WO2022193662A1 - Produit d'étanchéité monocomposant à base d'un polyéther modifié par un silane, procédé de préparation associé et son application - Google Patents
Produit d'étanchéité monocomposant à base d'un polyéther modifié par un silane, procédé de préparation associé et son application Download PDFInfo
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- WO2022193662A1 WO2022193662A1 PCT/CN2021/126416 CN2021126416W WO2022193662A1 WO 2022193662 A1 WO2022193662 A1 WO 2022193662A1 CN 2021126416 W CN2021126416 W CN 2021126416W WO 2022193662 A1 WO2022193662 A1 WO 2022193662A1
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- WIPO (PCT)
- Prior art keywords
- silane
- modified polyether
- resin
- epoxy resin
- modified
- Prior art date
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- 239000004526 silane-modified polyether Substances 0.000 title claims abstract description 136
- 239000000565 sealant Substances 0.000 title claims abstract description 107
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 103
- 239000011347 resin Substances 0.000 claims abstract description 103
- 239000004014 plasticizer Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000003381 stabilizer Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000005034 decoration Methods 0.000 claims abstract description 5
- 230000003137 locomotive effect Effects 0.000 claims abstract description 3
- 239000003822 epoxy resin Substances 0.000 claims description 54
- 229920000647 polyepoxide Polymers 0.000 claims description 54
- 239000003054 catalyst Substances 0.000 claims description 27
- 230000003014 reinforcing effect Effects 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 14
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 14
- 239000002516 radical scavenger Substances 0.000 claims description 14
- 229910000077 silane Inorganic materials 0.000 claims description 12
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229920000570 polyether Polymers 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 9
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 238000000518 rheometry Methods 0.000 claims description 8
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 5
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 claims description 5
- 229920004482 WACKER® Polymers 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 239000013008 thixotropic agent Substances 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 10
- 239000007822 coupling agent Substances 0.000 description 7
- 239000003292 glue Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 6
- 238000001723 curing Methods 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 239000004611 light stabiliser Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000012763 reinforcing filler Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 etc. Chemical compound 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000013008 moisture curing Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 206010035653 pneumoconiosis Diseases 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004588 polyurethane sealant Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Definitions
- the invention belongs to the technical field of sealants, and relates to a one-component silane-modified polyether sealant and a preparation method and application thereof, in particular to a high-transparency and high-strength one-component silane-modified polyether sealant and preparation thereof methods and applications.
- Silane-modified polyether adhesive also known as modified silicone adhesive, is a high-performance adhesive prepared from silane-terminated polyether polymer as the base resin.
- Silane-terminated polyether was first developed by Japan Zhongyuan Chemical in 1979. Its main chain is polyether, and its end groups are hydrolyzable silane end groups, which are similar to silicone glue.
- the silane-terminated polyether has a macromolecular pure ether chain structure on the main chain. It does not contain urethane bonds and urea bonds with high cohesive energy like the main chain of polyurethane, which not only brings good flexibility to the base resin.
- silane-terminated polyether It has good flexibility, high elongation and hydrolysis resistance, and significantly reduces the viscosity of silane-terminated polyether, which is beneficial to the silane-modified polyether sealant system that can obtain good process performance without or with less solvent or plasticizer. And maintain the balance of excellent overall performance of the system.
- Silane-modified polyether sealants have the advantages of environmental friendliness, paintability, and the versatility of bonding materials, but conventional silane-modified polyether sealants are mostly opaque paste-like compounds with relatively low strength. , which limits its application in applications requiring high bonding strength, high tensile strength and high transparency, such as in the field of high-end residential interior decoration and automotive windshield bonding, it still cannot replace transparent silicone glue and high mechanical strength polyurethane sealant.
- the more commonly used method is to use fumed silica as a reinforcing filler.
- fumed silica can improve the transparent silane-modified polyether sealant to a certain extent.
