CN112646541A - Dual-curing system organic silicon composition and preparation method thereof - Google Patents
Dual-curing system organic silicon composition and preparation method thereof Download PDFInfo
- Publication number
- CN112646541A CN112646541A CN202011506508.0A CN202011506508A CN112646541A CN 112646541 A CN112646541 A CN 112646541A CN 202011506508 A CN202011506508 A CN 202011506508A CN 112646541 A CN112646541 A CN 112646541A
- Authority
- CN
- China
- Prior art keywords
- component
- coo
- dual
- sio
- silicone composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 15
- 229910052710 silicon Inorganic materials 0.000 title claims description 15
- 239000010703 silicon Substances 0.000 title claims description 15
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 31
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 24
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 16
- SNVLJLYUUXKWOJ-UHFFFAOYSA-N methylidenecarbene Chemical compound C=[C] SNVLJLYUUXKWOJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 10
- 229910004674 SiO0.5 Inorganic materials 0.000 claims abstract description 4
- 229910020381 SiO1.5 Inorganic materials 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- 238000001723 curing Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- 230000009977 dual effect Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 10
- 230000005494 condensation Effects 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 9
- 150000001451 organic peroxides Chemical class 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical group N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 8
- 239000003063 flame retardant Substances 0.000 claims description 8
- HSLFISVKRDQEBY-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)cyclohexane Chemical group CC(C)(C)OOC1(OOC(C)(C)C)CCCCC1 HSLFISVKRDQEBY-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 125000003944 tolyl group Chemical group 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 125000004423 acyloxy group Chemical group 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract 2
- 229920005989 resin Polymers 0.000 description 16
- 239000011347 resin Substances 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000004590 silicone sealant Substances 0.000 description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000000565 sealant Substances 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000013008 moisture curing Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- -1 polysiloxane Polymers 0.000 description 1
- 239000004945 silicone rubber 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
- 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a dual-curing system organosilicon composition which comprises (R)3SiO0.5)a(R2SiO)b(R1SiO1.5)c(SiO)dAnd linear organopolysiloxanes, wherein R1、R2And R3Are the same or different from each other and are independently selected from alkoxy and CH2=CH‑COO(CH)m‑、CH2=C(CH3)‑COO(CH)m-, methyl or phenyl; a. b, c and d are each an integer of 1 to 200; the linear organopolysiloxane has alkoxy and CH in the molecular structure2=CH‑COO(CH)m‑、CH2=C(CH3)‑COO(CH)m-one or more of; the invention also discloses a method for preparing the dual-curing system organosilicon compositionA preparation method. According to the method, the crosslinking density of the material is enhanced by adopting a dual-curing system, and the bonding capacity of the product can be effectively improved by using acyloxy in the system, so that the purposes of improving the hardness and the strength are achieved, and the application field and the application range of the product are further expanded.
Description
Technical Field
The invention relates to the technical field of silicon compositions, in particular to a dual-curing system organic silicon composition and a preparation method thereof.
Background
There are many types of silicone sealants, and the performance of different types of silicone sealants varies greatly. The condensed type silicon sulfide rubber is a moisture-cured one-component organic silicon adhesive, and has excellent aging resistance, high insulation, temperature resistance and medium resistance, so that the condensed type silicon sulfide rubber is widely applied to various industries. The dealcoholized room temperature vulcanized silicone rubber is one of single-component room temperature vulcanized silicone rubbers, and has better development prospect compared with other kinds of room temperature silicone rubbers due to the characteristics of no corrosion, low odor and rapid curing.
The general condensed type solidified organic silicon has low hardness and mechanical strength, and the colloid is easy to damage when being subjected to external force. Therefore, it is highly desirable to develop a silicone sealant with high hardness and mechanical strength to meet the requirements of various applications.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a dual-curing system organic silicon composition and a preparation method thereof.
The invention discloses a dual-curing system organic silicon composition, which comprises a component A and a component B, wherein the component A is a three-dimensional reticular organic polysiloxane with the following formula (I):
(R3SiO0.5)a(R2SiO)b(R1SiO1.5)c(SiO)d (Ⅰ)
in the formula (I), R1Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; r2Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; r3Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; a. b, c and d are each an integer of 1 to 200;
the component B is straight-chain organopolysiloxane with alkoxy and CH in the molecule2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)m-one or more of (a) and (b).
