CN105754159B - Latex composite, preparation and the application of a kind of high intensity, antistatic - Google Patents

Latex composite, preparation and the application of a kind of high intensity, antistatic Download PDF

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CN105754159B
CN105754159B CN201610147271.9A CN201610147271A CN105754159B CN 105754159 B CN105754159 B CN 105754159B CN 201610147271 A CN201610147271 A CN 201610147271A CN 105754159 B CN105754159 B CN 105754159B
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latex
cnts
water soluble
soluble polymer
preparation
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CN105754159A (en
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华静
耿洁婷
薛梅玉
金鑫铮
武歧
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00—Compositions of natural rubber
    • C08L7/02—Latex
    • 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

Abstract

The present invention relates to a kind of high intensity, latex composite, preparation and the application of antistatic, belong to the preparation field of polymer nanocomposites.A kind of high intensity, the latex composite of antistatic, using simple mechanical milling method by water soluble polymer to the processing of carbon nano tube surface physics cladding, add it in the aqueous solution and be ultrasonically treated, then this carbon nano tube dispersion liquid is mixed with prevulcanized latex, mechanical agitation is well mixed, emulsion intercalation method is high, so as to fully play CNTs performance, and the viscosity of latex system will not increase, good leveling property, dipping plastic film mulch technique can be used, it also is adapted for linkage production line dipping production, be advantageous to the large-scale production of latex product, make obtained latex product intensity high, being folded without breaking, static electricity resistance.

