Further, the weight ratio of the wall material to the core material to the water is 1:2.8:1.2.
Preferably, the stirring speed in the step S1 is 3000-7000r/min, and the emulsifying time is 5-30min.
Preferably, in the step S3, the pH value is regulated to be 4-4.5, the stirring speed is 300-700r/min, the heat preservation temperature is 65-75 ℃, and the heat preservation time is 80-150min.
In order to improve the coating rate of the emulsifying agent and the essential oil composed of the composition of the horse oil, the grape seed oil and the shea butter as the core material wall material, the inventor finds that the coating rate and the stability of the emulsifying agent and the essential oil composed of the composition of the horse oil, the grape seed oil and the shea butter as the core material wall material can be improved by adding the citric acid solution to adjust the pH value of the mixed solution to be 4-4.5, the stirring speed to be 300-700r/min, the heat preservation temperature to be 65-75 ℃ and the heat preservation time to be 80-150min, the weight ratio of the wall material, the core material and the water is 1 (2.6-3): (1-1.5), particularly, when the weight ratio of the wall material, the core material and the water is 1:2.8:1.2, the coating rate and the stability of the essential oil composed of the composition of the horse oil, the grape seed oil and the shea butter can be improved, and the essential oil can be improved by controlling the pH value of the mixed solution, the stirring speed, the heat preservation time and the heat preservation temperature to be improved, the melamine, the urea and the formaldehyde can be dehydrated and condensed into the melamine-urea-formaldehyde resin prepolymer in the mixed solution to form the quantity of a polymer with a three-dimensional network structure through dehydration, and the quantity of the polymer in the mixed solution, and the quantity of the polymer with the three-dimensional network structure can be further dehydrated and the quantity of the essential oil, and the essential oil composed of the emulsified oil and the shea butter can be more coated with the essential oil and the essential oil can be improved by the coating rate and the essential oil; however, when the pH of the mixed solution is too high, the amount of the polymer having a three-dimensional network structure formed by further dehydrating and condensing the melamine-urea-formaldehyde resin prepolymer is affected, thereby affecting the coating ratio of the emulsifier and the composition comprising horse oil, grape seed oil and shea butter.
The third aspect of the invention provides application of the skin care microcapsule in fabric.
Preferably, the skin care microcapsules are applied as a finish to the facestock after being mixed with the binder.
An application of skin care microcapsules, comprising the following steps:
(1) Mixing the skin care microcapsules with an adhesive to obtain a finishing agent;
(2) Adding finishing agent into a liquid tank of a shaping machine, and passing fabric through the liquid tank and a roller;
(3) And heating and drying the fabric.
Preferably, the binder is a self-crosslinking polymer.
Further, the self-crosslinking polymer is self-crosslinking polyether polyurethane.
Preferably, the self-crosslinking polyether polyurethane has a viscosity of 30-70mpa.s.
The present invention is not limited to the manufacturers of self-crosslinking polyether polymers, and examples include the manufacturers of Tuo Nami Chemie, model numberThe self-crosslinking polyether polyurethane of the NANO PU has the viscosity of 50mPa.s.
Preferably, the weight ratio of the skin care microcapsules to the binder is 1 (0.5-1).
Preferably, the mass concentration of the finishing agent in the finishing liquid is 4-7%.
Preferably, the weight ratio of the finishing liquid to the fabric is (40-60): 1.
Preferably, the fabric is a cotton fiber textile fabric.
Preferably, the temperature for heating and drying the fabric is 140-160 ℃ and the drying time is 40-60 seconds.
The inventor finds that the skin care type microcapsule and the self-crosslinking polyether polyurethane are matched for use, so that the skin care type microcapsule has excellent retention durability on cotton fiber textile fabric and better water washing resistance, and the possible reasons are that the self-crosslinking polyether polyurethane is used as a connecting bridge of the cotton fiber textile fabric and the skin care type microcapsule, the self-crosslinking polyether polyurethane and the skin care type microcapsule form certain interaction and form a certain film layer on the surface of the skin care type microcapsule, and meanwhile, the self-crosslinking polyether polyurethane can permeate into the cotton fiber textile fabric and generate an intertwining structure with cotton fibers, so that the firmness of the microcapsule in the cotton fiber textile fabric is improved, the wrapped horse oil can be slowly released during application, the contact time of the horse oil and skin is prolonged, and an effective skin care effect is achieved on the skin.
