CN109527702A - A kind of Antistatic shoe-pad and its production method - Google Patents
A kind of Antistatic shoe-pad and its production method Download PDFInfo
- Publication number
- CN109527702A CN109527702A CN201811272296.7A CN201811272296A CN109527702A CN 109527702 A CN109527702 A CN 109527702A CN 201811272296 A CN201811272296 A CN 201811272296A CN 109527702 A CN109527702 A CN 109527702A
- Authority
- CN
- China
- Prior art keywords
- parts
- layer
- polyurethane
- conductive
- component
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
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- 238000000034 method Methods 0.000 claims description 9
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- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 claims description 5
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- CWZPGMMKDANPKU-UHFFFAOYSA-L butyl-di(dodecanoyloxy)tin Chemical compound CCCC[Sn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O CWZPGMMKDANPKU-UHFFFAOYSA-L 0.000 claims 1
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 4
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Classifications
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- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B17/00—Insoles for insertion, e.g. footbeds or inlays, for attachment to the shoe after the upper has been joined
- A43B17/003—Insoles for insertion, e.g. footbeds or inlays, for attachment to the shoe after the upper has been joined characterised by the material
- A43B17/006—Insoles for insertion, e.g. footbeds or inlays, for attachment to the shoe after the upper has been joined characterised by the material multilayered
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
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- A—HUMAN NECESSITIES
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- A43B17/02—Insoles for insertion, e.g. footbeds or inlays, for attachment to the shoe after the upper has been joined wedge-like or resilient
-
- A—HUMAN NECESSITIES
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- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B17/00—Insoles for insertion, e.g. footbeds or inlays, for attachment to the shoe after the upper has been joined
- A43B17/10—Insoles for insertion, e.g. footbeds or inlays, for attachment to the shoe after the upper has been joined specially adapted for sweaty feet; waterproof
- A43B17/102—Moisture absorbing socks; Moisture dissipating socks
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
- B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2437/00—Clothing
- B32B2437/02—Gloves, shoes
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Ceramic Engineering (AREA)
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- Wood Science & Technology (AREA)
- Footwear And Its Accessory, Manufacturing Method And Apparatuses (AREA)
Abstract
The invention discloses a kind of Antistatic shoe-pad and its production methods, it is related to footwear, Antistatic shoe-pad includes the ox-hide surface layer contacted with people vola, the nylon sheath contacted with inner sole, layer of polyurethane is provided between the ox-hide surface layer and nylon sheath, the nylon sheath and layer of polyurethane all have static electricity resistance, are provided through conductive hole at the ox-hide surface layer half sole.The electrostatic of human body accumulation can be oriented to layer of polyurethane and nylon sheath with certain conductive capability from conductive hole, and then be oriented in the shoes used with insole collocation in bottom, be finally directed at the earth, play the role of preventing accumulation of static electricity.Layer of polyurethane has excellent flexibility and resilience, therefore the comfort of people's dress greatly improves;Ox-hide surface layer has stronger moisture absorbing and sweat releasing ability, it is not easy to lead to bacteria breed, and sufficiently flexible, long service life.
Description
Technical field
The present invention relates to shoes industry, in particular to a kind of Antistatic shoe-pad and its production method.
Background technique
Static electricity on human body's accumulation is excessive to be easy to cause damages to physical and mental health, such as: irritated, headache, insomnia, and be easy
Electronics Factory damages electronic component in workshop.Anti-static shoes are the protective footwears that can eliminate static electricity on human body's accumulation, are commonly used
In the workshop of microelectronics industry, pharmaceutical factory etc., the principle is as follows: antistatic agent being added when shoe sole production, makes it have
Faint conducting function, can be the extra charge guiding of human body greatly.Anti-static shoes are generally required arranges in pairs or groups with Antistatic shoe-pad
It uses.
Notification number is that the Chinese patent of CN202179193U discloses a kind of Antistatic shoe-pad, including bound edge face, suture,
Insole surfaces are sewed with conductive filament on the insole surfaces, contact it with the conductive nail of sole by the weight of human body.
Above-mentioned Antistatic shoe-pad is by the setting of conductive filament and conductive nail, can be with so that insole has certain electric conductivity
By the extra charge guiding sole of human body, the earth is finally flowed into.But conductive filament and conductive nail are generally metal material, have one
Determine hardness, the bradyseism of insole and flexibility are poor, wear not comfortable enough;In addition, conductive filament is exposed outside, and it is easy to oxidize, it influences
Electric conductivity.
Summary of the invention
In view of the above technical defects, the first object of the present invention is to provide a kind of Antistatic shoe-pad, have it is good prevent it is quiet
Electric effect and comfort.
To achieve the above object, the present invention provides the following technical scheme that
A kind of Antistatic shoe-pad, including the ox-hide surface layer contacted with people vola, the nylon sheath contacted with inner sole, the ox-hide
Layer of polyurethane is provided between surface layer and nylon sheath, the nylon sheath and layer of polyurethane all have static electricity resistance, the ox
Conductive hole is provided through at veneer half sole.
