CN112961622B - Sealing adhesive tape and preparation method and application thereof - Google Patents
Sealing adhesive tape and preparation method and application thereof Download PDFInfo
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- CN112961622B CN112961622B CN202110287097.9A CN202110287097A CN112961622B CN 112961622 B CN112961622 B CN 112961622B CN 202110287097 A CN202110287097 A CN 202110287097A CN 112961622 B CN112961622 B CN 112961622B
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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
- 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
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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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/26—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers modified by chemical after-treatment
- C09J123/28—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
- C09J123/283—Halogenated homo- or copolymers of iso-olefines
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention provides a sealing adhesive tape and a preparation method and application thereof. The sealing adhesive tape comprises the following raw materials in parts by weight: 5-30 parts of natural rubber, 70-95 parts of brominated butyl rubber, 1-3 parts of a homogenizing agent, 20-50 parts of polyisobutylene, 2-4 parts of tackifying resin, 0.5-5 parts of an active agent, 2-5 parts of a plasticizer, 100-150 parts of a filler, 0.1-2 parts of a vulcanization accelerator and 2-6 parts of a vulcanization aid. The invention exerts the excellent comprehensive performance of the sealing adhesive tape material, endows the sealing adhesive tape with better high temperature resistance, oil resistance, high viscosity, excellent air tightness at 230 ℃, and has the characteristics of no residual adhesive remaining on the mold when the sealing adhesive tape is separated from a manufacturing mold. The sealing tape can be widely applied to the molding production of components such as fan blades, airplanes and the like.
Description
Technical Field
The invention belongs to the technical field of rubber, particularly relates to a sealing adhesive tape, a preparation method and application thereof, and particularly relates to a high-temperature vacuum bag sealing adhesive tape with high strength, good cleaning performance and high resistance, and a preparation method and application thereof.
Background
Advanced airplanes, missiles, rockets, wind power generation blades and the like are widely made of resin-based composite materials. At present, the molding of the composite material is mostly prepared by an autoclave molding process, and vacuum bag sealing is needed in the curing molding process of the part, namely the vacuum bag molding process. The vacuum bag forming process has the characteristics of flexibility, simplicity, convenience, high efficiency and the like, so that the vacuum bag forming process is widely applied to various large host factories, wind power generation assembly centers and the like. In the manufacturing process of the fan blade and the airplane component, the vacuum bag and the mold need to be sealed while vacuumizing, and therefore an adhesive tape with good sealing performance is needed for sealing. The resin matrix of the high-performance composite material is epoxy resin, bismaleimide, cyanate ester and the like, the curing temperature is high, and continuous heat preservation and pressure maintaining are needed in the resin prepreg forming process, so that more rigorous requirements on the performance of the sealing adhesive tape with the air sealing effect are provided.
CN104861895A discloses a high temperature resistant low-viscosity vacuum bag sealing tape, which uses butyl rubber and brominated butyl rubber as base materials, polyisobutylene as tackifier, calcium carbonate, kaolin and talc powder as fillers, and other additives are stirred, mixed and extruded to form. The sealing adhesive tape mainly adopts brominated butyl rubber, has low strength, cannot ensure the cleaning performance of the contact surface of the sealing adhesive tape and a tool after the sealing adhesive tape is taken out of a tank, has limited applicable temperature, and has limited hot press molding process capable of being matched.
CN101402764A discloses a wind navigation room temperature vacuum sealing adhesive tape and its production method, which uses butyl rubber, chlorosulfonated polyethylene, polyisobutylene, calcium carbonate, 201 brominated hydroxymethyl tert-octyl phenolic resin, etc. as main matrix to prepare the vacuum sealing adhesive tape. The mentioned sealing adhesive tape adopts chlorosulfonated polyethylene as a high-activity rubber matrix, and influences the elasticity, high temperature resistance and air tightness of the sealant.
