CN112341986B - Single-component polythioether sealant and preparation method thereof - Google Patents
Single-component polythioether sealant and preparation method thereof Download PDFInfo
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- CN112341986B CN112341986B CN202011114605.5A CN202011114605A CN112341986B CN 112341986 B CN112341986 B CN 112341986B CN 202011114605 A CN202011114605 A CN 202011114605A CN 112341986 B CN112341986 B CN 112341986B
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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
- C09J181/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Adhesives based on polysulfones; Adhesives based on derivatives of such polymers
- C09J181/02—Polythioethers; Polythioether-ethers
-
- 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
- C09J11/08—Macromolecular additives
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a single-component polythioether sealant and a preparation method thereof, belonging to the technical field of aviation sealing materials. The invention relates to a single-component sealant product, and the polythioether sealant related to the invention has excellent heat resistance and shorter surface drying time, and the prepared sealant is a single-component product and does not need additional processing. Compared with the current brushing type sealant, the invention reduces the operation difficulty and has higher controllability in the construction process.
Description
Technical Field
The invention belongs to the technical field of aviation sealing materials, and relates to a single-component polythioether sealing agent and a preparation method thereof.
Technical Field
The polysulfide sealant is widely applied to the field of aviation manufacture due to good oil resistance, air tightness, weather resistance and chemical medium resistance, and is one of the most important non-metallic materials for aircraft manufacture. However, the molecular chain of polysulfide rubber contains a large amount of disulfide bonds, which are easy to break at high temperature, and limit the heat resistance of the sealant.
Various forms of sealing are involved in aircraft manufacturing including fillet sealing, face sealing, and the like. The surface sealing is to brush the sealant on the sealing surface, which has a decisive effect on the appearance and the sealing quality of the product, so that the requirement on the construction performance of the sealant is high. Most of the sealing agents used in the field of aviation at present are two-component sealing agents and multi-component sealing agent products, when the sealing agent is used, a plurality of components of the sealing agent are required to be fully mixed and then coated, the mixing uniformity is difficult to guarantee due to the limitation of construction site conditions in the mixing process, and even a site with too fast local vulcanization or no local vulcanization occurs. In addition, for some sealant products with higher viscosity, a proper amount of solvent is added for dilution before brushing, the process is extremely complicated, and the operation process is not easy to control.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems, the invention provides the single-component polythioether sealant and the preparation method thereof, on one hand, the heat resistance of the sealant is improved, and the surface drying time is short, on the other hand, the prepared single-component sealant completely changes the current using situation of the current brushing type sealant, reduces the operation difficulty, and ensures that the controllability of the construction process is higher.
The technical scheme of the invention is as follows: the single-component polythioether sealant comprises solid polythioether rubber, a reinforcing filler, a curing agent, a silane coupling agent, tackifying resin and a mixed solvent, and the mass fractions of the components are shown in the following table:
| composition of matter | Parts by mass |
| Solid polythioether rubber | 100 portions of |
| Reinforcing filler | 15 to 50 portions of |
| Silane coupling agent | 0.1 to 5 portions |
| Mixed solvent | 200 to 600 parts by weight |
| Curing agent | 8 to 20 portions of |
| Tackifying resins | 7 to 20 portions of |
The solid polythioether rubber is sulfhydryl-terminated polythioether rubber, the relative weight of the solid polythioether rubber is about 3 to 5 million, and the structural formula is as follows:
the reinforcing filler is one or a mixture of two of fumed silica and carbon black.
The curing agent is prepared from zinc oxide and phenolic resin, and the preparation process of the curing agent comprises the following steps: preparing 30% ethanol solution of phenolic resin, slowly stirring zinc oxide in a beaker at 60 ℃, spraying the phenolic resin solution on the surface of the zinc oxide 20 times without stirring the powder, wherein the spraying amount is 5% of the mass of the zinc oxide each time, no wet powder is observed visually after spraying each time, and then spraying the next time. Wherein the structural formula of the phenolic resin is shown as the following, and the viscosity of 50% ethanol solution at 20 ℃ is between 0.11 Pa.s and 0.14 Pa.s.
The silane coupling agent is one or a mixture of KH-560, KH-590 and KH-550.
The tackifying resin is epoxy resin F44.
The mixed solvent is prepared from ethyl acetate and butanone according to the mass ratio of ethyl acetate: butanone 1: 1.75.
