CN113802214A - Medicinal ink phase change microcapsule fiber and preparation method thereof - Google Patents
Medicinal ink phase change microcapsule fiber and preparation method thereof Download PDFInfo
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- CN113802214A CN113802214A CN202111247770.2A CN202111247770A CN113802214A CN 113802214 A CN113802214 A CN 113802214A CN 202111247770 A CN202111247770 A CN 202111247770A CN 113802214 A CN113802214 A CN 113802214A
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 98
- 239000000835 fiber Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 230000008859 change Effects 0.000 title claims abstract description 24
- 238000009987 spinning Methods 0.000 claims abstract description 53
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims abstract description 39
- 235000011613 Pinus brutia Nutrition 0.000 claims abstract description 39
- 241000018646 Pinus brutia Species 0.000 claims abstract description 39
- 239000000779 smoke Substances 0.000 claims abstract description 34
- 239000012188 paraffin wax Substances 0.000 claims abstract description 32
- 229920000642 polymer Polymers 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 23
- 239000011162 core material Substances 0.000 claims abstract description 13
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims abstract description 12
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000010556 emulsion polymerization method Methods 0.000 claims abstract description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 6
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 6
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 6
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 6
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 55
- 238000003756 stirring Methods 0.000 claims description 35
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000012153 distilled water Substances 0.000 claims description 20
- 239000000839 emulsion Substances 0.000 claims description 16
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 15
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 10
- 239000002562 thickening agent Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 230000001112 coagulating effect Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000002775 capsule Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical group O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 5
- 229910001626 barium chloride Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 230000008719 thickening Effects 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 238000002166 wet spinning Methods 0.000 claims description 5
- 230000015271 coagulation Effects 0.000 claims description 2
- 238000005345 coagulation Methods 0.000 claims description 2
- 239000004753 textile Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 9
- 239000012782 phase change material Substances 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 3
- 230000007721 medicinal effect Effects 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 235000019504 cigarettes Nutrition 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
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- 238000002485 combustion reaction Methods 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
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- 239000002657 fibrous material Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
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Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
- B01J13/06—Making microcapsules or microballoons by phase separation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to the technical field of textile fibers, and discloses a medicinal ink phase change microcapsule fiber which comprises the following raw materials in parts by weight: the phase-change microcapsule comprises pine smoke drug ink powder, alkane phase-change paraffin, a phase-change microcapsule wall material and a polymer spinning solution, wherein the alkane phase-change paraffin is n-hexadecane or n-octadecane, the phase-change microcapsule wall material is polymethyl methacrylate or polyacrylonitrile, the polymer spinning solution is 20-30% of polyethylene terephthalate, the pine smoke drug ink powder and the alkane phase-change paraffin are combined together to be used as a core material, and the phase-change microcapsule is prepared through an emulsion polymerization method. The medicinal ink phase-change microcapsule fiber and the preparation method thereof provide a novel fiber raw material for the development of functional fiber textiles, effectively reduce the leakage problem of the pine smoke medicinal ink, and enable the medicinal effect of the medicinal ink to be better played through the heat release effect during the state transition of the phase-change material, thereby endowing the medicinal ink fiber with a new function of thermal moxibustion.
Description
Technical Field
The invention relates to the technical field of textile fibers, in particular to a medicinal ink phase change microcapsule fiber and a preparation method thereof.
Background
Pine cigarette medicinal ink is a traditional Chinese medicine preparation which can be taken orally or externally, wherein pine cigarette is carbon dust which is formed by incomplete combustion of pine trunk, pine branches and the like and flocculation of the cooled dense smoke, the pine cigarette medicinal ink has the longest history in ancient ink preparation types, and has tiny particle size, so that people who have great attention to ink preparation crafts are concerned by taking the medicinal ink into the ink, and the pine cigarette medicinal ink is always in contact with the skin, is easy to permeate into the skin, and can generate the health-care effects of relaxing muscles and tendons, promoting blood circulation and conditioning the body.