Description

Latex composite, preparation and the application of a kind of high intensity, antistatic
Technical field
The present invention relates to a kind of high intensity, latex composite, preparation and the application of antistatic, belong to polymer nanocomposite and answer The preparation field of condensation material.
Background technology
CNT (CNTs) is (logical because of its unique structure and characteristic such as high-flexibility, low mass density and big L/D ratio Normal 300-1000), also as it possesses outstanding electrical property, thermal conductivity and high mechanical properties.The conductance of single beam CNT It can reach 104S/cm value, (copper is 59 × 10 with the conductance of metal4S/cm, iron are 9.9 × 104S/cm) approach, and carbon The density of nanotube is very low, also can significantly mitigate weight.It is well known that carbon material generally has high thermal conductivity, and carbon is received (experimental measurements of single nanotube thermal conductivity are 3000W/ (mK) to mitron, and the predicted value calculated in theory is up to 6600W/ (mK), then make this uncommon advantageous characteristic more prominent, therefore such a material is classified as since the dawn of human civilization thermal conductivity is most High material.Due to the covalent sp formed between its single carbon atom2Key, CNT are rated as the intensity found so far most Material high, rigidity is best, its tensile strength is that (Kevlar is 3.5MPa to 10~150MPa by contrast, and stainless steel is 1MPa), modulus of elasticity is about 1TPa (Kevlar is about 0.15TPa by contrast, and stainless steel is about 0.2TPa).
There is very strong Van der Waals interaction, so that hundreds of carbon pipes tangle between CNT (CNTs) Together, larger aggregate is formed, it is difficult to separate, greatly weakens excellent mechanics and electricity that single carbon pipe is shown Characteristic.By carrying out effective surface modification to CNT, then the problem of above-mentioned can be overcome, so as to improve CNT Dispersive property, its compatibility between matrix material is improved, and strengthen the interaction between them.In addition, by it Carry out surface modification and can also impart to the new performance of CNT, realize the molecule assembling of CNT, it is excellent to obtain various performances Different nano material, before molectronics, nanoelectronics and nano biological molecules etc. have wide application Scape.
The surface-functionalized of CNT mainly has two kinds of covalent bond method and non-covalent bond method.Covalent bond method modified carbon nano tube Pipe mainly pass through chemical modification, carbon nano tube surface in the form of covalent bond with reference to a number of chemical functional group with up to To modified purpose.And non-covalent bond rule is to carbon by modes such as surfactant modified, polymer wrapped, winding and absorption Nanotube carries out surface modification.For the modification of covalent bond method, the advantages of this method is main is exactly being capable of anti-blocking pipe sp2Atomic structure of carbon and conjugated system are destroyed, and maintain the electronic structure of CNT, so as to not interfere with its excellent electricity , optics, magnetics, calorifics and mechanical performance.
At present, in rubber industry, its production scale is very big in China for latex product, but there is also with low content of technology, matter Measure the shortcomings of unstable.Come modified latex product inorganic filler can be brought easily heavy by adding the method for inorganic filler in latex Product is not easy to the industrialized production of infusion process, low production efficiency, and because the accumulation of inorganic filler easily makes product defect occur, drops The problem of low Mechanical Properties of Products.Chinese patent at present on inorganic filler modified latex is seldom.Chinese patent 201010200667.8th, 2007100492970,2007100492932 main research inorganic powder mill base modified latexs are prepared color The preparation method of color latex product.
CNT (CNTs) is the quite varied functional material of purposes, because its unique structure and characteristic such as high intensity, High-flexibility, low mass density and big L/D ratio, also as it possesses outstanding electrical property, thermal conductivity and high mechanical properties.I Using water soluble polymer reason cladding CNTs, make it dispersed in latex, do not influence the stable state of emulsion, do not increase Add the viscosity of latex, linkage production line continuous production can be used, while CNTs is uniformly dispersed in latex product, gained breast Glue product strength height, being folded without breaking while antistatic, the frictional static in work can be prevented for latex products such as emgloves Generation.
Chinese patent 201210450491.0 " a kind of High-conductivity carbon nanotube/rubber composite and preparation method thereof " is adopted With a kind of oriented growth of carbon nanometer tube beam, add it to aqueous surfactant solution and successively carry out ultrasonic place with different power Reason, makes CNT be dispersed in water.Carbon nano tube dispersion liquid is mixed with prevulcanized latex, mechanical agitation is well mixed Utilize " dipping plastic film mulch " technique that CNT/latex mixed liquor is poured onto in lucite grinding tool afterwards, drying at room temperature is sulfided into Type.There is higher draw ratio and preferably dispersiveness using CNT in CNT/rubber composite obtained by this method, Good with the compatibility of rubber matrix, the electrical conductivity of its vulcanizate is significantly increased.
What this method added CNT in emulsion contains aqueous surfactant solution, makes the solid content of emulsion reduce, because This this method is mainly for the natural concentrating glue breast that solid content is 60%, and the preparation technology of product is using dipping plastic film mulch technique.And A large amount of latex products are using linkage production line dipping production, and production scale is big, and this process conditions are to emulsion intercalation method requirement Height, viscosity requirement are low.
The content of the invention
