CN114395367A - High-strength RTV-2 sealant and preparation method thereof - Google Patents

High-strength RTV-2 sealant and preparation method thereof Download PDF

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Publication number
CN114395367A
CN114395367A CN202210098071.4A CN202210098071A CN114395367A CN 114395367 A CN114395367 A CN 114395367A CN 202210098071 A CN202210098071 A CN 202210098071A CN 114395367 A CN114395367 A CN 114395367A
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component
parts
mass
mpa
sealant
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郑玉娜
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Shenzhen Victory On Trust New Material Technology Co ltd
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Shenzhen Victory On Trust New Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention belongs to the technical field of organosilicon sealants, and discloses a high-strength RTV-2 sealant and a preparation method thereof. The high-strength RTV-2 sealant comprises a component A and a component B, wherein the mixing ratio of the A, B components is 0.8-1.2: 0.8-1.2, wherein the component A comprises A1 polydimethylsiloxane, A2 reinforcing base glue, A3 plasticizer, A4 inorganic filler and A5 color paste; the component B comprises B1 polydimethylsiloxane, B2 reinforcing base glue, B3 plasticizer, B4 inorganic filler, B5 cross-linking agent, B6 tackifier and B7 catalyst. The mixing proportion of the A, B component in the sealant can be 1:1, easy ratio use, and even there is certain deviation when mixing, it is little to the glue performance influence. In addition, the sealant has the advantages of high curing speed, high strength and high elasticity, and is suitable for the field of quick bonding and sealing with high strength requirement.

Description

High-strength RTV-2 sealant and preparation method thereof
Technical Field
The invention relates to the technical field of organosilicon sealants, in particular to a high-strength RTV-2 sealant and a preparation method thereof.
Background
Since the introduction of organosilicon materials in the middle of the 20 th century, the organosilicon material industry in China is developed vigorously, the yield and the sales volume are continuously and rapidly increased, and the liquid silicone rubber is one of the most promising products in the organosilicon industry and is widely applied to the national economy pillar industries such as buildings, automobiles, electronic and electrical products, aviation, machinery and the like. The room temperature condensed type double-component (RTV-2) liquid silicone rubber not only has the characteristics of high and low temperature resistance, aging resistance, chemical corrosion resistance, electric insulation and the like of room temperature condensed type single-component (RTV-1) liquid silicone rubber, but also has the characteristics of high internal curing efficiency, good storage stability and the like. However, the unreinforced RTV silicone rubber has low strength (about 0.3-0.4 MPa) after vulcanization, has no practical application value, needs to be reinforced by adding a filler, and a common reinforcing method is a gas phase method or a white carbon black precipitation method, but because a large amount of active hydroxyl groups exist on the surface of white carbon black, the probability of forming intermolecular hydrogen bonds is high, so that the white carbon black is difficult to be uniformly dispersed in a silicone rubber system.
In the prior art, for example, patent CN107805481 discloses a two-component silicone sealant, which comprises a component a and a component B, wherein the component a comprises 100 parts of end-capped polydimethylsiloxane, 20-80 parts of alkyl end-capped polydimethylsiloxane, 50-80 parts of inorganic filler and 1-5 parts of pigment, and the component B comprises 100 parts of end-capped polydimethylsiloxane, 10-30 parts of cross-linking agent, 1-4 parts of coupling agent, 4-8 parts of catalyst, 3-7 parts of anti-aging agent and 2-6 parts of ultraviolet absorbent. For another example, patent CN111500251 describes a two-component condensed type adhesive sealant and a preparation method thereof, the sealant comprises a component a and a component B, the component a comprises a1 organic siloxane, a2 filler, A3 moisture and a4 catalyst; the B component comprises B1 organic siloxane, B2 filler, B3 cross-linking agent and B4 adhesion promoter. The A, B component of the sealant can be freely matched from 0.5:1 to 5:1, and the product still can keep better final performance and is suitable for popularization and application, but the product has lower strength and needs to be improved.