The phase-change microcapsule is a new research technology formed by applying a microcapsule technology to a phase-change material, consists of a core material and a capsule wall, different phase-change materials can be selected as the core material to meet various required functional requirements, the phase-change material is encapsulated, the reaction of the phase-change material and the external environment is reduced, the heat transfer efficiency is improved, when the phase-change temperature of the phase-change material is reached, the state of the material is changed to release certain heat, meanwhile, the phase-change microcapsule can be effectively controlled for the material which is easy to leak, the phase-change microcapsule technology receives more and more attention in the field of textiles, and the phase-change microcapsule is a research hotspot in recent years.
With the continuous improvement of living standard, the development of modern textiles also puts forward more and more requirements, the development of functional synthetic fibers is a hot spot of research, more and better basic fiber materials can be provided for the requirements of clothes and textiles of people, if the pine smoke medicinal ink is added into the spinning solution, pine smoke medicinal ink fiber is prepared by the traditional spinning process and then is woven into textile, so that the textile not only has basic functions of beauty, heat preservation and the like, but also has the pharmacological function of the pine smoke medicinal ink, particularly is spun into underwear, under the help of the heat release effect of the phase-change material, the utility model can generate benefit for regulating human body to achieve the efficacy of thermal moxibustion, however, if the medicinal ink is directly combined with the spinning solution, the leakage problem is easy to occur, and thus the spinning process and the generated effect are greatly influenced, so that the medicinal ink phase-change microcapsule fiber and the preparation method thereof are provided to solve the problems.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the medicinal ink phase-change microcapsule fiber and the preparation method thereof, which have the advantages of effectively reducing the leakage of medicinal ink, developing a new-function textile fiber with a modern health-preserving concept, and solving the problems that the leakage is easy to occur when the medicinal ink is directly combined with spinning solution, and the great influence is caused on the spinning process and the generated effect.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the medicinal ink phase change microcapsule fiber comprises the following raw materials in parts by weight: pine smoke medicinal ink powder, alkane phase-change paraffin, phase-change microcapsule wall materials and polymer spinning solution.
Preferably, the alkane phase-change paraffin is n-hexadecane or n-octadecane
Preferably, the wall material of the phase-change microcapsule is polymethyl methacrylate or polyacrylonitrile.
Preferably, the polymer spinning solution is 20 to 30 mass percent of polyethylene terephthalate.
The invention aims to solve another technical problem of providing a preparation method of the medicinal ink phase-change microcapsule fiber, which comprises the following steps:
1) pine smoke medicinal ink powder and alkane phase-change paraffin are combined together to be used as core materials, and the phase-change microcapsules are prepared by an emulsion polymerization method.
2) Which is then added to the polymer dope.
3) The medicinal ink phase-change microcapsule fiber is prepared by adopting a wet spinning process.
Preferably, the phase-change microcapsule is prepared by the following steps: step 1) adding pine smoke medicinal ink into distilled water to prepare medicinal ink suspension, and then adding the medicinal ink suspension, a surfactant, a thickening agent and the distilled water into a beaker according to a certain proportion; step 2) adding the alkane phase-change paraffin and the microcapsule wall material into the solution obtained in the step 1), placing the beaker in a constant-temperature water bath, and continuously stirring the mixture by using a stirrer to uniformly disperse the mixture; step 3), adding an emulsifier, absolute ethyl alcohol and deionized water, uniformly stirring the mixture, and dispersing the mixture by using ultrasound to form stable emulsion; step 4) placing the emulsion obtained in the step 3) in a constant-temperature water bath, stirring for 1.5h, then dropwise adding an ammonia water solution to adjust the pH value of the solution to 8-9, stirring at constant temperature until the reaction is finished, and then standing at room temperature for 24h to fully solidify the capsule wall; and 5) finally, pouring out the supernatant in the solution after standing, adding absolute ethyl alcohol into the precipitate, centrifuging, repeating the steps for three times, cleaning the precipitate, and drying to obtain the medicinal ink paraffin microcapsule.
Preferably, the preparation steps of the fiber are as follows: step 1) adding the prepared pine smoke medicinal ink microcapsules into a polymer spinning solution, and uniformly distributing the medicinal ink microcapsules in the solution by an ultrasonic machine; step 2) stirring the spinning solution obtained in the step 1) in a constant-temperature water bath by adopting a stirrer to defoam the spinning solution to obtain a medicinal ink spinning solution; and 3) pouring the spinning solution into a stainless steel storage tank, pushing the spinning solution to a spinneret orifice by a metering pump under the action of nitrogen, spraying the spinning solution out, then entering a coagulating bath and a drafting bath, and performing post-treatment to obtain the medicinal ink phase change microcapsule fiber.
