CN105802248A - Method for preparing conductive composite with attapulgite as substrate - Google Patents
Method for preparing conductive composite with attapulgite as substrate Download PDFInfo
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- CN105802248A CN105802248A CN201610224881.4A CN201610224881A CN105802248A CN 105802248 A CN105802248 A CN 105802248A CN 201610224881 A CN201610224881 A CN 201610224881A CN 105802248 A CN105802248 A CN 105802248A
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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
- C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C08L87/005—Block or graft polymers not provided for in groups C08L1/00 - C08L85/04
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides a method for preparing a conductive composite with attapulgite as a substrate. The method comprises steps as follows: activating attapulgite serving as the substrate, preparating a novel polyaniline conductive layer and compositng the substrate and the polyaniline conductive layer. The activation process is simple, the efficiency is high, and the cost is low; the prepared novel polyaniline conductive layer has excellent conductive performance, and the preparation cost is moderate; the adsorption effect of the attapulgite substrate and the novel polyaniline conductive layer is excellent, and the stability is high.
Description
Technical field
The invention belongs to conductive material preparing technical field, be specifically related to a kind of method with attapulgite for substrate fabrication conducing composite material.
Background technology
Attapulgite be a kind of layer of chain excessive structural based on the clay pit containing Shuifu County's zeopan, there is fibrous or rough club shaped structure, show the physicochemical properties of various excellence, be widely used in the fields such as chemical industry.
Simultaneously, polyaniline is as one of conducting polymer composite, because its chemical stability is good, weatherability is good, cheaper starting materials is easy to get, synthetic method is simple and electric conductivity etc., it is considered as the structural conducting polymer most with commercial application value, in fields such as power technologies, there is the huge market demand.The conductivity of polyaniline own is not high, need doping could improve electric conductivity, but polyaniline has bigger difficulty in the processed in later stage, by the impact of difficulty of processing and processing cost, the composite material electric conductivity of polyaniline is not very good, and processing cost also has to be reduced simultaneously.
Therefore, developing a kind of for problem above is those skilled in the art institute urgent need to solve the problem in the manufacture method of conductive material carrying out both combining on the basis of initial processing.
Summary of the invention
For solving the problems referred to above, the invention discloses a kind of method with attapulgite for substrate fabrication conducing composite material.
In order to achieve the above object, the present invention provides following technical scheme:
A kind of method with attapulgite for substrate fabrication conducing composite material, step includes: activation attapulgite is as substrate, the compound making New Polyaniline conductive layer and substrate and layer/polyaniline conductive layer；
Further, concrete steps include:
(1), to attapulgite it is ground pulverizing, and sieves；
(2), will step (1) be that 1:5～15 mix through grinding with the attapulgite sieved with deionized water according to mass ratio, and stir 20～30min；Stand more than 30min after stirring and filter；Put in baking oven after filtration and be dried, it is thus achieved that pure attapulgite；
(3), polyvinylpyrrolidone is soluble in water, and be warming up to 220～230 DEG C generate polyvinylpyrrolidone steam；Simultaneously using noble gas as carrier gas, polyvinylpyrrolidone steam is made to contact with the pure attapulgite obtained in step (2)；Further heat up to 600～900 DEG C, and start cooling after being incubated 1～2h, stop adding polyvinylpyrrolidone steam simultaneously；After being cooled to room temperature, take out the attapulgite activated；
(4), in pre-converter, add polyaniline monomer, polrvinyl chloride and adjuvant, be polymerized；Generate the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer；The quality of the polyaniline polyvinyl chloride polymer that polymerization proceeds to formation accounts for the 70～95% of total mixture quality；
(5), the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer formed in step (4) is easily separated, is separated into the first logistics comprising 74～90wt% of mixture in step (4) and comprises the second logistics of mixture surplus in step (4)；
(6), in the second reactor, add the first logistics, be polymerized further；
(7), by the first logistics of inversion of phases in step (6) and the second logistics in step (5) with 28～35s-1Shear rate mix in static mixer, it is thus achieved that polyaniline polyvinyl chloride composite；
(8), the polyaniline polyvinyl chloride composite fluidization that will obtain in step (7), it is incubated after being warming up to 30～40 DEG C, the attapulgite that the activation obtained in step (3) completes is put into wherein, treats that it fully absorbs the polyaniline polyvinyl chloride composite of fluidization, obtain Compound Punch rod soil；
(9), put into step (8) obtains Compound Punch rod soil in mould, and hot-forming.