In order to overcome problem of the prior art and shortcoming, it is an object of the invention to provide one kind to prepare novel C NTs/ glue The preparation of newborn composite article.This method using principle be to CNT (CNTs) surface carry out physical modification, i.e., using letter Single mechanical milling method to the processing of CNTs surface physicses cladding, adds it to water soluble polymer in the aqueous solution at ultrasound Reason, this carbon nano tube dispersion liquid is mixed with prevulcanized latex, and mechanical agitation is well mixed, and emulsion intercalation method is high, so as to To fully play CNTs performance, and the viscosity of latex system will not increase, good leveling property, can use dipping plastic film mulch technique, Linkage production line dipping production also is adapted for, is advantageous to the large-scale production of latex product, makes obtained latex product intensity high, resistance to Pierce through, static electricity resistance.
The purpose of the present invention is achieved through the following technical solutions：
The latex composite of a kind of high intensity, antistatic, it is made of polymer emulsion and CNT blending.
Preferably：Cladding processing is carried out to carbon nano tube surface with water soluble polymer using polishing, then with gathering Compound latex is blended.After above-mentioned technical proposal, CNTs sufficiently uniformly can be distributed in latex, and latex system Viscosity will not increase, good leveling property, can use dipping plastic film mulch technique, also be adapted for linkage production line dipping production, be advantageous to latex The large-scale production of product, obtained latex product intensity height, being folded without breaking, static electricity resistance.
The method of Chinese patent 201210450491.0 adds aqueous surfactant solution, makes the solid content of emulsion reduce.Only Can be less demanding to emulsion intercalation method using dipping plastic film mulch technique for the natural concentrating glue breast that solid content is 60%.This is specially Dissolubility of the CNT of water soluble polymer reason cladding prepared by sharp method in water is high, and consolidating for available latex contains Amount can be in 60-40%, and emulsion intercalation method is good, and the viscosity of latex system will not increase, good leveling property, can use dipping paving Membrane process, linkage production line dipping production also is adapted for, is advantageous to the large-scale production of latex product.Gained latex product is except tool There is certain electric conductivity, intensity further increases, and cutting resistance is obviously improved.
Preferably：Polymer emulsion is Heveatex, styrene-butadiene latex, acrylonitrile-butadiene-phenylethylene copolymer glue Breast, styrene-butadiene-styrene latex, NBR latex, polyvinyl acetate emulsion, polyaminoester emulsion, acrylic acid At least one of ester homopolymer or copolymer emulsion, methacrylic acid homo thing or copolymer emulsion.
Preferably：CNT is at least one of single armed CNT or multi-walled carbon nanotube.
Preferably：Length of carbon nanotube is 5-10 μm.It is demonstrated experimentally that length is too short, and it is, for example, less than 5 μm, enhancing effect It is bad；Length is excessive, is greater than 10 μm, is easily snapped off in process of lapping.The present invention also provides above-mentioned latex composite Preparation method, comprise the following steps：
1) water soluble polymer parcel CNTs preparation
Water soluble polymer and CNTs are ground, water is added, ultrasonic disperse, obtains finely dispersed mixed solution；
2) preparation of CNTs/ latex composite
The above-mentioned of 0.5%~5% mass fraction is added in presulfurization centrifugal concentrate of the dry rubber content in 35%-45% CNTs, 10~30min is stirred, it is well mixed that blendlatex is made.
Preferably：In step 1), water soluble polymer and CNTs mass ratio are 1:4-4:1.
Preferably：In step 1), water soluble polymer parcel CNTs preparation condition is：By water soluble polymer with CNTs grinds 15min~5h, adds CNT:Water quality fraction is 1：100-1：1000,50~500W of power, frequency be 10~ Under conditions of 10000HZ, 10~100 DEG C of temperature, ultrasonic disperse 15min~2h.
Preferably：Tested according to national standard GB7544-2009 annex I, the film thickness of composite is in 0.170- Between 0.180mm, material lift 30-40% of the intensity than not adding CNT.
Preferably：The volume resistance of composite is 1.0 × 1012Ω·cm--1×1011Ω·cm。
Preferably：Water soluble polymer is polyvinylpyrrolidone, polyethylene glycol, kayexalate, starch derivatives Biology, carboxymethyl cellulose, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid, poly- second Enol, HPMA, poly-quaternary ammonium salt, starch, Arabic gum, algin sodium, bone meal, gelatin, at least one of casein.
The present invention also provides a kind of latex product, the blendlatex prepared according to method described above, utilizes the connection of routine Dynamic production line vulcanization process is made.
The present invention also provides above-mentioned latex product in high intensity emgloves, latex mould, conductive material, electromagnetic shielding material Or the application in barrier material.
Brief description of the drawings
Fig. 1 is respectively from left to right：MWCNTs is directly blended into day in Heveatex, the latex of embodiment 1, comparative example 1 The photo after 48h is stood in right latex；
Fig. 2 is the scanning electron microscope (SEM) photograph of unmodified CNTs/ latex composite article Tensile fracture；
Fig. 3 is the scanning electron microscope (SEM) photograph of modified CNTs/ latex composite article Tensile fractures.
Embodiment
Below by specific embodiment, the present invention will be further described, embodiment just to illustrate the present invention, It is not intended to limit the present invention.The protection content of the present invention is not limited to following examples, and following examples water soluble polymer is poly- Vinylpyrrolidone (PVP), latex are Heveatex.
Comparative example 1 and embodiment 1
The change of CNTs dispersivenesses after processing