Preferably, the surfactant is Sodium Dodecyl Sulfate (SDS), the thickener is polyvinyl alcohol, the emulsifier is selected from styrene maleic anhydride copolymer (SMA), sodium dodecyl sulfate or cetyl trimethyl sodium bromide, and the mass ratio of the pine smoke medicinal ink to the distilled water is 1: 2-5, the preparation concentration is 0.2-0.5 g/ml, and the ratio of the medicinal ink suspension, the surfactant, the thickening liquid and the distilled water is 5:1:1: 10.
Preferably, the core material and wall material solution is placed in a constant-temperature water bath kettle, the temperature is 60-80 ℃, the stirring speed of a stirrer is 700-1000 r/min, the ultrasonic time of the solution is 15-30 min, the temperature of the constant-temperature water bath kettle in which the emulsion is located is 90-120 ℃, and the mass ratio of the ink-drug phase-change microcapsules to the polymer is 1: 5-8, the method comprises the following steps: the ultrasonic time is 15-20 min, the temperature of the constant-temperature water bath is 80-100 ℃, the stirring time is 30-60 min, and the nitrogen pressure is 0.2 mpa.
Preferably, the coagulation bath is 7% BaCl2 and the draw bath is 3% BaCl 2; the speed ratio of the two yarn guide rollers in the drafting bath is 1: 2-5, and the post-treatment is to place the fiber subjected to the drawing bath in a glycerol aqueous solution for soaking treatment and then dry the fiber, wherein the mass fraction of the glycerol aqueous solution is 2%.
(III) advantageous effects
Compared with the prior art, the invention provides a medicinal ink phase change microcapsule fiber and a preparation method thereof, and the medicinal ink phase change microcapsule fiber has the following beneficial effects:
the medicinal ink phase-change microcapsule fiber and the preparation method thereof provide a novel fiber raw material for the development of functional fiber textiles, effectively reduce the leakage problem of pine smoke medicinal ink, and enable the medicinal effect of the medicinal ink to be better played through the temperature-adjusting and heat-releasing functions, achieve certain hot moxibustion effect, and adopt the traditional textile technology, the operation flow is simple and convenient, and the traditional textile technology is popular and easy to understand.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: the medicinal ink phase change microcapsule fiber comprises the following raw materials in parts by weight: pine smoke medicinal ink powder, alkane phase-change paraffin, phase-change microcapsule wall materials and polymer spinning solution.
Wherein the alkane phase-change paraffin is n-hexadecane or n-octadecane, the phase-change microcapsule wall material is polymethyl methacrylate or polyacrylonitrile, and the polymer spinning solution is polyethylene terephthalate with the mass fraction of 20%.
A preparation method of medicinal ink phase-change microcapsule fibers comprises the following steps:
1) pine smoke medicinal ink powder and alkane phase-change paraffin are combined together to be used as core materials, and the phase-change microcapsules are prepared by an emulsion polymerization method.
2) Which is then added to the polymer dope.
3) The medicinal ink phase-change microcapsule fiber is prepared by adopting a wet spinning process.
Specifically, the preparation method comprises the preparation of medicinal ink/paraffin microcapsules and the preparation of fibers, wherein the preparation process of the phase-change microcapsules comprises the following steps: step 1) adding pine smoke medicinal ink into distilled water to prepare medicinal ink suspension, and then adding the medicinal ink suspension, a surfactant, a thickening agent and the distilled water into a beaker according to a certain proportion; step 2) adding the alkane phase-change paraffin and the microcapsule wall material into the solution obtained in the step 1), placing the beaker in a constant-temperature water bath, and continuously stirring the mixture by using a stirrer to uniformly disperse the mixture; step 3), adding an emulsifier, absolute ethyl alcohol and deionized water, uniformly stirring the mixture, and dispersing the mixture by using ultrasound to form stable emulsion; step 4) placing the emulsion obtained in the step 3) in a constant-temperature water bath at 90 ℃ and stirring for 1.5h, then dropwise adding an ammonia water solution to adjust the pH value of the emulsion to 8-9, stirring at constant temperature until the reaction is finished, and then standing at room temperature for 24h to fully solidify the capsule wall; and 5) finally, pouring out the supernatant in the solution after standing, adding absolute ethyl alcohol into the precipitate, centrifuging, repeating the steps for three times, cleaning the precipitate, and drying to obtain the medicinal ink paraffin microcapsule.
