CN114395369A - Two-component addition type silicone adhesive and preparation method and application thereof - Google Patents
Two-component addition type silicone adhesive and preparation method and application thereof Download PDFInfo
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- CN114395369A CN114395369A CN202210121163.XA CN202210121163A CN114395369A CN 114395369 A CN114395369 A CN 114395369A CN 202210121163 A CN202210121163 A CN 202210121163A CN 114395369 A CN114395369 A CN 114395369A
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- silicone oil
- addition type
- silicone adhesive
- type silicone
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- 239000013464 silicone adhesive Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004753 textile Substances 0.000 claims abstract description 33
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 29
- 229920000570 polyether Polymers 0.000 claims abstract description 29
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000077 silane Inorganic materials 0.000 claims abstract description 21
- 239000000853 adhesive Substances 0.000 claims abstract description 12
- 230000001070 adhesive effect Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 claims description 58
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 54
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 38
- 229920002554 vinyl polymer Polymers 0.000 claims description 38
- 229910052739 hydrogen Inorganic materials 0.000 claims description 34
- 239000001257 hydrogen Substances 0.000 claims description 34
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 34
- 238000004898 kneading Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 28
- 239000011256 inorganic filler Substances 0.000 claims description 22
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 22
- 239000003112 inhibitor Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052697 platinum Inorganic materials 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 229910021485 fumed silica Inorganic materials 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000004526 silane-modified polyether Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000007792 addition Methods 0.000 description 54
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UEXCJVNBTNXOEH-UHFFFAOYSA-N Ethynylbenzene Chemical group C#CC1=CC=CC=C1 UEXCJVNBTNXOEH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 description 1
- 229920006052 Chinlon® Polymers 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a two-component addition type silicone adhesive and a preparation method and application thereof. The two-component addition type silicone adhesive comprises silane modified polyether with a structural formula shown in a formula (I), wherein n is 3-18. According to the invention, silane modified esterified polyether shown in formula (I) is added into the two-component addition type silicone adhesive, so that the bonding strength of the adhesive to textiles can be effectively improved, and the improvement range is preferably more than 15%. According to the invention, only the silane modified esterified polyether is directly added on the conventional process for preparing the double-component addition type silicone adhesive, the process is not required to be changed, the flow is simple, and the method is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of synthesis of adhesives for textiles, and particularly relates to a two-component addition type silicone adhesive as well as a preparation method and application thereof.
Background
With the development of textile technology and material technology, more and more adhesives are applied to the textile industry, besides printing and dyeing decorative patterns on textiles, the adhesives can also be coated on the surface of the textiles, so that the textiles have the functions of moisture permeability, water resistance, fire resistance, health care and the like, and different fibers or textiles can also be bonded together to form a composite material or non-woven fabric. Because of the high ductility of the organosilicon material and the characteristics of good skin-friendly property and water permeability, in some application scenes, such as the application of an anti-skid coating on clothes, or in the manufacture of underwear, compared with the traditional sewing method for textile industry, the method splices different textiles and uses the organosilicon adhesive to splice the textiles to achieve better use comfort of users. The two-component addition type silicone adhesive has the advantages of almost no small molecules generated in the curing process, low toxicity, environmental protection, high curing speed, suitability for flow line production and the like, and is widely applied. In recent years, with the development of the textile industry, various synthetic fiber materials such as chinlon, terylene and spandex are continuously appeared, so that the strength of the bonding and splicing of textiles using the new materials is higher, the traditional two-component addition type silicone adhesive faces more challenges, and therefore the two-component addition type silicone adhesive which is higher in affinity to the textile materials and higher in bonding and bonding strength needs to be developed.
Disclosure of Invention
The first purpose of the invention is to provide a two-component addition type silicone adhesive, wherein the components of the two-component addition type silicone adhesive contain silane modified polyether;
the molecular structural formula of the silane modified esterified polyether is shown as the formula (I):
wherein n is 3 to 18, and more preferably n is 7 to 18. Wherein n is a positive integer.
According to the invention, the silane modified esterified polyether shown in the formula (I) is added into the two-component addition type silicone adhesive, so that the bonding strength of the adhesive to fabrics can be effectively improved.
