CN114350309A - Flame-retardant silica gel pressure-sensitive adhesive, preparation method and adhesive tape - Google Patents
Flame-retardant silica gel pressure-sensitive adhesive, preparation method and adhesive tape Download PDFInfo
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- CN114350309A CN114350309A CN202111636843.7A CN202111636843A CN114350309A CN 114350309 A CN114350309 A CN 114350309A CN 202111636843 A CN202111636843 A CN 202111636843A CN 114350309 A CN114350309 A CN 114350309A
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- flame
- sensitive adhesive
- retardant
- silica gel
- gel pressure
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000003063 flame retardant Substances 0.000 title claims abstract description 101
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 70
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000000741 silica gel Substances 0.000 title claims abstract description 69
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 69
- 239000002390 adhesive tape Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 methyl phenyl vinyl Chemical group 0.000 claims abstract description 40
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 39
- 229920001971 elastomer Polymers 0.000 claims abstract description 23
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 238000009833 condensation Methods 0.000 claims abstract description 5
- 230000005494 condensation Effects 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229920002379 silicone rubber Polymers 0.000 claims description 6
- 239000004945 silicone rubber Substances 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- 229920002554 vinyl polymer Polymers 0.000 claims description 5
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 4
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 125000003944 tolyl group Chemical group 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000011247 coating layer Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- MOSXLDGILGBOSZ-UHFFFAOYSA-N ethenyl-methyl-phenylsilicon Chemical compound C=C[Si](C)C1=CC=CC=C1 MOSXLDGILGBOSZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000002459 sustained effect Effects 0.000 abstract description 4
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000013464 silicone adhesive Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical group C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/50—Adhesives in the form of films or foils characterised by a primer layer between the carrier and the adhesive
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2479/00—Presence of polyamine or polyimide
- C09J2479/08—Presence of polyamine or polyimide polyimide
- C09J2479/086—Presence of polyamine or polyimide polyimide in the substrate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
- C09J2483/003—Presence of polysiloxane in the primer coating
Abstract
The invention provides a flame-retardant silica gel pressure-sensitive adhesive which comprises the following raw materials in parts by weight: 100 portions of methyl phenyl vinyl silicone crude rubber and 120 portions of methyl phenyl vinyl silicone crude rubber; 120-180 parts of methyl polysiloxane resin; 20-50 parts of a flame retardant; 2-4 parts of an organotin condensation catalyst; 1-2 parts of a crosslinking agent; and 300 portions of solvent 250-. The invention also provides a preparation method and the adhesive tape. The intumescent flame retardant is used for enabling the flame-retardant silica gel pressure-sensitive adhesive to have flame retardant performance and environmental protection. Adopting methyl phenyl vinyl silicone crude rubber to introduce phenyl into the flame-retardant silica gel pressure-sensitive adhesive so as to improve the flame-retardant property of the flame-retardant silica gel pressure-sensitive adhesive; the methyl polysiloxane resin is adopted to improve the modulus of the flame-retardant silica gel pressure-sensitive adhesive, so that the viscosity of the flame-retardant silica gel pressure-sensitive adhesive is improved. The dosage of the methyl phenyl vinyl silicon and methyl polysiloxane resin is limited, so that the prepared flame-retardant silica gel pressure-sensitive adhesive has low initial viscosity and high sustained viscosity. The flame-retardant silica gel pressure-sensitive adhesive is used for preparing adhesive tapes, and the prepared adhesive tapes have the advantages of high temperature resistance, low initial adhesion, high lasting adhesion, high stripping force and high flame retardance.
Description
Technical Field
The invention belongs to the technical field of silica gel materials, and particularly relates to a flame-retardant silica gel pressure-sensitive adhesive, a preparation method and an adhesive tape.
Background
With the rapid development of industry, the existing adhesive tapes on the market meet partial requirements of people to a certain extent, and more environment-friendly adhesive tapes are used in electronic component systems in the fields of automobiles, household appliances, toy ornaments, communication, aviation, aerospace and the like, and especially the requirement on the adhesive tapes in the fields of aviation and aerospace is higher, and the requirement on flame retardance is required. The flame retardance refers to the condition that the flame-retardant material is non-combustible and self-extinguishes when meeting fire, and the purpose can be achieved by adding proper flame retardant. At present, the domestic flame-retardant organic adhesive is few in variety, most of flame-retardant products in the existing adhesive tape are halogen flame-retardant, byproducts pollute the environment, and the safety is low.
Disclosure of Invention
In order to achieve the above object, the present invention is achieved by the following technical solutions.