The invention provides a kind of method with attapulgite for substrate fabrication conducing composite material, by activation attapulgite as substrate, compound three acquisition making New Polyaniline conductive layer and substrate and layer/polyaniline conductive layer.
First attapulgite is activated, increase the specific surface area of attapulgite, to increase its adsorbance；Then prepare novel conductive layer with polyaniline and polrvinyl chloride for raw material, have on the basis of higher machinability, control production cost, it is ensured that its electrical conductivity；Finally both are adsorbed mutually, and hot pressing compound obtains novel conducing composite material.
When attapulgite is activated, purify firstly the need of to it, purification complete after using noble gas as carrier gas, polyvinylpyrrolidone steam is made to contact with the attapulgite clay after purifying soil phase, polyvinylpyrrolidone steam can react with the hydroxyl that contains in attapulgite, under the high temperature of 600～900 DEG C, with attapulgite generation graft reaction, can be well dispersed in attapulgite, bonding situation between the New Polyaniline conductive layer prepared in attapulgite and subsequent step can either be improved, grafting can also be passed through separated by the inorganic nano-particle contained in attapulgite simultaneously, prevent it from reuniting, play significant dispersion effect.Polyvinylpyrrolidone also has the feature improving electric conductivity simultaneously, contributes to promoting the electric conductivity of the New Polyaniline conductive layer obtained in subsequent step.
The present invention is when preparing New Polyaniline conductive layer, select polyaniline and polrvinyl chloride as primary raw material, coordinate again and carry out polyreaction with adjuvant, polymerization generates New Polyaniline conductive layer, have on the basis of better machinability, it is ensured that polymer has outstanding electric conductivity, stability and relatively low or moderate manufacturing cost.
Finally by obtained New Polyaniline conductive layer fluidization, attapulgite is put into wherein, the New Polyaniline conductive layer of fluidization is adsorbed to its surface, complete the absorption of the conducing composite material being substrate with attapulgite.
As preferably, the deionized water in step (2) has been also added with dispersant；Dispersant is sodium hexametaphosphate and the mixture of any one or two kinds in sodium orthophosphate.
The mixture of any one or two kinds that the present invention is added with in sodium hexametaphosphate and sodium orthophosphate in deionized water, as dispersant, to improve attapulgite dispersibility in deionized water, promotes refining effect.
As preferably, the quality of dispersant is the 3～4.5% of the quality of attapulgite.
As preferably, 20～25 times of the quality that quality is attapulgite of the polyvinylpyrrolidone steam in step (3)；Noble gas is He, N2And the one or any several combination in Ar.
In order to ensure purification and the activation effect of attapulgite, quality is attapulgite quality the 3～4.5% of the dispersant adopted in the present invention, the quality of polyvinylpyrrolidone steam is 20～25 times of the quality of attapulgite；And adopt He, N2And the one or any several combination in Ar is as carrier gas, ensure while polyvinylpyrrolidone steam is played carrier band effect not react with polyvinylpyrrolidone steam generation.
As preferably, in step (4), mass percent shared by polyaniline monomer, polrvinyl chloride and adjuvant is respectively as follows: 50～62%, 30～47%, 3～10%；Mass percent shared by the constituent of adjuvant and each composition is respectively as follows: adhesive: 5～15%, bulking agent: 65～80%, stabilizer: 7～20%.
In the present invention, adjuvant is made up of adhesive, bulking agent and stabilizer, and wherein adhesive can make prepared New Polyaniline conductive layer have certain intensity after absorption solidification, can improve its viscosity simultaneously, make it easier to combine with attapulgite；Adding bulking agent can by intermolecular bonding force so that polyaniline monomer and polrvinyl chloride are combined as a whole, and products therefrom is more stable；Add stabilizer and can keep chemical equilibrium, reduce products therefrom surface tension, it is prevented that light, thermal decomposition and oxidation Decomposition etc. act on.
As preferably, in step (9), the temperature of hot pressing is 55～70 DEG C, and the persistent period is 20～30min.
The present invention in the end adopts heat pressing process by attapulgite and New Polyaniline conductive layer molding.
Compared with prior art, activating process is simple, efficiency is high, cost is low for the present invention；The New Polyaniline conductive layer electric conductivity prepared is outstanding, and cost of manufacture is moderate；Attapulgite substrate is outstanding with the adsorption effect of New Polyaniline conductive layer, and stability is strong.
