CN113583446A - Antistatic silica gel protective film and preparation method thereof - Google Patents

Antistatic silica gel protective film and preparation method thereof Download PDF

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CN113583446A
CN113583446A CN202110819759.2A CN202110819759A CN113583446A CN 113583446 A CN113583446 A CN 113583446A CN 202110819759 A CN202110819759 A CN 202110819759A CN 113583446 A CN113583446 A CN 113583446A
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antistatic
silica gel
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CN113583446B (en
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周英杰
汪国明
麦启波
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Jiangsu Huangguan New Material Technology Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract

The invention belongs to the field of electronic product application, and particularly relates to an antistatic silica gel protective film and a preparation method thereof, wherein the antistatic silica gel protective film comprises an antistatic base material, a composite film arranged on the antistatic base material, and an antistatic silica gel layer arranged between the antistatic base material and the composite film, wherein the antistatic silica gel layer comprises the following components in parts by mass: 60-100 parts of high-low stripping silica gel, 0.05-3.0 parts of antistatic agent, 0.05-3.0 parts of conductive additive, 0.1-3 parts of dispersing additive, 0.5-2.5 parts of cross-linking agent, 0.5-2.5 parts of anchoring agent, 0.5-2.5 parts of catalyst and 50-200 parts of solvent. The invention adopts the compounding of the single-walled carbon nanotube and the antistatic agent, adopts the poisoning-prevention platinum catalyst to strengthen the curing, utilizes the synergy of the antistatic agent and the compounding of the single-walled carbon nanotube, reduces the using amount of the carbon tube, achieves the optical grade appearance requirement and reduces the resistance value, can effectively avoid the influence of the antistatic agent on the curing, plays a good antistatic effect, and can be used for the manufacturing process and the shipment protection process of electronic products.