In addition, because the proportion of A, B component in the bi-component is influenced by the metering proportion of the equipment, the requirement on the equipment is higher, and the deviation of the mixing proportion has obvious influence on the performance of the glue, the current bi-component product is difficult to carry out large-scale quantitative production, and has certain limitation in application and popularization.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provides a high-strength RTV-2 sealant and a preparation method thereof. The mixing proportion of the A, B component in the sealant can be 1:1, easy ratio use, and even there is certain deviation when mixing, it is little to the glue performance influence. In addition, the sealant has the advantages of high curing speed, high strength and high elasticity, and is suitable for the field of quick bonding and sealing with high strength requirement.
In order to achieve the aim of the invention, the high-strength RTV-2 sealant comprises a component A and a component B, wherein the mixing ratio of the A, B components is 0.8-1.2: 0.8-1.2, wherein the component A comprises A1 polydimethylsiloxane, A2 reinforcing base glue, A3 plasticizer, A4 inorganic filler and A5 color paste; the component B comprises B1 polydimethylsiloxane, B2 reinforcing base glue, B3 plasticizer, B4 inorganic filler, B5 cross-linking agent, B6 tackifier and B7 catalyst.
Further, in some embodiments of the present invention, the part A comprises 20 to 50 parts by mass of A2, 2 to 10 parts by mass of A3, 30 to 80 parts by mass of A4 and 1 to 5 parts by mass of A5 based on 100 parts by mass of A1.
Further, in some embodiments of the present invention, the B component comprises, based on 100 parts by mass of B1, 20 to 50 parts by mass of B2, 2 to 10 parts by mass of B3, 30 to 80 parts by mass of B4, 1 to 10 parts by mass of B5, 0.5 to 5 parts by mass of B6, and 0.1 to 3 parts by mass of B7.
Further, in some embodiments of the invention, the A1 is a hydroxyl terminated polydimethylsiloxane having a viscosity of 1500 to 50000 mPa.s and the B1 is an alkoxy terminated polydimethylsiloxane having a viscosity of 1500 to 50000 mPa.s.
Further, in some embodiments of the present invention, the reinforcing base adhesives a2 and B2 are reinforcing base adhesives obtained by mixing dimethyl silicone oil and fumed silica and performing surface treatment with a silane coupling agent, and the viscosity of the reinforcing base adhesives is 100 to 500 ten thousand mpa.s.
Further, in some embodiments of the present invention, the a2, B2 reinforcing base adhesive is prepared by: uniformly mixing dimethyl silicone oil and fumed silica in a vacuum kneading machine, adding a silane coupling agent, kneading at the temperature below 100 ℃, heating to 130-150 ℃ after uniform kneading, carrying out high-temperature kneading at the vacuum degree of-0.08-0.1 MPa for not less than 3h, transferring, grinding, and finally carrying out vacuum dispersion to obtain the reinforcing base rubber.
Preferably, in some embodiments of the present invention, the viscosity of the simethicone is 50 to 1000 mPa.s, and the specific surface area of the fumed silica is 100 to 400m2The silane coupling agent is a silane coupling agent containing vinyl or amino.
Further, in some embodiments of the present invention, the plasticizer A3 and B3 is dimethicone, and preferably, the viscosity of the plasticizer is 50 to 1000 mPa.s.
Further, in some embodiments of the present invention, the a4, B4 inorganic filler is nano calcium carbonate that is surface modified.
Further, in some embodiments of the present invention, the a5 color paste is a color paste prepared by mixing any one or more of carbon black, red iron oxide, yellow nickel chrome, brown chrome, blue chrome, green chrome, and iron blue with dimethyl silicone oil.
Further, in some embodiments of the present invention, the B5 crosslinker is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, or vinyltriethoxysilane.
Further, in some embodiments of the present invention, the B6 adhesion promoter is an amino or epoxy group-bearing alkoxysilane containing at least two alkoxy groups.
Further, in some embodiments of the present invention, the B7 catalyst is an organometallic catalyst that promotes moisture cure; preferably, the B7 catalyst is one or a mixture of isopropyl titanate, butyl titanate or dibutyltin dilaurate.
