CN103642068B - Antistatic slurry - Google Patents
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- CN103642068B CN103642068B CN201310605915.0A CN201310605915A CN103642068B CN 103642068 B CN103642068 B CN 103642068B CN 201310605915 A CN201310605915 A CN 201310605915A CN 103642068 B CN103642068 B CN 103642068B
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Abstract
The invention discloses an antistatic slurry containing a conductive filler and a silane coupling agent. The conductive filler comprises a conductive powder A and a conductive powder B in a weight ratio of 1:2-10. The conductive powder A is black and / or graphite with granularity of 800-2000 nm; the conductive powder B is carbon black with granularity of 20-200 nm. The conductive filler accounts for 0.5-5 wt% in the slurry; and the silane coupling agent accounts for 0.03-3 wt% of the conductive filler. The antistatic slurry has good dispersibility and small range of resistor change. Compared with the slurry with same content and employing individual nanometer order (or micron order) carbon black or graphite as conductive filler, the antistatic slurry, in the application to antistatic polyimide film, can improve the mechanical properties of the film by 20-30%, or in the preparation of a polyimide film with the same mechanical properties, the addition of the conductive filler in the slurry can be increased by 5-10%.
Description
Technical field
The present invention relates to a kind of antistatic polyimide film, be specifically related to the antistatic slurry used when making antistatic polyimide film.
Background technology
Antistatic macromolecule matrix material has slim and graceful soft, the feature such as involution mode is various of antistatic, electromagnetic shielding, resistance to chemical attack, physique, to meet Chemicals, microelectronic device etc. to have particular requirement field to wrapping material.
According to the difference of surface resistivity, material can be divided into conduction, antistatic and insulation three major types.
Polyimide (Polyimide is called for short PI) film refers to the class superpolymer containing imide ring on main chain, and it not only has good high-and low-temperature resistance performance, also has good physicals, electrical property and mechanical property.Polyimide can keep stable physical property in very large temperature range, can tolerate the envrionment temperature of-269 ~ 400 DEG C.In addition, select suitable filler and adopt suitable film technique can obtain anlistatig polyimide film, filler grain can form conductive network in polyimide film matrix, polymer surfaces resistivity is reduced, prevents gathering of electrostatic.
Since the sixties in 20th century, people conduct extensive research the antistatic property how improving macromolecular material, set up and define 4 kinds of typical composite modifying methods, respectively: (1) adds conductive filler material; (2) static inhibitor is added; (3) mixed with structural conductive macromolecular Huang; (4) surface-coated.
In the method for modifying adding conductive filler material, conventional conductive filler material can divide with carbon system and metal system two in class, and wherein carbon series conductive material adopts electrically conductive graphite or graphitized carbon black usually.If publication number is the patent of invention of CN102516574A, disclose a kind of preparation method of three layers of antistatic polyimide film, it realizes the object of modification in the antistatic polyimide precursor of preparation by adding nano level electrically conductive graphite, graphitized carbon black, antimony-doped stannic oxide or fluorine-doped tin dioxide.In addition, publication number is the patent of invention of CN102120826A, disclose a kind of preparation method of antistatic polyimide film, in the method, conductive filler material is added in aprotic polar organic solvent, add silane coupling agent, temperature controlled ultrasonic stirs, conductive filler material is made to be evenly dispersed in organic solution, make the conductive suspension of stable and uniform, described conductive filler material is micron size conductive graphite or micron size conductive carbon black, and wherein the mass ratio of conductive filler material and aprotic polar solvent is 0.005 ~ 0.25; The mass ratio 0.02 ~ 0.1 of silane coupling agent and conductive filler material.Above-mentioned patent is all using the electrically conductive graphite of single particle size scope or graphitized carbon black as conductive filler material, although the antistatic polyimide film obtained can be made to have certain antistatic property, the mechanical property of gained film is not ideal enough.
