CN111978906B - MS sealant with insect expelling and ultraviolet aging resisting functions and preparation method thereof - Google Patents
MS sealant with insect expelling and ultraviolet aging resisting functions and preparation method thereof Download PDFInfo
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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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
- C09J171/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/02—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of acids, salts or anhydrides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0058—Biocides
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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
- 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
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- 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
Abstract
The invention discloses an MS sealant with insect expelling and ultraviolet aging resistance and a preparation method thereof. The coating at least comprises the following components in parts by weight: 5-25 parts of silane oligomer, 5-20 parts of fluorine-containing hydroxyl-terminated polyether, 0.1-0.5 part of catalyst, 1-5 parts of dehydrating agent, 5-20 parts of plasticizer, 15-30 parts of filler and 0.1-0.5 part of multifunctional POSS-based microcapsule. According to the invention, silane oligomer and fluorine-containing hydroxyl-terminated polyether are adopted to generate silane modified polyether resin under the catalysis of an organic tin catalyst, and then the silane modified polyether resin is reacted with filler, a viscosity promoter, fumed silica, a plasticizer and a multifunctional POSS-based microcapsule together to prepare the MS sealant with insect expelling, ultraviolet ray aging resistance. The synthesis method has the advantages of mild reaction conditions, easily obtained reaction raw materials and easy operation of the reaction process; and compared with the traditional MS sealant, the sealant has excellent performances in the aspects of insect expelling, corrosion resistance, ultraviolet aging resistance and wetting resistance.
Description
Technical Field
The invention belongs to the field of adhesive materials, and relates to an MS sealant with insect expelling and ultraviolet aging resistance and a preparation method thereof.
Background
The MS sealant is a high-performance adhesive prepared by taking silane modified polyether resin as a base material, has the advantages of excellent cohesiveness, weather resistance, environmental protection, paintability and the like, and is widely applied to the fields of bonding, joint filling, joint sealing, water proofing, reinforcement and the like of building engineering and decoration.
Currently, research on MS sealants has been directed towards improving tack, but less functional research has been done for domestic applications, such as MS sealants often applied to the bonding of wood materials, and it is well known that wood is susceptible to insect attack. If MS sealant with insect resistance can be developed, and insect repellent medicine is encapsulated in the adhesive to achieve the effect of insect resistance, the application of the MS sealant in the aspect of life can be greatly improved. However, the MS sealant in the current market has the problem of tight molecular arrangement after curing, and the encapsulated drug cannot be released, so that the insect-expelling and corrosion-resisting effects cannot be realized. Therefore, it is a prerequisite to achieve this functionality if the molecular arrangement is effectively reduced so that the insect-resistant components in the system are effectively released. However, when the tightness of the MS sealant is effectively reduced, water molecules easily enter the inside of the colloid, so that the viscosity of the MS sealant is reduced. Besides, the MS sealant is easy to accelerate the aging of the colloid due to ultraviolet irradiation and short in service life, so that the damage of ultraviolet rays to the colloid can be effectively blocked by additionally adding the UV absorbent, but the existing UV absorbent is mostly micromolecules and is easy to volatilize, the blocking effect is difficult to realize, and the purpose of prolonging the service life cannot be achieved. Therefore, the multifunctional MS sealant with insect expelling and ultraviolet aging resistance is developed and has important significance in the aspect of life application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the MS sealant with functions of expelling insects and resisting ultraviolet aging and the preparation method thereof, the MS sealant provided by the invention not only can effectively expel insects, but also can absorb ultraviolet rays, reduce the damage effect of the ultraviolet rays on the MS sealant and prolong the service life of the MS sealant, and fluorine element is introduced into the MS sealant, so that the hydrophobicity of the MS sealant is improved, and the influence of moisture on the performance of the MS sealant is reduced; the adhesive is suitable for bonding between the building fields, and is particularly suitable for connecting wood bonding seams.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of an MS sealant with insect expelling and ultraviolet aging resistance, which comprises the following components in parts by weight:
the preparation method comprises the following steps:
1) adding fluorine-containing hydroxyl-terminated polyether into a reaction kettle, heating to 90-120 ℃, and carrying out reduced pressure dehydration.
2) And introducing inert gas into the reaction kettle, reducing the temperature to 50-80 ℃, adding the dehydrated silane oligomer and catalyst organotin, and reacting for 3-10 hours to obtain the silane modified polyether resin.