A preparation method of a single-component polythioether sealant comprises the following steps: the preparation method comprises the following steps of uniformly mixing solid polythioether rubber, a reinforcing filler and a curing agent on a two-roll open mill according to the mass parts in the following table to obtain a sizing material, putting the sizing material into a ball milling tank, adding a silane coupling agent, tackifying resin and a mixed solvent into the ball milling tank according to the mass parts of the silane coupling agent, the tackifying resin and the mixed solvent shown in the following table to obtain a mixture, and putting grinding balls into the ball milling tank to ball mill the mixture.
| Composition of matter | Parts by mass |
| Solid polythioether rubber | 100 portions of |
| Reinforcing filler | 15 to 50 portions of |
| Silane coupling agent | 0.1 to 5 portions |
| Mixed solvent | 200 to 600 parts by weight |
| Curing agent | 8 to 20 portions of |
| Tackifying resins | 7 to 20 portions of |
The rubber material is rolled into a thin rubber sheet, and then is placed into a ball milling tank after being cut up.
The mixture was ball milled with milling balls for more than 18 hours.
The invention has the beneficial effects that: compared with the traditional polysulfide sealant, the single-component polythioether sealant has higher temperature resistance level and quick surface drying time, and on the other hand, the single-component sealant does not need more operations in use, and only needs to be coated on the sealing surface and waits for surface drying and curing, so that the operation difficulty is greatly reduced, and the controllability of the construction process is higher.
Detailed Description
The single-component polythioether sealant comprises solid polythioether rubber, a reinforcing filler, a curing agent, a silane coupling agent, tackifying resin and a mixed solvent, wherein the mass fractions of the components are shown in the following table.
| Composition of matter | Parts by mass |
| Solid polythioether rubber | 100 portions of |
| Reinforcing filler | 15 to 50 portions of |
| Silane coupling agent | 0.1 to 5 portions |
| Mixed solvent | 200 to 600 parts by weight |
| Curing agent | 8 to 20 portions of |
| Tackifying resins | 7 to 20 portions of |
The solid polythioether rubber is sulfhydryl-terminated polythioether rubber, the relative weight of the solid polythioether rubber is about 3 to 5 million, and the structural formula is as follows:
the reinforcing filler is one or a mixture of two of fumed silica and carbon black.
The curing agent is prepared from zinc oxide and phenolic resin, and the preparation process of the curing agent comprises the following steps: preparing 30% ethanol solution of phenolic resin, slowly stirring zinc oxide in a beaker at 60 ℃, spraying the phenolic resin solution on the surface of the zinc oxide 20 times without stirring the powder, wherein the spraying amount is 5% of the mass of the zinc oxide each time, no wet powder is observed visually after spraying each time, and then spraying the next time. Wherein the structural formula of the phenolic resin is shown as the following, and the viscosity of 50% ethanol solution at 20 ℃ is between 0.11 Pa.s and 0.14 Pa.s.
The silane coupling agent is one or a mixture of KH-560, KH-590 and KH-550.
The tackifying resin is epoxy resin F44.
The mixed solvent is prepared from ethyl acetate and butanone according to the mass ratio of ethyl acetate: butanone 1: 1.75.
A preparation method of a single-component polythioether sealant comprises the following steps: mixing solid polythioether rubber, a reinforcing filler and a curing agent uniformly on a two-roll open mill according to the mass parts in the following table to obtain a sizing material, rolling the sizing material into a thin rubber sheet, chopping the thin rubber sheet, then putting the thin rubber sheet into a ball milling tank, adding a silane coupling agent, tackifying resin and a mixed solvent into the ball milling tank according to the mass parts of the silane coupling agent, the tackifying resin and the mixed solvent shown in the following table to obtain a mixture, putting grinding balls into the ball milling tank to ball mill the mixture, wherein the ball milling time is more than 18 hours.
| Composition of matter | Parts by mass |
| Solid polythioether rubber | 100 portions of |
| Reinforcing filler | 15 to 50 portions of |
| Silane coupling agent | 0.1 to 5 portions |
| Mixed solvent | 200 to 600 parts by weight |
| Curing agent | 8 to 20 portions of |
| Tackifying resins | 7 to 20 portions of |
Example 1
30g of phenolic resin is dissolved in 70g of absolute ethyl alcohol to prepare 30% ethanol solution in parts by mass, 100g of zinc oxide is placed in a beaker at 60 ℃ to be slowly stirred, then the phenolic resin solution is sprayed on the surface of the zinc oxide 20 times, zinc oxide powder is continuously stirred, the mass of the phenolic resin ethanol solution sprayed each time is 5g, no moist powder is observed visually after each spraying, and then the next spraying is carried out. Wherein the phenolic resin has a structural formula shown in the specification, and the viscosity of a 50% ethanol solution at 20 ℃ is 0.13 Pa.s.
