CN115304904B - Aging-resistant high-resilience earphone neck hanging wire and preparation method thereof - Google Patents
Aging-resistant high-resilience earphone neck hanging wire and preparation method thereof Download PDFInfo
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- 238000002844 melting Methods 0.000 claims abstract description 37
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 21
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 18
- 229920001577 copolymer Polymers 0.000 claims abstract description 17
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims abstract description 15
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims abstract description 15
- 229920001971 elastomer Polymers 0.000 claims abstract description 14
- 239000003921 oil Substances 0.000 claims abstract description 14
- 239000000806 elastomer Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- 239000010936 titanium Substances 0.000 claims abstract description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 52
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 47
- 239000004917 carbon fiber Substances 0.000 claims description 47
- 239000000463 material Substances 0.000 claims description 35
- 239000000725 suspension Substances 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000376 reactant Substances 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- 239000012768 molten material Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001746 injection moulding Methods 0.000 claims description 7
- 238000009832 plasma treatment Methods 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000002715 modification method Methods 0.000 claims description 2
- 210000004243 sweat Anatomy 0.000 abstract description 24
- 239000002537 cosmetic Substances 0.000 abstract description 20
- 210000002381 plasma Anatomy 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 17
- 238000012360 testing method Methods 0.000 description 16
- 238000005336 cracking Methods 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
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- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 229920001875 Ebonite Polymers 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000289 melt material Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
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- 239000000543 intermediate Substances 0.000 description 1
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- 239000006060 molten glass Substances 0.000 description 1
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- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
Abstract
The application relates to the technical field of composite materials, and particularly discloses an aging-resistant high-resilience earphone neck hanging wire and a preparation method thereof. The utility model provides an ageing-resistant high resilience earphone string neck line, its includes string neck frame, control area, string neck frame includes following raw materials by weight: 20-30 parts of thermoplastic polyurethane elastomer, 25-40 parts of naphthenic oil, 10-15 parts of organic silicon copolymer, 10-15 parts of ethylene propylene diene monomer, 15-20 parts of isobutyl triethoxysilane and 2-4 parts of anti-aging agent; the anti-aging agent is a composite anti-aging agent synthesized by taking low-melting glass powder as a carrier and titanium tetrachloride as a titanium source. The earphone neck hanging wire obtained by the application is excellent in artificial sweat resistance, cosmetics resistance and aging resistance.
Description
Technical Field
The application relates to the technical field of composite materials, in particular to an aging-resistant high-resilience earphone neck hanging wire and a preparation method thereof.
Background
The existing Bluetooth earphone is divided into a wired type and a wireless type, the two wired type Bluetooth earphone are connected through a cable, and the existing wireless Bluetooth earphone mainly comprises an in-ear type Bluetooth earphone, a head-wearing type Bluetooth earphone, a neck-hanging type Bluetooth earphone and the like; the Bluetooth headset is more and more popular with users because of convenient use and wearing.
The structure of the neck hanging type Bluetooth headset comprises a neck hanging frame and a control area, wherein the neck hanging frame is hung on the neck, and is made of elastic soft rubber materials such as TPU materials; the control area is connected to the neck hanging frame, is made of hard rubber, and is provided with a wire control and a battery box.
The neck hanging frame is easy to age under the influence of sweat stain, cosmetics, ultraviolet rays, high temperature and other factors, and can generate the phenomena of cracking, blushing, hair oil and the like, thereby influencing normal use.
Disclosure of Invention
In order to improve the ageing resistance effect of the earphone neck hanging wire, the application provides an ageing-resistant high-resilience earphone neck hanging wire and a preparation method thereof.
In a first aspect, the application provides an aging-resistant high-resilience earphone neck hanging wire and a preparation method thereof, and the following technical scheme is adopted:
the utility model provides an ageing-resistant high resilience earphone string neck line, its includes string neck frame, control area, string neck frame includes following raw materials by weight: 20-30 parts of thermoplastic polyurethane elastomer, 25-40 parts of naphthenic oil, 10-15 parts of organic silicon copolymer, 10-15 parts of ethylene propylene diene monomer, 15-20 parts of isobutyl triethoxysilane and 2-4 parts of anti-aging agent;
the anti-aging agent is a composite anti-aging agent synthesized by taking low-melting glass powder as a carrier and titanium tetrachloride as a titanium source.