Therefore, it is necessary to prepare an adhesive tape with high strength, good cleaning performance, high temperature resistance and good air tightness.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a sealing adhesive tape, a preparation method and application thereof. The sealing adhesive tape mainly aims to solve the problems that the high-temperature adhesive tape in the existing market is unstable in temperature resistance, has adhesive residue at high temperature, and is low in strength and poor in viscosity. The highest temperature resistance can reach 230 ℃, no residual adhesive is left after demoulding, and the adhesive tape can be integrally stripped from a corresponding tool.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a sealing tape, which comprises the following raw materials in parts by weight:
according to the invention, the combination of natural rubber and bromobutyl rubber with a certain proportion is used as the matrix rubber of the sealing adhesive tape, so that the sealing adhesive tape has the characteristic of high strength at normal temperature, the defect of poor cleaning performance of the adhesive tape after being taken out of a tank at the later stage is overcome, meanwhile, a homogenizing agent is adopted in the formula to improve the interface compatibility of polar rubber and non-polar rubber matrix rubber, improve the mixing uniformity of materials, and avoid the problems of unstable size of the adhesive tape in the extrusion process, dense hemp bubbles on the surface of the adhesive tape, which is in contact with a tool after being taken out of a hot-pressing tank, and the like. The components are mutually matched, so that the temperature resistance and the stability of the adhesive tape are further improved, the problems of adhesive residue, low strength and poor viscosity at high temperature are solved, the maximum temperature resistance reaches above 230 ℃, no adhesive residue exists after demolding, and the adhesive tape can be integrally stripped from a corresponding tool.
In the present invention, the natural rubber is contained in an amount of 5 to 30 parts, for example, 5 parts, 7 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts, 30 parts, etc.
In the present invention, the brominated butyl rubber is contained in an amount of 70 to 95 parts, and may be, for example, 70 parts, 72 parts, 75 parts, 76 parts, 78 parts, 80 parts, 82 parts, 84 parts, 86 parts, 88 parts, 90 parts, 92 parts, 93 parts, 95 parts, etc.
In the present invention, the content of the leveling agent is 1 to 3 parts, and may be, for example, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts, 3 parts, etc.
In the present invention, the polyisobutylene content is 20 to 50 parts, and may be, for example, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts, 30 parts, 32 parts, 34 parts, 36 parts, 38 parts, 40 parts, 42 parts, 44 parts, 46 parts, 48 parts, 50 parts, or the like.
In the present invention, the tackifier resin content is 2 to 4 parts, and may be, for example, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts, 3 parts, 3.2 parts, 3.4 parts, 3.6 parts, 3.8 parts, 4 parts, or the like.
In the present invention, the active agent is contained in an amount of 0.5 to 5 parts, and may be, for example, 0.5 part, 0.8 part, 1 part, 1.2 parts, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, or the like.
In the present invention, the plasticizer content is 2 to 5 parts, and may be, for example, 2 parts, 2.2 parts, 2.5 parts, 2.8 parts, 3 parts, 3.2 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, or the like.
In the present invention, the content of the filler is 100 to 150 parts, and may be, for example, 100 parts, 105 parts, 110 parts, 115 parts, 120 parts, 125 parts, 130 parts, 135 parts, 140 parts, 145 parts, 150 parts, or the like.
In the present invention, the content of the vulcanization accelerator is 0.1 to 2 parts, and may be, for example, 0.1 part, 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts or the like.
In the present invention, the content of the vulcanization aid is 2 to 6 parts, and may be, for example, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, or the like.
Preferably, the natural rubber is selected from any one of natural rubber 10#, natural rubber 20# or natural rubber SCR5 or the combination of at least two of the natural rubber.
Preferably, the brominated butyl rubber is selected from brominated butyl rubber 2030 and/or brominated butyl rubber 2255.
Preferably, the homogenizing agent is homogenizing agent RH-150.
In the invention, aiming at the mixture of polar rubber brominated butyl rubber and non-polar natural rubber, RH150 consisting of low molecular resins with different polarities such as aliphatic hydrocarbon, aromatic hydrocarbon, cyclane, petroleum resin and the like is adopted, and the multi-component characteristic provides various groups from polarity to non-polarity to adapt to different types of rubber with different polarities.
Preferably, the polyisobutene has a weight-average molecular weight of 2200 to 2400g/mol, which may be, for example, 2200g/mol, 2220g/mol, 2240g/mol, 2260g/mol, 2280g/mol, 2300g/mol, 2320g/mol, 2340g/mol, 2360g/mol, 2380g/mol, 2400g/mol, etc.
Preferably, the tackifying resin is a condensate of butyl phenol and acetylene.
In the present invention, the condensate of butyl phenol and acetylene is a commercially available product including, but not limited to, korein resin, 138# tackifying resin, and the like.
