CN105238342A - Organic silicon cementing compound and preparation method thereof - Google Patents
Organic silicon cementing compound and preparation method thereof Download PDFInfo
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- CN105238342A CN105238342A CN201510783100.0A CN201510783100A CN105238342A CN 105238342 A CN105238342 A CN 105238342A CN 201510783100 A CN201510783100 A CN 201510783100A CN 105238342 A CN105238342 A CN 105238342A
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Abstract
The invention discloses an organic silicon cementing compound and a preparation method thereof. The organic silicon cementing compound is prepared by adopting alpha, beta-dihydroxyl polydimethylsiloxane, inorganic filler, a silicon oil plasticizer, a flame-retardant agent, a cross-linking agent, a coupling agent and a catalyst, wherein the cross-linking agent is de-lactate ethyl cross-linking agent, and a molecular formula is R-Si-(OCHCH3COOCH2CH3)n, n is equal to 3 or 4, and when n is equal to 3, R is Me or Vi. Due to the application of the de-lactate ethyl cross-linking agent, non-corrosive lactate ethyl micro molecules are released during the reaction process, no corrosion is produced for a majority of cementing materials, and the cementing performance for a majority of metal materials, PBT, PET, PC, ABC and the like is relatively high; the organic silicon cementing compound has excellent anti-aging performance and is lower in volatilization performance and very suitable for the high-precision electron industry with high adhesive application requirement; and the production process is simple, the viscosity peak is relatively low, and the operation is convenient.
Description
Technical field
The invention belongs to organosilicon material technical field, particularly relate to organic silicon adhesive of a kind of demulsification acetoacetic ester new system and preparation method thereof.
Background technology
Rapidly, product category is enriched constantly in the nearly development of electronic enterprises during the last ten years, and product application environment and user require also to differ widely, and have higher requirement to the associated materials related to.Tackiness agent, as one of material indispensable in electronic enterprises, equally also will adapt to the more and more higher technical requirements that industrial chain Downstream Market proposes.Electronic apparatus stick with glue agent except the high and low temperature resistance, adhesiveproperties, heat conductivility, insulating property etc. of routine require higher except, also need tackiness agent to have environmental protection, low-volatile, performance to each side excellences such as material low corrosion.
Organic silicon adhesive, because of performances such as the high-low temperature resistant of its excellence, ageing-resistant, dielectric properties and low corrosion, is applied very general, as pcb board coating, electronic devices and components adhering and sealing etc. have use organic silicon adhesive in electronic enterprises.Current organic silicon adhesive Application comparison mainly contains widely and uses the de-oxime type of different linking agent, alcohol type and acetic acid type three kinds of systems, and for the requirement of environmental protection aspect, what be applicable to electronic enterprises is mainly dealcoholizing-type organic silicon adhesive.
Dealcoholizing-type organic silicon adhesive in use, there is larger volatile matter, and to a lot of materials such as copper sheets, there is certain corrodibility, along with electronic enterprises, the development of especially high-precision electron trade, common dealcoholizing-type organic silicon adhesive cannot be met the need of market, and develops a kind of novel organic silicon adhesive very necessary to the use glue demand meeting electronic enterprises higher.
Summary of the invention
Based on this, the object of the invention is to the defect overcoming above-mentioned prior art, provide a kind of and there is the ageing-resistant of excellence, low-volatile and non-corrosive novel demulsification acetoacetic ester type organic silicon adhesive.
In order to realize foregoing invention object, this invention takes following technical scheme:
A kind of organic silicon adhesive, described organic silicon adhesive is prepared by the component of following weight part and obtains:
Wherein, described linking agent is demulsification acetoacetic ester type linking agent, and molecular formula is R-Si-(OCHCH
3cOOCH
2cH
3)
n, n=3 or 4, and as n=3, substituent R=Me or Vi.
Wherein in some embodiments, described organic silicon adhesive is prepared by the component of following weight part and obtains:
Wherein, described linking agent is one or more in methyl three ethyl lactate siloxanes, vinyl three ethyl lactate siloxanes and four ethyl lactate siloxanes.
Wherein in some embodiments, described α, the structural formula of beta-dihydroxyl polydimethylsiloxane is HO-[SiO (CH
3)
2]
n-H, n=100-2000, when 25 DEG C, viscosity is 5Pa.s ~ 60Pa.s.
Wherein in some embodiments, described coupling agent is weight part ratio is (0 ~ 3): the diaminopropyl Trimethoxy silane of (3 ~ 0) and epoxypropyl Trimethoxy silane.