Summary of the invention
The technical problem to be solved in the present invention is to provide the antistatic slurry of a kind of dispersiveness and good stability.The antistatic polyimide film adopting this antistatic slurry and polyamic acid resin solution mixing system to obtain is compared with the antistatic polyimide film of identical conduction agent addition in prior art, and the mechanical property of film can improve 20 ~ 30%.
A kind of antistatic slurry, containing conductive filler material and silane coupling agent, described conductive filler material is made up of by the weight ratio of 1:2 ~ 10 conductive powder A and conductive powder B, described conductive powder A is carbon black and/or graphite, its granularity is 800 ~ 2000nm, the carbon black of described conductive powder B to be granularity be 20 ~ 200nm; Described conductive filler material weight percent is in the slurry 0.5 ~ 5%, and described silane coupling agent is 0.03 ~ 3% relative to the weight percent of conductive filler material.The present invention selects the conductive filler material of different-grain diameter to carry out specific proportioning, gained solution is after high speed shear, the carbon black pellet of very easily reuniting effectively is disperseed, to obtain good stability and the little antistatic slurry of resistance range, this slurry is especially applicable to preparing antistatic resin class material.
In technique scheme, also comprise the conventional constituents made used by antistatic slurry, as solvent, the selection of solvent is identical with existing routine techniques, particularly, solvent preferably adopts N-Methyl pyrrolidone, N,N-DIMETHYLACETAMIDE, dimethyl formamide or gamma-butyrolactone.
In technique scheme, when conductive powder A be chosen as the combination of carbon black and graphite time, the proportioning between them can be any proportioning.
In technique scheme, when the granularity selection of conductive powder A is 800 ~ 1200nm, when the granularity selection of conductive powder B is 30 ~ 50nm, electroconductibility and the better antistatic slurry of stability can be obtained.
In technique scheme, the weight ratio of described conductive powder A and conductive powder B is preferably 1:3 ~ 5.
In technique scheme, described conductive filler material weight percent is in the slurry preferably 0.9 ~ 5%.
In technique scheme, described silane coupling agent can be that routine of the prior art is selected, can be specifically be selected from γ-glycidoxypropyltrime,hoxysilane, γ-glycidoxypropyl diethoxy silane, N-(2-aminoethyl-3-aminopropyl) methyl dimethoxysilane, n-octyltri-ethoxysilane, γ aminopropyltriethoxy silane, N-β (amino-ethyl) gamma-amino propyl trimethoxy silicane, one or more combination in N-β (amino-ethyl) gamma-amino hydroxypropyl methyl dimethoxysilane and Sodium dodecylbenzene sulfonate.When silane coupling agent be chosen as above-mentioned combination two or more arbitrarily time, the proportioning between them can be any proportioning.
Antistatic slurry of the present invention can adopt existing ordinary method to prepare, specifically can be prepared as follows: the silane coupling agent adding formula ratio in the solvent of formula ratio, stir the conductive filler material adding formula ratio after 10 ~ 30 minutes, then ultrasonic pre-dispersed 10 ~ 60 minutes, and then high-pressure homogeneous, namely obtain Corona-resistant slurry.Wherein, the described pre-dispersed time is preferably 20 ~ 40 minutes, and described homogeneous carries out usually in high pressure homogenizer, and the time of homogeneous is generally 3 ~ 8 minutes.
Compared with prior art, the present invention carries out specific proportioning by selecting the conductive filler material of different-grain diameter, gained solution is after high speed shear, the carbon black pellet of very easily reuniting effectively is disperseed, to obtain good dispersity, resistance range is little, and is applicable to the antistatic slurry preparing antistatic resin class material.With other of same amount adopt separately the carbon black of nano level (or micron order) or graphite as conductive filler material slurry compared with, when being applied to antistatic polyimide film, the mechanical property of film can improve 20 ~ 30%; Or under the Kapton of preparation same mechanical performance, the conductive filler material content in slurry can add 5 ~ 10% more.