The invention provides a flame-retardant silica gel pressure-sensitive adhesive for preparing an adhesive tape, which comprises the following raw materials in parts by weight:
preferably, the methyl phenyl vinyl silicone crude rubber has a phenyl content of 5% -10% and a vinyl content of 2% -5%.
Preferably, the methyl polysiloxane resin has methyl groups at both ends of the molecular chain.
Preferably, the flame retardant is ammonium polyphosphate.
Preferably, the cross-linking agent is benzoyl peroxide.
Preferably, the solvent is toluene or xylene.
The invention also provides a preparation method of the flame-retardant silica gel pressure-sensitive adhesive, which comprises the following steps:
s1, taking a certain amount of solvent to dissolve methyl phenyl vinyl silicone crude rubber to obtain crude rubber dissolving liquid;
s2, introducing nitrogen, sequentially adding the rest solvent, methyl polysiloxane resin and the crude rubber dissolving solution prepared in the step S1 into a reaction container, and heating to dissolve to obtain a mixed solution;
s3, adding an organotin condensation catalyst into the mixed solution prepared in the step S2, heating, stirring and carrying out heat preservation reaction;
s4, adding a cross-linking agent into the reaction liquid obtained in the step S3, stirring, and reacting to obtain a glue liquid;
and S5, adding the intumescent flame retardant into the glue solution obtained in the step S4, stirring, reacting, and cooling to obtain the flame-retardant silica gel pressure-sensitive adhesive.
Preferably, in step S1, the weight ratio of the solvent to the methyl phenyl vinyl silicone gum is (10-12): (5-6); in step S2, the heating temperature is 80-90 ℃; in step S3, the heating temperature is 130-145 ℃, and the reaction time is 2-4 h.
Preferably, in the step S4, the reaction temperature is 130-145 ℃, and the reaction time is 15-40 min; in step S5, the reaction temperature is 130-145 ℃, and the reaction time is 25-50 min.
The third purpose of the invention is to provide the adhesive tape, which at least sequentially comprises a release film layer, a flame-retardant silica gel pressure-sensitive adhesive layer, a bottom coating and a flame-retardant substrate; the flame-retardant silica gel pressure-sensitive adhesive layer is formed by coating and curing the flame-retardant silica gel pressure-sensitive adhesive.
Compared with the prior art, the invention has the beneficial effects that:
according to the flame-retardant silica gel pressure-sensitive adhesive provided by the invention, the intumescent flame retardant is added, so that the prepared flame-retardant silica gel pressure-sensitive adhesive has good flame retardance, is environment-friendly and green and does not contain halogen; adopting methyl phenyl vinyl silicone crude rubber to introduce phenyl into the flame-retardant silica gel pressure-sensitive adhesive so as to improve the flame-retardant property of the flame-retardant silica gel pressure-sensitive adhesive; the methyl polysiloxane resin is adopted to improve the modulus of the flame-retardant silica gel pressure-sensitive adhesive, so that the viscosity of the flame-retardant silica gel pressure-sensitive adhesive is improved. The dosage of the methyl phenyl vinyl silicon and methyl polysiloxane resin is limited, so that the prepared flame-retardant silica gel pressure-sensitive adhesive has low initial viscosity and high sustained viscosity. The flame-retardant silica gel pressure-sensitive adhesive is used for preparing adhesive tapes, and the prepared adhesive tapes have the advantages of high temperature resistance, low initial adhesion, high lasting adhesion, high stripping force and high flame retardance.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a cross-sectional view of the flame-retardant silicone adhesive tape of the present invention;
FIG. 2 is a flow chart of the steps of the preparation method of the present invention.
In the figure: 100. a flame retardant silicone adhesive tape; 10. a release film layer; 20. a flame-retardant silica gel pressure-sensitive adhesive layer; 30. a primer layer; 40. a flame retardant substrate.