- the mechanical properties of the glue are limited, but the improvement is limited, and the tensile strength ( ⁇ 4MPa) and bonding strength are still low. Too much silica will harm human health and even cause pneumoconiosis.
- the two-component transparent sealant needs to be mixed evenly with the matching glue equipment before it can be constructed and used. The operation is complicated and its application is limited.
- CN111732924A discloses a one-component silane-modified polyether sealant and a preparation method thereof.
- the one-component silane-modified polyether sealant includes silane-modified polyether polymer, silane-modified polyether resin, plasticizer, Pigment and filler, dehydrating agent, silane coupling agent, catalyst, light stabilizer, ultraviolet absorber. Due to the introduction of amino groups and epoxy groups in this invention, the hardness, bulk strength and adhesion of the prepared sealant Strength is significantly increased. However, the transparency of the sealant of the invention needs to be further improved.
- CN111218248A discloses a transparent one-component silane-modified polyether sealant.
- the raw materials of the silane-modified polyether sealant include the following components: silane-modified polyether resin, plasticizer, inorganic filler, water removal agents, UV absorbers, light stabilizers, silane coupling agents and catalysts.
- the silane-modified polyether sealant of the invention has a simple preparation process, and has high transparency and/or good anti-ultraviolet performance. However, the transparency and tensile strength of the sealant of the invention need to be further improved.
- CN109337629A discloses a high-modulus transparent silane-modified polyether sealant, which is made from the following raw material components: silane-modified polyether resin, plasticizer, light stabilizer, antioxidant, color paste, white Carbon black, water scavengers, adhesion promoters and catalysts.
- the high-modulus transparent silane-modified polyether sealant of the invention has the characteristics of good transparency, good weather resistance, high tensile modulus, high bonding strength, paintability, and no free NCO. It has excellent comprehensive performance and can be applied In interior decoration, automobile manufacturing, electronic appliances and glass counters and other fields. However, the tensile strength of the sealant of the invention needs to be further improved, and the preparation raw material of the invention contains white carbon black, which will cause harm to human health.
- the purpose of the present invention is to provide a one-component silane-modified polyether sealant and its preparation method and application, especially to provide a high-transparency, high-strength one-component silane-modified polyether sealant Sealant and preparation method and application thereof.
- high transparency refers to the light transmittance of the silane-modified polyether sealant tested in accordance with GB/T2410-2008>85%
- high strength refers to the silane-modified polyether sealant tested in accordance with GB/T528-2009.
- the present invention provides a one-component silane-modified polyether sealant, and the raw materials for preparing the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- m, n are integers and 1 ⁇ m ⁇ 50, for example, m is 1, 2, 3, 5, 8, 10, 15, 20, 25, 30, 35, 40, 45 or 50, etc., 1 ⁇ n ⁇ 25, for example, n is 1, 2, 3, 5, 8, 10, 15, 20 or 25, etc.
- the ratio of m to n is (1 ⁇ 2):1, for example, the ratio of m to n is 1:1, 1.3 : 1, 1.5:1, 1.8:1 or 2:1, etc.
- R is any one of methyl, ethyl or phenyl or a combination of at least two, such as methyl and Ethyl, methyl and ethyl and phenyl and the like.
- the present invention uses ⁇ -silane-terminated silane-modified polyether resin as the base resin, adds reinforcing resin, and reasonably adjusts the mass percentage of each component to prepare the single-component silane-modified polyether sealant, which, on the one hand, retains the silane-modified polyether sealant.
- the reinforcing resin is also end-capped with -Si-OCH 3 , which can participate in the moisture curing process. Reaction, thereby increasing the crosslinking density of the sealant, thereby improving the mechanical properties of the sealant.
- the dosage of the silane-modified polyether resin can be 25 parts, 28 parts, 30 parts, 35 parts, 40 parts, 45 parts, 48 or 50, etc.