Detailed description of the invention
Below with reference to specific embodiment, technical scheme provided by the invention is described in detail, it should be understood that following detailed description of the invention is merely to illustrate the present invention rather than restriction the scope of the present invention.
Embodiment 1:
The invention provides a kind of method with attapulgite for substrate fabrication conducing composite material, step includes: activation attapulgite is as substrate, the compound making New Polyaniline conductive layer and substrate and layer/polyaniline conductive layer；
Concrete steps include:
(1), to attapulgite it is ground pulverizing, and sieves；
(2), will step (1) be that 1:5 mixes through grinding with the attapulgite sieved with deionized water according to mass ratio, and add sodium hexametaphosphate as dispersant, the quality of dispersant is the 3% of the quality of attapulgite；And stir 20min；Stand more than 30min after stirring and filter；Put in baking oven after filtration and be dried, it is thus achieved that pure attapulgite；
(3), polyvinylpyrrolidone is soluble in water, and be warming up to 220 DEG C generate polyvinylpyrrolidone steam；Simultaneously using He as noble gas as carrier gas, the polyvinylpyrrolidone steam of 20 times of the quality making quality be attapulgite contacts with the pure attapulgite obtained in step (2)；Further heat up to 600 DEG C, and start cooling after being incubated 1h, stop adding polyvinylpyrrolidone steam simultaneously；After being cooled to room temperature, take out the attapulgite activated；
(4), in pre-converter, add polyaniline monomer, polrvinyl chloride and adjuvant, be polymerized；Mass percent shared by polyaniline monomer therein, polrvinyl chloride and adjuvant is respectively as follows: 50%, 47%, 3%；Mass percent shared by the constituent of adjuvant and each composition is respectively as follows: adhesive: 5%, bulking agent: 80%, stabilizer: 15%；The quality of the polyaniline polyvinyl chloride polymer that polymerization proceeds to formation accounts for the 70% of total mixture quality；
(5), the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer formed in step (4) is easily separated, is separated into the first logistics comprising the 75wt% of mixture in step (4) and comprises the second logistics of mixture surplus in step (4)；
(6), in the second reactor, add the first logistics, be polymerized further；
(7), by the first logistics of inversion of phases in step (6) and the second logistics in step (5) with 35s-1Shear rate mix in static mixer, it is thus achieved that polyaniline polyvinyl chloride composite；
(8), the polyaniline polyvinyl chloride composite fluidization that will obtain in step (7), it is incubated after being warming up to 30 DEG C, the attapulgite that the activation obtained in step (3) completes is put into wherein, treats that it fully absorbs the polyaniline polyvinyl chloride composite of fluidization, obtain Compound Punch rod soil；
(9), put in mould by step (8) obtains Compound Punch rod soil, at the temperature of 55 DEG C, hot pressing 20min molding.
Embodiment 2:
The invention provides a kind of method with attapulgite for substrate fabrication conducing composite material, step includes: activation attapulgite is as substrate, the compound making New Polyaniline conductive layer and substrate and layer/polyaniline conductive layer；
Concrete steps include:
(1), to attapulgite it is ground pulverizing, and sieves；
(2), will step (1) be that 1:15 mixes through grinding with the attapulgite sieved with deionized water according to mass ratio, and add sodium orthophosphate as dispersant, the quality of dispersant is the 4.5% of the quality of attapulgite；And stir 25min；Stand more than 30min after stirring and filter；Put in baking oven after filtration and be dried, it is thus achieved that pure attapulgite；
(3), polyvinylpyrrolidone is soluble in water, and be warming up to 220 DEG C generate polyvinylpyrrolidone steam；Simultaneously using Ar as noble gas as carrier gas, the polyvinylpyrrolidone steam of 25 times of the quality making quality be attapulgite contacts with the pure attapulgite obtained in step (2)；Further heat up to 900 DEG C, and start cooling after being incubated 1.5h, stop adding polyvinylpyrrolidone steam simultaneously；After being cooled to room temperature, take out the attapulgite activated；
(4), in pre-converter, add polyaniline monomer, polrvinyl chloride and adjuvant, be polymerized；Mass percent shared by polyaniline monomer therein, polrvinyl chloride and adjuvant is respectively as follows: 62%, 30%, 8%；Mass percent shared by the constituent of adjuvant and each composition is respectively as follows: adhesive: 15%, bulking agent: 65%, stabilizer: 20%；The quality of the polyaniline polyvinyl chloride polymer that polymerization proceeds to formation accounts for the 95% of total mixture quality；
(5), the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer formed in step (4) is easily separated, is separated into the first logistics comprising the 90wt% of mixture in step (4) and comprises the second logistics of mixture surplus in step (4)；
(6), in the second reactor, add the first logistics, be polymerized further；
(7), by the first logistics of inversion of phases in step (6) and the second logistics in step (5) with 30s-1Shear rate mix in static mixer, it is thus achieved that polyaniline polyvinyl chloride composite；
(8), the polyaniline polyvinyl chloride composite fluidization that will obtain in step (7), it is incubated after being warming up to 40 DEG C, the attapulgite that the activation obtained in step (3) completes is put into wherein, treats that it fully absorbs the polyaniline polyvinyl chloride composite of fluidization, obtain Compound Punch rod soil；
(9), put in mould by step (8) obtains Compound Punch rod soil, at the temperature of 70 DEG C, hot pressing 20min molding.