Embodiment 1：It is 3 by weight ratio:1 PVP/CNTs mechanical lapping 15min, it is CNT 0.5mg/ according to concentration Ml adds appropriate parts by weight water, ultrasonic disperse 15min, obtains finely dispersed mixed solution.0.5% mass is added in latex The above-mentioned CNTs of fraction, dry rubber content is added in 45% presulfurization centrifugal concentrate, stir 30min, be configured to dry glue and contain The presulfurization centrifugal concentrate 45% is measured, a small amount of blended liquid is drawn, is added dropwise on PE films, utilizes the surface of blended liquid itself Power controls the thickness and size of drop.
The preparation method of comparative example 1：0.5% mass fraction is added in presulfurization centrifugal concentrate of the dry rubber content 45% Above-mentioned CNTs, stir 30min, draw a small amount of blended liquid, be added dropwise on PE films, utilize the surface tension control of blended liquid itself The thickness and size of drop processed.
Fig. 1 understands that the MWCNTs/PVP/NR rubber latex samples being obtained by this method have reached expected dispersion effect.
In documents 1, directly CNT is blended into Heveatex, the viscosity of latex is big, and carbon pipe is rolled into a ball wherein Poly- phenomenon is serious.
The emulsion viscosity of the embodiment 1 of falling ball method measure is 12Pa.s, and does not add the breast of the identical solid content of CNT The viscosity 11-13Pa.s of liquid is consistent.
As can be seen here, present invention, avoiding agglomeration caused by CNT addition and viscosity of latex increase phenomenon, carbon Nanotube dispersiveness and flow leveling are good.
Embodiment 2 and comparative example 2
The change of CNTs dispersivenesses after processing
Embodiment 2：It is 3 by weight ratio:1 PVP/CNTs mechanical lapping 15min, add appropriate parts by weight water, ultrasound point 15min is dissipated, obtains finely dispersed mixed solution.The above-mentioned CNTs of 0.5% mass fraction is added in latex, is added to dry glue Content in 45% presulfurization centrifugal concentrate, stir 30min, be configured to dry rubber content 35% presulfurization centrifugal concentrate by Latex product is made according to the conventional linkage production line vulcanization process of latex.
The preparation method of comparative example 2：0.5% mass fraction is added in presulfurization centrifugal concentrate of the dry rubber content 35% Above-mentioned CNTs, stir 30min, latex product be made according to the conventional linkage production line vulcanization process of latex.
Fig. 2 and Fig. 3 is the sem test result of CNTs/ latex composite article Tensile fractures.From the scanning electricity of amplification It can be seen that on mirror figure, deployment conditions of the CNT in rubber matrix are different.In Fig. 2, unmodified CNT is in rubber It is obvious to occur agglomeration in matrix.In Fig. 3, the CNT dispersiveness of PVP claddings substantially improves, and can also be clearly visible " wire drawing " phenomenon, illustrate that the adhesion of CNT and rubber interface becomes strong.
Embodiment 3-4 and comparative example 3-4
Influences of the CNTs to latex product mechanical property
Embodiment 3-4 preparation method：It is 3 by weight ratio:1 PVP/CNTs mechanical lapping 15min, add appropriate weight Part water is measured, ultrasonic disperse 15min, obtains finely dispersed mixed solution.In presulfurization centrifugal concentrate of the dry rubber content 45% It is middle add 0.4% and 0.5% mass fraction above-mentioned CNTs, stir 30min, be configured to dry rubber content be 40% presulfurization from Latex product is made according to the conventional linkage production line vulcanization process of latex in heart latex.Sample is tubbiness annulus, and wall wide 20mm is thick 0.170-0.180mm, girth 103mm.
The preparation method of comparative example 3：Dry rubber content 40% presulfurization centrifugal concentrate according to the conventional linkage of latex Latex product is made in production line vulcanization process.Sample is tubbiness annulus, wall wide 20mm, thick 0.170-0.180mm, girth 103mm.
The preparation method of comparative example 4：0.5% mass fraction is added in presulfurization centrifugal concentrate of the dry rubber content 40% Above-mentioned CNT, stir 30 minutes, latex product be made according to the conventional linkage production line vulcanization process of latex.Sample is tubbiness Annulus, wall wide 20mm, thick 0.170-0.180mm, girth 103mm.
With QC-II-DS type electronic tensile test machines, experimental condition:23 ± 2 DEG C of temperature, humidity 55 ± 15%, annular stretching Test piece, 500 ± 50mm/min of draw speed.
The sample pull-off force of table 1. and elongation rate of tensile failure
The pull-off force of the latex product of the CNTs after addition processing is improved with elongation rate of tensile failure as shown in Table 1, may The reason for be good dispersions of the CNTs in latex after processing, CNTs has humidification, therefore improves the toughness of sample And intensity.
Embodiment 5 and comparative example 5
Influences of the CNTs to latex product electric conductivity
The preparation method of embodiment 5:By weight than for 4:1 PVP/CNTs mechanical lapping 15min, add appropriate weight Part water, ultrasonic disperse 15min, obtains finely dispersed mixed solution.In the presulfurization centrifugal concentrate latex of dry rubber content 45% The middle above-mentioned CNTs aqueous solution for adding 0.5% mass fraction, stands 30min after shaking up, is configured to the pre- sulphur of dry rubber content 40% Change centrifugal concentrate, draw a small amount of above-mentioned emulsion and be added dropwise on PE films, utilize the surface tension transition drop of blended liquid itself Thickness and size.Obtained drop is positioned over natural air drying 48h at fume hood, obtains the sample of embodiment 4.
The preparation method of comparative example 5：The presulfurization centrifugal concentrate for drawing a small amount of 40% dry rubber content is added dropwise on PE films, profit With the thickness and size of the surface tension transition drop of emulsion itself.Obtained drop is positioned over natural air drying at fume hood 48h, obtain the sample of embodiment 5.
Table 2.CNTs before modified after latex film electrical property
Test sample size：15×15×(1.0±0.1)mm
By formulaResistance sizes are calculated, can calculate the resistance of the modified latex films of CNTs reduces, and says Bright addition CNTs can improve the electric conductivity of Heveatex.