Preferably, the A component is waxy or solid at 25 ℃.
One dual cure system silicone composition herein also includes an organic peroxide and a condensation catalyst.
Preferably, the organic peroxide is 1, 1-bis (t-butylperoxy) cyclohexane.
Preferably, the condensation catalyst is a zirconium catalyst or a titanium catalyst.
Preferably, a dual cure system silicone composition further comprises a filler.
Preferably, the filler is a flame retardant or heat resistant agent.
A preparation method of a dual-curing system organic silicon composition comprises the following steps:
(1) weighing the component A and the component B, dissolving the component A in a solvent with equal mass, and then uniformly mixing the component A with the component B;
(2) removing the solvent from the substances under the pressure of-0.8 to-1 Mpa at the temperature of 100 ℃, and cooling to room temperature;
(3) and (3) sequentially adding the filler, the organic peroxide and the condensation catalyst into the substances, and uniformly stirring to obtain a finished product.
Preferably, in step (1), the solvent is toluene.
The beneficial effect of this application lies in: the crosslinking density of the material is enhanced by adopting a dual-curing system, and the bonding capability of the product can be effectively improved by using acyloxy in the system, so that the aim of improving the hardness and the strength is fulfilled, and the application field and the application range of the product are further expanded.
Detailed Description
In the following description, numerous implementation details are set forth in order to provide a thorough understanding of the present invention. It should be understood, however, that these implementation details are not to be interpreted as limiting the invention. That is, in some embodiments of the invention, such implementation details are not necessary.
The invention discloses a dual-curing system organic silicon composition which comprises an A component and a B component, wherein
The component A is three-dimensional reticular organopolysiloxane with the following formula (I):
(R3SiO0.5)a(R2SiO)b(R1SiO1.5)c(SiO)d (Ⅰ)
in the formula (I), R1、R2And R3Equal to or different from each other, R1Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; r2Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; r3Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl. a. b, c and d are each an integer of 1 to 200. Preferably, the A component is waxy or solid at 25 ℃.
Specifically, the resin of the component A has different preparation methods, which are as follows:
synthesis of a1 component resin:
adding 324g of deionized water, 40g of absolute ethyl alcohol and 300g of toluene mixed solvent, 0.01mol of hexamethyldisiloxane and 9.4g of hydrochloric acid into a three-neck flask with a stirrer and a temperature control device in sequence, heating to 50-60 ℃, dripping a mixture of 3mol of methyltrimethoxysilane and 3mol of KH570 silane coupling agent within 1h, stirring and reacting for 1h after dripping, heating to 71 ℃ and maintaining the reaction for 2h, separating liquid while hot, taking out an oil phase, pouring the oil phase into distilled water, washing to be neutral, adding anhydrous magnesium sulfate, drying to be clear and transparent, pouring transparent liquid into the three-neck flask, adding 3.5g of tetramethylammonium hydroxide, heating to 110 ℃ under stirring, and carrying out reflux reaction for half an hour. Then slowly heating to 150 ℃ on a rotary evaporator, and then slowly vacuumizing to remove small molecules, thereby finally obtaining the colorless and transparent silicone resin.
Synthesis of a2 component resin:
adding 324g of deionized water, 40g of absolute ethyl alcohol and 300g of toluene mixed solvent, 0.01mol of hexamethyldisiloxane and 9.4g of hydrochloric acid into a three-neck flask with a stirrer and a temperature control device in sequence, heating to 50-60 ℃, dripping a mixture of 5mol of methyltrimethoxysilane and 1mol of KH570 silane coupling agent within 1h, stirring and reacting for 1h after dripping, heating to 71 ℃ and maintaining the reaction for 2h, separating liquid while hot, taking out an oil phase, pouring the oil phase into distilled water, washing to be neutral, adding anhydrous magnesium sulfate, drying to be clear and transparent, pouring transparent liquid into the three-neck flask, adding 3.5g of tetramethylammonium hydroxide, heating to 110 ℃ under stirring, and carrying out reflux reaction for half an hour. Then slowly heating to 150 ℃ on a rotary evaporator, and then slowly vacuumizing to remove small molecules, thereby finally obtaining the colorless and transparent silicone resin.