Advantageous effects
According to the invention, the skin care microcapsule with good stability is prepared by limiting the weight ratio of the emulsifier to the horse oil.
According to the invention, the pH value of the mixed solution, the stirring rotation speed, the temperature of heating and preserving heat and the preserving heat time are adjusted, so that the coating rate of the emulsifier and the horse oil is improved, and the stability of the skin care microcapsule is also improved.
The skin care microcapsule prepared by the method can be provided with excellent retention durability on the fabric and has better water resistance.
By adding the adhesive in the invention, the adhesive is mixed with the skin care type microcapsule, and then the mixture is used as a water washing resistant microcapsule product to increase the water washing resistance of the microcapsule, and the possible reason is that the adhesive forms a certain film on the surface of the skin care type microcapsule and the durability of the skin care type microcapsule in the fabric is increased.
According to the invention, the microcapsule is coated and entangled with the fiber, so that the firmness of the microcapsule in the fabric is improved, the horse oil coated in the skin care microcapsule can be slowly released during application, the contact time of the horse oil and the skin is prolonged, and the skin care effect is effectively achieved for a long time.
Drawings
Fig. 1 is a photograph of the skin care type microcapsule prepared in example 1 photographed microscopically by an electron microscope.
Fig. 2 is a graph showing the test results of the horse oil content of the treated fabric obtained by applying the skin care microcapsules prepared in example 1 to cotton fiber textile fabric by GC-MS.
Fig. 3 is a graph of a test of horse oil in a treated fabric obtained by applying the skin care microcapsules prepared in example 1 to a cotton fiber textile fabric, and performing GC-MS test on the treated fabric.
Fig. 4 is a graph of the test of treated horse oil standard.
Fig. 5 is a photograph of the treated fabric obtained in example 1 subjected to microscopic photographing with an electron microscope after washing 5 times.
Detailed Description
Example 1
A skin care microcapsule is prepared from wall material and core material;
the wall material is prepared from the following raw materials, by weight, 6.7 parts of melamine, 5.5 parts of urea, 26 parts of formaldehyde aqueous solution and 25 parts of water;
the preparation raw materials of the core material comprise an emulsifying agent and essential oil;
The essential oil is a composition of horse oil, grape seed oil and shea butter, and the weight ratio of the horse oil to the grape seed oil to the shea butter is 1:1:1.5.
The manufacturer of the horse oil is Shanghai Bin new material technology Co.
The purchasing manufacturer of the grape seed oil essential oil is Chengsheng biotechnology Co., ltd.
The manufacturer of the shea butter is Jiangxi Jingwang natural perfume limited company.
The CAS number of the melamine is 108-78-1.
The CAS number of the urea is 57-13-6.
The mass concentration of formaldehyde in the formaldehyde aqueous solution is 37%.
The preparation method of the wall material comprises the following steps:
and regulating the pH value of the aqueous solution of melamine, urea and formaldehyde in water to 8.5 by using an aqueous solution of NaOH with the mass concentration of 30%, stirring, heating, preserving heat for a certain time, cooling to 40 ℃ after the reaction is finished, and ending stirring to obtain the wall material.
The temperature rising speed is 1 ℃ per minute, the heat preservation temperature is 70 ℃, and the heat preservation time is 1h.
The raw materials for preparing the emulsifier comprise, by weight, 20 parts of a styrene-maleic anhydride copolymer, 2 parts of sodium hydroxide and 78 parts of water.
The preparation method of the emulsifier comprises the following steps:
20 parts of styrene-maleic anhydride copolymer, 2 parts of sodium hydroxide and 78 parts of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, so as to obtain the emulsifier.
The weight ratio of the emulsifier to the horse oil is 1:0.65.
The second aspect of the present embodiment provides a method for preparing a skin care microcapsule, comprising the steps of:
s1, adding essential oil and an emulsifying agent into a stirrer, stirring and emulsifying to obtain a core material;
S2, slowly adding the wall material into the core material, and adding water to mix to obtain a mixed solution;
And S3, adding the citric acid solution into the mixed solution to regulate the pH, stirring, heating and preserving heat for a certain time to obtain the skin care microcapsule.
The weight ratio of the wall material to the core material to the water is 1:3:1.05.
The core material is added in an amount of 150 parts by weight.
The rotation speed of stirring in the step S1 is 5500r/min, and the emulsification time is 20min.
And in the step S3, the pH value is regulated to be 4, the stirring speed is 550r/min, the heat preservation temperature is 70 ℃, and the heat preservation time is 110min.