By using above-mentioned technical proposal, the electrostatic of human body accumulation can be oriented to from conductive hole has certain conductive capability
Layer of polyurethane and nylon sheath, and then be oriented to and in bottom, be finally directed at the earth, playing prevents in the shoes that use of insole collocation
The effect of accumulation of static electricity.Layer of polyurethane has excellent flexibility and resilience, therefore the comfort of people's dress greatly improves;
On the one hand ox-hide surface layer can play the role of preventing polyurethane aging and mechanical wear, on the other hand have stronger moisture absorption
Perspire ability, it is not easy to lead to bacteria breed, and sufficiently flexible, long service life;Nylon sheath is between layer of polyurethane and shoes
Between interior bottom, due to its high mechanical strength, good toughness, it can play the role of protecting layer of polyurethane, prevent layer of polyurethane and shoes
The relative movement of interior bottom and caused by wear.
The present invention is further arranged to: the layer of polyurethane is made by first component and second component reaction, the first group subpackage
Include the component of following parts by weight:
50-70 parts of polytetramethylene ether diol;
5-8 parts of ethylene glycol;
0.3-0.6 parts of catalyst;
0.5-1.5 parts of antistatic agent;
1-2 parts of water;
0.5-1 parts of silicone oil;
2-4 parts of conductive black, partial size 30nm;
3-6 parts of nano-conductive fiber;
0.5-1 parts of mould inhibitor;
The component B includes the component of following parts by weight:
20-25 parts of polytetramethylene ether diol;
45-60 parts of liquefied mdi.
By using above-mentioned technical proposal, antistatic agent, conductive black and conductive nano joined in layer of polyurethane component
Fiber, three can be improved the conductive capability of layer of polyurethane and there is synergistic effect.The wherein volume electricity of conductive black itself
Resistance rate is small, is natural semiconductor, can be with when the carbon black particle being scattered in polymer matrix body directly contacts or gap is minimum
The catenulate conductive path of shape, so that layer of polyurethane has certain conductive capability;The surface area of nano-conductive fiber is larger,
More multiparticle near point can be promoted to contact, therefore conductive black can form preferable network knot by the bridge joint of nano-conductive fiber
Structure, so that the enhancing of conductive connection property, improves the conductive capability of layer of polyurethane.
The present invention is further arranged to: for the conductive black by being modified, modifying process is as follows: 100-120 parts are led
Electric carbon black, 5-8 part silane coupling agent, 95% ethanol solution of 200-250 part uniformly mix, and stir low temperature drying 24- after 10-12H
28H。
By using above-mentioned technical proposal, when the partial size of conductive black reaches nanoscale, there are nano effect, electric conductivity
It can become more excellent, but conductive black is easy to reunite and be difficult to be dispersed in layer of polyurethane, conductive black between each other
Surface can solve after silane coupler modified is difficult to disperse this disadvantage.
The present invention is further arranged to: the preparation process of the nano-conductive fiber is as follows:
Step 1, pyrroles, DEHS are first pressed (2-3): 1 molar ratio mixes, and is re-dissolved in 20% ethanol solution, is stirred continuously and adds
The APS for entering 3%, stirs 12-24h after being cooled to -15 DEG C, be finally washed with distilled water suction filtration and obtain powder;
Powder is dissolved in dichloroacetic acid by step 2, is made into the spinning solution that mass fraction is 10-15%;
Aqueous nylon is added to the water, is heated to 55-60 DEG C by step 3, be stirred continuously until aqueous nylon be completely dissolved, continue
Stirring is until be cooled to room temperature to obtain the nylon solution that mass fraction is 15%;
Step 4, it is isometric to mix nylon solution and spinning solution, it finally carries out electrostatic spinning and obtains nano-conductive fiber, spinning
40 DEG C of temperature, spinning speed 0.5mL/h.
By using above-mentioned technical proposal, nano-conductive fiber is by the excellent mechanical property of nylon, heat resistance and poly- pyrrole
It coughs up excellent electric conductivity to be combined together, therefore nano-conductive fiber is as follows as that can play in filler addition layer of polyurethane
Effect: the mechanical properties such as layer of polyurethane tear-proof, wear-resisting, elastic improve;The electric conductivity of layer of polyurethane improves, anti-static effect
It is good.