Synthesis of a3 component resin:
324g of deionized water, 40g of absolute ethyl alcohol and 300g of toluene mixed solvent, 0.01mol of hexamethyldisiloxane and 9.4g of hydrochloric acid are added into a three-mouth flask with a stirrer and a temperature control device at a time, the temperature is raised to 50-60 ℃, 6mol of methyltrimethoxysilane is dropped in within 1h, stirring reaction is carried out for 1h after dropping is finished, the temperature is raised to 71 ℃, reaction is maintained for 2h after the temperature is raised, liquid is separated while the liquid is hot, the oil phase is taken out, the oil phase is poured into distilled water to be washed to be neutral, then anhydrous magnesium sulfate is added to be dried to be clear and transparent, 3.5g of tetramethylammonium hydroxide is added after the transparent liquid is poured into the three-mouth flask, and the mixture is heated. Then slowly heating to 150 ℃ on a rotary evaporator, and then slowly vacuumizing to remove small molecules, thereby finally obtaining the colorless and transparent silicone resin.
The component B is straight-chain organopolysiloxane with alkoxy and CH in the molecule2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)m-one or more of (a) and (b). In specific applications, the following two linear organopolysiloxanes can be used as the component B:
the B1 component is the following organopolysiloxane:
the B2 component is the following organopolysiloxane:
one dual cure system silicone composition herein also includes an organic peroxide and a condensation catalyst.
Preferably, the organic peroxide is 1, 1-bis (t-butylperoxy) cyclohexane.
Preferably, the condensation catalyst is a zirconium catalyst or a titanium catalyst, and further, the condensation catalyst can be tetrabutyl titanate.
Preferably, a dual cure system silicone composition herein further comprises a filler. The filler can be selected from a heat-resistant agent and a flame-retardant auxiliary agent, and further the flame retardant is selected from Xinyue KR-2710.
A preparation method of a dual-curing system organic silicon composition comprises the following steps:
(1) weighing the component A and the component B, dissolving the component A in a solvent with equal mass, and then uniformly mixing the component A with the component B;
(2) removing the solvent from the substances under the pressure of-0.8 to-1 Mpa at the temperature of 100 ℃, and cooling to room temperature;
(3) and (3) sequentially adding the filler, the organic peroxide and the condensation catalyst into the substances, and uniformly stirring to obtain a finished product.
Preferably, in step (1), the solvent is toluene.
The double curing system is formed by moisture curing by using hydroxyl or alkoxy in the system and peroxide curing by using KH570 silane coupling agent in the system.
The present invention will be described in more detail below by showing a plurality of examples.
Example 1
Weighing 30g of A1 component resin, dissolving the resin in toluene with the same mass, uniformly mixing the resin with 70g of organopolysiloxane of B1 component, removing toluene under the condition that the pressure is-0.8 to-1 Mpa and the temperature is 100 ℃, adding 5g of Xinyue KR-2710 flame retardant, 0.5g of 1, 1-bis (tert-butylperoxy) cyclohexane and 0.8g of tetrabutyl titanate to the mixture till the mixture returns to the room temperature, and uniformly stirring to obtain a finished product for later use.
Example 2
Weighing 30g of A2 component resin, dissolving the resin in toluene with the same mass, uniformly mixing the resin with 35g of organopolysiloxane of component B1 and organopolysiloxane of component 35g of component B2, removing toluene at the pressure of-0.8 to-1 Mpa and the temperature of 100 ℃, returning to room temperature, adding 5g of Xinyue KR-2710 flame retardant, 0.5g of 1, 1-bis (tert-butylperoxy) cyclohexane and 0.8g of tetrabutyl titanate, and uniformly stirring to obtain a finished product for later use.
Example 3
Weighing 30g of A3 component resin, dissolving the resin in toluene with the same mass, uniformly mixing the resin with 35g of organopolysiloxane of component B1 and organopolysiloxane of component 35g of component B2, removing toluene at the pressure of-0.8 to-1 Mpa and the temperature of 100 ℃, returning to room temperature, adding 5g of Xinyue KR-2710 flame retardant, 0.5g of 1, 1-bis (tert-butylperoxy) cyclohexane and 0.8g of tetrabutyl titanate, and uniformly stirring to obtain a finished product for later use.