Embodiment
With specific embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the γ aminopropyltriethoxy silane of 0.36g, after stirring 15min, add conductive powder A (granularity is the carbon black 2g of 1000 ~ 2000nm) and conductive powder B (granularity is the carbon black 10g of 30nm) successively, ultrasonic pre-dispersed 30min, then use high pressure homogenizer homogeneous 5min, obtain the antistatic slurry of stable dispersion.
Comparative example 1-1
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the γ aminopropyltriethoxy silane of 0.36g, after stirring 15min, add conductive powder A (granularity is the carbon black 2g of 2000 ~ 2500nm) and conductive powder B (granularity is the carbon black 10g of 200 ~ 250nm) successively, ultrasonic pre-dispersed 30min, then use high pressure homogenizer homogeneous 5min, obtain antistatic slurry.
Comparative example 1-2
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the γ aminopropyltriethoxy silane of 0.36g, after stirring 15min, add conductive powder A (granularity is the carbon black 6g of 1000 ~ 2000nm) and conductive powder B (granularity is the carbon black 6g of 30nm) successively, ultrasonic pre-dispersed 30min, then use high pressure homogenizer homogeneous 5min, obtain antistatic slurry.
Embodiment 2
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the Sodium dodecylbenzene sulfonate of 0.2g, after stirring 15min, add conductive powder A (granularity is the graphite 1.5g of 1000nm) and conductive powder B (granularity is the carbon black 7.5g of 30nm) successively, ultrasonic pre-dispersed 20min, then use high pressure homogenizer homogeneous 5min, obtain the antistatic slurry of stable dispersion.
Embodiment 3
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the Sodium dodecylbenzene sulfonate of 0.075g, after stirring 10min, add conductive powder A (granularity is the graphite 1.5g of 1000 ~ 2000nm) and conductive powder B (granularity is the carbon black 6.0g of 30nm) successively, ultrasonic pre-dispersed 40min, then use high pressure homogenizer homogeneous 5min, obtain the antistatic slurry of stable dispersion.
Embodiment 4
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the Sodium dodecylbenzene sulfonate of 0.3g, after stirring 15min, add conductive powder A (granularity is the graphite 2.4g of 1000nm) and conductive powder B (granularity is the carbon black 9.6g of 30nm) successively, ultrasonic pre-dispersed 20min, then use high pressure homogenizer homogeneous 10min, obtain the antistatic slurry of stable dispersion.
Comparative example 4-1
The N,N-dimethylacetamide taking 1000g, as solvent, adds the γ aminopropyltriethoxy silane of 0.5g, after stirring 15min, add the carbon black 12g that granularity is 30nm, ultrasonic pre-dispersed 30min, use high pressure homogenizer homogeneous 5min again, obtain antistatic slurry.
Comparative example 4-2
The N,N-dimethylacetamide taking 1000g, as solvent, adds the γ aminopropyltriethoxy silane of 0.5g, after stirring 15min, add the carbon black 12g that granularity is 1000 ~ 2000nm, ultrasonic pre-dispersed 30min, use high pressure homogenizer homogeneous 5min again, obtain antistatic slurry.
Comparative example 4-3
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the Sodium dodecylbenzene sulfonate of 0.3g, after stirring 15min, add conductive powder A (granularity is the graphite 2.4g of 500nm) and conductive powder B (granularity is the carbon black 9.6g of 30nm) successively, ultrasonic pre-dispersed 20min, then use high pressure homogenizer homogeneous 10min, obtain antistatic slurry.
Embodiment 5
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the Sodium dodecylbenzene sulfonate of 0.3g, after stirring 20min, add conductive powder A (the graphite 0.9g that the carbon black 0.6g that granularity is 800 ~ 1000nm, granularity are 1000 ~ 1200nm) and conductive powder B (granularity is the carbon black 14.5g of 50 ~ 80nm) successively, ultrasonic pre-dispersed 20min, then use high pressure homogenizer homogeneous 5min, obtain the antistatic slurry of stable dispersion.