Specifically, the preparation steps of the fiber are as follows: step 1) adding the prepared pine smoke medicinal ink microcapsules into a polymer spinning solution, and uniformly distributing the medicinal ink microcapsules in the solution by an ultrasonic machine; step 2) stirring the spinning solution obtained in the step 1) in a constant-temperature water bath by adopting a stirrer to defoam the spinning solution to obtain a medicinal ink spinning solution; and 3) pouring the spinning solution into a stainless steel storage tank, pushing the spinning solution to a spinneret orifice by a metering pump under the action of nitrogen, spraying the spinning solution out, then entering a coagulating bath and a drafting bath, and performing post-treatment to obtain the medicinal ink phase change microcapsule fiber.
Wherein the surfactant is Sodium Dodecyl Sulfate (SDS), the thickener is polyvinyl alcohol, the emulsifier is styrene maleic anhydride copolymer (SMA), sodium dodecyl sulfate or cetyl trimethyl sodium bromide, and the mass ratio of the pine smoke medicinal ink to the distilled water is 1: 2, the preparation concentration is 0.2g/ml, and the proportion of the medicinal ink suspension, the surfactant, the thickening liquid and the distilled water is 5:1:1: 10.
The core material and wall material solution is placed in a constant-temperature water bath kettle, the temperature is 60 ℃, the stirring speed of a stirrer is 700r/min, the ultrasonic time of the solution is 10min, the temperature of the constant-temperature water bath kettle where the emulsion is located is 90 ℃, and the mass ratio of the medicinal ink phase-change microcapsule to the polymer is 1: 5, the ultrasonic time is 15min, the constant temperature water bath temperature is 80 ℃, the stirring time is 30min, and the nitrogen pressure is 0.2 mpa.
Wherein the coagulating bath is 7% BaCl2, and the drawing bath is 3% BaCl 2; the speed ratio of the two yarn guide rollers in the drafting bath is 1: and 2, post-treatment, namely soaking the fiber subjected to the drawing bath in a glycerol aqueous solution, and then drying, wherein the mass fraction of the glycerol aqueous solution is 2%.
Example two: the medicinal ink phase change microcapsule fiber comprises the following raw materials in parts by weight: pine smoke medicinal ink powder, alkane phase-change paraffin, phase-change microcapsule wall materials and polymer spinning solution.
Wherein the alkane phase-change paraffin is n-hexadecane or n-octadecane, the phase-change microcapsule wall material is polymethyl methacrylate or polyacrylonitrile, and the polymer spinning solution is 25 mass percent of polyethylene terephthalate.
A preparation method of medicinal ink phase-change microcapsule fibers comprises the following steps:
1) pine smoke medicinal ink powder and alkane phase-change paraffin are combined together to be used as core materials, and the phase-change microcapsules are prepared by an emulsion polymerization method.
2) Which is then added to the polymer dope.
3) The medicinal ink phase-change microcapsule fiber is prepared by adopting a wet spinning process.
Specifically, the preparation method comprises the preparation of medicinal ink/paraffin microcapsules and the preparation of fibers, wherein the preparation process of the phase-change microcapsules comprises the following steps: step 1) adding pine smoke medicinal ink into distilled water to prepare medicinal ink suspension, and then adding the medicinal ink suspension, a surfactant, a thickening agent and the distilled water into a beaker according to a certain proportion; step 2) adding the alkane phase-change paraffin and the microcapsule wall material into the solution obtained in the step 1), placing the beaker in a constant-temperature water bath, and continuously stirring the mixture by using a stirrer to uniformly disperse the mixture; step 3), adding an emulsifier, absolute ethyl alcohol and deionized water, uniformly stirring the mixture, and dispersing the mixture by using ultrasound to form stable emulsion; step 4) placing the emulsion obtained in the step 3) in a constant-temperature water bath at 110 ℃ and stirring for 1.5h, then dropwise adding an ammonia water solution to adjust the pH value of the mixture to 8-9, stirring at constant temperature until the reaction is finished, and then standing at room temperature for 24h to fully solidify the capsule wall; and 5) finally, pouring out the supernatant in the solution after standing, adding absolute ethyl alcohol into the precipitate, centrifuging, repeating the steps for three times, cleaning the precipitate, and drying to obtain the medicinal ink paraffin microcapsule.