Claims (4)

  1. A kind of 1. latex composite of high intensity, antistatic, it is characterised in that：Using polishing water soluble polymer to carbon Nanotube surface carries out cladding processing, is then made with polymer emulsion blending；Specific method comprises the following steps：
    1）Water soluble polymer wraps up CNTs preparation
    Water soluble polymer and CNTs are ground, water is added, ultrasonic disperse, obtains finely dispersed mixed solution；
    2）The preparation of CNTs/ latex composites
    The above-mentioned CNTs of 0.5% ~ 5% mass fraction, stirring 10 are added in presulfurization centrifugal concentrate of the dry rubber content in 35%-45% ~30min, it is well mixed that blendlatex is made；
    Step 1）In, water soluble polymer and CNTs mass ratio are 1:4-4:1；
    Step 1）In, water soluble polymer parcel CNTs preparation condition is：By water soluble polymer and CNTs grinding 15min ~ 5h, add CNT:Water quality fraction is 1：100-1：1000, it is 10 ~ 10000Hz, temperature 10 ~ 100 in 50 ~ 500W of power, frequency Under conditions of DEG C, ultrasonic disperse 15min ~ 2h；
    Water soluble polymer is polyvinylpyrrolidone, polyethylene glycol, kayexalate, starch derivatives, carboxymethyl fibre Tie up element, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid, polyvinyl alcohol, poly Acid anhydride, poly-quaternary ammonium salt, starch, Arabic gum, algin sodium, bone meal, gelatin, at least one of casein.
  2. 2. a kind of high intensity, the latex composite of antistatic as claimed in claim 1, it is characterised in that：Polymer emulsion is Heveatex, styrene-butadiene latex, acrylonitrile-butadiene-phenylethylene copolymer emulsion, styrene-butadiene-styrene glue Breast, NBR latex, polyvinyl acetate emulsion, polyaminoester emulsion, Voncoat R 3310 or copolymer emulsion, methacrylic acid At least one of homopolymer or copolymer emulsion.
  3. A kind of 3. latex product, it is characterised in that：The blendlatex prepared according to specific method described in claim 1, using normal The linkage production line vulcanization process of rule is made.
  4. 4. latex product described in claim 3 is in high intensity emgloves, latex mould, conductive material, electromagnetic shielding material or resistance Application in barrier material.
CN201610147271.9A 2016-03-15 2016-03-15 Latex composite, preparation and the application of a kind of high intensity, antistatic Active CN105754159B (en)

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Publication number Priority date Publication date Assignee Title
CN106432850A (en) * 2016-08-31 2017-02-22 邝月辉 Rubber material for making gloves
CN106782875B (en) * 2016-11-22 2019-01-01 叶静 A kind of preparation method of polymolecularity combined conductive agent
CN107955224B (en) * 2017-12-21 2020-08-21 新奥石墨烯技术有限公司 Carbon material reinforced rubber and preparation method thereof
CN110078983A (en) * 2019-05-10 2019-08-02 中国电力科学研究院有限公司 Gloves made of latex slurry with touch screen functionality and preparation method thereof
CN111941710B (en) * 2020-08-21 2021-06-22 安丹达工业技术(上海)有限公司 Antistatic antichemical latex gloves and preparation method thereof
CN113337200B (en) * 2021-05-26 2021-12-31 安徽辅朗光学材料有限公司 Carbon nano tube antistatic coating and preparation method and application thereof
CN114921202B (en) * 2022-04-28 2023-09-22 深圳市通泰盈科技股份有限公司 High-temperature-resistant acrylic pressure-sensitive adhesive and preparation method thereof, pressure-sensitive adhesive tape and preparation method thereof
CN115975273B (en) * 2022-12-26 2023-10-20 江苏恒辉安防股份有限公司 Biodegradable latex composite material and preparation method thereof

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CN101418089A (en) * 2008-12-03 2009-04-29 中国热带农业科学院农产品加工研究所 Method for preparing natural rubber-carbon nano tube composite material by using static electricity self-assembly

Patent Citations (2)

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CN1673261A (en) * 2005-03-18 2005-09-28 清华大学 Natural liquid rubber slurry with added carbon nanotube and its prepn process
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