By adopting the technical scheme, the thermoplastic polyurethane elastomer has good compatibility with the organic silicon copolymer, and the thermoplastic polyurethane elastomer and the organic silicon copolymer cooperate with naphthenic oil to ensure the higher tearing strength of the material, simultaneously provide the silky touch feeling of the material, and improve the waterproof and sweat pollution resistance of the material. The ethylene propylene diene monomer has good elasticity and compression deformation resistance, weather resistance, aging resistance, ozone resistance and chemical resistance, and the elasticity and the aging resistance of the material are improved by adding the ethylene propylene diene monomer. The addition of the isobutyl triethoxy silicon improves the ultraviolet ray resistance and sweat stain resistance of the material and the capacity of cosmetics.
The low-temperature molten glass powder is an inorganic nonmetallic material which is nontoxic, odorless and pollution-free, has the excellent performances of good temperature resistance, acid and alkali corrosion resistance, poor thermal conductivity, high insulation, low expansion, stable chemical property, large hardness and the like, is not easy to react with other substances, does not react with most of acid and alkali, and effectively improves the ultraviolet ray resistance, sweat stain resistance and cosmetic damage resistance of the material.
The composite anti-aging agent is synthesized by taking low-melting glass powder as a carrier titanium tetrachloride as a titanium source, the surface of the anti-aging agent is formed by arranging numerous tiny titanium oxide particles, and the titanium oxide nano particles are orderly arranged to avoid a large amount of agglomeration, so that the composite anti-aging agent has larger specific surface area and active reaction sites, can absorb and reflect ultraviolet light in a very wide wave band, scatter the ultraviolet light in all directions, greatly improve the shielding effect of the material on the ultraviolet light, and improve the anti-aging capability of the material.
Preferably, the preparation method of the composite anti-aging agent comprises the following steps:
1) Soaking low-melting glass powder in 20-25wt% sodium hydroxide solution, heating to 40-45 ℃, stirring and soaking for 1-2h, filtering and washing until the pH value is 7, then soaking the treated low-melting glass powder in 10-15wt% hydrochloric acid solution, stirring and soaking for 1-2h at 23-27 ℃, filtering and washing until the pH value is 7, and drying to obtain pretreated low-melting glass powder;
2) Adding the pretreated low-melting-point glass powder into water to prepare a low-melting-point glass powder suspension, heating the low-melting-point glass powder suspension to 50-55 ℃ and keeping the temperature unchanged, and then dropwise adding 10-15 wt/percent hydrochloric acid to enable the pH value of the low-melting-point glass powder suspension to be 5-6, wherein the ratio of the low-melting-point glass powder to the water is 300-400ml corresponding to 1g of the low-melting-point glass powder; dropwise adding titanium tetrachloride absolute ethyl alcohol solution into the low-melting glass powder suspension, maintaining the pH and the temperature of the suspension unchanged until the dropwise adding of the titanium tetrachloride absolute ethyl alcohol solution is completed, and keeping the temperature and the pH of the system for continuous reaction for 1h after the dropwise adding is completed; and (3) after the reactant is cooled to room temperature, washing the reactant to be neutral, drying the reactant at 100-120 ℃ for 10-12h, and finally roasting the reactant at 500-550 ℃ for 2h to obtain the composite anti-aging agent.
By adopting the technical scheme, the acid-base pretreatment is firstly carried out on the low-melting glass powder, the roughness of the low-melting glass powder is improved, convenient conditions are provided for the loading of titanium oxide particles, and then titanium tetrachloride is dripped, so that the titanium oxide particles are orderly and tightly arranged on the low-melting glass powder, an inorganic nano composite anti-aging agent is obtained, and the ultraviolet resistance effect of the inorganic nano composite anti-aging agent is greatly improved; meanwhile, the dispersibility of the low-melting-point glass powder in the organic matrix is improved, the bonding strength of the low-melting-point glass powder and the organic matrix is improved, and the ageing resistance of the material is further improved.
The treatment temperature, treatment time, solution concentration, etc. may be any value within the limits defined herein, such as 20-25 wt/wt% sodium hydroxide solution, 20 wt/wt% sodium hydroxide solution, 22 wt/wt% sodium hydroxide solution, 25 wt/wt% sodium hydroxide solution, etc.
Preferably, the particle size of the low melting point glass powder is 5-10 μm.