Specifically, the preparation steps of the fiber are as follows: step 1) adding the prepared pine smoke medicinal ink microcapsules into a polymer spinning solution, and uniformly distributing the medicinal ink microcapsules in the solution by an ultrasonic machine; step 2) stirring the spinning solution obtained in the step 1) in a constant-temperature water bath by adopting a stirrer to defoam the spinning solution to obtain a medicinal ink spinning solution; and 3) pouring the spinning solution into a stainless steel storage tank, pushing the spinning solution to a spinneret orifice by a metering pump under the action of nitrogen, spraying the spinning solution out, then entering a coagulating bath and a drafting bath, and performing post-treatment to obtain the medicinal ink phase change microcapsule fiber.
Wherein the surfactant is Sodium Dodecyl Sulfate (SDS), the thickener is polyvinyl alcohol, the emulsifier is styrene maleic anhydride copolymer (SMA), sodium dodecyl sulfate or cetyl trimethyl sodium bromide, and the mass ratio of the pine smoke medicinal ink to the distilled water is 1: 4, the preparation concentration is 0.4g/ml, and the proportion of the medicinal ink suspension, the surfactant, the thickening liquid and the distilled water is 5:1:1: 10.
The core material and wall material solution is placed in a constant-temperature water bath kettle, the temperature is 70 ℃, the stirring speed of a stirrer is 800r/min, the ultrasonic time of the solution is 5min, the temperature of the constant-temperature water bath kettle where the emulsion is located is 110 ℃, and the mass ratio of the medicinal ink phase-change microcapsule to the polymer is 1: 6, the ultrasonic time is 20min, the constant temperature water bath temperature is 90 ℃, the stirring time is 40min, and the nitrogen pressure is 0.2 mpa.
Wherein the coagulating bath is 7% BaCl2, and the drawing bath is 3% BaCl 2; the speed ratio of the two yarn guide rollers in the drafting bath is 1: and 6, post-treatment, namely soaking the fiber subjected to the drawing bath in a glycerol aqueous solution, and then drying, wherein the mass fraction of the glycerol aqueous solution is 2%.
Example three: the medicinal ink phase change microcapsule fiber comprises the following raw materials in parts by weight: pine smoke medicinal ink powder, alkane phase-change paraffin, phase-change microcapsule wall materials and polymer spinning solution.
Wherein the alkane phase-change paraffin is n-hexadecane or n-octadecane, the phase-change microcapsule wall material is polymethyl methacrylate or polyacrylonitrile, and the polymer spinning solution is polyethylene terephthalate with the mass fraction of 30%.
A preparation method of medicinal ink phase-change microcapsule fibers comprises the following steps:
1) pine smoke medicinal ink powder and alkane phase-change paraffin are combined together to be used as core materials, and the phase-change microcapsules are prepared by an emulsion polymerization method.
2) Which is then added to the polymer dope.
3) The medicinal ink phase-change microcapsule fiber is prepared by adopting a wet spinning process.