Example 4
Weighing 30g of A3 component resin, dissolving the resin in toluene with the same mass, uniformly mixing the resin with 70g of organopolysiloxane of B2 component, removing toluene under the condition that the pressure is-0.8 to-1 Mpa and the temperature is 100 ℃, adding 5g of Xinyue KR-2710 flame retardant, 0.5g of 1, 1-bis (tert-butylperoxy) cyclohexane and 0.8g of tetrabutyl titanate to the mixture till the mixture returns to the room temperature, and uniformly stirring to obtain a finished product for later use.
The silicone compositions obtained in examples 1 to 4 above were tested and the results are shown in the following table:
as can be seen from the above data, the shear force values of the silicone sealants obtained in examples 1 to 3 are greater than the shear force value of the silicone sealant obtained in example 4, i.e., the silicone sealant containing the organopolysiloxane of component B1 has better mechanical strength. And the hardness and the shear force value of the organic silicon sealant prepared in the embodiment 1 and the embodiment 2 are both larger than those of the organic silicon sealant prepared in the embodiment 4, namely, the hardness and the shear force value of the organic silicon sealant are improved to a certain extent by adding the KH570 silane coupling agent.
To sum up: according to the dual-curing system organosilicon composition and the dual-curing system organosilicon composition, moisture curing is carried out by utilizing hydroxyl or alkoxy in the system, peroxide curing is carried out by utilizing a KH570 silane coupling agent in the system, so that a dual-curing system is formed, the crosslinking density of materials is enhanced by adopting the dual-curing system, and meanwhile, the bonding capability of products can be effectively improved by virtue of acyloxy in the system, so that the purposes of improving the hardness and the strength are achieved, and the application field and the application range of the products are further expanded.
The above is merely an embodiment of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (9)
1. A dual cure system silicone composition characterized by comprising an a-component and a B-component; wherein the component A is a three-dimensional network organopolysiloxane with the following formula (I):
(R3SiO0.5)a(R2SiO)b(R1SiO1.5)c(SiO)d (Ⅰ)
in the formula (I), R1Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; r2Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; r3Is alkoxy, CH2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)mAny one of methyl, phenyl; a. b, c and d are each an integer of 1 to 200;
the component B is straight-chain organopolysiloxane with alkoxy and CH in the molecule2=CH-COO(CH)m-、CH2=C(CH3)-COO(CH)m-one or more of (a) and (b).
2. The dual cure system silicone composition according to claim 1, wherein the a component is waxy or solid at 25 ℃.
3. The dual cure system silicone composition according to claim 1, characterized in that it further comprises an organic peroxide and a condensation catalyst.
4. The dual cure system silicone composition according to claim 3, wherein the organic peroxide is 1, 1-bis (t-butylperoxy) cyclohexane.
5. The dual cure system silicone composition according to claim 3, characterized in that the condensation catalyst is a zirconium catalyst or a titanium catalyst.
6. The dual cure system silicone composition according to claim 3, characterized in that it further comprises a filler.
7. The dual cure system silicone composition according to claim 6, characterized in that the filler is a flame retardant or a heat resistant agent.
8. A preparation method of a dual-curing system organic silicon composition is characterized by comprising the following steps:
(1) weighing the component A and the component B, dissolving the component A in a solvent with equal mass, and then uniformly mixing the component A with the component B;
(2) removing the solvent from the substances under the pressure of-0.8 to-1 Mpa at the temperature of 100 ℃, and cooling to room temperature;
(3) and (3) sequentially adding the filler, the organic peroxide and the condensation catalyst into the substances, and uniformly stirring to obtain a finished product.