- the dosage of the reinforcing resin in the preparation raw materials of the one-component silane-modified polyether sealant, can be 5 parts, 10 parts, 15 parts, 20 parts, 25 parts or 30 parts, etc.
- the amount of plasticizer in the preparation raw materials of the one-component silane-modified polyether sealant, can be 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 or 50, etc.
- the dosage of the rheological agent in the preparation raw materials of the one-component silane-modified polyether sealant, can be 0.1 part, 0.3 part, 0.5 part, 0.8 part, 1 part, 1.5 part, 2 part, 2.5 servings or 3 servings etc.
- the amount of the stabilizer in the preparation raw materials of the one-component silane-modified polyether sealant, can be 0.5 parts, 0.8 parts, 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts, etc.
- the amount of the water scavenger in the raw materials for the preparation of the one-component silane-modified polyether sealant, can be 0.5, 0.8, 1, 1.5, 2, 2.5 or 3 parts, etc. .
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- Me is methyl
- the silane-modified polyether resin includes any one or a combination of at least two of STP-E10 resin, STP-E30 resin or STP-XB502 resin produced by WACKER, Germany.
- a combination of the at least two kinds such as STP-E10 resin and STP-E30 resin, STP-E10 resin and STP-E30 resin, and STP-XB502 resin, etc.
- the preparation method of the reinforced resin comprises the following steps:
- step (2) heating up, adding trialkoxysilane to the modified epoxy resin in step (1), then adding a catalyst, and performing a vacuum stirring reaction to obtain the reinforced resin.
- the reaction mechanism is as follows:
- the reinforced resin is prepared by the reaction of epoxy resin, polyetheramine, alkyl trialkoxy silane or phenyl trialkoxy silane, so that it retains the characteristics of epoxy resin and amino silane at the same time, and has High strength and high adhesion, so the one-component silane-modified polyether sealant with reinforcing resin has good adhesion to various substrates, and does not need to add silane coupling agent to improve adhesion.
- the ⁇ -silane-terminated silane-modified polyether resin does not need to add an organotin catalyst, and can be cross-linked and cured with moisture in the air under the catalysis of only aminosilane, which reduces the harm of organotin and is not immune to certain These areas limit the influence of organotin, thereby expanding the scope of use.
- the polyetheramine is a bifunctional polyetheramine resin whose main chain is a polyether structure and the terminal active functional group is a bifunctional amine group.
- the molecular weight of the polyetheramine is 100-3000, such as 100, 300, 500, 800, 1000, 1500, 1800, 2000, 2500 or 3000, and the like.
- the polyetheramine comprises any one or a combination of at least two of Huntsman D230, D400 or D2000.
- the epoxy resin is a bisphenol A epoxy resin.
- the molecular weight of the epoxy resin is 600-5000, such as 600, 800, 1000, 2000, 3000, 4000 or 5000, etc.
- the epoxy resin comprises any one or a combination of at least two of E44, E51 or E35 commercially available in Nanya, Taiwan.
- the trialkoxysilane includes alkyltrialkoxysilane and/or aryltrialkoxysilane, preferably methyltrimethoxysilane, ethyltrimethoxysilane or phenyltrimethoxysilane Any one or a combination of at least two, such as methyltrimethoxysilane and ethyltrimethoxysilane, ethyltrimethoxysilane and phenyltrimethoxysilane, etc., Methyltrimethoxysilane is preferred.
- the catalyst comprises dibutyltin dilaurate.
- epoxy resin is added to polyetheramine in step (1), and the molar ratio of polyetheramine to epoxy resin is 1:(0.5-1.5), for example, 1:0.5, 1:0.8, 1 :1, 1:1.2 or 1:1.5 etc.
- step (2) add trialkoxysilane to the modified epoxy resin of step (1), and the ratio of the number of moles of trialkoxysilane to the number of moles of hydroxyl groups in the modified epoxy resin is 1: (0.1 ⁇ 1), such as 1:0.1, 1:0.2, 1:0.3, 1:0.5, 1:0.8 or 1:1, etc.