3) Adding plasticizer, filler, dehydrating agent and multifunctional POSS-based microcapsule into a double-planetary power stirrer, heating to 80-150 ℃, and reacting for 2-5 h. Then the temperature is reduced to 50-80 ℃, and the reaction is carried out for 1-2h by vacuumizing.
4) And introducing nitrogen to reduce the temperature to 50-80 ℃, adding the silane modified polyether resin, and stirring and dispersing for 2-3h to obtain the MS sealant with insect expelling and ultraviolet aging resistance.
Preferably, the multifunctional POSS-based microcapsule is prepared by the following specific steps:
1) dissolving 0.5-2g of styrene, 0.5-2g of methyl methacrylate, 1-4g of insect repellent essential oil, 0.5-2gUV absorbent, 0.5-2g of octa-ammonium chloride propyl silsesquioxane, 0.1-1g of alkylphenol polyoxyethylene ether, 0.1-0.2g of sodium dodecyl benzene sulfonate, 0.1-2g of sodium bicarbonate and 1-5ml of acrylic acid in 80-120ml of distilled water, then emulsifying the mixture at the speed of 300-400rpm/min for 15-30 minutes, finally pouring the obtained emulsion into a 500ml four-neck flask, introducing argon for 30-40min, heating to 60-80 ℃, then starting to dropwise add 5-30ml of 1-2 wt% initiator ammonium persulfate solution until the dropwise addition is finished, and then continuously stirring for reaction for 3-3.5h to obtain the polymer containing the insect-repellent essential oil.
2) Dissolving 0.1-1g of vinyl triethoxysilane, 2-10g of butyl acrylate, 0.1-1g of alkylphenol polyoxyethylene, 1-5g of vinyl POSS and 0.01-0.1g of sodium dodecyl benzene sulfonate in 10-100ml of distilled water, emulsifying the mixture for 15-30 minutes at 300-400rpm/min, adding the obtained emulsion and 5-30ml of 1-2 wt% initiator ammonium persulfate solution into the polymer containing the insect repellent essential oil, stirring for 2-3 hours, heating to 50-80 ℃, placing in a culture dish, drying at room temperature, washing with ethanol for multiple times, and drying at room temperature to obtain the multifunctional POSS-based microcapsule.
Preferably, the hydroxyl-terminated fluorine-containing polyether in the step 1) is hydroxyl-terminated polyether containing 1-5 wt% of fluorine element and having molecular weight of 2000-10000;
preferably, the silane oligomer in the step 2) is one or more of a silane oligomer containing isocyanate groups and a silane oligomer containing epoxy groups;
preferably, the plasticizer in step 3) is one or more of dioctyl phthalate, dibutyl phthalate, dioctyl adipate and dibutyl sebacate;
preferably, the filler in the step 3) is one or more of calcium carbonate and fumed silica;
preferably, the dehydrating agent in the step 3) is one or more of vinyltriethoxysilane, vinyldimethoxymethylsilane and trimethyl orthoacetate;
preferably, the insect-repellent essential oil in step 1) comprises one or more of citronella essential oil, eucalyptus essential oil, clove essential oil and mint essential oil;
preferably, the ultraviolet absorbent of step 1) comprises one or more of ethyl 2- [3- (2-benzotriazol-2-yl) -4-hydroxyphenyl ] methacrylate and ethyl 2- (4-benzo-3-hydroxyphenoxy) acrylate;
the MS sealant with the functions of expelling parasites and resisting ultraviolet aging is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the conventional MS sealant, the MS sealant has great breakthrough in the aspect of life application, and has the function of expelling insects particularly aiming at wood.
2. Compared with the conventional MS sealant, the invention introduces the POSS microcapsule, has good physical and mechanical properties, and is not easy to damage in the process of processing and stirring by using a double-planet power stirrer. Meanwhile, the POSS microcapsules are used as a micron-sized shell-core structure, so that the space structure is increased, and the release of the insect-proof essential oil is facilitated.
3. The invention introduces the UV absorbent, and the covalent bond polymerizes the POSS microcapsule, so that the prepared MS sealant has the effect of blocking the damage of ultraviolet rays, can effectively reduce the aging speed and prolong the service time.
Drawings
FIG. 1 scanning electron microscopy images of multifunctional POSS-based microcapsules of example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further described below by means of specific examples.