The present invention is further arranged to: the preparation process of the antistatic agent is as follows:
4-6 parts of chlorinated dodecanes are dissolved in 50-60 parts of dehydrated alcohols by the first step, are stirred continuously and are heated to 70-80 DEG C, then plus
Enter 1-3 parts of diethanol amine, be stirring evenly and then adding into 0.5-1 parts of sodium hydroxide powders, be warming up to 90-100 DEG C, reacts 4-6h, mention
It is pure obtain crude product after be evaporated under reduced pressure, obtain product A;
12-15 parts of diethanol amine and 12-15 parts of succinic anhydrides are dissolved in DMAC by second step respectively, then again that diethanol amine is molten
Liquid is heated to 30-35 DEG C for use, is then slowly added to succinic anhydride solution, and rate control is added in 40-50min, 25 DEG C of reactions
3h obtains product B;
Product A is added in product B, is mixed evenly by third step, adds 50-60 parts of toluene, 0.1-0.3 parts of toluene
Sulfonic acid is stirred continuously and is heated to 50-60 DEG C, and reaction 3-5h is finally evaporated under reduced pressure and obtains product C;
Product C is dissolved in DMAC, is passed through nitrogen protection by the 4th step, adds 1-2 parts of sodium hydroxides, 5-6 parts of epoxy chloropropionates
Alkane is warming up to 70-80 DEG C of reaction 4-5h, takes filtrate to obtain product D after suction filtration;
5th step, product D are warming up to 40-50 DEG C in the case where being passed through nitrogen protection, and 2-4 parts of triethylamines are added, and react 5-7h,
Vacuum distillation removes solvent, finally dries 12-24h at 30-35 DEG C, obtains antistatic agent.
By using above-mentioned technical proposal, antistatic agent is other than the conductivity that can be improved layer of polyurethane, relative to biography
It unites for antistatic agent, the compatibility and stability between layer of polyurethane are very excellent, therefore layer of polyurethane is with good
Good water-wash resistance, will not be such that conductivity declines because of repeated multiple times washing.
The present invention is further arranged to: the first component further includes 1-3 parts of sisal fibers.
By using above-mentioned technical proposal, sisal fiber is added as filler, on the one hand can be improved the tough of layer of polyurethane
The mechanical properties such as property, elasticity and the chemical properties such as corrosion-resistant;Another aspect sisal fiber can reduce conductive black, nanometer is led
The percolation threshold of electric fiber, so that layer of polyurethane has more excellent electric conductivity.
The present invention is further arranged to: the catalyst is the dibutyltin dilaurate and three second of equal mass mixings
Amine.
The second object of the present invention is to provide a kind of production method of Antistatic shoe-pad.
A kind of production method of Antistatic shoe-pad, comprising the following steps:
S1 ox-hide surface layer: natural Kraft fabric is cut into the ox-hide surface layer of required shape by the size of design drawing, is connect
At ox-hide surface layer half sole punching and form conductive hole;
S2 nylon sheath: Antistatic Nylon film is cut into the nylon sheath of required shape by the size of design drawing;
S3 layer of polyurethane first component: by 50-70 parts of polytetramethylene ether diols, 5-8 parts of ethylene glycol, 0.3-0.6 catalyst, 0.5-
1.5 parts of antistatic agents, 1-2 parts of water, 0.5-1 parts of silicone oil, 2-4 parts of conductive blacks, 3-6 parts of nano-conductive fibers, 0.5-1 parts it is mould proof
Agent is mixed and stirred for uniformly, being preheated to 50-60 DEG C for use;
S4 layer of polyurethane component B: taking 45-60 parts of liquefied mdis, be warming up to 50-55 DEG C, adds 20-25 parts of polytetramethylene ethers
Glycol, quickly stirring makes it heat up naturally, and 80-90 DEG C is heated to when temperature is constant, vacuumizes 30-60min after reacting 2-3h,
Finally it is cooled to 50-60 DEG C for use;
S5 insole: coating release agent on toward mold, then nylon sheath is laid at lower die, ox-hide surface layer is laid at upper mold, then will
The mixed first component of injection and component B, finally mold in lower die, and demoulding obtains Antistatic shoe-pad after layer of polyurethane molding.
By using above-mentioned technical proposal, layer of polyurethane, ox-hide surface layer, being completely embedded between nylon sheath, it is not easy to
Segregation phenomenon, long service life occurs.
In conclusion the invention has the following advantages:
1. Antistatic shoe-pad is combined by ox-hide surface layer, layer of polyurethane, nylon sheath, not only there is excellent electric conductivity,
Also there is good comfort, resilience etc.;
2. conductive black, nano-conductive fiber, antistatic agent are added in the formula of layer of polyurethane, it is original to can solve layer of polyurethane
The high problem of resistivity, makes it have excellent electric conductivity.
Detailed description of the invention
Fig. 1 is the broken section structural schematic diagram of embodiment one;
Fig. 2 is the structural schematic diagram of one heifer surface layer of embodiment.
Description of symbols: 1, ox-hide surface layer;11, conductive hole;2, nylon sheath;3, layer of polyurethane.
Specific embodiment
Below in conjunction with attached drawing, invention is further described in detail.