Wherein in an embodiment, diaminopropyl Trimethoxy silane and the epoxypropyl Trimethoxy silane of described coupling agent to be weight part ratio be 1:1.
Wherein in some embodiments, described silicone oil softening agent is polydimethylsiloxane, and described catalyzer is organo-tin compound.
Wherein in some embodiments, described catalyzer is dibutyl tin dilaurate or two neodecanoic acid dibutyl tins.
Wherein in some embodiments, described mineral filler is one or more in activated Calcium carbonate, water-ground limestone, silicon powder.
Present invention also offers the preparation method of above-mentioned organic silicon adhesive, take following technical scheme:
A preparation method for organic silicon adhesive, comprises the following steps:
(1) by α, beta-dihydroxyl polydimethylsiloxane and mineral filler, in temperature 80 ~ 150 DEG C, vacuum tightness 0.085 ~ 0.099MPa, dewater blended kneading 120 ~ 200min, and cooling obtains base-material;
(2) silicone oil softening agent is added in base-material, under 200 ~ 600rpm, stir 60 ~ 200min;
(3) add linking agent, fire retardant and coupling agent, under 200 ~ 600rpm, stir 60 ~ 200min;
(4) add catalyzer, stir 60 ~ 200min under 200 ~ 600rpm, to obtain final product.
Demulsification acetoacetic ester type organic silicon adhesive of the present invention employs demulsification acetoacetic ester type linking agent, create a kind of novel reaction system, the mechanism of its crosslinking reaction is: generate silanol after the hydrolysis of ethyl lactate base, then with hydroxy-terminated polysiloxane condensation reaction, non-toxic, environmental friendly ethyl lactate small molecules is discharged.Compared with prior art, the present invention has following beneficial effect:
1, demulsification acetoacetic ester type organic silicon adhesive of the present invention is owing to employing demulsification acetoacetic ester type linking agent, non-corrosive ethyl lactate small molecules is discharged in reaction process, to most of adhesives almost non-corrosiveness, to most metallic substance, PBT, PET, PC, ABS etc., all there is stronger cementability; The ageing-resistant performance more more excellent than dealcoholizing-type organic silicon adhesive, lower fugitive constituent, the high-precision electron trade that very applicable height glue requires;
2, demulsification acetoacetic ester type organic silicon adhesive production process of the present invention is simple, and viscosity peak is less, handled easily.
Embodiment
For a better understanding of the present invention; below by embodiment, elaboration concrete is further done to the present invention; but it is unintelligible for define of the present invention; for some nonessential improvement and adjustment that those skilled in the art does according to foregoing invention content, also should be considered as dropping in protection scope of the present invention.
Except specified otherwise, the raw material used in following examples all derives from commercially available.
Embodiment 1 one kinds of demulsification acetoacetic ester type organic silicon adhesives
Organic silicon adhesive described in the present embodiment is prepared by the component of following weight part and obtains:
Wherein, described coupling agent is diaminopropyl Trimethoxy silane and the epoxypropyl Trimethoxy silane of weight ratio 1:1.
The preparation method of the demulsification acetoacetic ester type organic silicon adhesive of the present embodiment, comprises the following steps:
(1) be the α of 10Pa.s by the viscosity of 25 DEG C, beta-dihydroxyl polydimethylsiloxane 100 parts and activated Calcium carbonate 10 parts, join in kneader, in temperature 150 DEG C, and vacuum tightness 0.085MPa, dewater blended kneadings 120min, cools and obtain base-material;
(2) by the viscosity of 25 DEG C be the silicone oil softening agent polydimethylsiloxane 5 parts of 1Pa.s add above-mentioned base-material is housed planetary mixer in, stir 60min under 300rpm;
(3) 5 parts of methyl three ethyl lactate siloxane crosslinkers, 0.01 part of fire retardant and 1 part of coupling agent (diaminopropyl Trimethoxy silane: epoxypropyl Trimethoxy silane=1:1) are added in described planetary mixer, under rotating speed 300rpm, stir 60min;
(4) 0.05 part of dibutyltin dilaurate catalyst is added in described planetary mixer, stir 60min under rotating speed 300rpm, to obtain final product.
The product performance index of the demulsification acetoacetic ester type organic silicon adhesive of the present embodiment is in table 1.
Embodiment 2 one kinds of demulsification acetoacetic ester type organic silicon adhesives
Organic silicon adhesive described in the present embodiment is prepared by the component of following weight part and obtains:
Wherein, described coupling agent is diaminopropyl Trimethoxy silane and the epoxypropyl Trimethoxy silane of weight ratio 1:1.