By adopting the technical scheme, the particle size of the low-melting-point glass powder is limited, so that the load of titanium oxide particles is ensured, the dispersion of the glass powder in an organic matrix and the bonding strength of the glass powder with the organic matrix are ensured, and the comprehensive properties such as ageing resistance, mechanical property and the like of the material are improved.
Preferably, the low-melting glass powder is subjected to surface modification treatment by a silane coupling agent.
By adopting the technical scheme, the silane coupling agent is used for carrying out surface treatment on the low-melting-point glass powder, so that the bonding strength of the glass powder and an organic matrix is improved, the cracking probability of the material under the actions of ultraviolet rays, sweat stains, cosmetics and the like is reduced, and the ageing resistance of the material is further improved.
Preferably, the neck hanging frame further comprises 5-7 parts by weight of carbon fibers.
Through adopting above-mentioned technical scheme, carbon fiber itself nature is stable, and is high to sweat stain, cosmetic tolerance, adds the back of carbon fiber, and carbon fiber plays the effect of pulling in the material, reduces the material and takes place the probability of fracture under the effect such as ultraviolet ray, sweat stain, cosmetic, further improves the ageing resistance effect of material.
Preferably, the carbon fiber is modified carbon fiber, and the modification method comprises the following steps:
1) Pretreatment of
Sequentially ultrasonically treating the carbon fiber in absolute ethyl alcohol and water for 5-8min, and then drying at 60-65 ℃ to obtain pretreated carbon fiber;
2) Plasma treatment
Treating the carbon fiber obtained in the step 1) by using plasma jet, wherein the treatment time is 2-3min, and the condition parameters of the plasma jet are as follows: argon is used as reaction gas, the gas flow rate is 3L/min, the discharge voltage is 25kV, the current is 1mA, and the frequency is 10kHz; obtaining plasma-treated carbon fibers;
3) Acid treatment
Soaking the carbon fiber subjected to the plasma treatment obtained in the step 2) in 60-65wt% nitric acid for reaction for 80-90min, taking out and cleaning for 2-3 times, and drying to obtain the modified carbon fiber.
By adopting the technical scheme, the carbon fiber is cooperatively treated by using the plasmas and the acid oxidation, and the active sites and the oxygen-containing functional groups are introduced into the surface of the carbon fiber material, wherein the plasmas mainly play a role in activating the surface of the carbon fiber, and promote the contact of the carbon fiber with the acid solution so as to improve the acid oxidation efficiency; the roughness of the treated carbon fiber is improved, the hydrophilicity is enhanced, the bonding strength of the carbon fiber and an organic matrix is effectively improved, and the cracking resistance effect of the material is further improved, so that the ageing resistance is improved.
The treatment temperature, treatment time and the like can be any value in the limiting range of the application, such as 5-8min of ultrasound, 5min of ultrasound, 7min of ultrasound, 8min of ultrasound and the like.
Preferably, the silicone copolymer is a silicone and urethane copolymer.
By adopting the technical scheme, the organic silicon and carbamate copolymer is a thermoplastic material, and because the molecular chain of the organic silicon and carbamate copolymer contains more organic silicon units similar to silicon rubber, the organic silicon and carbamate copolymer has the characteristic of excellent touch and silky, and can endow the composite material with better silky touch through blending modification, and improve the body feel using effect of the neck hanging frame.
Preferably, the control region is a general-purpose or impact-resistant ABS material.
In a second aspect, the present application provides a method for manufacturing an aging-resistant high resilience earphone neck hanging wire, which adopts the following technical scheme:
a preparation method of an anti-aging high-resilience earphone neck hanging wire comprises the following steps:
s1, preparing molten materials of neck hanging frame
Uniformly mixing a thermoplastic polyurethane elastomer, naphthenic oil, a thermoplastic polyester elastomer, an organosilicon copolymer, ethylene propylene diene monomer rubber and isobutyl triethoxysilane according to parts by weight, then adding the rest raw materials, uniformly mixing, and melt blending at 200-220 ℃ to obtain a neck-hanging frame melt material;
s2, preparing a control area melting material
Melting the ABS material at 180-240 ℃ to obtain a control region melting material;
s3, injection molding
And (3) carrying out injection molding on the molten material of the neck hanging frame obtained in the step (S1) and the molten material of the control area obtained in the step (S2) to obtain the earphone neck hanging line.