Embodiment one:
A kind of Antistatic shoe-pad, as shown in Figure 1 and Figure 2, including the ox-hide surface layer 1 contacted with people vola, the Buddhist nun contacted with inner sole
Imperial sheath 2, is provided with layer of polyurethane 3 between ox-hide surface layer 1 and nylon sheath 2.Ox-hide surface layer 1 is made of natural Kraft fabric,
10 conductive holes, 11,10 conductive holes 11 are provided through at half sole to divide for two rows, every row 5 and along insole outside close to arch of foot
The oblique direction interval of place towards close shoes tip on the inside of insole is arranged.Nylon sheath 2 and layer of polyurethane 3 all have antistatic
Property, therefore the intracorporal electrostatic of people can flow to layer of polyurethane 3 from conductive hole 11, using nylon sheath 2, matched with insole anti-
The sole of electrostatic shoes and be oriented to the earth.
Embodiment two:
Layer of polyurethane is made by first component and second component reaction in embodiment one, and first component includes the component of following parts by weight:
50 parts of polytetramethylene ether diol;
5 parts of ethylene glycol;
0.3 part of catalyst, catalyst is the dibutyltin dilaurate and triethylamine of equal mass mixings;
0.5 part of antistatic agent;
1 part of water;
0.5 part of silicone oil, model 201 is bought from Hua Gu organosilicon Co., Ltd, Foshan City;
It 2 parts of conductive black, partial size 30nm, buys from De Long Chemical Co., Ltd., Xinxiang City;
3 parts of nano-conductive fiber;
It 0.5 part of mould inhibitor, model KP-M20, buys from Foshan science popularization mattress antimildew and antibacterial company;
It 1 part of sisal fiber, buys from Guangdong east sisal hemp group.
Component B includes the component of following parts by weight:
20 parts of polytetramethylene ether diol;
It 45 parts of liquefied mdi, model MDI-100LL, buys from Xin Dian chemical material Co., Ltd.
For conductive black by being modified, modifying process is as follows: by 100 parts of conductive blacks, 5 parts of Silane coupling agent KH550s,
200 part of 95% ethanol solution uniformly mixes, and stirs low temperature drying 24H after 10H.
The preparation process of nano-conductive fiber is as follows:
Step 1, first by purity be 99% pyrroles, DEHS (decanedioic acid two (2- ethylhexyl) ester) it is mixed by 2: 1 molar ratio
It closes, is re-dissolved in 20% ethanol solution, is stirred continuously and is added 3% APS for accounting for pyrroles and DEHS mixture quality, be cooled to-
12h is stirred after 15 DEG C, is finally washed with distilled water suction filtration and is obtained powder;
Powder is dissolved in dichloroacetic acid by step 2, is made into the spinning solution that mass fraction is 10%;
Aqueous nylon (buying from toray company) is added to the water, is heated to 55 DEG C, is stirred continuously until aqueous by step 3
Nylon is completely dissolved, and continues stirring until being cooled to room temperature to obtain the nylon solution that mass fraction is 15%;
Step 4, it is isometric to mix nylon solution and spinning solution, electrostatic is carried out finally by NF-103 series electrostatic spinning machine
Spinning obtains nano-conductive fiber, and 40 DEG C of spinning temperature, voltage 25kV, spinning speed 0.5mL/h.
The preparation process of antistatic agent is as follows:
4 parts of chlorinated dodecanes are dissolved in 50 parts of dehydrated alcohols by the first step, are stirred continuously and are heated to 70 DEG C, add 1 part of diethyl
Hydramine is stirring evenly and then adding into 0.5 part of sodium hydroxide powder, is warming up to 90 DEG C, reacts 4h, and purification depressurizes steaming after obtaining crude product
It evaporates, obtains product A;
12 parts of diethanol amine and 12 parts of succinic anhydrides are dissolved in DMAC (dimethyl acetamide), then again by two by second step respectively
Ethanolamine solutions are heated to 30 DEG C for use, are then slowly added to succinic anhydride solution, and rate control is added in 40min, and 25 DEG C anti-
3h is answered to obtain product B;
Product A is added in product B, is mixed evenly by third step, adds 50 parts of toluene, 0.1 part of toluenesulfonic acid, no
It is disconnected to be stirred and heated to 50 DEG C, 3h is reacted, finally vacuum distillation obtains product C;
Product C is dissolved in DMAC, is passed through nitrogen protection by the 4th step, adds 1 part of sodium hydroxide, 5 parts of epoxychloropropane, rises
Temperature takes filtrate to obtain product D to 70 DEG C of reaction 4h after suction filtration;
5th step, product D are warming up to 40 DEG C in the case where being passed through nitrogen protection, and 2 parts of triethylamines are added, and react 5h, and decompression is steamed
Solvent is removed in distillation, finally dries 12h at 30 DEG C, obtains antistatic agent.