- the added amount of the catalyst is 0.1-1% of the mass of the trialkoxysilane, such as 0.1%, 0.2%, 0.3%, 0.5%, 0.8% or 1%, etc.
- the temperature increase in step (1) is to increase the temperature to 50-60°C, for example, 50°C, 52°C, 54°C, 56°C, 58°C, or 60°C.
- the reaction time of step (1) is 4-8h, such as 4h, 5h, 5.5h, 6h, 7h or 8h, etc.
- the temperature is raised to 80-120°C, such as 80°C, 85°C, 90°C, 95°C, 100°C, 110°C or 120°C, and the like.
- the time of the vacuum stirring reaction in step (2) is 1-6h, such as 1h, 2h, 3h, 4h, 5h or 6h, etc.
- the plasticizer includes any one or a combination of at least two of the polyether polyols PPG1000, PPG2000, PPG3000, PPG4000 or PPG8000. Combinations of the at least two, such as PPG1000 and PPG2000, PPG3000 and PPG4000, and PPG8000, etc.
- the rheological agent is a liquid thixotropic agent, preferably BYK-410 from BYK.
- the stabilizer is a liquid stabilizer, preferably BASF B75.
- the water scavenger is a vinyl functional silane type water scavenger, including any one or at least one of vinyltrimethoxysilane, vinyltriethoxysilane or vinylmethyldimethoxysilane combination of the two. Combinations of the at least two such as vinyltrimethoxysilane and vinyltriethoxysilane, vinyltriethoxysilane and vinylmethyldimethoxysilane, and the like.
- the present invention provides the above-mentioned preparation method of one-component silane-modified polyether sealant, and the preparation method comprises the following steps:
- silane-modified polyether resin Mix the silane-modified polyether resin, rheology agent, stabilizer, part of plasticizer and water scavenger evenly, then add the remaining plasticizer and reinforcing resin, stir under vacuum conditions, and defoaming to obtain the monolayer.
- Components Silane-modified polyether sealant Components Silane-modified polyether sealant.
- the rotating speed of the mixing is 5-15rpm, such as 5rpm, 8rpm, 10rpm, 13rpm or 15rpm, etc.
- the mixing time is 20-60min, such as 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60min, etc.
- the vacuum degree of the vacuum condition is -0.09 to -0.1 MPa, such as -0.09 MPa, -0.092 MPa, -0.093 MPa, -0.095 MPa, -0.098 MPa or -0.1 MPa, and the like.
- the rotational speed of the stirring is 5-10rpm, 5rpm, 6rpm, 7rpm, 8rpm, 9rpm or 10rpm, etc.
- the stirring time is 15-60min, such as 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min , 55min or 60min, etc.
- the present invention provides the application of the above-mentioned one-component silane-modified polyether sealant in interior decoration, automobile windshield or locomotive structural bonding.
- the present invention at least has the following beneficial effects:
- the present invention uses silane-modified polyether resin as the base resin, and adds reinforcing resin to prepare a one-component silane-modified polyether sealant, which on the one hand retains the flexibility and durability of silane-modified polyether resin. On the other hand, its mechanical properties (tensile strength: 5.3-8.8MPa, tensile shear strength: 4.1-7.3MPa) are improved;
- the single-component silane-modified polyether sealant prepared by the present invention retains the properties of epoxy resin and amino silane because the preparation raw materials contain reinforcing resin. It has high strength and high adhesion, so it has good adhesion to various substrates, and does not need to add silane coupling agent to improve adhesion.