Then weighing the following raw materials in parts by weight:
100 portions of solid polythioether rubber
Fumed silica 15 parts
13 portions of curing agent
Uniformly mixing the raw materials on a two-roll open mill to obtain a sizing material, rolling the sizing material into a thin rubber sheet, cutting the thin rubber sheet, putting the thin rubber sheet into a ball milling tank, weighing the raw materials in parts by weight, and adding the raw materials into the ball milling tank:
wherein the mixed solvent is ethyl acetate: mixing butanone 1:1.75, then adding a proper amount of grinding balls, and performing ball milling for 24 hours; and finally filtering and packaging the ground glue solution to obtain the single-component polythioether sealant.
Example 2
30g of phenolic resin is dissolved in 70g of absolute ethyl alcohol to prepare 30% ethanol solution in parts by mass, 100g of zinc oxide is placed in a beaker at 60 ℃ to be slowly stirred, then the phenolic resin solution is sprayed on the surface of the zinc oxide 20 times, zinc oxide powder is continuously stirred, the mass of the phenolic resin ethanol solution sprayed each time is 5g, no moist powder is observed visually after each spraying, and then the next spraying is carried out. Wherein the phenolic resin has a structural formula shown in the specification, and the viscosity of a 50% ethanol solution at 20 ℃ is 0.13 Pa.s.
Then weighing the following raw materials in parts by weight:
uniformly mixing the raw materials on a two-roll open mill to obtain a sizing material, rolling the sizing material into a thin rubber sheet, cutting the thin rubber sheet, putting the thin rubber sheet into a ball milling tank, weighing the raw materials in parts by weight, and adding the raw materials into the ball milling tank:
wherein the mixed solvent is ethyl acetate: mixing butanone 1:1.75, then adding a proper amount of grinding balls, and performing ball milling for 24 hours; and finally filtering and packaging the ground glue solution to obtain the single-component polythioether sealant.
Example 3
30g of phenolic resin is dissolved in 70g of absolute ethyl alcohol to prepare 30% ethanol solution in parts by mass, 100g of zinc oxide is placed in a beaker at 60 ℃ to be slowly stirred, then the phenolic resin solution is sprayed on the surface of the zinc oxide 20 times, zinc oxide powder is continuously stirred, the mass of the phenolic resin ethanol solution sprayed each time is 5g, no moist powder is observed visually after each spraying, and then the next spraying is carried out. Wherein the phenolic resin has a structural formula shown in the specification, and the viscosity of a 50% ethanol solution at 20 ℃ is 0.13 Pa.s.
Weighing the following raw materials in parts by mass:
uniformly mixing the raw materials on a two-roll open mill to obtain a sizing material, rolling the sizing material into a thin rubber sheet, cutting the thin rubber sheet, putting the thin rubber sheet into a ball milling tank, weighing the raw materials in parts by weight, and adding the raw materials into the ball milling tank:
wherein the mixed solvent is ethyl acetate: mixing butanone 1:1.75, then adding a proper amount of grinding balls, and performing ball milling for 24 hours; and finally filtering and packaging the ground glue solution to obtain the single-component polythioether sealant.
The relevant performance test methods for the one-component polythioether sealants of examples 1 to 3 are shown below
1. Surface drying time: reference is made to GB/T13477.5-2002.
2. The adhesive property is as follows: adhering the anodized aluminum alloy, coating 5 layers of sealant on the surface of the anodized aluminum alloy, coating the next layer after the surface of the former layer of sealant is dried, coating a piece of canvas on the surface of the former layer of sealant after the last layer of sealant is coated, covering the canvas on the surface of the coating, and coating a layer of sealant on the back of the canvas. Standing at room temperature for more than 24h, placing into a 60 deg.C oven, accelerating vulcanization for 48h, taking out, and testing peel strength according to HB 5249
3. Double-layer liquid resistance: the prepared adhesive sample was placed in a container containing an aqueous solution of jet fuel No. 3 and 3% sodium chloride, half of the sealant was kept in the aqueous solution and half in jet fuel No. 3, and was left standing in an oven at 60 ℃ for 7 days, and then the peel strength was tested according to HB 5249.