The preparation method of the demulsification acetoacetic ester type organic silicon adhesive of the present embodiment, comprises the following steps:
(1) be the α of 20Pa.s by the viscosity of 25 DEG C, beta-dihydroxyl polydimethylsiloxane 100 parts and activated Calcium carbonate 10 parts, join in kneader, in temperature 150 DEG C, and vacuum tightness 0.085MPa, dewater blended kneadings 120min, cools and obtain base-material;
(2) by the viscosity of 25 DEG C be the silicone oil softening agent polydimethylsiloxane 5 parts of 1Pa.s add above-mentioned base-material is housed planetary mixer in, stir 60min under 300rpm;
(3) 10 parts of vinyl three ethyl lactate siloxane crosslinkers, 0.01 part of fire retardant and 1 part of coupling agent (diaminopropyl Trimethoxy silane: epoxypropyl Trimethoxy silane=1:1) are added in described planetary mixer, under rotating speed 300rpm, stir 60min;
(4) 0.05 part of dibutyltin dilaurate catalyst is added in described planetary mixer, stir 60min under rotating speed 300rpm, to obtain final product.
The demulsification acetoacetic ester type organic silicon adhesive product performance index of the present embodiment is in table 1.
Embodiment 3 one kinds of demulsification acetoacetic ester type organic silicon adhesives
Organic silicon adhesive described in the present embodiment is prepared by the component of following weight part and obtains:
Wherein, described linking agent is methyl three ethyl lactate siloxanes and the vinyl three ethyl lactate siloxanes of weight ratio 1:1, and described coupling agent is diaminopropyl Trimethoxy silane and the epoxypropyl Trimethoxy silane of weight ratio 1:1.
The preparation method of the demulsification acetoacetic ester type organic silicon adhesive of the present embodiment, comprises the following steps:
(1) be the α of 40Pa.s by the viscosity of 25 DEG C, beta-dihydroxyl polydimethylsiloxane 100 parts and activated Calcium carbonate 40 parts, join in kneader, in temperature 50 C, and vacuum tightness 0.085MPa, dewater blended kneadings 120min, cools and obtain base-material;
(2) by the viscosity of 25 DEG C be the silicone oil softening agent polydimethylsiloxane 30 parts of 1Pa.s add above-mentioned base-material is housed planetary mixer in, stir 60min under 300rpm;
(3) 20 parts of linking agents (methyl three ethyl lactate siloxanes: vinyl three ethyl lactate siloxanes=1:1), 0.01 part of fire retardant and 1 part of coupling agent (diaminopropyl Trimethoxy silane: epoxypropyl Trimethoxy silane=1:1) are added in described planetary mixer, under rotating speed 300rpm, stir 60min;
(4) 0.5 part of dibutyltin dilaurate catalyst is added in described planetary mixer, stir 60min under rotating speed 300rpm, to obtain final product.
The demulsification acetoacetic ester type organic silicon adhesive product performance index of the present embodiment is in table 1.
Embodiment 4 one kinds of demulsification acetoacetic ester type organic silicon adhesives
Organic silicon adhesive described in the present embodiment is prepared by the component of following weight part and obtains:
Wherein, described linking agent is methyl three ethyl lactate siloxanes and the vinyl three ethyl lactate siloxanes of weight ratio 1:1, and described coupling agent is diaminopropyl Trimethoxy silane and the epoxypropyl Trimethoxy silane of weight ratio 1:1.
The preparation method of the demulsification acetoacetic ester type organic silicon adhesive of the present embodiment, comprises the following steps:
(1) be the α of 60Pa.s by the viscosity of 25 DEG C, beta-dihydroxyl polydimethylsiloxane 100 parts and activated Calcium carbonate 40 parts, join in kneader, in temperature 50 C, and vacuum tightness 0.085MPa, dewater blended kneadings 120min, cools and obtain base-material;
(2) by the viscosity of 25 DEG C be the silicone oil softening agent polydimethylsiloxane 30 parts of 1Pa.s add above-mentioned base-material is housed planetary mixer in, stir 60min under 300rpm;
(3) 20 parts of linking agents (methyl three ethyl lactate siloxanes: vinyl three ethyl lactate siloxanes=1:1), 0.5 part of fire retardant and 5 parts of coupling agents (diaminopropyl Trimethoxy silane: epoxypropyl Trimethoxy silane=1:1) are added in described planetary mixer, under rotating speed 300rpm, stir 60min;
(4) 0.5 part of two neodecanoic acid dibutyl tin catalyzer is added in described planetary mixer, stir 60min under rotating speed 300rpm, to obtain final product.