Embodiment 6
Take the N of 1000g, N-N,N-DIMETHYLACETAMIDE is as solvent, add the Sodium dodecylbenzene sulfonate of 0.25g, after stirring 10min, add conductive powder A (granularity is the carbon black 3g of 1500 ~ 2000nm) and conductive powder B (granularity is the carbon black 6g of 100 ~ 200nm) successively, ultrasonic pre-dispersed 20min, then use high pressure homogenizer homogeneous 5min, obtain the antistatic slurry of stable dispersion.
Prepare film sample 1:
4 of 86.16g is added in the antistatic slurry that embodiment 1 is obtained, 4 ˊ-amino-diphenylethers, after dissolving, add pyromellitic acid anhydride adjusting viscosity again, the viscosity of final gained polyamic acid solution is made to be 60,000 centipoises, after vacuumizing froth breaking, technique salivation routinely, stretching and imidization masking.The thickness of gained film sample 1 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6.25%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Preparation contrast film sample 1:
Repeat the method preparing film sample 1, unlike the antistatic slurry that the antistatic slurry obtained with comparative example 1-1 replaces embodiment 1 obtained.The thickness of gained contrast film sample 1 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6.25%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Preparation contrast film sample 2:
Repeat the method preparing film sample 1, unlike the antistatic slurry that the antistatic slurry obtained with comparative example 1-2 replaces embodiment 1 obtained.The thickness of gained contrast film sample 1 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6.25%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Prepare film sample 2
81.84g4 is added in the Corona-resistant slurry that embodiment 2 is obtained, 4 ˊ-amino-diphenylethers, after dissolving, add pyromellitic acid anhydride adjusting viscosity again, the viscosity of final gained polyamic acid solution is made to be 5.6 ten thousand centipoises, after vacuumizing froth breaking, technique salivation routinely, stretching and imidization masking.The thickness of gained film sample 2 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 5%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Prepare film sample 3:
86.16g4 is added in the Corona-resistant slurry that embodiment 3 is obtained, 4 ˊ-amino-diphenylethers, after dissolving, add pyromellitic acid anhydride adjusting viscosity again, the viscosity of final gained polyamic acid solution is made to be 5.2 ten thousand centipoises, after vacuumizing froth breaking, technique salivation routinely, stretching and imidization masking.The thickness of gained film sample 3 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 4%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Prepare film sample 4:
89.98g4 is added in the Corona-resistant slurry that embodiment 4 is obtained, 4 ˊ-amino-diphenylethers, after dissolving, add pyromellitic acid anhydride adjusting viscosity again, the viscosity of final gained polyamic acid solution is made to be 5.5 ten thousand centipoises, after vacuumizing froth breaking, technique salivation routinely, stretching and imidization masking.The thickness of gained film sample 4 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Preparation contrast film sample 3:
Repeat the method preparing film sample 4, unlike the antistatic slurry that the antistatic slurry obtained with comparative example 4-1 replaces embodiment 4 obtained.The thickness of gained contrast film sample 3 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Preparation contrast film sample 4:
Repeat the method preparing film sample 1, unlike the antistatic slurry that the antistatic slurry obtained with comparative example 4-2 replaces embodiment 1 obtained.The thickness of gained contrast film sample 4 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Preparation contrast film sample 5:
Repeat the method preparing film sample 1, unlike the antistatic slurry that the antistatic slurry obtained with comparative example 4-3 replaces embodiment 1 obtained.The thickness of gained contrast film sample 5 is 25 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 6%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Prepare film sample 5:
88.07g4 is added in the Corona-resistant slurry that embodiment 5 is obtained, 4 ˊ-amino-diphenylethers, after dissolving, add pyromellitic acid anhydride adjusting viscosity again, the viscosity of final gained polyamic acid solution is made to be 4.8 ten thousand centipoises, after vacuumizing froth breaking, technique salivation routinely, stretching and imidization masking.The thickness of gained film sample 5 is 20 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 8%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Prepare film sample 6:
90.93g4 is added in the Corona-resistant slurry that embodiment 6 is obtained, 4 ˊ-amino-diphenylethers, after dissolving, add pyromellitic acid anhydride adjusting viscosity again, the viscosity of final gained polyamic acid solution is made to be 5.5 ten thousand centipoises, after vacuumizing froth breaking, technique salivation routinely, stretching and imidization masking.The thickness of gained film sample 6 is 20 microns, and wherein conductive filler material accounts for the weight ratio of whole film is 5%, and survey its surface resistivity and mechanical property, data are as shown in table 1 below.