A kind of production method of Antistatic shoe-pad, comprising the following steps:
S1 ox-hide surface layer: natural Kraft fabric is cut into the ox-hide surface layer of required shape by the size of design drawing, is connect
At ox-hide surface layer half sole punching and form conductive hole;
S2 nylon sheath: Antistatic Nylon film is cut into the nylon sheath of required shape by the size of design drawing;
S3 layer of polyurethane first component: by 50 parts of polytetramethylene ether diols, 5 parts of ethylene glycol, 0.3 catalyst, 0.5 part it is antistatic
Agent, 1 part of water, 0.5 part of silicone oil, 2 parts of conductive blacks, 3 parts of nano-conductive fibers, 0.5 part of mould inhibitor, 1 part of sisal fiber mixing are simultaneously
It stirs evenly, is preheated to 50 DEG C for use;
S4 layer of polyurethane component B: taking 45 parts of liquefied mdis, be warming up to 50 DEG C, adds 20 parts of polytetramethylene ether diols, quickly
Stirring makes it heat up naturally, is heated to 80 DEG C when temperature is constant, vacuumizes 30min after reaction 2h, be finally cooled to 50 DEG C to
With;
S5 insole: applying silicone oil on toward mold, then nylon sheath is laid at lower die, ox-hide surface layer is laid at upper mold, then will under
The mixed first component of injection and component B, finally mold in mould, and demoulding obtains Antistatic shoe-pad after layer of polyurethane molding.
Embodiment three:
Layer of polyurethane is made by first component and second component reaction in embodiment one, and first component includes the component of following parts by weight:
70 parts of polytetramethylene ether diol;
8 parts of ethylene glycol;
0.6 part of catalyst, catalyst is the dibutyltin dilaurate and triethylamine of equal mass mixings;
1.5 parts of antistatic agent;
2 parts of water;
1 part of silicone oil, model 201 is bought from Hua Gu organosilicon Co., Ltd, Foshan City;
It 4 parts of conductive black, partial size 30nm, buys from De Long Chemical Co., Ltd., Xinxiang City;
6 parts of nano-conductive fiber;
It 1 part of mould inhibitor, model KP-M20, buys from Foshan science popularization mattress antimildew and antibacterial company;
It 3 parts of sisal fiber, buys from Guangdong east sisal hemp group.
Component B includes the component of following parts by weight:
25 parts of polytetramethylene ether diol;
It 60 parts of liquefied mdi, model MDI-100LL, buys from Xin Dian chemical material Co., Ltd.
For conductive black by being modified, modifying process is as follows: by 120 parts of conductive blacks, 8 parts of Silane coupling agent KH550s,
250 part of 95% ethanol solution uniformly mixes, and stirs low temperature drying 28H after 12H.
The preparation process of nano-conductive fiber is as follows:
Step 1, first by purity be 99% pyrroles, DEHS (decanedioic acid two (2- ethylhexyl) ester) it is mixed by 3: 1 molar ratio
It closes, is re-dissolved in 20% ethanol solution, is stirred continuously and is added 3% APS for accounting for pyrroles and DEHS mixture quality, be cooled to-
It is stirred after 15 DEG C for 24 hours, is finally washed with distilled water suction filtration and obtains powder;
Powder is dissolved in dichloroacetic acid by step 2, is made into the spinning solution that mass fraction is 15%;
Aqueous nylon (buying from toray company) is added to the water, is heated to 60 DEG C, is stirred continuously until aqueous by step 3
Nylon is completely dissolved, and continues stirring until being cooled to room temperature to obtain the nylon solution that mass fraction is 15%;
Step 4, it is isometric to mix nylon solution and spinning solution, electrostatic is carried out finally by NF-103 series electrostatic spinning machine
Spinning obtains nano-conductive fiber, and 40 DEG C of spinning temperature, voltage 25kV, spinning speed 0.5mL/h.
The preparation process of antistatic agent is as follows:
6 parts of chlorinated dodecanes are dissolved in 60 parts of dehydrated alcohols by the first step, are stirred continuously and are heated to 80 DEG C, add 3 parts of diethyls
Hydramine is stirring evenly and then adding into 1 part of sodium hydroxide powder, is warming up to 100 DEG C, reacts 6h, and purification depressurizes steaming after obtaining crude product
It evaporates, obtains product A;
15 parts of diethanol amine and 15 parts of succinic anhydrides are dissolved in DMAC (dimethyl acetamide), then again by two by second step respectively
Ethanolamine solutions are heated to 35 DEG C for use, are then slowly added to succinic anhydride solution, and rate control is added in 50min, and 25 DEG C anti-
3h is answered to obtain product B;
Product A is added in product B, is mixed evenly by third step, adds 60 parts of toluene, 0.3 part of toluenesulfonic acid, no
It is disconnected to be stirred and heated to 60 DEG C, 5h is reacted, finally vacuum distillation obtains product C;
Product C is dissolved in DMAC, is passed through nitrogen protection by the 4th step, adds 2 parts of sodium hydroxides, 6 parts of epoxychloropropane, rises
Temperature takes filtrate to obtain product D to 80 DEG C of reaction 5h after suction filtration;
5th step, product D are warming up to 50 DEG C in the case where being passed through nitrogen protection, and 4 parts of triethylamines are added, and react 7h, and decompression is steamed
Solvent is removed in distillation, finally dries for 24 hours at 35 DEG C, obtains antistatic agent.