Description

Antistatic silica gel protective film and preparation method thereof
Technical Field
The invention belongs to the field of electronic product application, and particularly relates to an antistatic silica gel protective film and a preparation method thereof.
Background
In the production and transportation process of electronic products, protective films are required to carry out corresponding protection, bottom supporting, waste discharge and other working procedures on corresponding parts, and silica gel protective films are increasingly applied in the electronic industry due to excellent uniform air exhaust performance and stable bonding performance. However, the silicone protective film has a limitation in some applications due to its inherent properties: for example, the resistance of a general silica gel protective film product is generally 10 because silica gel is a poor conductor for a high-requirement antistatic product12Above omega, static electricity can be gathered in the use, higher tear film voltage is produced, electronic components can be punctured in serious cases, the defects are caused, and the production cost of enterprises is increased.
At present, antistatic products of silica gel protective films are generally realized by adopting antistatic base materials, and high-requirement antistatic protective films are improved by superposing schemes of internally adding antistatic agents, wherein the internally adding schemes mainly comprise two categories of internally adding antistatic agents and conductive slurry, the currently commonly used internally adding antistatic agents easily cause platinum catalyst poisoning, the problems of poor curing, insufficient colloid strength and the like are generated, the stripping force of the protective film products in use is unstable, and under the serious condition, the problems of silicon transfer, even residual gum, degumming and the like can occur, so that the pasted objects are polluted, and electronic components are scrapped; in order to achieve a good conductive effect, most of the carbon nanotubes used in the conductive slurry are single-walled carbon nanotubes with a high length-diameter ratio, the length of the carbon nanotubes is usually more than 10 μm, the carbon nanotubes in the colloid can be mutually overlapped to form a conductive channel, and the resistance of the product is reduced.
Disclosure of Invention
The invention aims to solve the problems and provides an antistatic silica gel protective film and a preparation method thereof, which can effectively reduce the resistance value of a colloid, have good antistatic effect and can be used for the manufacturing process and the shipment protection process of electronic products.
According to the technical scheme of the invention, the antistatic silica gel protective film comprises an antistatic base material, a composite film arranged on the antistatic base material and an antistatic silica gel layer arranged between the antistatic base material and the composite film, wherein the antistatic silica gel layer comprises the following components in parts by mass: 60-100 parts of high-low stripping silica gel, 0.05-3.0 parts of antistatic agent, 0.05-3.0 parts of conductive auxiliary agent, 0.1-3 parts of dispersing auxiliary agent, 0.5-2.5 parts of cross-linking agent, 0.5-2.5 parts of anchoring agent, 0.5-2.5 parts of catalyst and 50-200 parts of solvent, wherein the catalyst is an allyl coordination complex platinum catalyst and is an anti-poisoning platinum catalyst.
In order to achieve a better antistatic effect, the antistatic agent and the conductive additive are mixed for use, and further, the poisoning-prevention platinum catalyst is adopted to strengthen the curing, so that the bad curing condition is prevented.
Furthermore, the substrate used by the antistatic substrate is PET (polyethylene terephthalate), PE (polyethylene) or PP (polypropylene), and the resistance value of the antistatic substrate is 104-109Ω。
Further, the composite film is made of PET, can be a PET original film, a non-silicon release film or a fluorine release film, and is specifically screened according to the peeling force of the protective film, so that the tearing force of the composite film is less than 15 g.
Further, the antistatic agent is a polythiophene system antistatic agent.
Further, the antistatic agent PEDOT (poly (3, 4-ethylenedioxythiophene)) and/or PEDOT: PSS (polyethylenedioxythiophene-poly (styrenesulfonate)).
Further, the conductive auxiliary agent is selected from one or more of carbon black slurry, carbon nanotube slurry, graphite slurry and graphene slurry.
Preferably carbon nanotube slurry, the carbon nanotubes in the carbon nanotube slurry are single-wall carbon nanotubes with the length of 2-10 mu m and the diameter of 1-10 nm. The single-walled carbon nanotube and the antistatic agent are compounded for use, the poisoning-prevention platinum catalyst is used for reinforcing curing, the antistatic agent is used for compounding the single-walled carbon nanotube in a synergistic manner, the using amount of the carbon tube is reduced, the optical-grade appearance requirement is met, the resistance value is reduced, meanwhile, the influence of the antistatic agent on curing can be effectively avoided, and a good antistatic effect is achieved.
Further, the dispersing auxiliary agent is organic silicon modified polyester.
Further, the high-low peeling silica gel is conventional organic silicon pressure-sensitive adhesive glue sold in the market, such as Dow high peeling silica gel
Figure BDA0003171445120000021
7657 and Low Peel glue Dow