Table 1:
From table 1, the present invention by selecting the conductive filler material of different-grain diameter to carry out the antistatic slurry good dispersity of specific proportioning gained, resistance range is little, with other of same amount adopt separately the carbon black of nano level (or micron order) or graphite as conductive filler material slurry compared with, when being applied to antistatic polyimide film, the mechanical property of film can improve 20 ~ 30%; Or under the Kapton of preparation same mechanical performance, the conductive filler material content in slurry can add 5 ~ 10% more.
Claims (6)
1. an antistatic slurry, containing conductive filler material and silane coupling agent, it is characterized in that: described conductive filler material is made up of by the weight ratio of 1:2 ~ 10 conductive powder A and conductive powder B, described conductive powder A is carbon black and/or graphite, its granularity is 800 ~ 2000nm, the carbon black of described conductive powder B to be granularity be 20 ~ 200nm; Described conductive filler material weight percent is in the slurry 0.5 ~ 5%, and described silane coupling agent is 0.03 ~ 3% relative to the weight percent of conductive filler material.
2. antistatic slurry according to claim 1, is characterized in that: the granularity of described conductive powder A is 800 ~ 1200nm.
3. antistatic slurry according to claim 1, is characterized in that: the granularity of described conductive powder B is 30 ~ 50nm.
4. antistatic slurry according to claim 1, is characterized in that: the weight ratio of described conductive powder A and conductive powder B is 1:3 ~ 5.
5. the antistatic slurry according to any one of Claims 1 to 4, is characterized in that: described conductive filler material weight percent is in the slurry 0.9 ~ 5%.
6. the antistatic slurry according to any one of Claims 1 to 4, it is characterized in that: described silane coupling agent is for being selected from γ-glycidoxypropyltrime,hoxysilane, γ-glycidoxypropyl diethoxy silane, N-(2-aminoethyl-3-aminopropyl) methyl dimethoxysilane, n-octyltri-ethoxysilane, γ aminopropyltriethoxy silane, N-β (amino-ethyl) gamma-amino propyl trimethoxy silicane, one or more combination in N-β (amino-ethyl) gamma-amino hydroxypropyl methyl dimethoxysilane and Sodium dodecylbenzene sulfonate.
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| CN105482115B (en) * | 2015-12-11 | 2017-11-24 | 宁波今山电子材料有限公司 | A kind of preparation method of high insulated high-strength polyimides black film |
| JP6944811B2 (en) * | 2017-05-22 | 2021-10-06 | 大豊工業株式会社 | Resin material for sliding members and sliding members |
| JP6385026B1 (en) * | 2017-06-13 | 2018-09-05 | アーテック株式会社 | Water-based paint composition, air purification mechanism and air purification method |
| CN109536114A (en) * | 2018-12-03 | 2019-03-29 | 苏州市陆氏新材料有限公司 | A kind of preparation method of the dedicated Antistatic type PU Flock Adhesive of metal |
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| CN102432939A (en) * | 2011-11-07 | 2012-05-02 | 中国蓝星（集团）股份有限公司 | Antistatic flame-retardant ultra high molecular weight polyethylene composition and preparation method thereof |
| CN102532469A (en) * | 2011-12-28 | 2012-07-04 | 南京双威生物医学科技有限公司 | Graphite composite modified fire-retardant anti-static polyurethane and adhesive plaster |
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