A kind of production method of Antistatic shoe-pad, comprising the following steps:
S1 ox-hide surface layer: natural Kraft fabric is cut into the ox-hide surface layer of required shape by the size of design drawing, is connect
At ox-hide surface layer half sole punching and form conductive hole;
S2 nylon sheath: Antistatic Nylon film is cut into the nylon sheath of required shape by the size of design drawing;
S3 layer of polyurethane first component: by 70 parts of polytetramethylene ether diols, 8 parts of ethylene glycol, 0.6 catalyst, 1.5 parts it is antistatic
Agent, 2 parts of water, 1 part of silicone oil, 4 parts of conductive blacks, 6 parts of nano-conductive fibers, 1 part of mould inhibitor, 3 parts of sisal fibers are mixed and stirred for
Uniformly, 60 DEG C are preheated to for use;
S4 layer of polyurethane component B: taking 60 parts of liquefied mdis, be warming up to 55 DEG C, adds 25 parts of polytetramethylene ether diols, quickly
Stirring makes it heat up naturally, is heated to 90 DEG C when temperature is constant, vacuumizes 60min after reaction 3h, be finally cooled to 60 DEG C to
With;
S5 insole: applying silicone oil on toward mold, then nylon sheath is laid at lower die, ox-hide surface layer is laid at upper mold, then will under
The mixed first component of injection and component B, finally mold in mould, and demoulding obtains Antistatic shoe-pad after layer of polyurethane molding.
Example IV:
Layer of polyurethane is made by first component and second component reaction in embodiment one, and first component includes the component of following parts by weight:
60 parts of polytetramethylene ether diol;
6 parts of ethylene glycol;
0.4 part of catalyst, catalyst is the dibutyltin dilaurate and triethylamine of equal mass mixings;
1 part of antistatic agent;
1.5 parts of water;
0.7 part of silicone oil, model 201 is bought from Hua Gu organosilicon Co., Ltd, Foshan City;
It 3 parts of conductive black, partial size 30nm, buys from De Long Chemical Co., Ltd., Xinxiang City;
4 parts of nano-conductive fiber;
It 0.8 part of mould inhibitor, model KP-M20, buys from Foshan science popularization mattress antimildew and antibacterial company;
It 2 parts of sisal fiber, buys from Guangdong east sisal hemp group.
Component B includes the component of following parts by weight:
23 parts of polytetramethylene ether diol;
It 50 parts of liquefied mdi, model MDI-100LL, buys from Xin Dian chemical material Co., Ltd.
For conductive black by being modified, modifying process is as follows: by 110 parts of conductive blacks, 7 parts of Silane coupling agent KH550s,
230 part of 95% ethanol solution uniformly mixes, and stirs low temperature drying 26H after 11H.
The preparation process of nano-conductive fiber is as follows:
Step 1, first by purity be 99% pyrroles, DEHS (decanedioic acid two (2- ethylhexyl) ester) it is mixed by 2.5: 1 molar ratio
It closes, is re-dissolved in 20% ethanol solution, is stirred continuously and is added 3% APS for accounting for pyrroles and DEHS mixture quality, be cooled to-
18h is stirred after 15 DEG C, is finally washed with distilled water suction filtration and is obtained powder;
Powder is dissolved in dichloroacetic acid by step 2, is made into the spinning solution that mass fraction is 12%;
Aqueous nylon (buying from toray company) is added to the water, is heated to 58 DEG C, is stirred continuously until aqueous by step 3
Nylon is completely dissolved, and continues stirring until being cooled to room temperature to obtain the nylon solution that mass fraction is 15%;
Step 4, it is isometric to mix nylon solution and spinning solution, electrostatic is carried out finally by NF-103 series electrostatic spinning machine
Spinning obtains nano-conductive fiber, and 40 DEG C of spinning temperature, voltage 25kV, spinning speed 0.5mL/h.
The preparation process of antistatic agent is as follows:
5 parts of chlorinated dodecanes are dissolved in 55 parts of dehydrated alcohols by the first step, are stirred continuously and are heated to 75 DEG C, add 2 parts of diethyls
Hydramine is stirring evenly and then adding into 0.8 part of sodium hydroxide powder, is warming up to 95 DEG C, reacts 5h, and purification depressurizes steaming after obtaining crude product
It evaporates, obtains product A;
13 parts of diethanol amine and 13 parts of succinic anhydrides are dissolved in DMAC (dimethyl acetamide), then again by two by second step respectively
Ethanolamine solutions are heated to 33 DEG C for use, are then slowly added to succinic anhydride solution, and rate control is added in 45min, and 25 DEG C anti-
3h is answered to obtain product B;
Product A is added in product B, is mixed evenly by third step, adds 55 parts of toluene, 0.2 part of toluenesulfonic acid, no
It is disconnected to be stirred and heated to 55 DEG C, 4h is reacted, finally vacuum distillation obtains product C;
Product C is dissolved in DMAC, is passed through nitrogen protection by the 4th step, adds 1.5 parts of sodium hydroxides, 4.5 parts of epoxy chloropropionates
Alkane is warming up to 75 DEG C of reaction 4.5h, takes filtrate to obtain product D after suction filtration;
5th step, product D are warming up to 45 DEG C in the case where being passed through nitrogen protection, and 3 parts of triethylamines are added, and react 6h, and decompression is steamed
Solvent is removed in distillation, finally dries 18h at 33 DEG C, obtains antistatic agent.