4. Heat resistance: baking at 180 deg.C for 3 hr, and observing the state of the sealant.
The results of the related performance tests of the single-component polythioether sealants of examples 1-3 and the related performance results of similar polysulfide sealant products are shown in the following table:
| item | Example 1 | Example 2 | Example 3 | Polysulfide sealant |
| Time to surface dry | 20min | 20min | 20min | 1h |
| Adhesive strength, kN/m | 5.6 | 6.2 | 7.5 | 6.0 |
| Resistance to double layer liquids, kN/m | 5.3 | 5.9 | 7.0 | 5.6 |
| Heat resistance | Without obvious change | Without obvious change | Without obvious change | Surface becomes sticky |
As can be seen from the table, the product has the characteristics of quick surface drying, fuel oil resistance and good water resistance, and has higher temperature resistance grade compared with the common polysulfide sealant.
Claims (8)
1. The single-component polythioether sealant is characterized by comprising solid polythioether rubber, a reinforcing filler, a curing agent, a silane coupling agent, tackifying resin and a mixed solvent, wherein the mass fractions of the components are as follows:
solid polythioether rubber: 100 parts of (A);
15-50 parts of reinforcing filler;
0.1-5 parts of a silane coupling agent;
200-600 parts of a mixed solvent;
8-20 parts of a curing agent;
7-20 parts of tackifying resin;
the curing agent is characterized by being prepared from zinc oxide and phenolic resin, and the preparation process of the curing agent comprises the following steps: preparing 30% by mass of an ethanol solution from phenolic resin, slowly stirring zinc oxide in a beaker at 60 ℃, spraying the phenolic resin solution on the surface of the zinc oxide 20 times without stirring the powder, wherein the spraying amount is 5% of the mass of the zinc oxide, no wet powder is observed visually after each spraying, and then spraying the next time, wherein the structural formula of the phenolic resin is as follows:
and the viscosity of the 50% ethanol solution at 20 ℃ is between 0.11 Pa.s and 0.14 Pa.s.
2. The one-component polythioether sealant of claim 1 wherein the reinforcing filler is one or a mixture of fumed silica and carbon black.
3. The one-component polythioether sealant according to claim 1, wherein the silane coupling agent is one or a mixture of KH-560, KH-590 and KH-550.
4. The one-component polythioether sealant of claim 1 wherein the tackifying resin is epoxy resin F44.
5. The single-component polythioether sealant according to claim 1, wherein the mixed solvent is prepared from ethyl acetate and butanone according to the mass ratio of ethyl acetate: butanone 1: 1.75.
6. The method for preparing the single-component polythioether sealant as claimed in any one of claims 1 to 5, characterized in that the method comprises the following steps: uniformly mixing the solid polythioether rubber, the reinforcing filler and the curing agent on a two-roller open mill according to the mass parts to obtain a sizing material, putting the sizing material into a ball milling tank, adding the silane coupling agent, the tackifying resin and the mixed solvent into the ball milling tank according to the mass parts to obtain a mixture, and putting grinding balls into the ball milling tank to ball mill the mixture.
7. The method for preparing the single-component polythioether sealant according to claim 6, wherein the sizing material is rolled into a thin rubber sheet, and then the thin rubber sheet is chopped and placed into a ball milling tank.
8. The method of claim 6, wherein the mixture is ball milled for more than 18 hours with milling balls.
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| CN110234676A (en) * | 2017-01-31 | 2019-09-13 | Prc-迪索托国际公司 | Low-density aerospace composition and sealant |
| CN110869445A (en) * | 2017-07-07 | 2020-03-06 | Prc-迪索托国际公司 | Hydraulic fluid and fuel resistant sealant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7645840B2 (en) * | 2002-02-26 | 2010-01-12 | Advanced Chemistry And Technology, Inc. | Frozen, lightweight curable sealant |
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| GB1084893A (en) * | 1965-05-13 | 1967-09-27 | Ciba Ltd | Curable polythioether compositions |
| US3509112A (en) * | 1965-05-13 | 1970-04-28 | Ciba Ltd | Polymeric adducts of monoepisulfides and primary amines |
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