On the other hand, the invention also provides a preparation method of the high-strength RTV-2 sealant, which comprises the following steps:
(1) preparing A2 and B2 reinforcing base glue;
(1) preparation of component A: uniformly mixing A1, A2, A4 and A5, then controlling the temperature of the materials to be not more than 100 ℃, stirring for 90-150 minutes, cooling the materials to be below 40 ℃, then adding A3, vacuumizing to ensure that the vacuum degree is-0.08-0.1 MPa, stirring for 30-60 minutes, discharging, and hermetically packaging to obtain a component A;
(2) preparation of the component B: uniformly mixing B1, B2 and B4, simultaneously heating the materials to 130-150 ℃, controlling the vacuum degree to be-0.08 to-0.1 MPa, stirring for 90-150 minutes, then cooling the materials to below 40 ℃, then adding B3 and B5, controlling the temperature of the materials not to exceed 50 ℃, simultaneously vacuumizing, controlling the vacuum degree to be-0.08 to-0.1 MPa, stirring for 30-60 minutes, then adding B6 and B7, controlling the temperature of the materials not to exceed 50 ℃, simultaneously vacuumizing, controlling the vacuum degree to be-0.08 to-0.1 MPa, stirring for 30-60 minutes, then discharging, sealing and packaging to obtain the component B.
Compared with the prior art, the invention has the following advantages:
(1) the sealant has reasonable component collocation, the A, B component mixing proportion can be 1:1, so that the influence of the metering proportion error is small, the metering requirement on mixing equipment is low, and the production efficiency and the product quality are favorably improved;
(2) the invention adopts the matching of the polydimethylsiloxanes with different end closures and uses the self-made reinforcing base adhesive for reinforcing, so that the two-component sealant can realize higher curing speed, higher strength and better elasticity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
Furthermore, the description below of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily for the same embodiment or example. Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Examples 1 to 4
Preparing raw materials according to the components and the proportion (the proportion of each component is mass percent) shown in the standard 1, and preparing the high-strength RTV-2 sealant by the following method:
(1) preparing a reinforcing base adhesive: uniformly mixing dimethyl silicone oil and fumed silica in a vacuum kneader, adding a silane coupling agent, kneading at the temperature of below 100 ℃, setting the temperature to 140 ℃ after the mixture is uniform, kneading at high temperature for 5 hours with the vacuum degree of-0.1 Mpa, transferring to a three-roll machine, grinding for 2 times, and finally dispersing uniformly in vacuum to obtain a reinforcing base adhesive;
(2) preparation of component A: uniformly mixing A1, A2, A4 and A5 by using a power mixer, controlling the revolution speed to be 20Hz and the dispersion speed to be 20Hz, and then stirring for 2 hours while controlling the temperature of the materials not to exceed 100 ℃; cooling the materials to below 40 ℃, adding A3, setting the revolution speed at 20Hz and the dispersion speed at 10Hz, simultaneously vacuumizing the materials at the vacuum degree of-0.1 MPa, stirring for 60 minutes, finally discharging the materials, and hermetically packaging to obtain a component A;
(3) preparation of the component B: uniformly mixing B1, B2 and B4 by using a power mixer, wherein the revolution speed is 20Hz, the dispersion speed is 20Hz, simultaneously heating the materials to 140 ℃, controlling the vacuum degree to be-0.1 MPa, and stirring for 2 hours; cooling the materials to below 40 ℃, adding B3 and B5, setting the revolution speed to be 20Hz and the dispersion speed to be 10Hz, controlling the temperature of the materials to be not more than 50 ℃ by using cold circulating water, simultaneously vacuumizing to the vacuum degree of-0.1 MPa, and stirring for 60 minutes; then adding B6 and B7, setting the revolution speed at 20Hz and the dispersion speed at 10Hz, controlling the temperature of the materials not to exceed 50 ℃ by using cold circulating water, simultaneously vacuumizing to the vacuum degree of-0.1 MPa, stirring for 60 minutes, finally discharging, and sealing and packaging to obtain the component B.
