CN109486168A - A kind of preparation method of graphite-silver-conductive polyurethane laminated film - Google Patents
A kind of preparation method of graphite-silver-conductive polyurethane laminated film Download PDFInfo
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- CN109486168A CN109486168A CN201710816859.3A CN201710816859A CN109486168A CN 109486168 A CN109486168 A CN 109486168A CN 201710816859 A CN201710816859 A CN 201710816859A CN 109486168 A CN109486168 A CN 109486168A
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- silver
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- polyurethane
- laminated film
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
Abstract
The invention discloses a kind of graphite-silver-conductive polyurethane laminated film preparation methods, it include: that (1) silver acetate solution and graphite powder are added in dimethylacetamide solvent, 30~60min of ultrasonic disperse under 50~60 DEG C of water bath conditions, it is warming up to 70~80 DEG C, 10~20min of magnetic agitation, obtains mixing suspension；(2) a certain amount of polyaminoester emulsion is added in Xiang Shangshu mixing suspension, is uniformly mixed, obtains graphite-silver-polyurethane suspension；(3) above-mentioned graphite-silver-polyurethane suspension is uniformly applied on round glass slide, carries out spin coating with spin coater, obtain graphite-silver in homogeneous thickness-polyurethane wet film；(4) gained graphite-silver-polyurethane wet film is placed under 60~120 DEG C of vacuum condition dry 5~8h, obtains graphite-silver-conductive polyurethane laminated film.In the present invention in graphite-silver-conductive polyurethane laminated film obtained, silver particles are evenly dispersed in polyurethane matrix, therefore have good electric conductivity.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation of graphite-silver-conductive polyurethane laminated film
Method.
Background technique
With the rapid development of the industries such as electronics industry and information technology, for the polymer material with conducting function
Demand is more more and more urgent.Since conducting polymer materials have light weight, easy processing at various complicated shapes, good stability of the dimension
And resistivity it is adjustable in a big way the features such as, make it in fields such as antistatic, microwave absorption, electromagnetic shielding and electrochemistry
Tool has been widely used.
The common method of conducting polymer composite material is that various conductive fillers, conductive filler are filled in matrix polymer
Type it is very much, can commonly be divided into charcoal system, metal system, metal oxide three classes.Charcoal system includes carbon black, graphite and carbon fiber
Deng metal system mainly has the metal powders such as silver, aluminium, copper, nickel, iron, sheet metal and metallic fiber etc..Due to the cost of charcoal based material
Lower, research at present and application are more.But in the prior art, the high filler loading capacity of charcoal based material also brings a series of problem,
For example, filler grain is easy to fall off, dispersion is not uniform enough, to influence the electric conductivity of compound.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of graphite-silver-conductive polyurethane laminated film,
It is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of graphite-silver-conductive polyurethane laminated film preparation methods, existing to overcome
There is the deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of graphite-silver-conductive polyurethane laminated film, comprising:
(1) silver acetate solution and graphite powder are added in dimethylacetamide solvent, are surpassed under 50~60 DEG C of water bath conditions
Sound disperses 30~60min, is warming up to 70~80 DEG C, 10~20min of magnetic agitation obtains mixing suspension；
(2) a certain amount of polyaminoester emulsion is added in Xiang Shangshu mixing suspension, is uniformly mixed, obtains the poly- ammonia of graphite-silver-
Ester suspension；
(3) above-mentioned graphite-silver-polyurethane suspension is uniformly applied on round glass slide, carries out spin coating with spin coater,
Obtain graphite-silver in homogeneous thickness-polyurethane wet film；
(4) gained graphite-silver-polyurethane wet film is placed under 60~120 DEG C of vacuum condition dry 5~8h, obtains stone
Mo-silver-conductive polyurethane laminated film.
Preferably, in step (2), the preparation method of the polyaminoester emulsion includes: 1) pure and mild polyether polyols of polyester polyols
Alcohol and isophorone diisocyanate are in the presence of dibutyl tin laurate catalyst, isocyanates in proportion: polyalcohol=2.7
The molar ratio of~3.2:1 molar ratio, polyester polyol and polyether polyol is 50~30:50~70, and catalyst is that performed polymer is total
2/10000ths of weight obtain performed polymer in 75~80 DEG C of reaction 1h；2) it based on 0.1mol polyalcohol, is followed by added and contains
The compound dihydromethyl propionic acid 0.09mol of hydrophilic radical and the cosolvent N- crassitude for accounting for lotion total weight 3~4%
Ketone, in 65~70 DEG C of reaction 2h；3) based on 0.1mol polyalcohol, be added 0.09mol triethylamine in and performed polymer, and by this
Performed polymer is added in 300~400g water and emulsifies, and adds in 25~30min, maintains 10min after adding again；4) it is followed by added
2.5~3g amine chainextender, feed time are 10~15min, are stirred for 30min after adding, are defoamed, filtered, and polyurethane is made
Lotion.