In the examples of the present invention, the raw materials used are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
Example 1
A preparation method of an MS sealant with insect expelling and ultraviolet aging resistance comprises the following steps:
1) 0.5g of styrene, 0.5g of methyl methacrylate, 1g of citronella essential oil, 0.5g of 2- [3- (2-benzotriazole-2-yl) -4-hydroxyphenyl ] ethyl methacrylate, 0.5g of octa-ammoniumshloride propyl silsesquioxane, 0.1g of alkylphenol polyoxyethylene ether, 0.1g of sodium dodecyl benzene sulfonate, 0.1g of sodium bicarbonate and 1ml of acrylic acid are dissolved in 80ml of distilled water, the mixture is emulsified for 15 minutes at the speed of 300rpm/min, finally the obtained emulsion is poured into a 500ml four-neck flask, argon is introduced for 30 minutes, after the temperature is raised to 60 ℃, 5ml of 1 wt% initiator ammonium persulfate solution is started to be dripped until the dripping is finished, and the reaction is continuously stirred for 3 hours to obtain the citronella essential oil-containing polymer.
2) Dissolving 0.1g of vinyl triethoxysilane, 2g of butyl acrylate, 0.1g of alkylphenol polyoxyethylene, 5g of vinyl POSS and 0.03g of sodium dodecyl benzene sulfonate in 20ml of distilled water, emulsifying the mixture at 300rpm/min for 15 minutes, adding the obtained emulsion and 5ml of 1 wt% initiator ammonium persulfate solution into a polymer containing citronella essential oil, stirring for 2 hours, heating to 50 ℃, placing in a culture dish, drying at room temperature, washing with ethanol for multiple times, and drying at room temperature to obtain the multifunctional POSS-based microcapsule.
3) 5 parts of hydroxyl-terminated polyether containing 1 wt% of fluorine element and having molecular weight of 2000 are added into a reaction kettle, and the temperature is raised to 90 ℃ for decompression and dehydration.
4) And introducing inert gas into the reaction kettle, reducing the temperature to 50 ℃, adding 5 parts of dehydrated silane oligomer containing isocyanate groups and 0.1 part of catalyst organotin, and reacting for 3 hours to obtain the silane modified polyether resin.
5) 5 parts of dioctyl phthalate, 15 parts of calcium carbonate, 1 part of vinyl triethoxysilane and 0.1 part of multifunctional POSS-based microcapsule are added into a double-planetary power mixer, the temperature is raised to 80 ℃, and the reaction is carried out for 2 hours. Then the temperature is reduced to 50 ℃, and the reaction is carried out for 1 hour by vacuumizing.
6) And introducing nitrogen to reduce the temperature to 50 ℃, adding 5 parts of silane modified polyether resin, stirring and dispersing for 2 hours to obtain the MS sealant with insect expelling, ultraviolet ray resistance and aging resistance.
Example 2
A preparation method of an MS sealant with insect expelling and ultraviolet aging resistance comprises the following steps:
1) 1g of styrene, 1g of methyl methacrylate, 2g of eucalyptus essential oil, 1g of ethyl 2- [3- (2-benzotriazole-2-yl) -4-hydroxyphenyl ] methacrylate, 1g of octa-ammoniumchloride propylsilsesquioxane, 0.5g of alkylphenol polyoxyethylene, 0.1g of sodium dodecyl benzene sulfonate, 0.5g of sodium bicarbonate and 2ml of acrylic acid are dissolved in 80ml of distilled water, the mixture is emulsified for 20 minutes at the speed of 300rpm/min, finally the obtained emulsion is poured into a 500ml four-neck flask, argon is introduced for 30 minutes, after the temperature is raised to 70 ℃, 15ml of 1 wt% initiator ammonium persulfate solution is added dropwise until the dropwise addition is finished, and the polymer containing the eucalyptus essential oil is obtained after continuous stirring reaction for 3 hours.
2) Dissolving 0.5g of vinyltriethoxysilane, 3g of butyl acrylate, 0.5g of alkylphenol ethoxylates, 2g of vinyl POSS and 0.05g of sodium dodecyl benzene sulfonate in 20ml of distilled water, emulsifying the mixture at 300rpm/min for 15 minutes, adding the obtained emulsion and 15ml of 1 wt% initiator ammonium persulfate solution into a polymer containing eucalyptus essential oil, stirring for 2 hours, heating to 60 ℃, placing in a culture dish, drying at room temperature, washing with ethanol for multiple times, and drying at room temperature to obtain the multifunctional POSS-based microcapsule.