Figure BDA0003171445120000022
7647;
The cross-linking agent is a conventional cross-linking agent sold in the market, such as Dow SYL-OFFTMSL 7028;
the anchoring agent is a conventional commercially available anchoring agent, such as Dow
Figure BDA0003171445120000031
297。
Further, the solvent is one or more of toluene, xylene and ethyl acetate.
In another aspect of the present invention, there is provided a method for preparing the above antistatic silica gel protective film, comprising the steps of,
s1: adding the high-low peeling silica gel, the conductive assistant, the dispersing assistant and part of the solvent into stirring equipment, and stirring for 30-60min at the rotating speed of 300-500 r/min;
s2: adding the residual solvent, the antistatic agent, the cross-linking agent, the anchoring agent and the catalyst into the material liquid obtained in the step S1, stirring at the rotating speed of 500-600r/min for 15-30min to ensure that the raw materials are fully stirred and uniformly dispersed to obtain antistatic silica gel material liquid;
s3: filtering the antistatic silica gel feed liquid, coating the antistatic silica gel feed liquid on an antistatic surface of an antistatic base material, drying, and covering a composite film to obtain the antistatic silica gel protective film;
the mass ratio of the high-low peeling silica gel to the low-peeling silica gel to the antistatic agent to the conductive auxiliary agent to the dispersing auxiliary agent to the crosslinking agent to the anchoring agent to the catalyst to the solvent is 60-100: 0.05-3.0: 0.05-3.0: 0.1-3: 0.5-2.5: 0.5-2.5: 0.5-2.5: 50-200.
Further, in the step S1, the change of components caused by overheating of the feed liquid is prevented, the temperature of the feed liquid is not higher than 45 ℃ during stirring, and when the temperature is too high, the circulating water can be connected for cooling.
Further, in the step S2, the remaining solvent, the antistatic agent, the crosslinking agent, the anchoring agent, and the catalyst are sequentially added, with the interval between the addition of the solvent and the catalyst being 3-5 min. By dispersing and adding, the reaction between components caused by high reactivity between small and medium materials of a platinum catalyst system is avoided.
Specifically, in the step S3, the filtering is performed by using 200-400 mesh filter cloth, and the coating is performed by using a micro-concave, slit or scraper.
Further, in the step, the thickness of the dried antistatic silica gel solution is 3-15 mu.
Compared with the prior art, the technical scheme of the invention has the following advantages: the short-chain single-wall carbon nano tube is adopted, and compared with the original carbon tube, the agglomeration condition is greatly improved; meanwhile, the compatibility of the dispersion auxiliary agent and a silica gel system is increased by matching with the dispersion auxiliary agent, so that the agglomeration degree can be further reduced; in addition, a proper amount of antistatic agent is added into the system for supplement, and the poisoning-prevention platinum catalyst is adopted for curing, through mixed use, the single-walled carbon nanotubes form a conductive network structure in the colloid, the antistatic agent is filled and enhanced, and the two are matched, so that on one hand, the aggregation degree is reduced, and simultaneously, the defect that the lapping effect of the short-chain carbon nanotubes is slightly weak is overcome, on the other hand, the using amount of the antistatic agent is reduced, and the defect of the antistatic agent in the using process is avoided to a certain extent.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Description of reference numerals: 1-antistatic base material, 2-antistatic silica gel layer and 3-composite film.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
The mass ratio of the high-low peeling silica gel in the following examples and comparative examples is 1: 1 Dow high-silica gel
Figure BDA0003171445120000041
7657 and Dow Low Peel glue
Figure BDA0003171445120000042
7647 the cross-linking agent is Dow SYL-OFFTMSL 7028, anchoring agent adopts Dow
Figure BDA0003171445120000043
297。
Example 1
As shown in fig. 1, an antistatic silica gel protective film includes an antistatic base material 1, a composite film 3 disposed on the antistatic base material 1, and an antistatic silica gel layer 2 disposed between the antistatic base material and the composite film. The antistatic silica gel layer comprises high-low peeling silica gel, PEDOT, single-wall carbon nanotube slurry (the length is 2-10 mu m, the diameter is 1-10nm, the same below), a dispersing auxiliary agent, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the addition mass ratio is 100: 0.3: 1: 1.5: 1.5: 1.0: 2.0: 180.
the preparation method of the antistatic silica gel protective film comprises the following steps:
s1, adding the high-low silica gel, the single-walled carbon nanotube slurry, the dispersing aid and part of toluene into stirring equipment, stirring at the rotating speed of 500r/min for 30-60min, controlling the temperature of the feed liquid not to be higher than 45 ℃ in the period, and switching on circulating water for cooling when the temperature is too high;
s2, after uniformly stirring, sequentially adding the residual toluene, PEDOT, cross-linking agent, anchoring agent and allyl coordination complex catalyst into the material liquid obtained in the step S1, wherein the feeding interval is 3-5min, and after all small materials are added, stirring at the rotating speed of 500-600r/min for 15-30 min;