The demulsification acetoacetic ester type organic silicon adhesive product performance index of the present embodiment is in table 1.
Test the organic silicon adhesive product performance of embodiment 1 ~ 4, test result is as shown in table 1 below.
The organic silicon adhesive product performance test result of table 1 embodiment 1 ~ 4
As can be seen from table 1 test result, this novel every test performance of demulsification acetoacetic ester organic silicon adhesive meets most of purposes demand, wherein to copper sheet all non-corrosivenesss, is the excellent properties not available for other systems.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. an organic silicon adhesive, is characterized in that, described organic silicon adhesive is prepared by the component of following weight part and obtains:
Wherein, described linking agent is demulsification acetoacetic ester type linking agent, and molecular formula is R-Si-(OCHCH
3cOOCH
2cH
3)
n, n=3 or 4, and as n=3, substituent R=Me or Vi.
2. organic silicon adhesive according to claim 1, is characterized in that, described organic silicon adhesive is prepared by the component of following weight part and obtains:
Wherein, described linking agent is one or more in methyl three ethyl lactate siloxanes, vinyl three ethyl lactate siloxanes and four ethyl lactate siloxanes.
3. organic silicon adhesive according to claim 1 and 2, is characterized in that, described α, and the structural formula of beta-dihydroxyl polydimethylsiloxane is HO-[SiO (CH
3)
2]
n-H, n=100-2000, when 25 DEG C, viscosity is 5Pa.s ~ 60Pa.s.
4. organic silicon adhesive according to claim 1 and 2, is characterized in that, described coupling agent is weight part ratio is (0 ~ 3): the diaminopropyl Trimethoxy silane of (3 ~ 0) and epoxypropyl Trimethoxy silane.
5. organic silicon adhesive according to claim 4, is characterized in that, diaminopropyl Trimethoxy silane and the epoxypropyl Trimethoxy silane of described coupling agent to be weight part ratio be 1:1.
6. organic silicon adhesive according to claim 1 and 2, is characterized in that, described silicone oil softening agent is polydimethylsiloxane, and described catalyzer is organo-tin compound.
7. organic silicon adhesive according to claim 6, is characterized in that, described catalyzer is dibutyl tin dilaurate or two neodecanoic acid dibutyl tins.
8. organic silicon adhesive according to claim 1 and 2, is characterized in that, described mineral filler is one or more in activated Calcium carbonate, water-ground limestone, silicon powder.
9. the preparation method of the organic silicon adhesive described in any one of claim 1 ~ 8, is characterized in that, comprises the following steps:
(1) by α, beta-dihydroxyl polydimethylsiloxane and mineral filler, in temperature 80 ~ 150 DEG C, vacuum tightness 0.085 ~ 0.099MPa, dewater blended kneading 120 ~ 200min, and cooling obtains base-material;
(2) silicone oil softening agent is added in base-material, under 200 ~ 600rpm, stir 60 ~ 200min;
(3) add linking agent, fire retardant and coupling agent, under 200 ~ 600rpm, stir 60 ~ 200min;
(4) add catalyzer, stir 60 ~ 200min under 200 ~ 600rpm, to obtain final product.