9. The dual cure system silicone composition according to claim 8, characterized in that, in step (1), the solvent is toluene.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011506508.0A CN112646541A (en) | 2020-12-18 | 2020-12-18 | Dual-curing system organic silicon composition and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011506508.0A CN112646541A (en) | 2020-12-18 | 2020-12-18 | Dual-curing system organic silicon composition and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112646541A true CN112646541A (en) | 2021-04-13 |
Family
ID=75355286
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011506508.0A Pending CN112646541A (en) | 2020-12-18 | 2020-12-18 | Dual-curing system organic silicon composition and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112646541A (en) |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1869125A (en) * | 2005-05-25 | 2006-11-29 | 信越化学工业株式会社 | Heat conductive silicone composition |
CN102408569A (en) * | 2010-09-21 | 2012-04-11 | 北京化工大学 | Dual-curable polysiloxane acrylate resin and preparation method thereof |
CN111040726A (en) * | 2019-12-26 | 2020-04-21 | 烟台德邦科技有限公司 | UV (ultraviolet) moisture dual-curing organic silicon coating adhesive |
KR20200076242A (en) * | 2018-12-19 | 2020-06-29 | 율촌화학 주식회사 | The double curing type silicone adhesive composition |
CN112062964A (en) * | 2020-08-12 | 2020-12-11 | 肇庆市武大环境技术研究院 | UV/moisture dual-curing acrylate polysiloxane and preparation method and application thereof |
-
2020
- 2020-12-18 CN CN202011506508.0A patent/CN112646541A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1869125A (en) * | 2005-05-25 | 2006-11-29 | 信越化学工业株式会社 | Heat conductive silicone composition |
CN102408569A (en) * | 2010-09-21 | 2012-04-11 | 北京化工大学 | Dual-curable polysiloxane acrylate resin and preparation method thereof |
KR20200076242A (en) * | 2018-12-19 | 2020-06-29 | 율촌화학 주식회사 | The double curing type silicone adhesive composition |
CN111040726A (en) * | 2019-12-26 | 2020-04-21 | 烟台德邦科技有限公司 | UV (ultraviolet) moisture dual-curing organic silicon coating adhesive |
CN112062964A (en) * | 2020-08-12 | 2020-12-11 | 肇庆市武大环境技术研究院 | UV/moisture dual-curing acrylate polysiloxane and preparation method and application thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104152104B (en) | A kind of autohension organic silicon pressure-sensitive adhesive and preparation method thereof | |
TWI447176B (en) | Curable polyorganosiloxane composition | |
TWI425031B (en) | A compound containing silicon, a hardened composition and a hardened product | |
JPS5931542B2 (en) | Solvent resistant silicone | |
JP2011190413A (en) | Siloxane polymer crosslinking-cured product | |
TW201247802A (en) | Composition for coating film formation purposes | |
KR20170018408A (en) | Room-temperature-curable organopolysiloxane composition, and moulded product comprising cured product of said room- temperature-curable organopolysiloxane composition | |
US4818805A (en) | Vulcanizable fluorinated silicone compositions | |
CN106381122A (en) | Phenyl-structure high-heat-resistance room-curing adhesive and preparation method thereof | |
TW201000563A (en) | Addition curable silicone rubber composition and cured silicone rubber | |
JP2015155541A (en) | Siloxane polymer crosslinked cured product | |
CN110156997A (en) | It is a kind of can moisture solidification organic silicon block copolymer and preparation method thereof | |
US2462640A (en) | Method of making methyl siloxanes | |
JPS632299B2 (en) | ||
JPH07165919A (en) | Additive for terpolymer fluid composition | |
CN104927058B (en) | A kind of hydroxyl polysiloxane blocking modification method | |
TWI447148B (en) | Silicon-containing polymer, method of manufacturing thereof, and curable polymer composition | |
CN112646541A (en) | Dual-curing system organic silicon composition and preparation method thereof | |
JP6319168B2 (en) | Method for producing condensation reaction product, method for producing room temperature curable organopolysiloxane composition containing the condensation reaction product | |
CN105209425B (en) | Aluminium chelate compound and the room temperature-curable resin composition containing aluminium chelate compound | |
CA2013472A1 (en) | Acrylamide polysiloxane composition with improved heat stability | |
JP7175249B2 (en) | Alkynyl group-containing organopolysiloxane and hydrosilylation reaction control agent | |
TW561169B (en) | Process for the preparation of a suspension of silica in an optionally crosslinkable silicone matrix | |
KR101757676B1 (en) | Silicone elastomer composition, silicone elastomer and silicone paste prepared using the same | |
JP7126999B2 (en) | Alkynyl group-containing cyclic organopolysiloxane and hydrosilylation reaction control agent |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210413 |
|
RJ01 | Rejection of invention patent application after publication |