By adopting the technical scheme, the preparation method is simple and easy to operate, has no special requirement on production equipment, and is suitable for industrial production.
In summary, the present application has the following beneficial effects:
1. the thermoplastic polyurethane elastomer, naphthenic oil, the organosilicon copolymer, ethylene propylene diene monomer and isobutyl triethoxysilane are compounded to serve as an organic matrix, and the composite anti-aging agent synthesized by taking low-melting glass powder as a carrier titanium tetrachloride as a titanium source is matched to prepare the neck hanging frame of the earphone neck hanging wire, so that the artificial sweat resistance, the cosmetic resistance and the aging resistance of the earphone neck hanging wire are improved.
2. In the application, the carbon fiber is preferably added and modified, so that the artificial sweat resistance, the cosmetic resistance and the ageing resistance of the neck line are further improved.
Detailed Description
The present application is described in further detail below with reference to examples.
Preparation examples of starting materials and intermediates
Raw materials
The raw materials of the examples of the present application can be obtained commercially:
the thermoplastic polyurethane elastomer is German Bayer injection molding TPU with the brand of 9392AU;
the naphthenic oil is analytically pure;
the organosilicon copolymer is an organosilicon and carbamate copolymer, wherein the proportion of organosilicon monomers is 65%;
the silane coupling agent is a silane coupling agent KH550;
the length of the carbon fiber is 10-15 mu m;
the ABS material is impact resistant.
Preparation example
Preparation example I-1
A silane coupling agent modified low-melting-point glass powder is prepared by the following steps:
and (3) soaking the low-melting-point glass powder in a silane coupling agent solution for 10min, fishing out, and drying at 60 ℃ for 1h to obtain the silane coupling agent modified low-melting-point glass powder.
Preparation example II-1
A preparation method of the composite anti-aging agent comprises the following steps:
1) Soaking low-melting-point glass powder with the particle size of 5-10 mu m in 25 wt/percent sodium hydroxide solution, heating to 40 ℃, stirring and soaking for 1.5 hours, filtering and washing until the pH value is 7, then soaking the treated low-melting-point glass powder in 10 wt/percent hydrochloric acid solution, stirring and soaking for 1.5 hours at 25 ℃, filtering and washing until the pH value is 7, and drying to obtain pretreated low-melting-point glass powder;
2) Taking 100g of pretreated low-melting-point glass powder, adding 40L of water to prepare low-melting-point glass powder suspension, heating the low-melting-point glass powder suspension to 50 ℃ and keeping the temperature unchanged, and then dropwise adding 10-wt/% hydrochloric acid to enable the pH value of the low-melting-point glass powder suspension to be 5; dropwise adding titanium tetrachloride absolute ethyl alcohol solution into the low-melting glass powder suspension, maintaining the pH and the temperature of the suspension unchanged, dropwise adding the titanium tetrachloride absolute ethyl alcohol solution for 20min, and keeping the temperature and the pH of the system for continuous reaction for 1h after the dropwise adding is completed; and after the reactant is cooled to room temperature, washing the reactant to be neutral, drying the reactant at 100 ℃ for 12 hours, and finally roasting the reactant at 500 ℃ for 2 hours to obtain the composite anti-aging agent.
Preparation example II-2
A preparation method of the composite anti-aging agent comprises the following steps:
1) Soaking low-melting-point glass powder with the particle size of 5-10 mu m in 25 wt/percent sodium hydroxide solution, heating to 40 ℃, stirring and soaking for 3 hours, filtering and washing until the pH value is 7, and drying to obtain pretreated low-melting-point glass powder;
2) Taking 100g of pretreated low-melting-point glass powder, adding 40L of water to prepare low-melting-point glass powder suspension, heating the low-melting-point glass powder suspension to 50 ℃ and keeping the temperature unchanged, and then dropwise adding 10-wt/% hydrochloric acid to enable the pH value of the low-melting-point glass powder suspension to be 5; dropwise adding titanium tetrachloride absolute ethyl alcohol solution into the low-melting glass powder suspension, maintaining the pH and the temperature of the suspension unchanged, dropwise adding the titanium tetrachloride absolute ethyl alcohol solution for 20min, and keeping the temperature and the pH of the system for continuous reaction for 1h after the dropwise adding is completed; and after the reactant is cooled to room temperature, washing the reactant to be neutral, drying the reactant at 100 ℃ for 12 hours, and finally roasting the reactant at 500 ℃ for 2 hours to obtain the composite anti-aging agent.