In the invention, the silane modified esterified polyether shown in formula (I) can be added into the component A or the component B of the two-component addition type silicone adhesive, and the silane modified esterified polyether and the inhibitor are required to be in the same component, preferably in the same component with hydrogen-containing silicone oil and the inhibitor and in different components with the catalyst. In a preferred embodiment of the invention, the two-component addition type silicone adhesive comprises a component A and a component B; wherein, the component A comprises vinyl silicone oil, inorganic filler, hexamethyldisilazane, water and platinum catalyst; wherein the component B comprises vinyl silicone oil, inorganic filler, hexamethyldisilazane, the silane modified polyether, hydrogen-containing silicone oil, an inhibitor and water.
In a preferred embodiment of the present invention, the vinyl silicone oil in the component A and the vinyl silicone oil in the component B are the same. Wherein, the content of vinyl in the vinyl silicone oil is preferably 0.5 wt% to 3 wt%. The vinyl silicone oil in the present invention contains at least 2 vinyl groups per molecule. The viscosity (25 ℃) of the vinyl silicone oil is preferably 1000 to 20000 mPas, more preferably 10000 to 15000 mPas.
In a preferred embodiment of the present invention, the inorganic fillers in the component A and the component B are the same in kind; the inorganic filler is one or more of fumed silica, light or heavy calcium carbonate, alumina, silica micropowder and carbon black, and the fumed silica is preferred.
In a preferred embodiment of the invention, the platinum catalyst in the component A is one or more of platinum-alkyne-based complex, isopropanol solution of chloroplatinic acid or platinum-vinylsiloxane complex.
In a preferred embodiment of the present invention, the content of active hydrogen (i.e., Si-H bonded to silicon) in the hydrogen-containing silicone oil in the B component is 0.3 wt% to 0.7 wt%. The viscosity of the hydrogen-containing silicone oil is preferably 30 to 100mPa.s, and in the present invention, the viscosity may be 30mPa.s, 40mPa.s, 50mPa.s, 60mPa.s, 70mPa.s, 80mPa.s, 90mPa.s, or 100 mPa.s. The inhibitor is preferably an alkynol compound, and can be one or more of 1-ethynyl-1-cyclohexanol, phenylacetylene, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butynyl-2-ol and 3-methyl-1-ethynyl-3-ol, and preferably is 1-ethynyl-1-cyclohexanol.
In a preferred embodiment of the invention, the mass ratio of the vinyl silicone oil, the inorganic filler, the hexamethyldisilazane, the water and the platinum catalyst in the component A is (80-180): (15-40): (2-10): (1-4): (1-5), preferably (140-160): (30-35): (5-8): (1-4): (1-5).
In a preferred embodiment of the invention, the mass ratio of the vinyl silicone oil, the inorganic filler, hexamethyldisilazane, water, the silane modified polyether, the hydrogen-containing silicone oil and the inhibitor in the component B is (60-120): (15-40): (2-10): (1-4): (2-10): (20-40): (0.5-5), preferably (90-110): (30-35): (5-8): (1-4): (2-10): (30-35): (0.5-5).
The two-component addition type silicone adhesive of the present invention can be prepared using preparation methods commonly used in the art, with the silane-modified esterified polyether and hydrogen-containing silicone oil added to the components along with the inhibitor. In a preferred embodiment of the present invention, the preparation method of the two-component addition type silicone adhesive comprises the following steps:
the component A comprises:
adding vinyl silicone oil, inorganic filler, hexamethyldisilazane and water into a kneading machine for multiple times, kneading for 0.5-1 h at room temperature, heating to 80-90 ℃, kneading for 2-3 h, heating to 140-150 ℃, kneading for 2-3 h, cooling, adding a platinum catalyst, and mixing in vacuum to obtain the composite material;
the component B comprises:
adding vinyl silicone oil, inorganic filler, hexamethyldisilazane and water into a kneading machine for multiple times, kneading for 0.5-1 h at room temperature, heating to 80-90 ℃, kneading for 2-3 h, heating to 140-150 ℃, kneading for 2-3 h, cooling, adding silane modified esterified polyether shown in formula (I), hydrogen-containing silicone oil and an inhibitor, and mixing in vacuum to obtain the silicone oil.