Preferably, the active agent is a combination of zinc oxide and stearic acid.
In the present invention, the reason why the combination of zinc oxide and stearic acid is employed as the active agent is: the two are mutually matched to form an organic matter of zinc stearate, thereby further improving the whole reaction activity.
Preferably, the mass ratio of the zinc oxide to the stearic acid is (1-3) to (0.5-2);
wherein "1 to 3" may be, for example, 1, 1.5, 2, 2.5, 3, etc.;
here, "0.5 to 2" may be, for example, 0.5, 0.8, 1, 1.2, 1.5, 2.
Preferably, the plasticizer is any one of rubber oil, paraffin oil, naphthenic oil or dioctyl phthalate or a combination of at least two of the rubber oil, the paraffin oil, the naphthenic oil and the dioctyl phthalate.
Preferably, the filler is any one or a combination of at least two of modified nano calcium carbonate, talcum powder, barium sulfate or heavy calcium carbonate.
Preferably, the modified nano calcium carbonate is nano calcium carbonate powder modified by stearic acid.
In the invention, the stearic acid and the calcium carbonate are bonded together through chemical bonds, so that the adhesive force can be further increased, the polymer chain is firmer, the thermal stability of the polymer is improved, the nano calcium carbonate modified by the stearic acid is filled in the organism of the sealant and can be well dispersed, and the interaction between particles and the adhesion between polymers are reduced.
Preferably, the vulcanization accelerator is a combination of a thiuram accelerator and a thiazole accelerator.
In the invention, the reason for the use form of compounding the cymbidium accelerator and the thiazole accelerator is as follows: the influence of a single accelerator on a system formula is avoided, and the influence of an ultra-fast accelerator and a fast accelerator on the overall vulcanization time of the rubber compound is synthesized.
Preferably, the mass ratio of the cymbidium accelerant to the thiazole accelerant is (1-5) to (3-8);
wherein "1 to 5" may be, for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, etc.;
here, "3 to 8" may be, for example, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, etc.
Preferably, the cymbidium accelerator is an accelerator TMTD.
Preferably, the thiazole accelerator is accelerator DM.
Preferably, the vulcanization aid is a combination of sulfur and a vulcanization resin.
In the present invention, the vulcanization system is adopted; the sulfur and the vulcanized resin are compounded to form a vulcanization auxiliary agent, the sulfur and the double-bond-containing natural rubber preferentially react to form a framework material under the action of an activating agent, and the vulcanized resin and the brominated butyl rubber are combined to produce a carbon-carbon double bond with higher bond energy, so that the integral temperature resistance of the adhesive tape is ensured.
Preferably, the mass ratio of the sulfur to the vulcanized resin is (0.1-0.4) to (1-2);
wherein "0.1 to 0.4" may be, for example, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, etc.;
here, "1-2" may be, for example, 1, 1.2, 1.4, 1.6, 1.8, 2, etc.
Preferably, the curing resin is a phenolic resin, preferably phenolic resin 2402 and/or SP1045.
Preferably, the raw materials for preparing the sealing tape also comprise an antifoaming agent and/or a toner.
Preferably, the amount of the defoamer added is 5 to 8 parts, and may be, for example, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, and the like.
Preferably, the defoaming agent is selected from any one or a combination of at least two of B-422, a calcium oxide defoaming agent or a grease calcium oxide defoaming agent.
Preferably, the toner is added in an amount of 0.1 to 0.3 parts, and may be, for example, 0.1 parts, 0.15 parts, 0.2 parts, 0.25 parts, 0.3 parts, or the like.
Preferably, the toner is selected from lemon yellow and/or phthalocyanine green.
Preferably, the raw materials for preparing the sealing tape comprise the following components in parts by weight:
in the present invention, the content of zinc oxide is 1 to 2.5 parts, and may be, for example, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, 2.1 parts, 2.3 parts, 2.5 parts, or the like.
In the present invention, the stearic acid is contained in an amount of 0.5 to 2 parts, for example, 0.5 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, etc.
In the present invention, the content of the Kalanchoe-type accelerator is 0.1 to 0.5 parts, and may be, for example, 0.1 part, 0.15 part, 0.2 part, 0.25 part, 0.3 part, 0.35 part, 0.4 part, 0.45 part, 0.5 part, or the like.
In the present invention, the thiazole accelerator is contained in an amount of 0.3 to 0.8 parts, and may be, for example, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, etc.