s3, filtering the feed liquid obtained in the step S2 through 300-mesh filter cloth, and applying a micro-concave coating head to an antistatic substrate for resisting staticElectric surface (10)4-6Omega), drying, and then compounding a PET original film to obtain the corresponding antistatic silica gel protective film, wherein the thickness of the dried dry gel is 5-8 mu.
Example 2
An antistatic silica gel protection film comprises an antistatic base material, a composite film arranged on the antistatic base material and an antistatic silica gel layer arranged between the antistatic base material and the composite film. The antistatic silica gel layer comprises high-low peeling silica gel, PEDOT, single-walled carbon nanotube slurry, a dispersing aid, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the addition mass ratio is 100: 0.6: 0.8: 1.0: 1.5: 1.0: 1.5: 180.
the preparation method of the antistatic silica gel protective film is the same as that described in example 1.
Example 3
An antistatic silica gel protection film comprises an antistatic base material, a composite film arranged on the antistatic base material and an antistatic silica gel layer arranged between the antistatic base material and the composite film. The antistatic silica gel layer comprises high-low peeling silica gel, PEDOT, single-walled carbon nanotube slurry, a dispersing aid, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the addition mass ratio is 100: 0.3: 2.0: 2.0: 1.5: 1.0: 2.0: 180.
the preparation method of the antistatic silica gel protective film is the same as that described in example 1.
Example 4
An antistatic silica gel protection film comprises an antistatic base material, a composite film arranged on the antistatic base material and an antistatic silica gel layer arranged between the antistatic base material and the composite film. The antistatic silica gel layer comprises high-low peeling silica gel, PEDOT, single-walled carbon nanotube slurry, a dispersing aid, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the addition mass ratio is 100: 0.1: 0.5: 0.5: 1.5: 1.0: 2.0: 180.
the preparation method of the antistatic silica gel protective film is the same as that described in example 1.
Example 5
The PEDOT was replaced with PEDOT PSS on the basis of example 2.
Example 6
An antistatic silica gel protection film comprises an antistatic base material, a composite film arranged on the antistatic base material and an antistatic silica gel layer arranged between the antistatic base material and the composite film. The antistatic silica gel layer comprises high-low peeling silica gel, PEDOT, single-walled carbon nanotube slurry, a dispersing aid, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the addition mass ratio is 80: 1.5: 3: 3: 2.5: 0.5: 2.5: 100.
the preparation method of the antistatic silica gel protective film is the same as that described in example 1.
Example 7
An antistatic silica gel protection film comprises an antistatic base material, a composite film arranged on the antistatic base material and an antistatic silica gel layer arranged between the antistatic base material and the composite film. The antistatic silica gel layer comprises high-low peeling silica gel, PEDOT, single-walled carbon nanotube slurry, a dispersing aid, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the addition mass ratio is 60: 3: 0.1: 0.1: 0.5: 2.5: 0.5: 50.
the preparation method of the antistatic silica gel protective film is the same as that described in example 1.
Examples 8 to 9
Toluene was replaced with xylene and ethyl acetate, respectively, on the basis of example 1.
Examples 10 to 12
The single-wall carbon nanotube slurry is replaced by carbon black slurry, graphite slurry and graphene slurry on the basis of the embodiment 1.
Comparative example 1
A protective film comprises an antistatic base material, a composite film arranged on the antistatic base material and a silica gel layer arranged between the antistatic base material and the composite film. The silica gel layer comprises high-low peeling silica gel, a conductive auxiliary agent, a cross-linking agent, an anchoring agent, an allyl coordination complex platinum catalyst and toluene, and the adding mass ratio is 100: 2.0: 1.5: 1.0: 2.0: 180, the conductive auxiliary agent is a long-chain single-walled carbon nanotube.
The protective film was prepared as described in example 1.
Comparative example 2
A protective film comprises an antistatic base material, a composite film arranged on the antistatic base material and a silica gel layer arranged between the antistatic base material and the composite film. The silica gel layer comprises high-low peeling silica gel, an antistatic agent, a cross-linking agent, an anchoring agent, a vinyl complexing and coordinating platinum catalyst and toluene, and the adding mass ratio is 100: 0.8: 1.5: 1.0: 2.0: 180.
the protective film was prepared as described in example 1.
The antistatic silica gel protective films obtained in examples 1 to 4 and the protective films obtained in comparative examples 1 to 2 were subjected to comprehensive performance tests, and the test results are shown in the following table:
Figure BDA0003171445120000071
from the test result, the antistatic agent, the conductive additive, the dispersing additive and the anti-poisoning catalyst are mixed for use, so that the resistance value of the protective film can be reduced, the conductivity can be improved, meanwhile, the problems of rapid residual reduction, poor appearance and the like do not occur, and the product can achieve better comprehensive performance.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.