Preferably, in the graphite-silver-conductive polyurethane laminated film, the mass fraction of the graphite is 20~60%,
The mass fraction of silver is 5~25%.
Preferably, in the graphite-silver-conductive polyurethane laminated film, the mass fraction of the graphite is 30~50%,
The mass fraction of silver is 5~15%.
Compared with the prior art, the advantages of the present invention are as follows: graphite-silver-conductive polyurethane obtained is compound in the present invention
In film, silver particles are evenly dispersed in polyurethane matrix, therefore have good electric conductivity.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of graphite-silver-conductive polyurethane laminated film, comprising:
(1) silver acetate solution and graphite powder are added in dimethylacetamide solvent, are surpassed under 50~60 DEG C of water bath conditions
Sound disperses 30~60min, is warming up to 70~80 DEG C, 10~20min of magnetic agitation obtains mixing suspension；
(2) a certain amount of polyaminoester emulsion is added in Xiang Shangshu mixing suspension, is uniformly mixed, obtains the poly- ammonia of graphite-silver-
Ester suspension；
(3) above-mentioned graphite-silver-polyurethane suspension is uniformly applied on round glass slide, carries out spin coating with spin coater,
Obtain graphite-silver in homogeneous thickness-polyurethane wet film；
(4) gained graphite-silver-polyurethane wet film is placed under 60~120 DEG C of vacuum condition dry 5~8h, obtains stone
Mo-silver-conductive polyurethane laminated film.
In the graphite-silver according to obtained by the above method-conductive polyurethane laminated film, the mass fraction of the graphite is
20~60%, silver-colored mass fraction is 5~25%, it is preferred that the mass fraction of the graphite is 30~50%, silver-colored quality point
Number is 5~15%, it is further preferred that the mass fraction of the graphite is 40%, silver-colored mass fraction is 10%.
In one embodiment, the preparation method of the polyaminoester emulsion includes:
1) the pure and mild polyether polyol of polyester polyols and isophorone diisocyanate are deposited in dibutyl tin laurate catalyst
Under, isocyanates in proportion: the molar ratio of polyalcohol=2.7~3.2:1 molar ratio, polyester polyol and polyether polyol is
50~30:50~70, catalyst are 2/10000ths of performed polymer total weight, obtain performed polymer in 75~80 DEG C of reaction 1h；
2) based on 0.1mol polyalcohol, the compound dihydromethyl propionic acid containing hydrophilic radical is followed by added
0.09mol and the cosolvent N-Methyl pyrrolidone for accounting for lotion total weight 3~4%, in 65~70 DEG C of reaction 2h；
3) it based on 0.1mol polyalcohol, is added in 0.09mol triethylamine and performed polymer, and this performed polymer is added to
It emulsifies in 300~400g water, is added in 25~30min, maintain 10min after adding again；
4) 2.5~3g amine chainextender is followed by added, feed time is 10~15min, 30min is stirred for after adding, through disappearing
Bubble, filtering, are made polyaminoester emulsion.
Embodiment
1, polyaminoester emulsion is prepared
1) the pure and mild polyether polyol of polyester polyols and isophorone diisocyanate are deposited in dibutyl tin laurate catalyst
Under, isocyanates in proportion: the molar ratio of polyalcohol=3:1 molar ratio, polyester polyol and polyether polyol is 40:60,
Catalyst is 2/10000ths of performed polymer total weight, obtains performed polymer in 80 DEG C of reaction 1h；
2) based on 0.1mol polyalcohol, the compound dihydromethyl propionic acid containing hydrophilic radical is followed by added
0.09mol and the cosolvent N-Methyl pyrrolidone for accounting for lotion total weight 3%, in 70 DEG C of reaction 2h；
3) it based on 0.1mol polyalcohol, is added in 0.09mol triethylamine and performed polymer, and this performed polymer is added to
It emulsifies in 350g water, is added in 30min, maintain 10min after adding again；
4) 3g amine chainextender is followed by added, feed time 15min is stirred for 30min after adding, is defoamed, filtered, and makes
Obtain polyaminoester emulsion.
2, graphite-silver-conductive polyurethane laminated film is prepared
(1) silver acetate solution and graphite powder are added in dimethylacetamide solvent, the ultrasound point under 60 DEG C of water bath conditions
45min is dissipated, is warming up to 80 DEG C, magnetic agitation 20min obtains mixing suspension；
(2) a certain amount of polyaminoester emulsion is added in Xiang Shangshu mixing suspension, is uniformly mixed, obtains the poly- ammonia of graphite-silver-
Ester suspension；
(3) above-mentioned graphite-silver-polyurethane suspension is uniformly applied on round glass slide, carries out spin coating with spin coater,
Obtain graphite-silver in homogeneous thickness-polyurethane wet film；
(4) gained graphite-silver-polyurethane wet film is placed under 80 DEG C of vacuum condition dry 6h, it is poly- obtains graphite-silver-
Urethane conductive composite film.