In the present invention, the sulfur content is 0.2 to 0.8 parts, and may be, for example, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, or the like.
In the present invention, the content of the vulcanized resin is 2 to 4 parts, and may be, for example, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts, 3 parts, 3.2 parts, 3.4 parts, 3.6 parts, 3.8 parts, 4 parts, etc.
In a second aspect, the present invention provides a method for preparing a sealing tape according to the first aspect, comprising the steps of:
(1) Banburying master batch: plasticating natural rubber and brominated butyl rubber according to a formula amount to obtain a rubber material, mixing the rubber material with tackifying resin, an active agent, a plasticizer, a part of filler and a part of polyisobutylene, and carrying out mixing, rubber discharging and rubber standing to obtain a master batch;
(2) Kneading: mixing the master batch obtained in the step (1) with the rest components, and carrying out mixing, rubber discharging and rubber standing to obtain a semi-finished rubber block;
(3) And (3) extrusion molding: and (3) sending the semi-finished product rubber block obtained in the step (2) into a rubber extruder for extrusion molding to obtain the sealing adhesive tape.
The invention adopts a two-stage method of banburying and kneading to prepare the high-temperature-resistant vacuum bag sealing adhesive tape with high strength, good cleaning property and high temperature resistance, the preparation method is simple, and under the condition of a stable process, polar glue and non-polar glue form a homogeneous mixed system, so that the excellent comprehensive performance of the sealing adhesive tape material is exerted, and the sealing adhesive tape is endowed with better high temperature resistance, oil resistance and high viscosity.
Preferably, the plastication of step (1) is carried out in an LL0 internal mixer.
Preferably, the feeding sequence of the step (1) is as follows: stearic acid, tackifying resin, zinc oxide, a homogenizing agent, a plasticizer, part of a filler and part of polyisobutylene are sequentially added into the obtained rubber material.
Preferably, the filler of the part in the step (1) accounts for 1/5 to 3/5 of the total mass of the filler, and can be 1/5, 3/10, 2/5, 1/2, 3/5 and the like.
Preferably, the portion of the polyisobutylene in step (1) is 1/5 to 3/5 of the total mass of the polyisobutylene, and may be, for example, 1/5, 3/10, 2/5, 1/2, 3/5, etc.
Preferably, the temperature for mixing in step (1) is 20-120 deg.C, such as 20 deg.C, 40 deg.C, 60 deg.C, 80 deg.C, 90 deg.C, 100 deg.C, 110 deg.C, 120 deg.C, etc., and the mixing time is 25-35min, such as 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min, etc.
Preferably, the temperature of the sealing gel in the step (1) is 20-25 ℃, for example, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃ and the like, and the time of the sealing gel is 8-24h, for example, 8h, 9h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h and the like.
Preferably, the temperature for the kneading in the step (2) is 80 to 105 ℃, for example, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃ and the like, and the kneading time is 10 to 15min, for example, 10min, 11min, 12min, 13min, 14min, 15min and the like.
Preferably, the temperature of the gel-rising in the step (2) is 20-25 ℃, for example, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃ and the like, and the time of the gel-rising is 8-24h, for example, 8h, 9h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h and the like.
Preferably, after the extrusion molding in the step (3), the belt conveying, the winding of the winding machine and the cutting by the cutter are sequentially carried out, so as to obtain the sealing adhesive tape.
Preferably, after the extrusion molding in the step (3), the belt conveying, the winding of the winding machine and the cutting by the cutter are sequentially carried out, so as to obtain the sealing adhesive tape.