The component A (raw material in the component A) in the two-component addition type silicone adhesive preferably comprises vinyl silicone oil, inorganic filler, hexamethyldisilazane, water and a platinum catalyst. The component B (raw material in the component B) preferably consists of vinyl silicone oil, inorganic filler, hexamethyldisilazane, the silane-modified esterified polyether, hydrogen-containing silicone oil, an inhibitor and water.
In the invention, when the two-component addition type silicone adhesive provided by the invention is used, the prepared component A and the component B are mixed according to a proportion for use, and the mass ratio of the component A to the component B is 1 (1-1.2).
The invention also aims to provide a preparation method of the two-component addition type silicone adhesive, which comprises the following steps:
the component A comprises:
adding vinyl silicone oil, inorganic filler, hexamethyldisilazane and water into a kneading machine for multiple times, kneading for 0.5-1 h at room temperature, heating to 80-90 ℃, kneading for 2-3 h, heating to 140-150 ℃, kneading for 2-3 h, cooling, adding a platinum catalyst, and mixing in vacuum to obtain the composite material;
the component B comprises:
adding vinyl silicone oil, inorganic filler, hexamethyldisilazane and water into a kneading machine for multiple times, kneading for 0.5-1 h at room temperature, heating to 80-90 ℃, kneading for 2-3 h, heating to 140-150 ℃, kneading for 2-3 h, cooling, adding silane modified esterified polyether shown in formula (I), hydrogen-containing silicone oil and an inhibitor, and mixing in vacuum to obtain the silicone oil.
Wherein, in the component A, the dosage of the vinyl silicone oil, the inorganic filler, the hexamethyldisilazane, the water and the platinum catalyst is preferably 80-180 parts, 15-40 parts, 2-10 parts, 1-4 parts and 1-5 parts respectively. In the component B, the preferred amounts of the vinyl silicone oil, the inorganic filler, the hexamethyldisilazane, the water, the silane-modified esterified polyether, the hydrogen-containing silicone oil and the inhibitor are 60-120 parts, 15-40 parts, 2-10 parts, 1-4 parts, 2-10 parts, 20-40 parts and 0.5-5 parts by weight respectively.
In the present invention, the parts by weight may be in the units of μ g, mg, g, kg, etc. known in the art, or may be multiples thereof, such as 1/10, 1/100, 10, 100, etc.
When the two-component addition type silicone adhesive provided by the invention is used, the component A and the component B are mixed according to a proportion and then defoamed, and are applied to the surface of a textile fabric in a screen printing or steel mesh printing mode and the like, so that the two-component addition type silicone adhesive can be quickly cured at a temperature of over 100 ℃. The two-component addition type silicone adhesive provided by the invention can be preferably applied to the field of textiles, namely the two-component addition type silicone adhesive for textiles.
The invention also aims to provide the application of the two-component addition type silicone adhesive or the preparation method in preparing the textile adhesive.
According to the invention, silane modified esterified polyether shown in formula (I) is added into the two-component addition type silicone adhesive, so that the bonding strength of the adhesive to textiles can be effectively improved, and the bonding strength is improved by more than 8%, preferably more than 15%. According to the invention, only the silane modified esterified polyether is directly added on the conventional process for preparing the double-component addition type silicone adhesive, the process is not required to be changed, the flow is simple, and the method is suitable for industrial production. The silane modified esterified polyether used in the invention is cheap and has no influence on the overall cost of the formula after being added into the two-component addition type silicone adhesive as an additive.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment provides a two-component addition type silicone adhesive for textiles, which is prepared by the following steps:
the component A comprises:
1) 140 parts of vinyl silicone oil with the viscosity of 10000mPa.s, 30 parts of fumed silica, 5 parts of hexamethyldisilazane and 2.5 parts of water are added into a kneader for multiple times, and the mixture is kneaded for 3 minutes after each addition, and is kneaded for 1 hour at room temperature after all the additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) After cooling, the mixture was transferred to a planetary mixer, and 2 parts of a platinum catalyst (an ethanol solution of chloroplatinic acid, platinum content: 0.15%) was added thereto, followed by vacuum mixing for 40 minutes to obtain component A.