Table 1 examples 1-4 raw material compositions and ratios
Figure DEST_PATH_IMAGE001
Wherein, the modified nano calcium carbonate is purchased from Australian whitish chemical Co., Ltd in England; the epoxypropyltrimethoxysilane of B6 is also known as 3- (2, 3-epoxypropoxy) propyltrimethoxysilane with CAS number 2530-83-8. Example A part A and B part were mixed at a volume ratio of 1:1 and tested for properties, the results of which are shown in Table 2.
Table 2 examples performance test results
Test results Example 1 Example 2 Example 3 Example 4
Time to surface dry (min) 20 15 15 10
Initial fixed time (min) 120 100 100 80
Shear strength (MPa) 3.5 3.8 4.3 4.6
Tensile Strength (MPa) 4.0 4.3 4.6 4.1
Elongation at Break (%) 400 360 330 300
Shore hardness (A) 35 38 42 45
As can be seen from the data in the table 2, the sealant of the invention has the advantages of fast initial setting time, high strength of more than 4.0MP, good strength, high elongation at break of more than 300 percent and good elasticity.
The component A and the component B are mixed according to different mixing ratios, and the influence on the performance of the sealant is tested, and the test comparison results are shown in Table 3.
Table 3 example 3 comparison of performance tests of different mixing ratio
Figure DEST_PATH_IMAGE003
As can be seen from the data in Table 3 above, the example 3 was selected to have a change in the blend ratio of A, B, which has little effect on the cure rate, mechanical strength and elongation at break of the sealant of example 3, even though the blend deviates by 20%.
Therefore, the sealing glue is matched with polydimethylsiloxane with different end closures and reinforced by the reinforcing base glue produced by the self-made scheme, and the prepared sealing glue has higher strength and better elasticity; A. the component B comprises the following components in percentage by weight: the 1 proportion is easy to mix and use, has low requirement on the dispensing equipment, large range of use proportion and wide applicability, and is suitable for the field of quick bonding and sealing with high strength requirement.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.

Claims (10)

1. The high-strength RTV-2 sealant is characterized by comprising a component A and a component B, wherein the mixing ratio of A, B components is 0.8-1.2: 0.8-1.2, wherein the component A comprises A1 polydimethylsiloxane, A2 reinforcing base glue, A3 plasticizer, A4 inorganic filler and A5 color paste; the component B comprises B1 polydimethylsiloxane, B2 reinforcing base glue, B3 plasticizer, B4 inorganic filler, B5 cross-linking agent, B6 tackifier and B7 catalyst.
2. The high-strength RTV-2 sealant according to claim 1, wherein the component A comprises 100 parts by mass of A1, 20-50 parts by mass of A2, 2-10 parts by mass of A3, 30-80 parts by mass of A4 and 1-5 parts by mass of A5.
3. The high-strength RTV-2 sealant according to claim 1, wherein the B component comprises 100 parts by mass of B1, 20-50 parts by mass of B2, 2-10 parts by mass of B3, 30-80 parts by mass of B4, 1-10 parts by mass of B5, 0.5-5 parts by mass of B6, and 0.1-3 parts by mass of B7.
4. The high strength RTV-2 sealant according to claim 1, wherein A1 is hydroxyl terminated polydimethylsiloxane having viscosity of 1500-50000 mPa.s, and B1 is alkoxy terminated polydimethylsiloxane having viscosity of 1500-50000 mPa.s.
5. The high-strength RTV-2 sealant as claimed in claim 1, wherein the reinforcing base adhesives A2 and B2 are reinforcing base adhesives prepared by mixing dimethyl silicone oil and fumed silica and performing surface treatment with silane coupling agent, and the viscosity of the reinforcing base adhesives is 100 to 500 ten thousand mPa.s.