A third aspect of the present embodiment provides an application of a skin care microcapsule in a fabric.
The application of the skin care microcapsule comprises the following steps:
(1) Mixing the skin care microcapsules with an adhesive to obtain a finishing agent;
(2) Adding the finishing agent into a liquid tank of a setting machine, mixing with water to form finishing liquid, immersing the fabric in the liquid tank for 2min and rolling;
(3) And heating and drying the fabric.
The adhesive is self-crosslinking polyether type polymer, and the self-crosslinking polymer is self-crosslinking polyether polyurethane.
The self-crosslinking polyether polyurethane is purchased from the manufacturer of Tuo Naochi, model number isNANO PU。
The weight ratio of the skin care microcapsules to the binder is 1:0.8.
The mass concentration of the finishing agent in the finishing liquid is 5%.
The weight ratio of the finishing liquid to the fabric is 50:1.
The fabric is cotton fiber textile fabric.
The temperature of heating and drying the fabric is 150 ℃, and the drying is carried out for 50s.
Example 2
A skin care microcapsule is prepared from wall material and core material;
the wall material is prepared from the following raw materials, by weight, 7.5 parts of melamine, 6.5 parts of urea, 30 parts of formaldehyde aqueous solution and 30 parts of water;
the preparation raw materials of the core material comprise an emulsifying agent and essential oil;
The essential oil is a composition of horse oil, grape seed oil and shea butter, and the weight ratio of the horse oil to the grape seed oil to the shea butter is 1:1:1.5.
The manufacturer of the horse oil is Shanghai Bin new material technology Co.
The purchasing manufacturer of the grape seed oil essential oil is Chengsheng biotechnology Co., ltd.
The manufacturer of the shea butter is Jiangxi Jingwang natural perfume limited company.
The CAS number of the melamine is 108-78-1.
The CAS number of the urea is 57-13-6.
The mass concentration of formaldehyde in the formaldehyde aqueous solution is 37%.
The preparation method of the wall material comprises the following steps:
and regulating the pH value of the aqueous solution of melamine, urea and formaldehyde in water to 9 by using an aqueous solution of NaOH with the mass concentration of 30%, stirring, heating, preserving heat for a certain time, cooling to 50 ℃ after the reaction is finished, and ending stirring to obtain the wall material.
The temperature rising speed is 3 ℃ per minute, the heat preservation temperature is 75 ℃, and the heat preservation time is 2 hours.
The raw materials for preparing the emulsifier comprise, by weight, 25 parts of a styrene-maleic anhydride copolymer, 3 parts of sodium hydroxide and 85 parts of water.
The weight ratio of the emulsifier to the horse oil is 1:0.8.
The preparation method of the emulsifier comprises the following steps:
25 parts of styrene-maleic anhydride copolymer, 3 parts of sodium hydroxide and 85 parts of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, so as to obtain the emulsifier.
The second aspect of the present embodiment provides a method for preparing a skin care microcapsule, comprising the steps of:
s1, adding essential oil and an emulsifying agent into a stirrer, stirring and emulsifying to obtain a core material;
S2, slowly adding the wall material into the core material, and adding water to mix to obtain a mixed solution;
And S3, adding the citric acid solution into the mixed solution to regulate the pH, stirring, heating and preserving heat for a certain time to obtain the skin care microcapsule.
The weight ratio of the wall material to the core material to the water is 1:2.6:1.2.
The core material is added in an amount of 150 parts by weight.
The stirring speed in the step S1 is 7000r/min, and the emulsifying time is 10min.
And in the step S3, the pH value is regulated to be 4.5, the stirring speed is 700r/min, the heat preservation temperature is 75 ℃, and the heat preservation time is 150min.
A third aspect of the present embodiment provides an application of a skin care microcapsule in a fabric.
The application of the skin care microcapsule comprises the following steps:
(1) Mixing the skin care microcapsules with an adhesive to obtain a finishing agent;
(2) Adding the finishing agent into a liquid tank of a setting machine, mixing with water to form finishing liquid, immersing the fabric in the liquid tank for 2min and rolling;
(3) And heating and drying the fabric.
The adhesive is self-crosslinking polyether type polymer, and the self-crosslinking polymer is self-crosslinking polyether polyurethane.
The self-crosslinking polyether polyurethane is purchased from the manufacturer of Tuo Naochi, model number isNANO PU。
The weight ratio of the skin care microcapsules to the binder is 1:1.
The mass concentration of the finishing agent in the finishing liquid is 7%.