Detailed Description
The foregoing and other objects, features, aspects and advantages of the present invention will become more apparent to those skilled in the art from the following detailed description, which, taken in conjunction with the annexed drawings, discloses a full and partial embodiment of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
The invention provides a flame-retardant silica gel pressure-sensitive adhesive for preparing an adhesive tape, which comprises the following raw materials in parts by weight:
in the embodiment, the intumescent flame retardant is added, so that the prepared flame-retardant silica gel pressure-sensitive adhesive has good flame retardance, is environment-friendly and does not contain halogen. Methyl phenyl vinyl silicone crude rubber is adopted as a matrix material to participate in reaction to form the pressure-sensitive adhesive, and in addition, phenyl is introduced into the flame-retardant silica gel pressure-sensitive adhesive to improve the flame retardant property of the flame-retardant silica gel pressure-sensitive adhesive. The methyl polysiloxane resin is adopted to improve the modulus of the flame-retardant silica gel pressure-sensitive adhesive, so that the viscosity of the flame-retardant silica gel pressure-sensitive adhesive is improved. The dosage of the methyl phenyl vinyl silicon and methyl polysiloxane resin is limited, so that the prepared flame-retardant silica gel pressure-sensitive adhesive has low initial viscosity and high sustained viscosity.
In one embodiment, the methyl phenyl vinyl silicone rubber has a phenyl content of 5% to 10% and a vinyl content of 2% to 5%. Specifically, the phenyl content is 5-10% so as to improve the flame retardance of the flame-retardant silica gel pressure-sensitive adhesive and avoid the influence of overhigh phenyl content on the processability, high temperature resistance and vulcanization performance of the methyl phenyl vinyl silicone crude adhesive. The vinyl content of 2% -5% enables methyl phenyl vinyl silicone crude rubber to better participate in vulcanization reaction, reduces internal stress of the prepared flame-retardant silica gel pressure-sensitive adhesive, and further improves the bonding performance of the flame-retardant silica gel pressure-sensitive adhesive.
Further, the molecular weight of the methyl phenyl vinyl silicone rubber is 600000-700000.
In one embodiment, the methyl polysiloxane resin has methyl groups at both ends of the molecular chain.
Further, the molecule of the methylpolysiloxane resin was 5000-7000.
Further, the flame retardant is ammonium polyphosphate.
In one embodiment, the cross-linking agent is benzoyl peroxide, so that macromolecules of the methyl phenyl vinyl silicone rubber are converted into a three-dimensional network structure, thereby improving the strength, the heat resistance, the wear resistance and the solvent resistance.
In one embodiment, the solvent is toluene or xylene.
The invention also provides a preparation method of the flame-retardant silica gel pressure-sensitive adhesive, as shown in fig. 2, comprising the following steps:
s1, taking a certain amount of solvent to dissolve methyl phenyl vinyl silicone crude rubber to obtain crude rubber dissolving liquid;
s2, introducing nitrogen, sequentially adding the rest solvent, methyl polysiloxane resin and the crude rubber dissolving solution prepared in the step S1 into a reaction container, and heating to dissolve to obtain a mixed solution;
s3, adding an organotin condensation catalyst into the mixed solution prepared in the step S2, heating, stirring and carrying out heat preservation reaction;
s4, adding a cross-linking agent into the reaction liquid obtained in the step S3, stirring, and reacting to obtain a glue liquid;
and S5, adding the intumescent flame retardant into the glue solution obtained in the step S4, stirring, reacting, and cooling to obtain the flame-retardant silica gel pressure-sensitive adhesive.
In one embodiment, in step S1, the weight ratio of the solvent to the methyl phenyl vinyl silicone rubber is (10-12): (5-6) to adjust the viscosity of the methyl phenyl vinyl silicone rubber for subsequent operation.
In one embodiment, in step S2, the heating temperature is 80 ℃ to 90 ℃.
In one embodiment, in step S3, the heating temperature is 130-145 ℃, and the reaction time is 2-4 h.
In one embodiment, in step S4, the reaction temperature is 130-145 ℃ and the reaction time is 15-40 min.
In one embodiment, in step S5, the reaction temperature is 130-145 ℃ and the reaction time is 25-50 min.
The invention also provides an adhesive tape, as shown in fig. 1, comprising a flame-retardant silica gel adhesive tape 100, wherein the flame-retardant silica gel adhesive tape 100 at least sequentially comprises a release film layer 10, a flame-retardant silica gel pressure-sensitive adhesive layer 20, a primer layer 30 and a flame-retardant base material 40; the flame-retardant silica gel pressure-sensitive adhesive layer 20 is formed by coating and curing the flame-retardant silica gel pressure-sensitive adhesive.
In one embodiment, the primer layer 30 is a silicone layer having a thickness of less than 1 μm.
In one embodiment, the thickness of the flame retardant silicone pressure sensitive adhesive layer 20 is 15-30 μm.
In one embodiment, the flame retardant substrate 40 is a PI film.
In one embodiment, the release film layer 10 is a transparent fluorine release film layer.