The component B comprises:
1) 100 parts of vinyl silicone oil with the viscosity of 10000mPa.s, 30 parts of fumed silica, 5 parts of hexamethyldisilazane and 2.5 parts of water are added into a kneader for multiple times, and the mixture is kneaded for 3 minutes after each addition, and is kneaded for 1 hour at room temperature after all the additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) Cooling, transferring to a planetary stirrer, adding 2 parts of silane modified esterified polyether (wherein n is 3) shown as the formula (I), 30 parts of hydrogen-containing silicone oil with the viscosity of 50mPa.s and the hydrogen (active hydrogen) content of 0.4 percent and 0.6 part of 1-ethynyl-1-cyclohexanol inhibitor, and mixing for 40 minutes in vacuum to obtain a component B.
Example 2
The embodiment provides a two-component addition type silicone adhesive for textiles, which is prepared by the following steps:
the preparation of component A is the same as in example 1.
The component B comprises:
1) 100 parts of vinyl silicone oil with the viscosity of 10000mPa.s, 30 parts of fumed silica, 5 parts of hexamethyldisilazane and 2.5 parts of water are added into a kneader for multiple times, and the mixture is kneaded for 3 minutes after each addition, and is kneaded for 1 hour at room temperature after all the additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) Cooling, transferring to a planetary stirrer, adding 6 parts of silane modified esterified polyether shown as formula (I) (wherein n is 7), 30 parts of hydrogen-containing silicone oil with viscosity of 50mPa.s and hydrogen (active hydrogen) content of 0.4%, and 0.6 part of 1-ethynyl-1-cyclohexanol inhibitor, and vacuum mixing for 40 minutes to obtain component B.
Example 3
The embodiment provides a two-component addition type silicone adhesive for textiles, which is prepared by the following steps:
the preparation of component A is the same as in example 1.
The component B comprises:
1) 100 parts of vinyl silicone oil with the viscosity of 10000mPa.s, 30 parts of fumed silica, 5 parts of hexamethyldisilazane and 2.5 parts of water are added into a kneader for multiple times, and the mixture is kneaded for 3 minutes after each addition, and is kneaded for 1 hour at room temperature after all the additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) Cooling, transferring to a planetary stirrer, adding 10 parts of silane modified esterified polyether shown as the formula (I) (wherein n is 18), 30 parts of hydrogen-containing silicone oil with the viscosity of 50mPa.s and the hydrogen (active hydrogen) content of 0.4 percent, and 0.6 part of 1-ethynyl-1-cyclohexanol inhibitor, and mixing in vacuum for 40 minutes to obtain a component B.
Example 4
The embodiment provides a two-component addition type silicone adhesive for textiles, which is prepared by the following steps:
the preparation of component A is the same as in example 1.
The component B comprises:
1) 100 parts of vinyl silicone oil with the viscosity of 10000mPa.s, 30 parts of fumed silica, 5 parts of hexamethyldisilazane and 2.5 parts of water are added into a kneader for multiple times, and the mixture is kneaded for 3 minutes after each addition, and is kneaded for 1 hour at room temperature after all the additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) Cooling, transferring to a planetary stirrer, adding 8 parts of silane modified esterified polyether shown as the formula (I) (wherein n is 14), 30 parts of hydrogen-containing silicone oil with the viscosity of 50mPa.s and the hydrogen (active hydrogen) content of 0.4 percent, and 0.6 part of 1-ethynyl-1-cyclohexanol inhibitor, and mixing in vacuum for 40 minutes to obtain a component B.
Example 5
The embodiment provides a two-component addition type silicone adhesive for textiles, which is prepared by the following steps:
the component A comprises:
1) 80 parts of vinyl silicone oil with viscosity of 20000mPa.s, 40 parts of fumed silica, 10 parts of hexamethyldisilazane and 4 parts of water are added into a kneader for multiple times, and kneaded for 3 minutes after each addition, and kneaded for 1 hour at room temperature after all additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) After cooling, the mixture was transferred to a planetary mixer, and 5 parts of a platinum catalyst (an ethanol solution of chloroplatinic acid, platinum content: 0.15%) was added and mixed in vacuo for 40 minutes to obtain component A.