Specifically, the preparation method comprises the preparation of medicinal ink/paraffin microcapsules and the preparation of fibers, wherein the preparation process of the phase-change microcapsules comprises the following steps: step 1) adding pine smoke medicinal ink into distilled water to prepare medicinal ink suspension, and then adding the medicinal ink suspension, a surfactant, a thickening agent and the distilled water into a beaker according to a certain proportion; step 2) adding the alkane phase-change paraffin and the microcapsule wall material into the solution obtained in the step 1), placing the beaker in a constant-temperature water bath, and continuously stirring the mixture by using a stirrer to uniformly disperse the mixture; step 3), adding an emulsifier, absolute ethyl alcohol and deionized water, uniformly stirring the mixture, and dispersing the mixture by using ultrasound to form stable emulsion; step 4) placing the emulsion obtained in the step 3) in a constant-temperature water bath at 120 ℃ and stirring for 1.5h, then dropwise adding an ammonia water solution to adjust the pH value of the solution to 8-9, stirring at constant temperature until the reaction is finished, and then standing at room temperature for 24h to fully solidify the capsule wall; and 5) finally, pouring out the supernatant in the solution after standing, adding absolute ethyl alcohol into the precipitate, centrifuging, repeating the steps for three times, cleaning the precipitate, and drying to obtain the medicinal ink paraffin microcapsule.
Specifically, the preparation steps of the fiber are as follows: step 1) adding the prepared pine smoke medicinal ink microcapsules into a polymer spinning solution, and uniformly distributing the medicinal ink microcapsules in the solution by an ultrasonic machine; step 2) stirring the spinning solution obtained in the step 1) in a constant-temperature water bath by adopting a stirrer to defoam the spinning solution to obtain a medicinal ink spinning solution; and 3) pouring the spinning solution into a stainless steel storage tank, pushing the spinning solution to a spinneret orifice by a metering pump under the action of nitrogen, spraying the spinning solution out, then entering a coagulating bath and a drafting bath, and performing post-treatment to obtain the medicinal ink phase change microcapsule fiber.
Wherein the surfactant is Sodium Dodecyl Sulfate (SDS), the thickener is polyvinyl alcohol, the emulsifier is styrene maleic anhydride copolymer (SMA), sodium dodecyl sulfate or cetyl trimethyl sodium bromide, and the mass ratio of the pine smoke medicinal ink to the distilled water is 1: 5, the preparation concentration is 0.5g/ml, and the proportion of the medicinal ink suspension, the surfactant, the thickening liquid and the distilled water is 5:1:1: 10.
The core material and wall material solution is placed in a constant-temperature water bath kettle, the temperature is 80 ℃, the stirring speed of a stirrer is 1000r/min, the ultrasonic time of the solution is 20min, the temperature of the constant-temperature water bath kettle where the emulsion is located is 120 ℃, and the mass ratio of the medicinal ink phase-change microcapsule to the polymer is 1: 8, the ultrasonic time is 20min, the temperature of the constant-temperature water bath is 100 ℃, the stirring time is 60min, and the nitrogen pressure is 0.2 mpa.
Wherein the coagulating bath is 7% BaCl2, and the drawing bath is 3% BaCl 2; the speed ratio of the two yarn guide rollers in the drafting bath is 1: and 5, post-treatment, namely soaking the fiber subjected to the drawing bath in a glycerol aqueous solution, and then drying, wherein the mass fraction of the glycerol aqueous solution is 2%.
The pine smoke medicinal ink phase change microcapsule fibers prepared in the examples 1 to 3 are subjected to a test of basic fiber forming performance, and the specific data are as follows:
as can be seen from the above table, the fiber has good glossiness and no obvious color change, which indicates that the problem of leakage of the medicinal ink is effectively assisted under the wrapping effect of the phase-change microcapsule, and the average linear density of the fiber is increased along with the increase of the content of the medicinal ink, so that the fiber has better fiber forming effect.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The medicinal ink phase change microcapsule fiber is characterized by comprising the following raw materials in parts by weight: pine smoke medicinal ink powder, alkane phase-change paraffin, phase-change microcapsule wall materials and polymer spinning solution.
2. The medicinal ink phase change microcapsule fiber as claimed in claim 1, wherein the alkane phase change paraffin is n-hexadecane or n-octadecane.
3. The drug-ink phase change microcapsule fiber of claim 1, wherein the phase change microcapsule wall material is polymethyl methacrylate or polyacrylonitrile.
4. The drug-ink phase change microcapsule fiber of claim 1, wherein the polymer spinning solution is 20-30% by weight of polyethylene terephthalate.
5. A preparation method of a medicinal ink phase-change microcapsule fiber is characterized by comprising the following steps:
1) pine smoke medicinal ink powder and alkane phase-change paraffin are combined together to be used as core materials, and the phase-change microcapsules are prepared by an emulsion polymerization method.