6. The high-strength RTV-2 sealant according to claim 1, wherein the reinforcing base adhesives A2 and B2 are prepared by the following steps: uniformly mixing dimethyl silicone oil and fumed silica in a vacuum kneading machine, adding a silane coupling agent, kneading at the temperature below 100 ℃, heating to 130-150 ℃ after uniform kneading, carrying out high-temperature kneading at the vacuum degree of-0.08-0.1 MPa for not less than 3h, transferring, grinding, and finally carrying out vacuum dispersion to obtain a reinforcing base adhesive; preferably, the viscosity of the dimethyl silicone oil is 50-1000 mPa.s, and the specific surface area of the fumed silica is 100-400 m2The silane coupling agent is a silane coupling agent containing vinyl or amino.
7. The high-strength RTV-2 sealant according to claim 1, wherein the plasticizer A3 and B3 is dimethicone, and preferably the viscosity of the plasticizer is 50 to 1000 mPa.s.
8. The high strength RTV-2 sealant according to claim 1, wherein the A4 and B4 inorganic fillers are surface modified nano calcium carbonate.
9. The high-strength RTV-2 sealant according to claim 1, wherein the A5 color paste is a color paste prepared by mixing one or more of carbon black, red iron oxide, yellow iron oxide, Qinzi nickel yellow, Qinzi chrome brown, cobalt blue, cobalt green and iron blue with dimethyl silicone oil; preferably, the B5 crosslinking agent is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane or vinyltriethoxysilane; preferably, the B6 adhesion promoter is an amino or epoxy group-bearing alkoxysilane containing at least two alkoxy groups; preferably, the B7 catalyst is an organometallic catalyst that promotes moisture cure; preferably, the B7 catalyst is one or a mixture of isopropyl titanate, butyl titanate or dibutyltin dilaurate.
10. A process for the preparation of a high strength RTV-2 sealant according to any one of claims 1 to 9, characterized in that it comprises the following steps:
(1) preparing A2 and B2 reinforcing base glue;
(1) preparation of component A: uniformly mixing A1, A2, A4 and A5, then controlling the temperature of the materials to be not more than 100 ℃, stirring for 90-150 minutes, cooling the materials to be below 40 ℃, then adding A3, vacuumizing to ensure that the vacuum degree is-0.08-0.1 MPa, stirring for 30-60 minutes, discharging, and hermetically packaging to obtain a component A;
(2) preparation of the component B: uniformly mixing B1, B2 and B4, simultaneously heating the materials to 130-150 ℃, controlling the vacuum degree to be-0.08 to-0.1 MPa, stirring for 90-150 minutes, then cooling the materials to below 40 ℃, then adding B3 and B5, controlling the temperature of the materials not to exceed 50 ℃, simultaneously vacuumizing, controlling the vacuum degree to be-0.08 to-0.1 MPa, stirring for 30-60 minutes, then adding B6 and B7, controlling the temperature of the materials not to exceed 50 ℃, simultaneously vacuumizing, controlling the vacuum degree to be-0.08 to-0.1 MPa, stirring for 30-60 minutes, then discharging, sealing and packaging to obtain the component B.
CN202210098071.4A 2022-01-27 2022-01-27 High-strength RTV-2 sealant and preparation method thereof Pending CN114395367A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109971416A (en) * 2019-04-24 2019-07-05 陈果 A kind of modified bi-component silicone sealant and preparation method thereof
CN110205084A (en) * 2019-06-13 2019-09-06 罗青菊 A kind of expediting setting type organosilicon sealant
CN111057517A (en) * 2019-12-31 2020-04-24 广州机械科学研究院有限公司 Bi-component fast curing type organic silicon structural adhesive and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109971416A (en) * 2019-04-24 2019-07-05 陈果 A kind of modified bi-component silicone sealant and preparation method thereof
CN110205084A (en) * 2019-06-13 2019-09-06 罗青菊 A kind of expediting setting type organosilicon sealant
CN111057517A (en) * 2019-12-31 2020-04-24 广州机械科学研究院有限公司 Bi-component fast curing type organic silicon structural adhesive and preparation method thereof

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Application publication date: 20220426