- the reinforcing resin in the sealant of the present invention has a structure similar to that of the aminosilane coupling agent, the ⁇ -silane-terminated silane-modified polyether resin can be cross-linked with moisture in the air without adding an organotin catalyst. For curing, there is no need to add aminosilane coupling agent and organotin as catalyst, which reduces the harm of organotin, and is not affected by the restriction of organotin in some fields, thus expanding its scope of use;
- the one-component silane-modified polyether sealant of the present invention uses a reinforcing resin to improve its mechanical properties, and has better performance than the traditional transparent silane-modified polyether sealant using fumed silica as a reinforcing filler. High transparency (light transmittance: 92-93%) and can prevent human health from inhaling too much silica powder during the production process;
- the one-component silane-modified polyether sealant of the present invention has simpler construction and is compared with the conventional opaque paste-like one-component silane-modified polyether sealant. , Because powder with higher water content is not used as reinforcing filler in the formula system, high temperature dehydration is not required during production, the process is simple, easy to operate, and the production cost is low, which is conducive to industrial production and use.
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- the ratio of m to n is 1:1, and R is methyl.
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- the preparation method of the reinforced resin comprises the following steps:
- the addition amount of catalyst dibutyltin dilaurate is 0.1% of the mass of methyltrimethoxysilane.
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- the ratio of m to n is 1.1:1, and R is ethyl.
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- the preparation method of the reinforced resin comprises the following steps:
- the addition amount of catalyst dibutyltin dilaurate is 0.5% of the mass of ethyltrimethoxysilane.
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- Silane-modified polyether resin STP-E30, rheology agent BYK-410, stabilizer B75, part of plasticizer PPG8000 (20 parts) and water scavenger vinyltriethoxysilane were mixed at a low speed of 10rpm for 60min uniformly, then add the remaining plasticizer PPG8000 and reinforcing resin, stir for 60 minutes at a speed of 5 rpm under -0.1MPa vacuum condition, and defoaming to obtain the single-component silane-modified polyether sealant.
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- the ratio of m to n is 1.5:1, and R is phenyl.
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- the preparation method of the reinforced resin comprises the following steps:
- the addition amount of catalyst dibutyltin dilaurate is 1% of the mass of phenyltrimethoxysilane.
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- the ratio of m to n is 1.8:1, and R is phenyl.
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- the preparation method of the reinforced resin comprises the following steps:
- the addition amount of catalyst dibutyltin dilaurate is 1% of the mass of phenyltrimethoxysilane.
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- the ratio of m to n is 1.3:1, and R is methyl.
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- the preparation method of the reinforced resin comprises the following steps:
- the addition amount of catalyst dibutyltin dilaurate is 0.8% of the mass of methyltrimethoxysilane.
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- Silane-modified polyether resin STP-E10, rheology agent BYK-410, stabilizer B75, part of plasticizer PPG1000 (5 parts) and water scavenger vinylmethyldimethoxysilane were stirred at low speed at 5rpm Mix uniformly for 30min, then add the remaining plasticizer PPG1000 and reinforcing resin, stir at 8rpm for 35min under vacuum condition of -0.098MPa, and degassing to obtain the single-component silane-modified polyether sealant.
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the reinforcing resin has the following structural features:
- the ratio of m to n is 2:1, and R is ethyl.
- the silane-modified polyether resin is a silane-modified polyether resin end-capped with ⁇ -silane, and has the following structural features:
- the preparation method of the reinforced resin comprises the following steps:
- the addition amount of catalyst dibutyltin dilaurate is 0.3% of the mass of ethyltrimethoxysilane.
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- Silane-modified polyether resin Germany Wacker STP-E30, rheology agent BYK-410, stabilizer B75, part of plasticizer PPG2000 (20 parts) and water scavenger vinylmethyldimethoxysilane were mixed at 15rpm. Stir at a low speed for 50 minutes and mix evenly, then add the remaining plasticizer PPG2000 and reinforced resin, stir at a speed of 10 rpm for 15 minutes under -0.09MPa vacuum condition, and degassing to obtain the one-component silane-modified polyether sealant .