A kind of production method of Antistatic shoe-pad, comprising the following steps:
S1 ox-hide surface layer: natural Kraft fabric is cut into the ox-hide surface layer of required shape by the size of design drawing, is connect
At ox-hide surface layer half sole punching and form conductive hole;
S2 nylon sheath: Antistatic Nylon film is cut into the nylon sheath of required shape by the size of design drawing;
S3 layer of polyurethane first component: by 60 parts of polytetramethylene ether diols, 6 parts of ethylene glycol, 0.4 catalyst, 1 part of antistatic agent,
1.5 parts of water, 0.7 part of silicone oil, 3 parts of conductive blacks, 4 parts of nano-conductive fibers, 0.8 part of mould inhibitor, 2 parts of sisal fibers are mixed and are stirred
It mixes uniformly, is preheated to 55 DEG C for use;
S4 layer of polyurethane component B: taking 50 parts of liquefied mdis, be warming up to 53 DEG C, adds 23 parts of polytetramethylene ether diols, quickly
Stirring makes it heat up naturally, and 85 DEG C are heated to when temperature is constant, vacuumizes 45min after reacting 2.5h, is finally cooled to 55 DEG C
For use;
S5 insole: applying silicone oil on toward mold, then nylon sheath is laid at lower die, ox-hide surface layer is laid at upper mold, then will under
The mixed first component of injection and component B, finally mold in mould, and demoulding obtains Antistatic shoe-pad after layer of polyurethane molding.
Embodiment five:
Unlike example IV, conductive black is without modification.
Embodiment six:
Unlike example IV, layer of polyurethane does not include sisal fiber.
Comparative example one:
Unlike example IV, layer of polyurethane does not include antistatic agent.
Comparative example two:
Unlike example IV, layer of polyurethane does not include conductive black.
Comparative example three:
Unlike example IV, layer of polyurethane does not include nano-conductive fiber.
Comparative example four:
Unlike example IV, layer of polyurethane does not include nano-conductive fiber and conductive black.
Comparative example five:
Unlike example IV, layer of polyurethane does not include nm-class conducting wire fiber, conductive black, antistatic agent.
The test of layer of polyurethane antistatic:
According to the method recorded in national sector standard " test methods of GB/T20991-2007 Individual protection equitment shoes ", test
Layer of polyurethane antistatic performance, obtains resistance.
Layer of polyurethane is immersed in deionized water, bath raio 1: 100, be heated to 50 DEG C, 20min is handled, every 5min glass
Glass stick presses sample into the bottom, and drying tests polyurethane by above-mentioned test method after being repeated 5 times to constant weight again after the completion of processing
Layer antistatic performance, obtains resistance.
According to the regulation of national sector standard " GB 21146-2007 Individual protection equitment occupational footwear ", it is desirable that resistance is greater than
100k Ω and be less than 1000M Ω.
Layer of polyurethane flexibility test:
It is recorded according in national sector standard " measurement of GB/T6670-2008 flexible foam polymeric material falling ball method resilience performance "
Method, test the resilience performance of layer of polyurethane, obtain rebound degree.
Test result table
This specific embodiment is only explanation of the invention, is not limitation of the present invention, and those skilled in the art exist
It can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as in the present invention
Scope of the claims in all by the protection of Patent Law.
Claims (8)
1. a kind of Antistatic shoe-pad, it is characterised in that: including contacted with people vola ox-hide surface layer (1), contact with inner sole
Nylon sheath (2) is provided with layer of polyurethane (3) between the ox-hide surface layer (1) and nylon sheath (2), the nylon sheath (2)
Static electricity resistance is all had with layer of polyurethane (3), is provided through conductive hole (11) at ox-hide surface layer (1) half sole.
2. a kind of Antistatic shoe-pad according to claim 1, it is characterised in that: the layer of polyurethane (3) by first component and
Second component reaction is made, and the first component includes the component of following parts by weight:
50-70 parts of polytetramethylene ether diol;
5-8 parts of ethylene glycol;
0.3-0.6 parts of catalyst;
0.5-1.5 parts of antistatic agent;
1-2 parts of water;
0.5-1 parts of silicone oil;
2-4 parts of conductive black, partial size 30nm;
3-6 parts of nano-conductive fiber;
0.5-1 parts of mould inhibitor;
The component B includes the component of following parts by weight:
20-25 parts of polytetramethylene ether diol;
45-60 parts of liquefied mdi.