In a third aspect, the present invention provides a use of the sealing tape according to the first aspect for the preparation of a high temperature resistant vacuum bag.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts the combination of natural rubber and brominated butyl rubber with a certain proportion as the matrix rubber of the sealing adhesive tape, thereby endowing the sealing adhesive tape with the characteristic of high strength at normal temperature and overcoming the defect of poor cleaning property of the adhesive tape after the adhesive tape is taken out of a tank at the later stage;
(2) The invention adopts the homogenizing agent to improve the interface compatibility of polar rubber and non-polar rubber matrix rubber, improves the uniformity of material mixing, and avoids the problems of unstable size of the adhesive tape in the extrusion process, dense and hemp bubbles on the surface of the adhesive tape which is in contact with a tool after the adhesive tape is discharged from a hot pressing tank, and the like;
(3) The sealing adhesive tape disclosed by the invention has excellent comprehensive performance, good high temperature resistance, oil resistance and high viscosity, excellent air tightness at 230 ℃, and the like, and can not retain residual glue on a mold when being separated from a manufacturing mold. The sealing tape can be widely applied to the molding production of components such as fan blades, airplanes and the like.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a sealing tape, which comprises the following raw materials in parts by weight:
the preparation method of the sealing tape of the embodiment comprises the following steps:
(1) Adopting general rubber processing equipment, adding 70 parts of brominated butyl rubber and 30 parts of natural rubber which are proportioned into an LL0 internal mixer for plastication, sequentially adding 1.5 parts of stearic acid, 2 parts of tackifying resin, 1 part of zinc oxide, 1.5 parts of homogenizing agent RH-150, 2 parts of plasticizer rubber oil 2280, partially treated 40 parts of nano calcium carbonate and 8 parts of polyisobutylene into plasticated rubber, discharging rubber when the mixing temperature reaches 120 ℃, uniformly mixing to obtain masterbatch, and standing for 24 hours;
(2) After the glue is proofed, adding the beated master batch into a kneading machine, then sequentially adding the remaining 60 parts of nano calcium carbonate, the remaining 16 parts of polyisobutylene, 5 parts of defoaming agent, 0.3 part of accelerator DM,0.5 part of accelerator TMTD,2 parts of vulcanized resin, 0.5 part of sulfur and 0.2 part of toner, mixing at the mixing temperature of 105 ℃, uniformly mixing, then carrying out screw extrusion discharging, and carrying out glue proofing for 24 hours to obtain a semi-finished product glue block;
(3) And (3) sending the semi-finished rubber blocks into a rubber extruder for extrusion molding, and carrying out belt conveying, rolling by a rolling machine and cutting by a cutter to obtain a finished product.
Example 2
The embodiment provides a sealing tape, which comprises the following raw materials in parts by weight:
the preparation method of the sealing tape of the embodiment comprises the following steps:
(1) Adopting general rubber processing equipment, adding 80 parts of brominated butyl rubber and 20 parts of natural rubber which are proportioned well into an LL0 internal mixer for plastication, sequentially adding 1.3 parts of stearic acid, 2 parts of tackifying resin, 0.8 part of zinc oxide, 1.5 parts of homogenizing agent RH-150, 2 parts of plasticizer naphthenic oil, 30 parts of partially treated nano calcium carbonate and 10 parts of polyisobutylene into plasticated rubber, discharging rubber when the mixing temperature reaches 120 ℃, uniformly mixing to obtain master batch, and standing for 24 hours after the rubber is stirred;
(2) After the glue is removed, adding the prepared master batch into a kneading machine, then sequentially adding the remaining 90 parts of nano calcium carbonate, the remaining 12 parts of polyisobutylene, 6 parts of defoaming agent, 0.5 part of accelerator DM,0.5 part of accelerator TMTD,2.5 parts of vulcanized resin, 0.3 part of sulfur and 0.2 part of toner, controlling the mixing process to be 100 ℃, enabling the mixing temperature to reach 105 ℃, uniformly mixing, then performing screw extrusion and discharging, and removing glue for 24 hours to obtain a semi-finished glue block;
(3) And (3) feeding the semi-finished rubber blocks into a rubber extruder for extrusion molding, and carrying out belt conveying, winding by a winding machine and cutting by a cutter to obtain a finished product.
Example 3
The embodiment provides a sealing tape, which comprises the following raw materials in parts by weight:
the preparation method of the sealing tape of the embodiment comprises the following steps:
(1) Adopting general rubber processing equipment, adding 90 parts of brominated butyl rubber and 10 parts of natural rubber which are proportioned into an LL0 internal mixer for plastication, sequentially adding 1 part of stearic acid, 2.5 parts of tackifying resin, 1.2 parts of zinc oxide, 1.5 parts of homogenizing agent RH-150, 3 parts of plasticizer rubber oil 2280, 40 parts of nano calcium carbonate which is partially treated and 10 parts of polyisobutylene into plasticated rubber, discharging rubber when the mixing temperature reaches 120 ℃, uniformly mixing to obtain masterbatch, and standing for 24 hours after rubber standing.