The component B comprises:
1) 60 parts of vinyl silicone oil having a viscosity of 20000mPa.s, 40 parts of fumed silica, 10 parts of hexamethyldisilazane and 4 parts of water were added in a kneader in a plurality of times, kneaded for 3 minutes after each addition, and kneaded for 1 hour at room temperature after all the additions were completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) Cooling, transferring to a planetary stirrer, adding 6 parts of silane modified esterified polyether (wherein n is 7) shown as the formula (I), 40 parts of hydrogen-containing silicone oil with the viscosity of 50mPa.s and the hydrogen (active hydrogen) content of 0.4 percent and 5 parts of 1-ethynyl-1-cyclohexanol inhibitor, and mixing for 40 minutes in vacuum to obtain the component B.
Example 6
The embodiment provides a two-component addition type silicone adhesive for textiles, which is prepared by the following steps:
the component A comprises:
1) 180 parts of vinyl silicone oil with a viscosity of 1000mPa.s, 15 parts of fumed silica, 2 parts of hexamethyldisilazane and 4 parts of water are added into a kneader in multiple times, and kneaded for 3 minutes after each addition, and kneaded for 1 hour at room temperature after all additions are completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) After cooling, the mixture was transferred to a planetary mixer, and 5 parts of a platinum catalyst (an ethanol solution of chloroplatinic acid, platinum content: 0.15%) was added and mixed in vacuo for 40 minutes to obtain component A.
The component B comprises:
1) 120 parts of vinyl silicone oil having a viscosity of 1000mPa.s, 15 parts of fumed silica, 2 parts of hexamethyldisilazane, and 4 parts of water were added in a kneader in portions, kneaded for 3 minutes after each addition, and kneaded for 1 hour at room temperature after all the additions were completed.
2) The temperature was raised to 85 ℃ and kneaded for 2 hours.
3) The temperature was raised to 150 ℃ and vacuum kneading was carried out for 2 hours.
4) Cooling, transferring to a planetary stirrer, adding 6 parts of silane modified esterified polyether (wherein n is 7) shown as the formula (I), 20 parts of hydrogen-containing silicone oil with the viscosity of 50mPa.s and the hydrogen (active hydrogen) content of 0.4 percent and 0.5 part of 1-ethynyl-1-cyclohexanol inhibitor, and mixing for 40 minutes in vacuum to obtain a component B.
Comparative example 1
The comparative example provides a two-component addition type silicone adhesive for textiles, and the preparation method comprises the following steps:
the preparation of component A and component B is the same as in example 1, except that component B is not added with silane-modified esterified polyether.
Comparative example 2
The comparative example provides a two-component addition type silicone adhesive for textiles, and the preparation method comprises the following steps:
the preparation of component A and component B was the same as in example 2, except that component B was prepared without the addition of the silane-modified esterified polyether and the same amount of gamma-glycidoxypropyltrimethoxysilane was added.
Comparative example 3
The comparative example provides a two-component addition type silicone adhesive for textiles, and the preparation method comprises the following steps:
the preparation of component A and component B was the same as in example 2, except that component B was prepared without the addition of the silane-modified esterified polyether and with the addition of the same amount of gamma- (methacryloyloxy) propyl trimethoxysilane.
The adhesives prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to a peeling test, and the test results are shown in table 1.
The component A and the component B prepared in the examples and the comparative examples are mixed according to the mass ratio of 1: 1 mixing and defoaming, flatly paving a nylon textile fabric on glass, gluing the nylon textile fabric, controlling the thickness of a curing adhesive by using a tape with the thickness of 0.2 mm, then sequentially covering another piece of nylon textile fabric and the glass, placing 2 kilograms of weights on the glass, curing for 20 minutes at 120 ℃, removing the upper glass and the lower glass after cooling, cutting a sample piece into a stripping test sample strip with the width of 10 mm, and testing the 180-degree stripping strength on a universal stretching machine.
TABLE 1 Peel Strength results Table
Compared with the traditional mode of not adding an adhesion promoter or adding monomer silane, the double-component addition type silicone adhesive using the silane-modified esterified polyether provided by the application has better adhesive force on a nylon textile fabric, and the lifting amplitude reaches more than 8%, preferably more than 15%.
Finally, the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A double-component addition type silicone adhesive is characterized in that the components contain silane modified esterified polyether;
the molecular structural formula of the silane modified esterified polyether is shown as the formula (I):
wherein n is 3 to 18.