Embodiment 3:
The invention provides a kind of method with attapulgite for substrate fabrication conducing composite material, step includes: activation attapulgite is as substrate, the compound making New Polyaniline conductive layer and substrate and layer/polyaniline conductive layer；
Concrete steps include:
(1), to attapulgite it is ground pulverizing, and sieves；
(2) will step (1) be, that 1:10 mixes through grinding with the attapulgite sieved with deionized water according to mass ratio, and add sodium hexametaphosphate with the mixture in sodium orthophosphate as dispersant, the quality of dispersant is the 4% of the quality of attapulgite；And stir 30min；Stand more than 30min after stirring and filter；Put in baking oven after filtration and be dried, it is thus achieved that pure attapulgite；
(3), polyvinylpyrrolidone is soluble in water, and be warming up to 230 DEG C generate polyvinylpyrrolidone steam；Simultaneously with N2As noble gas as carrier gas, the polyvinylpyrrolidone steam of 22 times of the quality making quality be attapulgite contacts with the pure attapulgite obtained in step (2)；Further heat up to 780 DEG C, and start cooling after being incubated 2h, stop adding polyvinylpyrrolidone steam simultaneously；After being cooled to room temperature, take out the attapulgite activated；
(4), in pre-converter, add polyaniline monomer, polrvinyl chloride and adjuvant, be polymerized；Mass percent shared by polyaniline monomer therein, polrvinyl chloride and adjuvant is respectively as follows: 55%, 40%, 5%；Mass percent shared by the constituent of adjuvant and each composition is respectively as follows: adhesive: 10%, bulking agent: 75%, stabilizer: 15%；The quality of the polyaniline polyvinyl chloride polymer that polymerization proceeds to formation accounts for the 90% of total mixture quality；
(5), the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer formed in step (4) is easily separated, is separated into the first logistics comprising the 85wt% of mixture in step (4) and comprises the second logistics of mixture surplus in step (4)；
(6), in the second reactor, add the first logistics, be polymerized further；
(7), by the first logistics of inversion of phases in step (6) and the second logistics in step (5) with 28s-1Shear rate mix in static mixer, it is thus achieved that polyaniline polyvinyl chloride composite；
(8), the polyaniline polyvinyl chloride composite fluidization that will obtain in step (7), it is incubated after being warming up to 40 DEG C, the attapulgite that the activation obtained in step (3) completes is put into wherein, treats that it fully absorbs the polyaniline polyvinyl chloride composite of fluidization, obtain Compound Punch rod soil；
(9), put in mould by step (8) obtains Compound Punch rod soil, at the temperature of 60 DEG C, hot pressing 30min molding.
It is calculated by above three groups of embodiments are raw materials used, processing cost, and respectively three groups of embodiment products therefroms is carried out performance test；Embodiment 1 cost only increases by 10.5% relative to existing product, but electrical conductivity promotes about 30.2%；Embodiment 2 cost increases by 15% relative to existing product, and electrical conductivity promotes about 47%；Embodiment 3 cost increases by 17% relative to existing product, but electrical conductivity promotes about 73.3%；Integrated cost and products obtained therefrom performance consider, embodiment 3 is preferred.