(2) After the glue is removed, the kneaded masterbatch is added into a kneading machine, then the remaining 80 parts of nano calcium carbonate, the remaining 15 parts of polyisobutylene, 5 parts of defoaming agent, 0.3 part of accelerator DM,0.5 part of accelerator TMTD,3 parts of vulcanized resin, 0.3 part of sulfur and 0.2 part of toner are sequentially added, the mixing temperature is controlled at 100 ℃ in the mixing process, the mixing temperature reaches 105 ℃, the materials are uniformly mixed and then are extruded by a screw to discharge, and the semi-finished glue block is obtained after 24 hours of glue removal.
(3) And (3) sending the semi-finished rubber blocks into a rubber extruder for extrusion molding, and carrying out belt conveying, rolling by a rolling machine and cutting by a cutter to obtain a finished product.
Example 4
This example provides a sealing tape, which is different from example 1 only in that the leveling agent RH-150 is replaced with equal mass RH-100, and the contents of other components and the preparation method are the same as example 1.
Example 5
This example provides a sealing tape which differs from example 1 only in that the tackifying resin korein is replaced by an equal mass of tackifying resin RJ-551, and the contents of other components and the preparation method are the same as in example 1.
Example 6
This example provides a sealing tape, which is different from example 1 only in that zinc oxide is not added, the content of stearic acid is increased to 2.5 parts, and the contents of other components and the preparation method are the same as example 1.
Example 7
This example provides a sealing tape, which is different from example 1 only in that stearic acid is not added, the content of zinc oxide is increased to 2.5 parts, and the contents of other components and the preparation method are the same as example 1.
Example 8
This example provides a sealing tape, which is different from example 1 only in that modified nano calcium carbonate is replaced by nano calcium carbonate with equal mass, and the contents of other components and the preparation method are the same as example 1.
Example 9
The present example provides a sealing tape, which is different from example 1 only in that modified nano calcium carbonate is replaced by equal mass of talc powder, and the contents of other components and the preparation method are the same as example 1.
Example 10
This example provides a sealing tape which differs from example 1 only in that the content of the accelerator TMTD is not added, the content of the accelerator DM is increased to 0.8 part, and the contents of other components and the preparation method are the same as example 1.
Example 11
This example provides a sealing tape which differs from example 1 only in that the content of accelerator DM is not added, the content of accelerator TMTD is increased to 0.8 part, and the contents of other components and the preparation method are the same as example 1.
Example 12
This example provides a sealing tape, which is different from example 1 only in that sulfur is not added, the content of the vulcanized resin is increased to 2.5 parts, and the contents of other components and the preparation method are the same as example 1.
Example 13
This example provides a sealing tape, which is different from example 1 only in that the sulfur content is increased to 2.5 parts without adding a curing resin, and the contents of other components and the preparation method are the same as example 1.
Comparative example 1
This comparative example provides a sealing tape which differs from example 1 only in that no natural rubber is added, the brominated butyl rubber content is increased to 100 parts, and the other component contents and preparation method are the same as example 1.
Comparative example 2
This comparative example provides a sealing tape which is different from example 1 only in that brominated butyl rubber was not added, the natural rubber content was increased to 100 parts, and the contents of other components and the preparation method were the same as example 1.
Comparative example 3
This comparative example provides a sealing tape which is different from example 1 only in that the natural rubber content is increased to 50 parts, the bromobutyl rubber content is reduced to 50 parts, and the other component contents and preparation method are the same as example 1.
Comparative example 4
This comparative example provides a sealing tape, which is different from example 1 only in that the homogenizing agent is not added, the content of the rubber oil 2280 is increased to 3.5 parts, and the contents of other components and the preparation method are the same as example 1.
Performance testing
The properties of the sealing tapes provided in examples 1 to 13 and comparative examples 1 to 4 were measured, respectively, according to the following specific test methods:
the following process is adopted to test the airtightness vacuum value of the high-temperature-resistant adhesive tape: making a 600mm × 600mm vacuum bag, placing 4 layers of WF330/WF300N ventilated felts in the bag, pumping to the vacuum degree of 0.098MPa, placing the bag in a hot-pressing tank, applying external pressure of 0.6MPa, keeping the temperature at 200 ℃ for 6h, then closing a vacuum switch, and measuring the vacuum leakage value within 5min. And respectively recording the vacuum degree in the temperature rising process, the vacuum degree in the heat preservation process and the vacuum degree in the cooling process or after cooling. The removability after cooling was determined according to the method for determination of HB 5481 under conditions of 200 ℃ C.. Times.3 h.