2. The two-part addition type silicone adhesive according to claim 1, comprising a component A and a component B;
the component A comprises vinyl silicone oil, inorganic filler, hexamethyldisilazane, water and a platinum catalyst;
the component B comprises vinyl silicone oil, inorganic filler, hexamethyldisilazane, the silane-modified esterified polyether, hydrogen-containing silicone oil, an inhibitor and water.
3. The two-component addition type silicone adhesive according to claim 1 or 2, wherein the weight ratio of the component A to the component B is 1 (1-1.2).
4. The two-component addition type silicone adhesive according to claim 2 or 3, wherein the inorganic fillers in the component A and the component B are the same in kind; the inorganic filler is one or more of fumed silica, light or heavy calcium carbonate, alumina, silica micropowder and carbon black, and the fumed silica is preferred.
5. The two-component addition type silicone adhesive according to any one of claims 2 to 4, wherein the vinyl silicone oil in the component A and the vinyl silicone oil in the component B are the same in type; the vinyl silicone oil contains 0.5-3 wt% of vinyl and has a viscosity of 1000-20000 mPa.s.
6. The two-component addition type silicone adhesive according to any one of claims 2 to 5, wherein the hydrogen content in the hydrogen-containing silicone oil is 0.3 wt% to 0.7 wt%;
and/or the inhibitor is an alkynol compound;
and/or the platinum catalyst is one or more of platinum-alkyne base complex, isopropanol solution of chloroplatinic acid or platinum-vinyl siloxane complex.
7. The two-component addition type silicone adhesive according to any one of claims 2 to 6, wherein the mass ratio of the vinyl silicone oil, the inorganic filler, the hexamethyldisilazane, the water and the platinum catalyst in the component A is (80-180): (15-40): (2-10): (1-4): (1-5).
8. The two-component addition type silicone adhesive according to any one of claims 2 to 7, wherein the mass ratio of the vinyl silicone oil, the inorganic filler, hexamethyldisilazane, water, the silane-modified esterified polyether, the hydrogen-containing silicone oil and the inhibitor in the component B is (60-120): (15-40): (2-10): (1-4): (2-10): (20-40): (0.5-5).
9. The method of preparing the two-component addition type silicone adhesive according to any one of claims 2 to 8, comprising the steps of:
the component A comprises:
adding vinyl silicone oil, inorganic filler, hexamethyldisilazane and water into a kneading machine for multiple times, kneading for 0.5-1 h at room temperature, heating to 80-90 ℃, kneading for 2-3 h, heating to 140-150 ℃, kneading for 2-3 h, cooling, adding a platinum catalyst, and mixing in vacuum to obtain the composite material;
the component B comprises:
adding vinyl silicone oil, inorganic filler, hexamethyldisilazane and water into a kneading machine for multiple times, kneading for 0.5-1 h at room temperature, heating to 80-90 ℃, kneading for 2-3 h, heating to 140-150 ℃, kneading for 2-3 h, cooling, adding silane modified esterified polyether shown in formula (I), hydrogen-containing silicone oil and an inhibitor, and mixing in vacuum to obtain the silicone oil.
10. Use of the two-component addition silicone adhesive of any one of claims 1 to 8 in the preparation of an adhesive for textiles.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5552223A (en) * | 1992-10-30 | 1996-09-03 | Dow Corning Toray Silicone Co., Ltd. | Organopolysiloxane modified polyesters and method of the preparation thereof |
| CN108219671A (en) * | 2018-01-11 | 2018-06-29 | 佛山市天宝利硅工程科技有限公司 | A kind of bi-component addition type liquid silastic and preparation method thereof |
| CN113929897A (en) * | 2021-11-01 | 2022-01-14 | 江西晨光新材料股份有限公司 | Silane modified esterified polyether and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5552223A (en) * | 1992-10-30 | 1996-09-03 | Dow Corning Toray Silicone Co., Ltd. | Organopolysiloxane modified polyesters and method of the preparation thereof |
| CN108219671A (en) * | 2018-01-11 | 2018-06-29 | 佛山市天宝利硅工程科技有限公司 | A kind of bi-component addition type liquid silastic and preparation method thereof |
| CN113929897A (en) * | 2021-11-01 | 2022-01-14 | 江西晨光新材料股份有限公司 | Silane modified esterified polyether and preparation method and application thereof |
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