3) Hydroxyl-terminated polyether containing 2 wt% of fluorine element and having molecular weight of 5000 is added into a reaction kettle, and the temperature is raised to 100 ℃ for decompression and dehydration.
4) And introducing inert gas into the reaction kettle, reducing the temperature to 60 ℃, adding the dehydrated silane oligomer containing epoxy groups and catalyst organotin, and reacting for 5 hours to obtain the silane modified polyether resin.
5) Adding 10 parts of dibutyl phthalate, 15 parts of calcium carbonate, 3 parts of vinyl triethoxysilane and 0.2 part of multifunctional POSS-based microcapsules into a double-planetary power mixer, heating to 100 ℃, and reacting for 3 hours. Then the temperature is reduced to 60 ℃, and the reaction is carried out for 1 hour by vacuumizing.
6) And introducing nitrogen to reduce the temperature to 60 ℃, adding 7 parts of silane modified polyether resin, stirring and dispersing for 2 hours to obtain the MS sealant with insect expelling, ultraviolet ray resistance and aging resistance.
Example 3
A preparation method of an MS sealant with insect expelling and ultraviolet aging resistance comprises the following steps:
1) 1.5g of styrene, 1.5g of methyl methacrylate, 3g of clove essential oil, 1.5g of 2- [3- (2-benzotriazole-2-yl) -4-hydroxyphenyl ] ethyl methacrylate, 1.5g of octa-ammoniumshloride propylsilsesquioxane, 0.8g of alkylphenol polyoxyethylene ether, 0.2g of sodium dodecyl benzene sulfonate, 0.8g of sodium bicarbonate and 4ml of acrylic acid are dissolved in 100ml of distilled water, the mixture is emulsified for 20 minutes at the speed of 400rpm/min, the obtained emulsion is poured into a 500ml four-neck flask, argon is introduced for 35 minutes, after the temperature is raised to 70 ℃, 10ml of 1.5 wt% initiator ammonium persulfate solution is started to be dripped until the dripping is finished, and the reaction is continuously stirred for 3.5 hours to obtain the polymer containing the clove essential oil.
2) Dissolving 0.8g of vinyltriethoxysilane, 5g of butyl acrylate, 0.8g of alkylphenol ethoxylates, 5g of vinyl POSS and 0.08g of sodium dodecyl benzene sulfonate in 500ml of distilled water, emulsifying the mixture at 400rpm/min for 20 minutes, adding the obtained emulsion and 20ml of 1.5 wt% initiator ammonium persulfate solution into the polymer containing clove essential oil, stirring for 2.5 hours, heating to 70 ℃, placing in a culture dish, drying at room temperature, washing with ethanol for multiple times, and drying at room temperature to obtain the multifunctional POSS-based microcapsule.
3) 15 parts of hydroxyl-terminated polyether containing 4 wt% of fluorine and having a molecular weight of 7000 is added into a reaction kettle, and the temperature is raised to 110 ℃ for decompression and dehydration.
4) And introducing inert gas into the reaction kettle, reducing the temperature to 70 ℃, adding 20 parts of dehydrated silane oligomer containing isocyanate groups and 0.3 part of catalyst organotin, and reacting for 7 hours to obtain the silane modified polyether resin.
5) Adding 15 parts of dioctyl adipate, 15 parts of calcium carbonate, 3 parts of vinyl triethoxysilane and 0.5 part of multifunctional POSS-based microcapsules into a double-planetary power mixer, heating to 120 ℃, and reacting for 4 hours. Then the temperature is reduced to 70 ℃, and the reaction is carried out for 1.5h by vacuumizing.
6) And introducing nitrogen to reduce the temperature to 70 ℃, adding 10 parts of silane modified polyether resin, stirring and dispersing for 2.5 hours to obtain the MS sealant with insect expelling, ultraviolet ray aging resistance.