The weight ratio of the finishing liquid to the fabric is 50:1.
The fabric is cotton fiber textile fabric.
The temperature of heating and drying the fabric is 150 ℃, and the drying is carried out for 50s.
Example 3
A skin care microcapsule is prepared from wall material and core material;
The wall material is prepared from the following raw materials in parts by weight, namely 5.5 parts of melamine, 5 parts of urea, 20 parts of formaldehyde aqueous solution and 20 parts of water;
the preparation raw materials of the core material comprise an emulsifying agent and essential oil;
The essential oil is a composition of horse oil, grape seed oil and shea butter, and the weight ratio of the horse oil to the grape seed oil to the shea butter is 1:1:1.5.
The manufacturer of the horse oil is Shanghai Bin new material technology Co.
The purchasing manufacturer of the grape seed oil essential oil is Chengsheng biotechnology Co., ltd.
The manufacturer of the shea butter is Jiangxi Jingwang natural perfume limited company.
The CAS number of the melamine is 108-78-1.
The CAS number of the urea is 57-13-6.
The mass concentration of formaldehyde in the formaldehyde aqueous solution is 37%.
The preparation method of the wall material comprises the following steps:
And regulating the pH value of the aqueous solution of melamine, urea and formaldehyde in water to 8 by using an aqueous solution of NaOH with the mass concentration of 30%, stirring, heating, preserving heat for a certain time, cooling to 35 ℃ after the reaction is finished, and ending stirring to obtain the wall material.
The temperature rising speed is 0.5 ℃ per minute, the heat preservation temperature is 65 ℃, and the heat preservation time is 2 hours.
The raw materials for preparing the emulsifier comprise 15 parts by weight of styrene-maleic anhydride copolymer, 1.5 parts by weight of sodium hydroxide and 70 parts by weight of water.
15 Parts of styrene-maleic anhydride copolymer, 1.5 parts of sodium hydroxide and 70 parts of water are mixed and heated to 80 ℃ until the solution is transparent yellow liquid, so as to obtain the emulsifier.
The weight ratio of the emulsifier to the horse oil is 1:0.5.
The second aspect of the present embodiment provides a method for preparing a skin care microcapsule, comprising the steps of:
s1, adding essential oil and an emulsifying agent into a stirrer, stirring and emulsifying to obtain a core material;
S2, slowly adding the wall material into the core material, and adding water to mix to obtain a mixed solution;
And S3, adding the citric acid solution into the mixed solution to regulate the pH, stirring, heating and preserving heat for a certain time to obtain the skin care microcapsule.
The weight ratio of the wall material to the core material to the water is 1:2.6:1.2.
The core material is added in an amount of 120 parts by weight.
The stirring speed in the step S1 is 7000r/min, and the emulsifying time is 10min.
And in the step S3, the pH value is regulated to be 4.5, the stirring speed is 700r/min, the heat preservation temperature is 75 ℃, and the heat preservation time is 150min.
A third aspect of the present embodiment provides an application of a skin care microcapsule in a fabric.
The application of the skin care microcapsule comprises the following steps:
(1) Mixing the skin care microcapsules with an adhesive to obtain a finishing agent;
(2) Adding the finishing agent into a liquid tank of a setting machine, mixing with water to form finishing liquid, immersing the fabric in the liquid tank for 2min and rolling;
(3) And heating and drying the fabric.
The adhesive is self-crosslinking polyether type polymer, and the self-crosslinking polymer is self-crosslinking polyether polyurethane.
The self-crosslinking polyether polyurethane is purchased from the manufacturer of Tuo Naochi, model number isNANO PU。
The weight ratio of the skin care microcapsules to the binder is 1:0.5.
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 cotton fiber textile fabric.
The temperature of heating and drying the fabric is 150 ℃, and the drying is carried out for 50s.
Example 4
Example 4 provides a skin care microcapsule, a preparation method and an application technical scheme, which are different from example 1 in that in the preparation method of the skin care microcapsule, the pH value is adjusted to 5.5 in the step S3, and the temperature is kept at 80 ℃.
Example 5
Example 5 provides a skin care microcapsule, a preparation method and an application technical scheme, and the skin care microcapsule is different from example 1 in that the weight ratio of the emulsifier to the horse oil is 1:1.
Example 6
Example 6 provides a skin care microcapsule, a preparation method and an application technical scheme, and the skin care microcapsule is different from example 1 in that the adhesive is self-crosslinking acrylic latex, the year of the self-crosslinking acrylic latex is 60mPa.s, and the manufacturer is Graded New Material technology (Zhongshan).