The specific test results are shown in table 1 below:
TABLE 1
As can be seen from the test data in Table 1, the maximum vacuum degree of the sealing tape can reach-100KPa in the temperature rise process, the vacuum degree can reach more than-85 KPa in the constant temperature process at 200 ℃, the vacuum degree can reach more than-80 KPa in the cooling process or after cooling, and the cleanable rate is more than 90% after cooling. The sealing adhesive tape has excellent comprehensive performance, good high temperature resistance, oil resistance, high viscosity, excellent air tightness at 230 ℃, and the like, and can not retain residual adhesive on a mold when being separated from a manufacturing mold. The sealing tape can be widely applied to the molding production of components such as fan blades, airplanes and the like.
As can be seen from the comparison between example 1 and example 4, the selection of RH-150 as the homogenizing agent can further improve the interfacial compatibility between the polar rubber and the non-polar rubber matrix rubber, and improve the uniformity of the material mixing. As can be seen from the comparison between example 1 and example 5, the butyl phenol and acetylene condensate as the tackifying resin can be better matched with other components, so that the temperature resistance and stability of the adhesive tape can be further improved.
From a comparison of example 1 with examples 6 and 7, it can be seen that the reason for using a combination of zinc oxide and stearic acid as the active agent is: the two are mutually matched to form an organic matter of zinc stearate, so that the whole reaction activity is further improved, and the improvement of the vacuum degree in the cooling process or after cooling is ensured.
As can be seen from the comparison of example 1 with examples 8 and 9, the stearic acid and calcium carbonate are bonded together by chemical bonds, which further increases the adhesion, which makes the polymer chains stronger, thereby further improving the temperature resistance and stability of the tape.
From the comparison of example 1 with examples 10 and 11, it can be seen that the reason for using the compound of the mother autumn accelerator and the thiazole accelerator is that: the influence of a single accelerator on a system formula is avoided, and the influence of an ultra-fast accelerator and a fast accelerator on the overall vulcanization time of the rubber compound is synthesized.
As can be seen from a comparison of example 1 with examples 12 and 13, in the present invention, the vulcanization system is used; the sulfur and the vulcanized resin are compounded to form a vulcanization assistant, the sulfur and the double-bond-containing natural rubber preferentially react to form a framework material under the action of an activating agent, and the vulcanized resin and the brominated butyl rubber are combined to produce a carbon-carbon double bond with higher bond energy, so that the temperature resistance of the whole adhesive tape is ensured.
As can be seen from the comparison between the example 1 and the comparative examples 1 to 3, the invention adopts the combination of the natural rubber and the brominated butyl rubber in a certain proportion as the matrix rubber of the sealing adhesive tape, thereby endowing the sealing adhesive tape with the characteristic of high strength at normal temperature and overcoming the defect of poor cleaning property of the adhesive tape after the adhesive tape is taken out of a tank at the later stage. As can be seen from the comparison between the example 1 and the comparative example 4, the homogenizing agent is adopted in the formula to improve the interface compatibility of the polar rubber and the non-polar rubber matrix rubber, improve the mixing uniformity of the materials, and avoid the problems of unstable size of the adhesive tape in the extrusion process, dense and hemp bubbles on the surface of the adhesive tape which is in contact with a tool after being discharged from a hot pressing tank and the like.
The applicant states that the present invention is illustrated by the above examples to describe the sealing tape, the preparation method and the application thereof, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (29)
1. The sealing adhesive tape is characterized by comprising the following raw materials in parts by weight:
the homogenizing agent is RH-150;
the vulcanization accelerator is a combination of a cymbidium accelerator and a thiazole accelerator;
the vulcanization auxiliary agent is a combination of sulfur and vulcanized resin;
the tackifying resin is a condensation product of butyl phenol and acetylene;
the active agent is a combination of zinc oxide and stearic acid;
the filler is modified nano calcium carbonate, and the modified nano calcium carbonate is nano calcium carbonate powder modified by stearic acid.
2. The sealing tape according to claim 1, wherein the natural rubber is selected from any one of natural rubber 10#, natural rubber 20#, or natural rubber SCR5, or a combination of at least two of the same.