Specifically, the preparation method of the adhesive tape comprises the following steps: coating silica gel on one surface of the corona layer of the flame-retardant base material 40, and curing to form a base coat layer 30; the surface of the primer layer 30 is coated with the flame-retardant silica gel pressure-sensitive adhesive, cured at a high temperature of 180-190 ℃, and attached with the release film layer 10 to obtain the flame-retardant silica gel adhesive tape 100.
In order to illustrate the invention herein, specific examples are set forth below. It should be understood that these examples are for illustrative purposes only and are not to be construed as limiting the invention in any way.
Example 1
The invention provides an adhesive tape, which sequentially comprises a release film layer 10, a flame-retardant silica gel pressure-sensitive adhesive layer 20, a bottom coating layer 30 and a flame-retardant base material 40; wherein the release film layer 10 is a transparent fluorine release film layer with the thickness of 50 μm; the thickness of the flame-retardant silica gel pressure-sensitive adhesive layer 20 is 20 μm; the bottom coating 30 is a silica gel layer with a thickness of 0.9 μm; the flame-retardant base material 40 is a PI film layer with the thickness of 36 mu m; wherein, the flame-retardant silica gel pressure-sensitive adhesive layer 20 is coated and cured by adopting a flame-retardant silica gel pressure-sensitive adhesive; the flame-retardant silica gel pressure-sensitive adhesive comprises the following raw materials in parts by weight:
wherein the molecular weight of the methyl phenyl vinyl silicone crude rubber is 600000, the content of phenyl in the methyl phenyl vinyl silicone crude rubber is 8%, and the content of vinyl is 4%; methyl polysiloxane resin has methyl at both ends of molecular chain, and its molecular weight is 6000.
The preparation method of the flame-retardant silica gel pressure-sensitive adhesive comprises the following steps:
(1) dissolving 100 parts of methyl phenyl vinyl silicon crude rubber in 200 parts of dimethylbenzene to obtain crude rubber dissolving liquid;
(2) introducing nitrogen, sequentially adding 80 parts of dimethylbenzene, 120 parts of methyl polysiloxane resin and crude rubber dissolving liquid into a reaction container, and heating to 80 ℃ within 20 ℃ until the materials are dissolved to obtain mixed liquid;
(3) adding 2 parts of organic tin condensation catalyst into the mixed solution prepared in the step (2), heating, stirring and heating to 130 ℃, and carrying out heat preservation reaction for 3 hours;
(4) adding 1 part of benzoyl peroxide cross-linking agent into the reaction liquid in the step (3), and reacting for 20min at 130 ℃ to obtain glue liquid;
(5) and (4) adding 20 parts of ammonium polyphosphate into the glue solution obtained in the step (4), stirring for 30min at 130 ℃, and cooling to obtain the flame-retardant silica gel pressure-sensitive adhesive.
Example 2
The invention provides an adhesive tape, which is different from the adhesive tape in embodiment 1 in that a flame-retardant silica gel pressure-sensitive adhesive layer 20 is prepared by coating flame-retardant silica gel pressure-sensitive adhesive and comprises the following raw materials in parts by weight:
when the flame-retardant silica gel pressure-sensitive adhesive is prepared, 210 parts of dimethylbenzene is used for dissolving methyl phenyl vinyl silicone crude rubber. The rest of the preparation process is the same as in example 1.
Example 3
The invention provides an adhesive tape, which is different from the adhesive tape in embodiment 1 in that a flame-retardant silica gel pressure-sensitive adhesive layer 20 is prepared by coating flame-retardant silica gel pressure-sensitive adhesive and comprises the following raw materials in parts by weight:
when the flame-retardant silica gel pressure-sensitive adhesive is prepared, 220 parts of dimethylbenzene is used for dissolving methyl phenyl vinyl silicone crude rubber. The rest of the preparation process is the same as in example 1.
Comparative example 1
Flame retardant tape-DS 10B 6F.
Comparative example 2
An adhesive tape was different from example 2 in that methyl phenyl vinyl silicone was replaced with methyl vinyl silicone in the pressure-sensitive adhesive raw material.
Comparative example 3
An adhesive tape was different from example 2 in that methyl phenyl vinyl silicone gum in the pressure-sensitive adhesive raw material was replaced with methyl silicone gum.
Example 4
The tapes prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to a performance test.
And (3) testing the peel strength: testing according to standard GB 2792-81.
Tack-holding test: tested according to standard GB 4851-8.
Initial tack test: tested according to standard GB 4852-2002.