Preparation example II-3
A preparation method of the composite anti-aging agent comprises the following steps:
1) Soaking low-melting-point glass powder with the particle size of 5-10 mu m in a 10 wt/percent hydrochloric acid solution, stirring and soaking for 3 hours at 25 ℃, filtering and washing until the pH value is 7, and drying to obtain pretreated low-melting-point glass powder;
2) Taking 100g of pretreated low-melting-point glass powder, adding 40L of water to prepare low-melting-point glass powder suspension, heating the low-melting-point glass powder suspension to 50 ℃ and keeping the temperature unchanged, and then dropwise adding 10-wt/% hydrochloric acid to enable the pH value of the low-melting-point glass powder suspension to be 5; dropwise adding titanium tetrachloride absolute ethyl alcohol solution into the low-melting glass powder suspension, maintaining the pH and the temperature of the suspension unchanged, dropwise adding the titanium tetrachloride absolute ethyl alcohol solution for 20min, and keeping the temperature and the pH of the system for continuous reaction for 1h after the dropwise adding is completed; and after the reactant is cooled to room temperature, washing the reactant to be neutral, drying the reactant at 100 ℃ for 12 hours, and finally roasting the reactant at 500 ℃ for 2 hours to obtain the composite anti-aging agent.
Preparation example II-4
A preparation method of the composite anti-aging agent comprises the following steps:
taking 100g of low-melting-point glass powder with the particle size of 5-10 mu m, adding the low-melting-point glass powder into 40L of water to prepare low-melting-point glass powder suspension, heating the low-melting-point glass powder suspension to 50 ℃ and keeping the temperature unchanged, and then dropwise adding 10-wt/% hydrochloric acid to enable the pH value of the low-melting-point glass powder suspension to be 5; dropwise adding titanium tetrachloride absolute ethyl alcohol solution into the low-melting glass powder suspension, maintaining the pH and the temperature of the suspension unchanged, dropwise adding the titanium tetrachloride absolute ethyl alcohol solution for 20min, and keeping the temperature and the pH of the system for continuous reaction for 1h after the dropwise adding is completed; and after the reactant is cooled to room temperature, washing the reactant to be neutral, drying the reactant at 100 ℃ for 12 hours, and finally roasting the reactant at 500 ℃ for 2 hours to obtain the composite anti-aging agent.
Preparation example II-5
Unlike preparation II-1, the low melting point glass frit of preparation II-5 had a particle diameter of 10 to 13. Mu.m.
Preparation example II-6
Unlike preparation II-1, preparation II-6 had melting point glass frit derived from preparation I-1.
Preparation example III-1
A modified carbon fiber is prepared by the following steps:
1) Pretreatment of
Sequentially carrying out ultrasonic treatment on the carbon fiber in absolute ethyl alcohol and water for 6min, and then drying at 60 ℃ for 30min to obtain pretreated carbon fiber;
2) Plasma treatment
Treating the carbon fiber obtained in the step 1) by using plasma jet, introducing argon into a cavity of normal pressure plasma equipment as reaction gas, wherein the gas flow rate is 3L/min, the discharge voltage is 25kV, the current is 1mA, the frequency is 10kHz, igniting plasma to perform pre-discharge for 10min, adjusting the plasma discharge parameters and the position of a sample plate, after the discharge is stable, placing the carbon fiber obtained in the step 1) on the sample plate at the position of a plasma nozzle for fixing, and treating for 2min under the atmospheric pressure plasma jet to obtain the carbon fiber treated by the plasma;
3) Acid treatment
Soaking the carbon fiber subjected to the plasma treatment obtained in the step 2) in 60 wt/percent nitric acid for reaction for 90min, taking out, washing with water for 3 times, and drying at 60 ℃ for 30min to obtain the modified carbon fiber.