Example 4
A preparation method of an MS sealant with insect expelling and ultraviolet aging resistance comprises the following steps:
1) 2g of styrene, 2g of methyl methacrylate, 4g of mint essential oil, 2g of 2- [3- (2-benzotriazole-2-yl) -4-hydroxyphenyl ] ethyl methacrylate, 2g of octa-ammoniumshloride propylsilsesquioxane, 1g of alkylphenol ethoxylate, 0.2g of sodium dodecyl benzene sulfonate, 2g of sodium bicarbonate and 5ml of acrylic acid are dissolved in 120ml of distilled water, the mixture is emulsified at the speed of 400rpm/min for 30 minutes, finally the obtained emulsion is poured into a 500ml four-neck flask, argon is introduced for 40 minutes, after the temperature is increased to 80 ℃, 30ml of 2 wt% initiator ammonium persulfate solution is added dropwise until the dropwise addition is finished, and the stirring reaction is continued for 3.5 hours to obtain the polymer containing the mint essential oil.
2) Dissolving 1g of vinyltriethoxysilane, 10g of butyl acrylate, 1g of alkylphenol ethoxylates, 3g of vinyl POSS and 0.1g of sodium dodecyl benzene sulfonate in 100ml of distilled water, emulsifying the mixture at 400rpm/min for 30 minutes, adding the obtained emulsion and 30ml of 2 wt% initiator ammonium persulfate solution into the polymer containing the mint essential oil, stirring for 3 hours, heating to 80 ℃, placing in a culture dish, drying at room temperature, washing with ethanol for multiple times, and drying at room temperature to obtain the multifunctional POSS-based microcapsule.
3) Adding 20 parts of hydroxyl-terminated polyether with 5 wt% of fluorine element and molecular weight of 10000 into a reaction kettle, heating to 120 ℃, and carrying out reduced pressure dehydration.
4) And introducing inert gas into the reaction kettle, reducing the temperature to 70 ℃, adding 25 parts of dehydrated silane oligomer containing epoxy groups and 0.5 part of catalyst organotin, and reacting for 10 hours to obtain the silane modified polyether resin.
5) Adding 20 parts of dibutyl sebacate, 30 parts of calcium carbonate, 5 parts of vinyl triethoxysilane and 0.5 part of multifunctional POSS-based microcapsules into a double-planetary power mixer, heating to 150 ℃, and reacting for 5 hours. Then the temperature is reduced to 80 ℃, and the reaction is carried out for 2 hours in a vacuum pumping way.
6) And introducing nitrogen to reduce the temperature to 70 ℃, adding 15 parts of silane modified polyether resin, stirring and dispersing for 3 hours to obtain the MS sealant with insect expelling, ultraviolet ray resistance and aging resistance.
The following table shows the water absorption of the MS sealants with insect repellent and uv aging resistant properties prepared in examples 1-4 of the present invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A preparation method of MS sealant with insect expelling and ultraviolet aging resistance is characterized by comprising the following steps: the weight parts of the components are as follows:
the fluorine-containing hydroxyl-terminated polyether contains 5wt% of fluorine element and has a molecular weight of 2000-10000;
the preparation method comprises the following steps:
1) adding fluorine-containing hydroxyl-terminated polyether into a reaction kettle, heating to 90-120 ℃, and carrying out reduced pressure dehydration;
2) Introducing inert gas into the reaction kettle, reducing the temperature to 50-80 ℃, adding the dehydrated silane oligomer and catalyst organotin, and reacting for 3-10h to obtain silane modified polyether resin;
3) adding a plasticizer, a filler, a dehydrating agent and a multifunctional POSS-based microcapsule into a double-planetary power mixer, heating to 80-150 ℃, reacting for 2-5h, reducing the temperature to 50-80 ℃, and vacuumizing for 1-2 h;
4) introducing nitrogen to reduce the temperature to 50-80 ℃, adding silane modified polyether resin, stirring and dispersing for 2-3h to obtain the MS sealant with insect expelling, ultraviolet ray resistance and aging resistance;
the multifunctional POSS-based microcapsule is prepared by the following specific steps:
s1: dissolving 0.5-2g of styrene, 0.5-2g of methyl methacrylate, 1-4g of insect repellent essential oil, 0.5-2gUV absorbent, 0.5-2g of octa-ammonium chloride propyl silsesquioxane, 0.1-1 g of alkylphenol polyoxyethylene ether, 0.1-0.2 g of sodium dodecyl benzene sulfonate, 0.1-2g of sodium bicarbonate and 1-5ml of acrylic acid in 80-120 ml of distilled water, then the mixture is emulsified for 15 to 30 minutes at the speed of 300-400 rpm/min, and finally the obtained emulsion is poured into a 500ml four-neck flask, introducing argon for 30-40min, heating to 60-80 ℃, then starting to dropwise add 5-30ml of 1-2wt% initiator ammonium persulfate solution until the dropwise addition is finished, and then continuously stirring for reaction for 3-3.5h to obtain the polymer containing the insect-repellent essential oil;
S2: dissolving 0.1-1g of vinyl triethoxysilane, 2-10 g of butyl acrylate, 0.1-1g of alkylphenol polyoxyethylene, 1-5g of vinyl POSS and 0.01-0.1 g of sodium dodecyl benzene sulfonate in 10-100ml of distilled water, emulsifying the mixture for 15-30 minutes at 400 rpm/min of 300-.