3. The sealing tape of claim 1, wherein the brominated butyl rubber is selected from the group consisting of brominated butyl rubber 2030 and/or brominated butyl rubber 2255.
4. The sealing tape according to claim 1, wherein the polyisobutylene has a weight average molecular weight of 2200 to 2400g/mol.
5. The sealing tape according to claim 1, wherein the mass ratio of the zinc oxide to the stearic acid is (1-3): (0.5-2).
6. The sealing tape according to claim 1, wherein the plasticizer is any one of rubber oil, paraffin oil, naphthene oil or dioctyl phthalate or a combination of at least two thereof.
7. The sealing tape according to claim 1, wherein the mass ratio of the kauram accelerators to the thiazole accelerators is (1-5) to (3-8).
8. The sealing tape of claim 1, wherein the kauri-kava promoter is a promoter TMTD.
9. The sealing tape of claim 1, wherein the thiazole accelerator is accelerator DM.
10. The sealing tape according to claim 1, wherein the mass ratio of the sulfur to the vulcanized resin is (0.1-0.4): (1-2).
11. The sealing tape according to claim 1, wherein the curing resin is a phenol resin.
12. The sealing tape according to claim 11, wherein the curing resin is a phenol resin 2402 and/or SP1045.
13. The sealing tape according to claim 1, wherein the raw material for preparing the sealing tape further comprises an antifoaming agent and/or a toner.
14. The sealing tape of claim 13, wherein the defoamer is added in an amount of 5-8 parts.
15. The sealing tape of claim 13, wherein the defoamer is selected from B-422 and/or calcium oxide type defoamers.
16. The seal tape according to claim 13, wherein the toner is added in an amount of 0.1 to 0.3 parts.
17. The sealing tape according to claim 13, characterized in that the toner is selected from lemon yellow and/or phthalocyanine green.
18. The sealing tape according to claim 1, wherein the raw materials for preparing the sealing tape comprise the following components in parts by weight:
19. the method of manufacturing a sealing tape according to claim 1, comprising the steps of:
(1) Banburying master batch: plasticating natural rubber and brominated butyl rubber according to a formula amount to obtain a rubber material, mixing the rubber material with tackifying resin, an active agent, a homogenizing agent, a plasticizer, a part of filler and a part of polyisobutylene, and carrying out mixing, rubber discharging and rubber standing to obtain a master batch;
(2) Kneading: mixing the master batch obtained in the step (1) with the rest components, and carrying out mixing, rubber discharging and rubber standing to obtain a semi-finished rubber block;
(3) And (3) extrusion molding: and (3) sending the semi-finished product rubber block obtained in the step (2) into a rubber extruder for extrusion molding to obtain the sealing adhesive tape.
20. The method of preparing sealing tape according to claim 19, wherein the mastication in step (1) is performed in an LL0 internal mixer.
21. The method for preparing a sealing tape according to claim 19, wherein the step (1) is carried out in the order of: stearic acid, tackifying resin, zinc oxide, homogenizing agent, plasticizer, part of filler and part of polyisobutylene are sequentially added into the obtained rubber material.
22. The method of producing a sealing tape according to claim 19, wherein the filler in the portion of step (1) accounts for 1/5 to 3/5 of the total mass of the filler.
23. The method of claim 19, wherein the portion of polyisobutylene in step (1) is 1/5 to 3/5 of the total mass of polyisobutylene.
24. The method of preparing a sealing tape according to claim 19, wherein the temperature of the kneading in the step (1) is 20 to 120 ℃ and the kneading time is 25 to 35min.
25. The method for preparing sealing tape according to claim 19, wherein the temperature of the glue rinsing in the step (1) is 20-25 ℃, and the time of the glue rinsing is 8-24h.
26. The method of preparing a sealing tape according to claim 19, wherein the temperature of the kneading in the step (2) is 80 to 105 ℃ and the kneading time is 10 to 15min.
27. The method for preparing sealing tape according to claim 19, wherein the temperature of the glue rinsing in the step (2) is 20-25 ℃, and the time of the glue rinsing is 8-24h.
28. The method according to claim 20, wherein after the extrusion molding in step (3), a belt conveying, a winding machine and a cutter are sequentially performed to obtain the sealing tape.
29. Use of a sealing tape according to any one of claims 1-18 for the preparation of a high temperature resistant vacuum bag.
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