Preparation example III-2
A modified carbon fiber is prepared by the following steps:
1) Pretreatment of
Sequentially carrying out ultrasonic treatment on the carbon fiber in absolute ethyl alcohol and water for 6min, and then drying at 60 ℃ for 30min to obtain pretreated carbon fiber;
2) Plasma treatment
And (3) treating the carbon fiber obtained in the step (1) by using plasma jet, introducing argon into a cavity of normal pressure plasma equipment as reaction gas, wherein the gas flow rate is 3L/min, the discharge voltage is 25kV, the current is 1mA, the frequency is 10kHz, igniting plasma to perform pre-discharge for 10min, adjusting the plasma discharge parameters and the position of a sample plate, after discharge is stable, placing the carbon fiber obtained in the step (1) on the sample plate at the position of a plasma nozzle for fixing, and treating for 2min under the atmospheric pressure plasma jet to obtain the plasma treated carbon fiber, namely the modified carbon fiber.
Preparation example III-3
A modified carbon fiber is prepared by the following steps:
1) Pretreatment of
Sequentially carrying out ultrasonic treatment on the carbon fiber in absolute ethyl alcohol and water for 6min, and then drying at 60 ℃ for 30min to obtain pretreated carbon fiber;
2) Acid treatment
And (3) soaking the pretreated carbon fiber in 60 wt/percent nitric acid for reaction for 90min, taking out, washing with water for 3 times, and drying at 60 ℃ for 30min to obtain the modified carbon fiber.
Examples
Examples 1 to 6
The utility model provides an ageing-resistant high resilience earphone string neck line, includes string neck frame, control area, and its preparation method is:
s1, preparing molten materials of neck hanging frame
According to the proportion in the table 1, thermoplastic polyurethane elastomer, naphthenic oil, organic silicon copolymer, ethylene propylene diene monomer and isobutyl triethoxysilane are uniformly mixed, then inorganic anti-aging agent and carbon fiber are added to be uniformly mixed, and melt blending is carried out under the condition of 200 ℃ to obtain a neck-hanging frame melt material;
s2, preparing a control area melting material
Melting an ABS material at 220 ℃ to obtain a control region melting material;
s3, injection molding
And (3) carrying out injection molding on the molten material of the neck hanging frame obtained in the step (S1) and the molten material of the control area obtained in the step (S2) to obtain the earphone neck hanging line.
Table 1 examples 1-6 raw materials proportioning Table (kg)
Wherein the anti-aging agent is derived from preparation II-1.
Examples 7 to 11
In contrast to example 5, the anti-aging agents of examples 7 to 11 are derived from preparation examples II-2 to II-6, respectively
Examples 12 to 14
Unlike example 11, the carbon fibers in examples 12 to 14 were modified carbon fibers modified in preparation examples III-1 to III-3, respectively.
Comparative example
Comparative example 1
Unlike example 1, the silicone copolymer was replaced with an equivalent amount of thermoplastic polyurethane elastomer in comparative example 1.
Comparative example 2
Unlike example 1, the naphthenic oil was replaced with an equal amount of thermoplastic polyurethane elastomer in comparative example 2.
Comparative example 3
Unlike example 1, the same amount of thermoplastic polyurethane elastomer was used in comparative example 3 instead of isobutyl triethoxysilane.
Comparative example 4
Unlike example 1, the aging inhibitor in comparative example 4 was titanium oxide.
Comparative example 5
Unlike example 1, the anti-aging agent in comparative example 4 was UV622.
Performance test
Detection method/test method
The following performance tests were performed on the products of examples 1 to 14 and comparative examples 1 to 5:
test for artificial sweat resistance: test environment: 35 ℃,75% rh, test method: soaking filter paper in artificial sweat, and filtering with adhesive tapeThe paper was stuck on the surface of the neck frame and ensured that the test paper was in full contact with the surface of the product, and then placed in the test environment, after 72 hours, the sample was taken out of the test environment and after 2 hours of placement, the product was inspected and scored according to the criteria of table 2: scoring by 30 professionals and taking an average value; a sweat formulation; artificial sweat test: solution component (1)clean drinking water,100g, (2) Na 2 HPO 4 ·12H 2 O,5g, (3) NaCl,5g, (4)Acetic Acid glacial,2g; the solution was mixed and placed in a 45 ℃ test chamber for 24 hours.
Cosmetic resistance test: smearing vaseline at the neck hanging frame, heating to 35deg.C, standing for 72H at 75% humidity, cooling to room temperature, waiting for 2H, and wiping with dust-free cloth; after testing the products were checked and scored according to the criteria of table 2: the average was scored by 30 professionals.