And (3) testing the flame retardance: the expression "oxygen index" means that a material of a predetermined size is charged into an experimental apparatus, a mixed gas of oxygen and nitrogen is introduced under a predetermined condition, the material is ignited by an igniter, and the minimum oxygen concentration (%) necessary for maintaining the wax-like sustained combustion is measured. The lowest oxygen concentration in the oxygen/nitrogen mixed system required for the smooth combustion of the adhesive tape was determined with an oxygen index meter according to GB/T5454-1997 standard.
The test results are shown in table one.
Watch 1
As can be seen from table one, the flame-retardant silicone adhesive tape 100 of the present invention maintains a high 180 ° peel strength, has high tensile strength, is resistant to high temperature, has significantly improved permanent adhesion, has good stability, and reduces initial adhesion. Compared with comparative examples 2 and 3, the introduction of phenyl groups in example 2 can obviously improve the flame retardant property of the adhesive tape.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can readily practice the invention as shown and described in the drawings and detailed description herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the scope of the invention as defined by the appended claims; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The flame-retardant silica gel pressure-sensitive adhesive is characterized by being used for preparing an adhesive tape and comprising the following raw materials in parts by weight:
2. the flame-retardant silicone pressure-sensitive adhesive according to claim 1, wherein the methyl phenyl vinyl silicone rubber has a phenyl content of 5% to 10% and a vinyl content of 2% to 5%.
3. The pressure-sensitive adhesive according to claim 1, wherein the methyl polysiloxane resin has methyl groups at both ends of the molecular chain.
4. The flame-retardant silica gel pressure-sensitive adhesive as claimed in claim 1, wherein the flame retardant is ammonium polyphosphate.
5. The flame-retardant silicone pressure-sensitive adhesive of claim 1, wherein the cross-linking agent is benzoyl peroxide.
6. The flame-retardant silica gel pressure-sensitive adhesive according to claim 1, wherein the solvent is toluene or xylene.
7. The preparation method of the flame-retardant silica gel pressure-sensitive adhesive according to any one of 1 to 6, which is characterized by comprising the following steps:
s1, taking a certain amount of solvent to dissolve methyl phenyl vinyl silicone crude rubber to obtain crude rubber dissolving liquid;
s2, introducing nitrogen, sequentially adding the rest solvent, methyl polysiloxane resin and the crude rubber dissolving solution prepared in the step S1 into a reaction container, and heating to dissolve to obtain a mixed solution;
s3, adding an organotin condensation catalyst into the mixed solution prepared in the step S2, heating, stirring and carrying out heat preservation reaction;
s4, adding a cross-linking agent into the reaction liquid obtained in the step S3, stirring, and reacting to obtain a glue liquid;
and S5, adding the intumescent flame retardant into the glue solution obtained in the step S4, stirring, reacting, and cooling to obtain the flame-retardant silica gel pressure-sensitive adhesive.
8. The method according to claim 7, wherein in step S1, the weight ratio of the solvent to the methyl phenyl vinyl silicone gum is (10-12): (5-6); in step S2, the heating temperature is 80-90 ℃.
9. The preparation method according to claim 7, wherein in step S3, the heating temperature is 130-145 ℃, the reaction time is 2-4 h; in step S4, the reaction temperature is 130-145 ℃, and the reaction time is 15-40 min; in step S5, the reaction temperature is 130-145 ℃, and the reaction time is 25-50 min.
10. The adhesive tape is characterized by at least sequentially comprising a release film layer (10), a flame-retardant silica gel pressure-sensitive adhesive layer (20), a bottom coating layer (30) and a flame-retardant base material (40); the flame-retardant silica gel pressure-sensitive adhesive layer (20) is formed by coating and curing the flame-retardant silica gel pressure-sensitive adhesive according to any one of claims 1 to 6.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492390A (en) * | 2011-12-12 | 2012-06-13 | 长春中科应化特种材料有限公司 | Silicon rubber self-melting belt and production method thereof |
| CN109705766A (en) * | 2018-12-24 | 2019-05-03 | 昆山诺泰普复合新材料有限公司 | A kind of high-performance refractory type silicon rubber self-adhesive tape and its preparation process |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492390A (en) * | 2011-12-12 | 2012-06-13 | 长春中科应化特种材料有限公司 | Silicon rubber self-melting belt and production method thereof |
| CN109705766A (en) * | 2018-12-24 | 2019-05-03 | 昆山诺泰普复合新材料有限公司 | A kind of high-performance refractory type silicon rubber self-adhesive tape and its preparation process |
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| Title |
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| 曾广根 等, 四川大学出版社 * |
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