According in graphite-silver-conductive polyurethane laminated film obtained in above-described embodiment, the quality of the graphite is divided
Number is 40%, and silver-colored mass fraction is 10%.
In the present invention, by the way that silver acetate is added in polyurethane body, by heat treatment, silver ion reduction at silver atoms simultaneously
It is evenly dispersed in polyurethane matrix, therefore there is good electric conductivity.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (4)
1. a kind of graphite-silver-conductive polyurethane laminated film preparation method characterized by comprising
(1) silver acetate solution and graphite powder are added in dimethylacetamide solvent, the ultrasound point under 50~60 DEG C of water bath conditions
30~60min is dissipated, is warming up to 70~80 DEG C, 10~20min of magnetic agitation obtains mixing suspension；
(2) a certain amount of polyaminoester emulsion is added in Xiang Shangshu mixing suspension, is uniformly mixed, it is outstanding to obtain graphite-silver-polyurethane
Supernatant liquid；
(3) above-mentioned graphite-silver-polyurethane suspension is uniformly applied on round glass slide, carries out spin coating with spin coater, obtained
Graphite-silver in homogeneous thickness-polyurethane wet film；
(4) gained graphite-silver-polyurethane wet film is placed under 60~120 DEG C of vacuum condition dry 5~8h, obtains graphite-
Silver-conductive polyurethane laminated film.
2. graphite-silver according to claim 1-conductive polyurethane laminated film preparation method, which is characterized in that step
(2) in, the preparation method of the polyaminoester emulsion includes: 1) the pure and mild polyether polyol of polyester polyols and isophorone diisocyanate
Ester is in the presence of dibutyl tin laurate catalyst, isocyanates in proportion: polyalcohol=2.7~3.2:1 molar ratio, polyester are more
The molar ratio of first alcohol and polyether polyol is 50~30:50~70, and catalyst is 2/10000ths of performed polymer total weight, in 75~
80 DEG C of reaction 1h obtain performed polymer；2) based on 0.1mol polyalcohol, the compound dihydroxy containing hydrophilic radical is followed by added
Methylpropanoic acid 0.09mol and the cosolvent N-Methyl pyrrolidone for accounting for lotion total weight 3~4%, in 65~70 DEG C of reaction 2h；3)
It based on 0.1mol polyalcohol, is added in 0.09mol triethylamine and performed polymer, and this performed polymer is added to 300~400g
It emulsifies in water, is added in 25~30min, maintain 10min after adding again；4) 2.5~3g amine chainextender is followed by added, when charging
Between be 10~15min, be stirred for 30min after adding, defoamed, filtered, be made polyaminoester emulsion.
3. graphite-silver according to claim 1-conductive polyurethane laminated film preparation method, which is characterized in that described
In graphite-silver-conductive polyurethane laminated film, the mass fraction of the graphite is 20~60%, silver-colored mass fraction is 5~
25%.
4. graphite-silver according to claim 3-conductive polyurethane laminated film preparation method, which is characterized in that described
In graphite-silver-conductive polyurethane laminated film, the mass fraction of the graphite is 30~50%, silver-colored mass fraction is 5~
15%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710816859.3A CN109486168A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of graphite-silver-conductive polyurethane laminated film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710816859.3A CN109486168A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of graphite-silver-conductive polyurethane laminated film |
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| CN109486168A true CN109486168A (en) | 2019-03-19 |
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| CN201710816859.3A Withdrawn CN109486168A (en) | 2017-09-12 | 2017-09-12 | A kind of preparation method of graphite-silver-conductive polyurethane laminated film |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740206A (en) * | 2005-09-22 | 2006-03-01 | 上海市合成树脂研究所 | Prepn process of water thinned polyurethane emulsion |
| CN105131563A (en) * | 2015-09-30 | 2015-12-09 | 中北大学 | Preparation method for Fe3O4/graphene oxide/waterborne polyurethane composite |
-
2017
- 2017-09-12 CN CN201710816859.3A patent/CN109486168A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740206A (en) * | 2005-09-22 | 2006-03-01 | 上海市合成树脂研究所 | Prepn process of water thinned polyurethane emulsion |
| CN105131563A (en) * | 2015-09-30 | 2015-12-09 | 中北大学 | Preparation method for Fe3O4/graphene oxide/waterborne polyurethane composite |
Non-Patent Citations (1)
| Title |
|---|
| 洪凤宏: "聚氨酯/纳米银导电复合薄膜的制备及结构与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20190319 |
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