Performance testing
1. Stability test
The skin care microcapsules prepared in examples 1 to 6 were stored at 60 ℃ for 72 hours, the existence state of the skin care microcapsules was observed, whether turbidity and precipitation occurred or not was observed, the appearance of no turbidity and no precipitation was marked as class a, the appearance of turbidity and no precipitation was marked as class B, the appearance of turbidity and no precipitation was marked as class C, and the test results are shown in table 1.
2. Dimensional testing
The skin care microcapsule prepared in example 1 is subjected to microscopic photographing by an electron microscope, and a photographing diagram is shown in fig. 1.
The treated fabric obtained in example 1 was subjected to microscopic photographing by using an electron microscope, and the photographing chart is shown in fig. 5.
3. Testing of horse oil content in fabric
The skin care microcapsules prepared in example 1 were applied to cotton fiber textile fabric to obtain treated fabric, and the content of horse oil in the fabric was tested by GC-MS, and the test results are shown in FIGS. 2-4.
The figure 3 is a test spectrum of qualitative test of horse oil in the treated fabric obtained by applying the skin care microcapsule prepared in the example 1 to the cotton fiber textile fabric, and the GC-MS test is adopted to test the fabric, the figure 4 is a test spectrum of horse oil standard product after treatment, and as can be seen from the figure 4, ma Youbiao standard product after GC-MS treatment is obtained, different ion fragments are obtained, the ion fragments appear in the range of 19-23, as can be seen from the figure 3, the ion fragments obtained after GC-MS treatment of horse oil in the extracted fabric also appear in the range of 19-23, and the correspondence of peak type and peak intensity is the same as the correspondence of test result obtained in the figure 4, so that a certain amount of horse oil is contained in the fabric, and the content of horse oil in the obtained fabric is 2174mg/kg through GC-MS quantitative test.
4. Test of Water washing resistance
The treated fabric obtained by applying the skin care microcapsules prepared in examples 1 to 6 to cotton fiber textile fabric was washed with water once a week for 30 minutes, after 5 times of washing, the change rate of the horse oil content in the fabric before washing with water and without washing was measured, the change rate of the horse oil content was designated as a grade of less than 20%, the change rate of the horse oil content was designated as B grade of more than 20% and less than or equal to 30%, the change rate of the horse oil content was designated as C grade of more than 30% and less than or equal to 40%, the change rate of the horse oil content was designated as D grade of more than 40%, and the measurement results are shown in table 1.
TABLE 1
| Examples | Stability of | Resistance to washing with water |
| Example 1 | A | A |
| Example 2 | A | A |
| Example 3 | A | A |
| Example 4 | C | C |
| Example 5 | B | B |
| Example 6 | A | D |
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| CN108004788A (en) * | 2017-12-20 | 2018-05-08 | 贺州宝兴新材料有限公司 | A kind of preparation method of modified melamine resin essence microcapsule finishing agent |
| CN111455675A (en) * | 2020-04-23 | 2020-07-28 | 罗莱生活科技股份有限公司 | Skin-care microcapsule and preparation method and application thereof |
| CN114133984A (en) * | 2021-12-10 | 2022-03-04 | 东莞波顿香料有限公司 | Essence capsule capable of releasing fragrance by friction and preparation method thereof |
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| KR100415442B1 (en) * | 2001-02-15 | 2004-01-24 | 우리켐테크(주) | Health functional textile adhered by microcapsule containing muscone or natural oil |
| CN111021061B (en) * | 2019-12-24 | 2022-10-11 | 淄博大染坊丝绸集团有限公司 | After-finishing process of hyaluronic acid real silk fabric |
| CN112144290A (en) * | 2020-08-25 | 2020-12-29 | 深圳全棉时代科技有限公司 | Production method of skin-care fabric |
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| CN108004788A (en) * | 2017-12-20 | 2018-05-08 | 贺州宝兴新材料有限公司 | A kind of preparation method of modified melamine resin essence microcapsule finishing agent |
| CN111455675A (en) * | 2020-04-23 | 2020-07-28 | 罗莱生活科技股份有限公司 | Skin-care microcapsule and preparation method and application thereof |
| CN114133984A (en) * | 2021-12-10 | 2022-03-04 | 东莞波顿香料有限公司 | Essence capsule capable of releasing fragrance by friction and preparation method thereof |
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