Claims (10)

1. The utility model provides an antistatic silica gel protection film, is in including antistatic substrate, setting complex film on the antistatic substrate with set up in antistatic substrate with antistatic silica gel layer between the complex film, its characterized in that, according to the mass fraction, antistatic silica gel layer includes: 60-100 parts of high-low stripping silica gel, 0.05-3.0 parts of antistatic agent, 0.05-3.0 parts of conductive auxiliary agent, 0.1-3 parts of dispersing auxiliary agent, 0.5-2.5 parts of cross-linking agent, 0.5-2.5 parts of anchoring agent, 0.5-2.5 parts of catalyst and 50-200 parts of solvent, wherein the catalyst is a platinum catalyst complexed by allyl coordination.
2. The antistatic silica gel protective film of claim 1 wherein the antistatic agent is a polythiophene system antistatic agent.
3. The antistatic silica gel protective film of claim 2 wherein the antistatic agent is PEDOT and/or PEDOT: PSS.
4. The antistatic silica gel protective film of claim 1 wherein the conductive additive is selected from one or more of carbon black slurry, carbon nanotube slurry, graphite slurry and graphene slurry.
5. The antistatic silica gel protective film of claim 4 wherein the carbon nanotubes in the carbon nanotube slurry are single-walled carbon nanotubes having a length of 2 to 10 μm and a diameter of 1 to 10 nm.
6. The antistatic silicone protective film of claim 1 wherein the dispersing aid is a silicone modified polyester.
7. The antistatic silica gel protective film of claim 1 wherein the solvent is one or more of toluene, xylene and ethyl acetate.
8. The method for preparing an antistatic silica gel protective film according to any one of claims 1 to 7, comprising the steps of,
s1: adding the high-low peeling silica gel, the conductive assistant, the dispersing assistant and part of the solvent into stirring equipment, and stirring for 30-60min at the rotating speed of 300-500 r/min;
s2: adding the residual solvent, the antistatic agent, the cross-linking agent, the anchoring agent and the catalyst into the feed liquid obtained in the step S1, and stirring at the rotating speed of 500-600r/min for 15-30min to obtain antistatic silica gel feed liquid;
s3: filtering the antistatic silica gel feed liquid, coating the antistatic silica gel feed liquid on an antistatic surface of an antistatic base material, drying, and covering a composite film to obtain the antistatic silica gel protective film;
the mass ratio of the high-low peeling silica gel to the low-peeling silica gel to the antistatic agent to the conductive auxiliary agent to the dispersing auxiliary agent to the crosslinking agent to the anchoring agent to the catalyst to the solvent is 60-100: 0.05-3.0: 0.05-3.0: 0.1-3: 0.5-2.5: 0.5-2.5: 0.5-2.5: 50-200.
9. The method according to claim 8, wherein in the step S1, the temperature of the feed liquid during stirring is not higher than 45 ℃.
10. The method of claim 8, wherein the residual solvent, the antistatic agent, the crosslinking agent, the anchoring agent and the catalyst are added sequentially at an interval of 3-5min in step S2.
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Citations (6)

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US20150267063A1 (en) * 2012-10-11 2015-09-24 Byk-Chemie Gmbh Coating Composition and Use Thereof
CN104995257A (en) * 2013-02-15 2015-10-21 信越聚合物株式会社 Curable antistatic organopolysiloxane composition and antistatic silicone film
CN107312471A (en) * 2017-07-28 2017-11-03 宁波启合新材料科技有限公司 A kind of antistatic protection film and its manufacture method
CN107602861A (en) * 2017-08-28 2018-01-19 哈尔滨工业大学无锡新材料研究院 A kind of waterborne flame retardant fluorine containing silicone oil and preparation method thereof
CN109666402A (en) * 2018-12-29 2019-04-23 中山市聚力有机硅技术有限公司 A kind of anti-static release lotion and preparation method thereof with good stability energy
CN109913142A (en) * 2019-03-01 2019-06-21 苏州格睿光电科技有限公司 A kind of antistatic property organic pressure-sensitive gel product

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150267063A1 (en) * 2012-10-11 2015-09-24 Byk-Chemie Gmbh Coating Composition and Use Thereof
CN104995257A (en) * 2013-02-15 2015-10-21 信越聚合物株式会社 Curable antistatic organopolysiloxane composition and antistatic silicone film
CN107312471A (en) * 2017-07-28 2017-11-03 宁波启合新材料科技有限公司 A kind of antistatic protection film and its manufacture method
CN107602861A (en) * 2017-08-28 2018-01-19 哈尔滨工业大学无锡新材料研究院 A kind of waterborne flame retardant fluorine containing silicone oil and preparation method thereof
CN109666402A (en) * 2018-12-29 2019-04-23 中山市聚力有机硅技术有限公司 A kind of anti-static release lotion and preparation method thereof with good stability energy
CN109913142A (en) * 2019-03-01 2019-06-21 苏州格睿光电科技有限公司 A kind of antistatic property organic pressure-sensitive gel product

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