2) Which is then added to the polymer dope.
3) The medicinal ink phase-change microcapsule fiber is prepared by adopting a wet spinning process.
6. The preparation method of the medicinal ink phase-change microcapsule fiber according to claim 5, which comprises the preparation of medicinal ink/paraffin microcapsules and the preparation of fiber, wherein the preparation process of the phase-change microcapsule comprises the following steps: step 1) adding pine smoke medicinal ink into distilled water to prepare medicinal ink suspension, and then adding the medicinal ink suspension, a surfactant, a thickening agent and the distilled water into a beaker according to a certain proportion; step 2) adding the alkane phase-change paraffin and the microcapsule wall material into the solution obtained in the step 1), placing the beaker in a constant-temperature water bath, and continuously stirring the mixture by using a stirrer to uniformly disperse the mixture; step 3), adding an emulsifier, absolute ethyl alcohol and deionized water, uniformly stirring the mixture, and dispersing the mixture by using ultrasound to form stable emulsion; step 4) placing the emulsion obtained in the step 3) in a constant-temperature water bath, stirring for 1.5h, then dropwise adding an ammonia water solution to adjust the pH value of the solution to 8-9, stirring at constant temperature until the reaction is finished, and then standing at room temperature for 24h to fully solidify the capsule wall; and 5) finally, pouring out the supernatant in the solution after standing, adding absolute ethyl alcohol into the precipitate, centrifuging, repeating the steps for three times, cleaning the precipitate, and drying to obtain the medicinal ink paraffin microcapsule.
7. The preparation method of the medicinal ink phase change microcapsule fiber according to claim 6, wherein the preparation steps of the fiber are as follows: step 1) adding the prepared pine smoke medicinal ink microcapsules into a polymer spinning solution, and uniformly distributing the medicinal ink microcapsules in the solution by an ultrasonic machine; step 2) stirring the spinning solution obtained in the step 1) in a constant-temperature water bath by adopting a stirrer to defoam the spinning solution to obtain a medicinal ink spinning solution; and 3) pouring the spinning solution into a stainless steel storage tank, pushing the spinning solution to a spinneret orifice by a metering pump under the action of nitrogen, spraying the spinning solution out, then entering a coagulating bath and a drafting bath, and performing post-treatment to obtain the medicinal ink phase change microcapsule fiber.
8. The method for preparing the medicinal ink phase-change microcapsule fiber as claimed in claim 6, wherein the surfactant is Sodium Dodecyl Sulfate (SDS), the thickener is polyvinyl alcohol, the emulsifier is styrene maleic anhydride copolymer (SMA), sodium dodecyl sulfate or cetyl trimethyl sodium bromide, and the mass ratio of the pine smoke medicinal ink to the distilled water is 1: 2-5, the preparation concentration is 0.2-0.5 g/ml, and the ratio of the medicinal ink suspension, the surfactant, the thickening liquid and the distilled water is 5:1:1: 10.
9. The preparation method of the drug-ink phase-change microcapsule fiber according to claim 7, wherein the core material and wall material solution is placed in a constant temperature water bath kettle, the temperature is 60-80 ℃, the stirring speed of a stirrer is 700-1000 r/min, the ultrasonic time of the solution is 15-30 min, the temperature of the constant temperature water bath kettle in which the emulsion is located is 90-120 ℃, and the mass ratio of the drug-ink phase-change microcapsule to the polymer is 1: 5-8, the method comprises the following steps: the ultrasonic time is 15-20 min, the temperature of the constant-temperature water bath is 80-100 ℃, the stirring time is 30-60 min, and the nitrogen pressure is 0.2 mpa.
10. The method for preparing the medicated ink phase-change microcapsule fiber according to claim 7, wherein the coagulation bath is 7% BaCl2, the drawing bath is 3% BaCl 2; the speed ratio of the two yarn guide rollers in the drafting bath is 1: 2-5, and the post-treatment is to place the fiber subjected to the drawing bath in a glycerol aqueous solution for soaking treatment and then dry the fiber, wherein the mass fraction of the glycerol aqueous solution is 2%.
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Application publication date: 20211217 |