2. The preparation method of the MS sealant with insect repelling and ultraviolet aging resistance as claimed in claim 1, is characterized in that: the silane oligomer in the step 2) is one or more of silane oligomer containing isocyanate and silane oligomer containing epoxy groups.
3. The preparation method of the MS sealant with insect expelling and ultraviolet aging resistance as claimed in claim 1, is characterized in that: the plasticizer in the step 3) is one or more of dioctyl phthalate, dibutyl phthalate, dioctyl adipate and dibutyl sebacate.
4. The preparation method of the MS sealant with insect expelling and ultraviolet aging resistance as claimed in claim 1, is characterized in that: the filler in the step 3) is one or more of calcium carbonate and fumed silica.
5. The preparation method of the MS sealant with insect repelling and ultraviolet aging resistance as claimed in claim 1, is characterized in that: the dehydrating agent in the step 3) is one or more of vinyltriethoxysilane, vinyldimethoxymethylsilane and trimethyl orthoacetate.
6. The preparation method of the MS sealant with insect expelling and ultraviolet aging resistance as claimed in claim 1, is characterized in that: the insect-repellent essential oil in the step S1 includes one or more of citronella essential oil, eucalyptus essential oil, clove essential oil, and peppermint essential oil.
7. The preparation method of the MS sealant with insect expelling and ultraviolet aging resistance as claimed in claim 1, is characterized in that: the ultraviolet absorbent of step S1 is 2- [3- (2-benzotriazole-2-yl) -4-hydroxyphenyl ] ethyl methacrylate.
8. An MS sealant with insect repelling and ultraviolet aging resistance prepared according to the preparation method of any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010790225.7A CN111978906B (en) | 2020-08-07 | 2020-08-07 | MS sealant with insect expelling and ultraviolet aging resisting functions and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010790225.7A CN111978906B (en) | 2020-08-07 | 2020-08-07 | MS sealant with insect expelling and ultraviolet aging resisting functions and preparation method thereof |
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| CN112608703B (en) * | 2020-11-25 | 2022-07-12 | 广州市白云化工实业有限公司 | Antifouling silane modified polyether adhesive and preparation method thereof |
| CN114045689A (en) * | 2021-11-22 | 2022-02-15 | 国佳凝胶科创中心(深圳)有限公司 | Preparation method of hydrogel cooling cloth |
| CN114874747B (en) * | 2022-05-05 | 2023-01-03 | 安徽斯迈特新材料股份有限公司 | Preparation method of high-temperature-resistant and strong-ultraviolet-resistant MS (Murashige & Skoog) adhesive |
| CN115386209B (en) * | 2022-08-17 | 2023-12-19 | 万华化学（宁波）有限公司 | Long-acting fragrance-retaining PLA wire applied to 3D printing field and preparation method and application thereof |
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| CN111001363A (en) * | 2019-11-15 | 2020-04-14 | 温州科技职业学院 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
| CN111100590A (en) * | 2019-12-04 | 2020-05-05 | 湖南柯盛新材料有限公司 | Silane modified polyether sealant and preparation method thereof |
| CN111109255A (en) * | 2020-01-06 | 2020-05-08 | 温州科技职业学院 | Insect-attracting microcapsule for insect sticking plate and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111001363A (en) * | 2019-11-15 | 2020-04-14 | 温州科技职业学院 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
| CN111100590A (en) * | 2019-12-04 | 2020-05-05 | 湖南柯盛新材料有限公司 | Silane modified polyether sealant and preparation method thereof |
| CN111109255A (en) * | 2020-01-06 | 2020-05-08 | 温州科技职业学院 | Insect-attracting microcapsule for insect sticking plate and preparation method and application thereof |
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