3. a kind of Antistatic shoe-pad according to claim 2, it is characterised in that: the conductive black changes by being modified
Property process is as follows: 100-120 parts of conductive blacks, 5-8 parts of silane coupling agents, 95% ethanol solution of 200-250 part uniformly mixed,
Low temperature drying 24-28H after stirring 10-12H.
4. a kind of Antistatic shoe-pad according to claim 2, it is characterised in that: the preparation process of the nano-conductive fiber
It is as follows:
Step 1, pyrroles, DEHS are first pressed (2-3): 1 molar ratio mixes, and is re-dissolved in 20% ethanol solution, is stirred continuously and adds
The APS for entering 3%, stirs 12-24h after being cooled to -15 DEG C, be finally washed with distilled water suction filtration and obtain powder;
Powder is dissolved in dichloroacetic acid by step 2, is made into the spinning solution that mass fraction is 10-15%;
Aqueous nylon is added to the water, is heated to 55-60 DEG C by step 3, be stirred continuously until aqueous nylon be completely dissolved, continue
Stirring is until be cooled to room temperature to obtain the nylon solution that mass fraction is 15%;
Step 4, it is isometric to mix nylon solution and spinning solution, it finally carries out electrostatic spinning and obtains nano-conductive fiber, spinning
40 DEG C of temperature, spinning speed 0.5mL/h.
5. a kind of Antistatic shoe-pad according to claim 2, it is characterised in that: the preparation process of the antistatic agent is such as
Under:
4-6 parts of chlorinated dodecanes are dissolved in 50-60 parts of dehydrated alcohols by the first step, are stirred continuously and are heated to 70-80 DEG C, then plus
Enter 1-3 parts of diethanol amine, be stirring evenly and then adding into 0.5-1 parts of sodium hydroxide powders, be warming up to 90-100 DEG C, reacts 4-6h, mention
It is pure obtain crude product after be evaporated under reduced pressure, obtain product A;
12-15 parts of diethanol amine and 12-15 parts of succinic anhydrides are dissolved in DMAC by second step respectively, then again that diethanol amine is molten
Liquid is heated to 30-35 DEG C for use, is then slowly added to succinic anhydride solution, and rate control is added in 40-50min, 25 DEG C of reactions
3h obtains product B;
Product A is added in product B, is mixed evenly by third step, adds 50-60 parts of toluene, 0.1-0.3 parts of toluene
Sulfonic acid is stirred continuously and is heated to 50-60 DEG C, and reaction 3-5h is finally evaporated under reduced pressure and obtains product C;
Product C is dissolved in DMAC, is passed through nitrogen protection by the 4th step, adds 1-2 parts of sodium hydroxides, 5-6 parts of epoxy chloropropionates
Alkane is warming up to 70-80 DEG C of reaction 4-5h, takes filtrate to obtain product D after suction filtration;
5th step, product D are warming up to 40-50 DEG C in the case where being passed through nitrogen protection, and 2-4 parts of triethylamines are added, and react 5-7h,
Vacuum distillation removes solvent, finally dries 12-24h at 30-35 DEG C, obtains antistatic agent.
6. a kind of Antistatic shoe-pad according to claim 2, it is characterised in that: the first component further includes 1-3 portions of sisal hemps
Fiber.
7. a kind of Antistatic shoe-pad according to claim 2, it is characterised in that: the catalyst is the two of equal mass mixings
Butyl tin dilaurate and triethylamine.
8. a kind of production method of Antistatic shoe-pad as claimed in claim 2, which comprises the following steps:
S1 ox-hide surface layer: natural Kraft fabric is cut into the ox-hide surface layer of required shape by the size of design drawing, is connect
At ox-hide surface layer half sole punching and form conductive hole;
S2 nylon sheath: Antistatic Nylon film is cut into the nylon sheath of required shape by the size of design drawing;
S3 layer of polyurethane first component: by 50-70 parts of polytetramethylene ether diols, 5-8 parts of ethylene glycol, 0.3-0.6 catalyst, 0.5-
1.5 parts of antistatic agents, 1-2 parts of water, 0.5-1 parts of silicone oil, 2-4 parts of conductive blacks, 3-6 parts of nano-conductive fibers, 0.5-1 parts it is mould proof
Agent is mixed and stirred for uniformly, being preheated to 50-60 DEG C for use;
S4 layer of polyurethane component B: taking 45-60 parts of liquefied mdis, be warming up to 50-55 DEG C, adds 20-25 parts of polytetramethylene ethers
Glycol, quickly stirring makes it heat up naturally, and 80-90 DEG C is heated to when temperature is constant, vacuumizes 30-60min after reacting 2-3h,
Finally it is cooled to 50-60 DEG C for use;
S5 insole: coating release agent on toward mold, then nylon sheath is laid at lower die, ox-hide surface layer is laid at upper mold, then will
The mixed first component of injection and component B, finally mold in lower die, and demoulding obtains Antistatic shoe-pad after layer of polyurethane molding.
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