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| CN105713552A (en) * | 2016-03-24 | 2016-06-29 | 深圳市安品有机硅材料有限公司 | Preparation method of thixotropic organic silicon packaging adhesive |
| CN105838319A (en) * | 2016-03-24 | 2016-08-10 | 深圳市安品有机硅材料有限公司 | Preparation method of pre-dispersed high-thixotropy packaging silica gel |
| CN106753203A (en) * | 2016-12-26 | 2017-05-31 | 广州市白云化工实业有限公司 | A kind of depickling type organic silicon adhesive and preparation method thereof |
| CN107033835A (en) * | 2016-11-22 | 2017-08-11 | 广州市高士实业有限公司 | A kind of demulsification acetoacetic ester transparent neutral silicone sealant and preparation method thereof |
| CN107523257A (en) * | 2017-09-29 | 2017-12-29 | 山东三泽硅胶有限公司 | A kind of cold curing demulsification acetoacetic ester type silicone sealant |
| WO2019069706A1 (en) * | 2017-10-06 | 2019-04-11 | 信越化学工業株式会社 | Method for manufacturing room-temperature-curable organopolysiloxane composition, room-temperature-curable organopolysiloxane composition, and article |
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| JPWO2020203607A1 (en) * | 2019-04-03 | 2020-10-08 | ||
| WO2020226076A1 (en) * | 2019-05-09 | 2020-11-12 | 信越化学工業株式会社 | Room-temperature-vulcanizing organopolysiloxane composition, silicone rubber, and article |
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| CN105838319A (en) * | 2016-03-24 | 2016-08-10 | 深圳市安品有机硅材料有限公司 | Preparation method of pre-dispersed high-thixotropy packaging silica gel |
| CN105713552B (en) * | 2016-03-24 | 2018-09-18 | 深圳市安品有机硅材料有限公司 | Preparation method of thixotropic organic silicon packaging adhesive |
| CN105838319B (en) * | 2016-03-24 | 2019-01-04 | 深圳市安品有机硅材料有限公司 | Preparation method of pre-dispersed high-thixotropy packaging silica gel |
| CN105713552A (en) * | 2016-03-24 | 2016-06-29 | 深圳市安品有机硅材料有限公司 | Preparation method of thixotropic organic silicon packaging adhesive |
| CN107033835A (en) * | 2016-11-22 | 2017-08-11 | 广州市高士实业有限公司 | A kind of demulsification acetoacetic ester transparent neutral silicone sealant and preparation method thereof |
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| CN106753203A (en) * | 2016-12-26 | 2017-05-31 | 广州市白云化工实业有限公司 | A kind of depickling type organic silicon adhesive and preparation method thereof |
| CN107523257A (en) * | 2017-09-29 | 2017-12-29 | 山东三泽硅胶有限公司 | A kind of cold curing demulsification acetoacetic ester type silicone sealant |
| CN111183186A (en) * | 2017-10-06 | 2020-05-19 | 信越化学工业株式会社 | Method for producing room-temperature-curable organopolysiloxane composition, and article |
| JPWO2019069706A1 (en) * | 2017-10-06 | 2020-11-05 | 信越化学工業株式会社 | Method for Producing Room Temperature Curable Organopolysiloxane Composition, Room Temperature Curable Organopolysiloxane Composition and Articles |
| WO2019069706A1 (en) * | 2017-10-06 | 2019-04-11 | 信越化学工業株式会社 | Method for manufacturing room-temperature-curable organopolysiloxane composition, room-temperature-curable organopolysiloxane composition, and article |
| US11525057B2 (en) | 2017-10-06 | 2022-12-13 | Shin-Etsu Chemical Co., Ltd. | Method for manufacturing room-temperature-curable organopolysiloxane composition, room-temperature-curable organopolysiloxane composition, and article |
| CN111183186B (en) * | 2017-10-06 | 2022-09-16 | 信越化学工业株式会社 | Method for producing room-temperature-curable organopolysiloxane composition, and article |
| WO2020203607A1 (en) * | 2019-04-03 | 2020-10-08 | 信越化学工業株式会社 | Organopolysiloxane modified with lactate silyl at both ends and method for producing same |
| JPWO2020203607A1 (en) * | 2019-04-03 | 2020-10-08 | ||
| JP7424369B2 (en) | 2019-04-03 | 2024-01-30 | 信越化学工業株式会社 | Lactate silyl-modified organopolysiloxane at both ends and method for producing the same |
| WO2020226076A1 (en) * | 2019-05-09 | 2020-11-12 | 信越化学工業株式会社 | Room-temperature-vulcanizing organopolysiloxane composition, silicone rubber, and article |
| JPWO2020226076A1 (en) * | 2019-05-09 | 2020-11-12 | ||
| JP7355105B2 (en) | 2019-05-09 | 2023-10-03 | 信越化学工業株式会社 | Room temperature curable organopolysiloxane compositions, silicone rubbers and articles |
| CN110903807A (en) * | 2019-11-27 | 2020-03-24 | 烟台德邦科技有限公司 | Preparation method of environment-friendly room temperature vulcanized silicone rubber |
| CN115058062A (en) * | 2022-07-26 | 2022-09-16 | 北京天罡助剂有限责任公司 | Composition for crosslinked polyethylene, preparation method thereof and polyethylene film |
| CN115058062B (en) * | 2022-07-26 | 2024-03-15 | 北京天罡助剂有限责任公司 | Composition for crosslinked polyethylene, preparation method thereof and polyethylene film |
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Application publication date: 20160113 |