Finally it should be noted that, above example is only in order to illustrate technical scheme and non-limiting technical scheme, it will be understood by those within the art that, technical scheme is modified or equivalent replacement by those, without deviating from objective and the scope of the technical program, all should be encompassed in the middle of scope of the presently claimed invention.
Claims (7)
1. the method with attapulgite for substrate fabrication conducing composite material, it is characterised in that: step includes: activation attapulgite is as substrate, the compound making New Polyaniline conductive layer and substrate and layer/polyaniline conductive layer.
2. a kind of method with attapulgite for substrate fabrication conducing composite material according to claim 1, it is characterised in that: concrete steps include:
(1), to attapulgite it is ground pulverizing, and sieves；
(2), will step (1) be that 1:5～15 mix through grinding with the attapulgite sieved with deionized water according to mass ratio, and stir 20～30min；Stand more than 30min after stirring and filter；Put in baking oven after filtration and be dried, it is thus achieved that pure attapulgite；
(3), polyvinylpyrrolidone is soluble in water, and be warming up to 220～230 DEG C generate polyvinylpyrrolidone steam；Simultaneously using noble gas as carrier gas, polyvinylpyrrolidone steam is made to contact with the pure attapulgite obtained in step (2)；Further heat up to 600～900 DEG C, and start cooling after being incubated 1～2h, stop adding polyvinylpyrrolidone steam simultaneously；After being cooled to room temperature, take out the attapulgite activated；
(4), in pre-converter, add polyaniline monomer, polrvinyl chloride and adjuvant, be polymerized；Generate the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer；The quality of the polyaniline polyvinyl chloride polymer that described polymerization proceeds to formation accounts for the 70～95% of total mixture quality；
(5), the mixture comprising polyaniline, polrvinyl chloride and polyaniline polyvinyl chloride polymer formed in step (4) is easily separated, is separated into the first logistics comprising 74～90wt% of mixture in step (4) and comprises the second logistics of mixture surplus in step (4)；
(6), in the second reactor, add the first logistics, be polymerized further；
(7), by the first logistics of inversion of phases in step (6) and the second logistics in step (5) with 28～35s-1Shear rate mix in static mixer, it is thus achieved that polyaniline polyvinyl chloride composite；
(8), the polyaniline polyvinyl chloride composite fluidization that will obtain in step (7), it is incubated after being warming up to 30～40 DEG C, the attapulgite that the activation obtained in step (3) completes is put into wherein, treats that it fully absorbs the polyaniline polyvinyl chloride composite of fluidization, obtain Compound Punch rod soil；
(9), put into step (8) obtains Compound Punch rod soil in mould, and hot-forming.
3. a kind of method with attapulgite for substrate fabrication conducing composite material according to claim 2, it is characterised in that: the deionized water in described step (2) has been also added with dispersant；Described dispersant is sodium hexametaphosphate and the mixture of any one or two kinds in sodium orthophosphate.
4. a kind of method with attapulgite for substrate fabrication conducing composite material according to claim 3, it is characterised in that: the quality of described dispersant is the 3～4.5% of the quality of attapulgite.
5. a kind of method with attapulgite for substrate fabrication conducing composite material according to claim 2, it is characterised in that: 20～25 times of the quality that quality is attapulgite of the polyvinylpyrrolidone steam in described step (3)；Described noble gas is He, N2And the one or any several combination in Ar.
6. a kind of method with attapulgite for substrate fabrication conducing composite material according to claim 2, it is characterised in that: in described step (4), mass percent shared by polyaniline monomer, polrvinyl chloride and adjuvant is respectively as follows: 50～62%, 30～47%, 3～10%；Mass percent shared by the constituent of described adjuvant and each composition is respectively as follows: adhesive: 5～15%, bulking agent: 65～80%, stabilizer: 7～20%.
7. a kind of method with attapulgite for substrate fabrication conducing composite material according to claim 2, it is characterised in that: in described step (9), the temperature of hot pressing is 55～70 DEG C, and the persistent period is 20～30min.
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| CN106947222A (en) * | 2017-03-16 | 2017-07-14 | 张丹丹 | A kind of 3D printing material for being used to produce electric-conductor |
| CN107042302A (en) * | 2017-03-16 | 2017-08-15 | 张丹丹 | It is a kind of to be used for the 3D printing material of pipe fitting in hot-cast technique |
| CN110591442A (en) * | 2019-09-12 | 2019-12-20 | 浙江工业大学之江学院 | Preparation method of water-based thickening agent |
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