Aging test: the samples were baked at 120 ℃ for 3 days and then at 60 ℃ for 1 day, with the aid of uv light during baking, the products were inspected and scored according to the criteria of table 3: the average was scored by 30 professionals.
The results of the performance tests are shown in Table 4.
TABLE 2 Artificial sweat resistance and cosmetic scoring criteria
| Product status | Score of |
| The surface has no color change, peeling, falling off, fading and cracking | 90-100 |
| The surface has slight color change, peeling, falling off, fading and cracking | 60-80 |
| The surface has obvious color change, peeling, falling off, fading and cracking | 0-50 |
TABLE 3 anti-aging scoring criteria
| Product status | Score of |
| No blushing, oil and cracking on the surface | 90-100 |
| The surface has slight blushing, hair oil and cracking | 60-80 |
| The surface has obvious blushing, oiling and cracking | 0-50 |
TABLE 4 Performance test results
As can be seen by combining examples 1-14 and comparative examples 1-5 and combining Table 4, the products in examples 1-14 have higher scores for artificial sweat resistance, cosmetic resistance and aging resistance than those in comparative examples 1-5, which indicates that the artificial sweat resistance, cosmetic resistance and aging resistance of the earphone neck strap prepared by the method are better.
As can be seen from the combination of examples 1 and comparative examples 1 to 3 and Table 4, the raw materials in comparative examples 1 to 3 lack the silicone copolymer, naphthenic oil, and isobutyl triethoxysilane, respectively, and the scores of artificial sweat resistance, cosmetic resistance, and aging resistance in comparative examples 1 to 3 are reduced compared with those in example 1, probably because the raw materials in the present application are mutually matched, and the aging resistance of the earphone neck line is improved.
By combining the embodiment 2 with the embodiment 4-6 and combining the table 4, it can be seen that the product in the embodiment 4-6 has higher scores of artificial sweat resistance, cosmetic resistance and aging resistance than the product in the embodiment 2, which indicates that the addition of carbon fiber can further improve the artificial sweat resistance, cosmetic resistance and aging resistance of the earphone neck line.
By combining the embodiment 5 with the embodiment 7-10 and combining the table 4, the scores of the product in the embodiment 5 for resisting artificial sweat, cosmetics and aging are higher than those in the embodiment 7-10, which shows that the roughness of the low-melting glass powder can be improved by carrying out acid-base pretreatment on the low-melting glass powder, and a convenient condition is provided for loading the titanium oxide particles, so that the titanium oxide particles are orderly and tightly arranged on the low-melting glass powder, and the ultraviolet resistance effect of the titanium oxide particles is greatly improved; meanwhile, the dispersibility of the low-melting-point glass powder in the organic matrix is improved, the bonding strength of the low-melting-point glass powder and the organic matrix is improved, and the artificial sweat resistance, the cosmetic resistance and the ageing resistance of the material are further improved.
As can be seen by combining examples 11-14 and Table 4, the products in examples 12-13 have higher scores for artificial sweat resistance, cosmetic resistance and aging resistance than those in example 11, which shows that the plasma and acid oxidation synergistic treatment can be used for carbon fiber, active sites and oxygen-containing functional groups are introduced into the surface of the carbon fiber material, the roughness of the carbon fiber is improved, the hydrophilicity is enhanced, the bonding strength of the carbon fiber and an organic matrix is effectively improved, and the cracking resistance of the material is further improved, so that the artificial sweat resistance, the cosmetic resistance and the aging resistance are improved.
The headphone neck strap in examples 1 to 14 was subjected to a headphone expansion test: putting hardware on the head hard rubber sleeve, stretching for 30cm, and then recovering to the original shape to be a cycle, and testing 10000 times; standing for 2 hours after testing, and measuring the width of the head; the judgment standard is as follows: the change of the head wearing width is less than 20%, and the head wearing shape is unchanged; the soft and hard glue can not be separated, and the gap can be automatically recovered. The earphone neck line tests in examples 1-14 were all acceptable.