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- Example 1 The difference between this comparative example and Example 1 is that the preparation raw materials do not include reinforcing resin, the weight part of silane-modified polyether resin (WACKER STP-E10, Germany) is 65 parts, and 2 parts of amino silane are used for coupling Agent KH550 was used as the catalyst, and the rest were the same as in Example 1.
- WACKER STP-E10 weight part of silane-modified polyether resin
- 2 parts of amino silane are used for coupling Agent KH550 was used as the catalyst, and the rest were the same as in Example 1.
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- Example 2 The difference between this comparative example and Example 2 is that the preparation raw materials do not include reinforcing resin, the weight part of silane-modified polyether resin (WACKER STP-E30, Germany) is 57 parts, and 1 part of amino silane is used for coupling Agent KH540 was used as the catalyst, and the rest were the same as in Example 2.
- WACKER STP-E30, Germany weight part of silane-modified polyether resin
- 1 part of amino silane is used for coupling Agent KH540 was used as the catalyst, and the rest were the same as in Example 2.
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- Example 3 The difference between this comparative example and Example 3 is that the preparation raw materials do not include reinforcing resin, the weight parts of silane-modified polyether resin (German Wacker STP-E30) is 43 parts, and the weight of plasticizer (PPG4000) is 43 parts by weight. The number of parts is 50 parts, and 0.5 part of aminosilane coupling agent KH792 is used as a catalyst, and the rest are the same as in Example 3.
- a one-component silane-modified polyether sealant is provided, and the preparation raw materials of the one-component silane-modified polyether sealant, in parts by weight, include the following components:
- the preparation method of one-component silane-modified polyether sealant comprises the following steps:
- Transparency test according to GB/T2410-2008, use SM-2 type light transmittance tester to test the light transmittance of the sealant, and the film thickness is 2mm.
- the sealants prepared in Examples 1-6 can be cured without adding an aminosilane coupling agent, and the cured mechanical strength (tensile strength: 5.3-8.8 MPa, tensile shear strength: 4.1-7.3MPa) and transparency (transmittance: 92-93%) are significantly improved, meeting the requirements of high strength and high transparency of silane-modified polyether sealants, that is, according to GB/T 528-2009 test tensile strength>5Mpa, according to GB/T2410-2008 test light transmittance>85%.
- the present invention illustrates the one-component silane-modified polyether sealant of the present invention and its preparation method and application through the above-mentioned examples, but the present invention is not limited to the above-mentioned examples, that is, it does not mean that the present invention must Implementation depends on the above-mentioned embodiment.
- Those skilled in the art should understand that any improvement of the present invention, the equivalent replacement of each raw material of the product of the present invention, the addition of auxiliary components, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Sealing Material Composition (AREA)
Abstract
La présente invention concerne un produit d'étanchéité monocomposant à base d'un polyéther modifié par un silane, un procédé de préparation associé et son application. Les matières premières de la préparation du produit d'étanchéité monocomposant à base d'un polyéther modifié par un silane comprennent, en parties en poids, les constituants suivants : 25 à 50 parties d'une résine de polyéther modifiée par un silane, 5 à 30 parties d'une résine de renfort, 10 à 50 parties d'un plastifiant, 0,1 à 3 parties d'un agent rhéologique, 0,5 à 3 parties d'un stabilisant et 0,5 à 3 parties d'un déshydratant. Le produit d'étanchéité monocomposant à base d'un polyéther modifié par un silane, préparé dans le cadre de la présente invention, présente les caractéristiques d'une grande transparence et d'une grande résistance mécanique et convient aux domaines de la décoration intérieure, du collage des pare-brises pour automobile, du collage de structures de locomotive, etc.
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CN113943415B (zh) * | 2021-11-30 | 2022-07-08 | 武汉理工大学 | 一种韧性阻燃环氧树脂及其制备方法和使用方法 |
CN114854353B (zh) * | 2022-06-24 | 2023-06-09 | 郑州中原思蓝德高科股份有限公司 | 一种阻燃型硅烷改性聚醚组合物以及密封胶 |
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