The earphone neck line in examples 1-14 was subjected to a two shot product bonding force test: measuring the binding force of soft and hard glue, fixing the hard glue of a product, and hanging 3.5kg of the software part for 1min; all four directions are tested; the judgment standard is as follows: the soft and hard glue can not be separated, and the gap can be automatically recovered. The earphone neck line tests in examples 1-14 were all acceptable.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (6)
1. The utility model provides an ageing-resistant high resilience earphone string neck line, its includes string neck frame, control area, its characterized in that, string neck frame includes following raw materials by weight: 20-30 parts of thermoplastic polyurethane elastomer, 25-40 parts of naphthenic oil, 10-15 parts of organic silicon copolymer, 10-15 parts of ethylene propylene diene monomer, 15-20 parts of isobutyl triethoxysilane and 2-4 parts of anti-aging agent; 5-7 parts of carbon fiber;
the carbon fiber is modified carbon fiber, and the modification method comprises the following steps:
1) Pretreatment of
Sequentially ultrasonically treating the carbon fiber in absolute ethyl alcohol and water for 5-8min, and then drying at 60-65 ℃ to obtain pretreated carbon fiber;
2) Plasma treatment
Treating the carbon fiber obtained in the step 1) by using plasma jet, wherein the treatment time is 2-3min, and the condition parameters of the plasma jet are as follows: argon is used as reaction gas, the gas flow rate is 3L/min, the discharge voltage is 25kV, the current is 1mA, and the frequency is 10kHz; obtaining plasma-treated carbon fibers;
3) Acid treatment
Soaking the carbon fiber subjected to the plasma treatment obtained in the step 2) in 60-65wt/% nitric acid for reaction for 80-90min, taking out and cleaning for 2-3 times, and drying to obtain modified carbon fiber;
the anti-aging agent is a composite anti-aging agent synthesized by taking low-melting glass powder as a carrier and titanium tetrachloride as a titanium source;
the preparation method of the composite anti-aging agent comprises the following steps:
1) Soaking low-melting glass powder in 20-25wt% sodium hydroxide solution, heating to 40-45 ℃, stirring and soaking for 1-2h, filtering and washing until the pH value is 7, then soaking the treated low-melting glass powder in 10-15wt% hydrochloric acid solution, stirring and soaking for 1-2h at 23-27 ℃, filtering and washing until the pH value is 7, and drying to obtain pretreated low-melting glass powder;
2) Adding the pretreated low-melting-point glass powder into water to prepare a low-melting-point glass powder suspension, heating the low-melting-point glass powder suspension to 50-55 ℃ with 300-400ml of water corresponding to 1g of low-melting-point glass powder, and then dropwise adding 10-15wt/% hydrochloric acid to enable the p H value of the low-melting-point glass powder suspension to be 5-6; dropwise adding titanium tetrachloride absolute ethyl alcohol solution into the low-melting glass powder suspension, maintaining the pH and the temperature of the suspension unchanged until the dropwise adding of the titanium tetrachloride absolute ethyl alcohol solution is completed, and keeping the temperature and the pH of the system for continuous reaction for 1h after the dropwise adding is completed; and (3) after the reactant is cooled to room temperature, washing the reactant to be neutral, drying the reactant at 100-120 ℃ for 10-12h, and finally roasting the reactant at 500-550 ℃ for 2h to obtain the composite anti-aging agent.
2. The aging-resistant high resilience earphone neck strap of claim 1, wherein: the particle size of the low-melting glass powder is 5-10 mu m.
3. The aging-resistant high resilience earphone neck strap of claim 2, wherein: the low-melting-point glass powder is subjected to surface modification treatment by a silane coupling agent.
4. The aging-resistant high resilience earphone neck strap of claim 1, wherein: the organosilicon copolymer is an organosilicon and carbamate copolymer.
5. The aging-resistant high resilience earphone neck strap of claim 1, wherein: the control area is a general-purpose or impact-resistant ABS material.
6. A method for manufacturing the aging-resistant high resilience earphone neck line according to any one of claims 1 to 5, comprising the following steps:
s1, preparing molten materials of neck hanging frame
Uniformly mixing a thermoplastic polyurethane elastomer, naphthenic oil, an organosilicon copolymer, ethylene propylene diene monomer and isobutyl triethoxysilane according to parts by weight, then adding the rest raw materials, uniformly mixing, and melt blending at 200-220 ℃ to obtain a neck-hanging frame melt;
s2, preparing a control area melting material
Melting the ABS material at 180-240 ℃ to obtain a control region melting material;
s3, injection molding
And (3) carrying out injection molding on the molten material of the neck hanging frame obtained in the step (S1) and the molten material of the control area obtained in the step (S2) to obtain the earphone neck hanging line.
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