CN1058735C - Single-component catalytic curing system for curing silastic at atmospheric temp. - Google Patents
Single-component catalytic curing system for curing silastic at atmospheric temp. Download PDFInfo
- Publication number
- CN1058735C CN1058735C CN96116911.7A CN96116911A CN1058735C CN 1058735 C CN1058735 C CN 1058735C CN 96116911 A CN96116911 A CN 96116911A CN 1058735 C CN1058735 C CN 1058735C
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- CN
- China
- Prior art keywords
- curing
- curing system
- alpha
- substitution
- catalytic
- 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.)
- Expired - Fee Related
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- 230000003197 catalytic effect Effects 0.000 title claims description 21
- 229920000260 silastic Polymers 0.000 title description 2
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 5
- 239000003292 glue Substances 0.000 claims description 15
- 238000006467 substitution reaction Methods 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 12
- 229920002379 silicone rubber Polymers 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 125000000547 substituted alkyl group Chemical group 0.000 claims description 2
- 125000003107 substituted aryl group Chemical group 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000007711 solidification Methods 0.000 abstract description 3
- 230000008023 solidification Effects 0.000 abstract description 3
- 150000001412 amines Chemical class 0.000 abstract 2
- 239000000741 silica gel Substances 0.000 abstract 2
- 229910002027 silica gel Inorganic materials 0.000 abstract 2
- 239000000499 gel Substances 0.000 abstract 1
- 229920001971 elastomer Polymers 0.000 description 9
- 239000005060 rubber Substances 0.000 description 9
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000005470 impregnation Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- VRAIHTAYLFXSJJ-UHFFFAOYSA-N alumane Chemical compound [AlH3].[AlH3] VRAIHTAYLFXSJJ-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- -1 methyl siloxanes Chemical class 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000010074 rubber mixing Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a dealcoholized monocomponent RTV silica gel solidification catalyzing system which takes ortho silicate and phenyl trialkoxysilane as solidifying agents, and takes trialkoxysilane containing amine and dialkoxysilane containing amine as solidifying catalysts. The RTV silica gel has the characteristics of quick solidification, adjustability, good elasticity and adhesiveness, and low price, and the storage period of the gel is longer than six months.
Description
The present invention relates to dealcoholizing-type single-component self-vulcanizing (RTV) silicon rubber, particularly its catalytic curing system.
The core technology of single-component (or claim single packing) RTV silicon rubber is its catalytic curing system (or claiming cross-linking system), and the catalytic curing system is the curing speed, the package stability that influence single-component RTV silicon rubber, there have to be pollution-free, the principal element of corrodibility and electrophysics performance thereof etc.
The present single-component RTV silicon rubber of dealcoholizing-type, having with the methyltrimethoxy silane is solidifying agent, is that the catalytic curing system of catalyzer (is seen United States Patent (USP) 4,257,932 with the complex compound of titanium; Germany patent 3,032,059; The clear 57-141447 of Japanese Patent), it emits methyl alcohol in solidification process, to the metal non-corrosiveness, can be used for electronic isolation and building aspect, but exists curing speed slow, the shortcoming of package stability difference.The purity for preparing this glue requirement MTMS is very high, otherwise after the period of storage length, with retardation of curing, even solidifies.
The single-component RTV silicon rubber of other dealcoholizing-type has (the seeing United States Patent (USP) 3,280,072) of making solidifying agent with γ-An Bingjisanyiyangjiguiwan, solidifies halfway critical defect but exist.
United States Patent (USP) 3,560,442 with general formula (RO)
3The silane of SiCHR ' NR " R " is made curing agent, DRP 1,794, and 197 with general formula [(C
2H
5O)
3SiCH
2]
2NCH
2(R is CH to R
2=CH-, n-C
3H
7-, C
6H
5-etc.) make curing agent, but their storage period is too short, can only 3-4 month.
Newer dealcoholizing-type kind is to make the RTV silicon rubber [seeing " special synthetic rubber " 1,43 (1982)] of catalyzer with the trialkoxy silane coupling agent.This class catalytic curing agent has two groups: (C
2H
5)
2NCH
2Si (OC
2H
5)
3+ Cl
2CHSi (OC
2H
5)
3I (C
2H
5)
2NCH
2Si (OC
2H
5)
3+ C
6H
5NHCH
2Si (OC
2H
5)
3II emits ethanol during their curing, but shortcoming is: 1. curing rate is unadjustable, and range of application is restricted; 2. the tackify peak occurs during encapsulating, be difficult for encapsulating.Be difficult to realize the mechanize encapsulating for stiff glue, therefore can not make the kind of high strength (increase reinforced filling) and low price (increasing non-reinforced filling); 3. elasticity and poor adhesion.
The catalytic curing system of the disclosed single-component RTV silicon rubber of Chinese patent (application number 94111301.9) is made up of amino dialkoxy silicane of alpha-substitution and ortho-silicate, and there is the slow shortcoming of curing speed in it.
The purpose of this invention is to provide a kind of single-component RTV silicon rubber curing speed that makes and comparatively fast also can regulate, the tackify peak does not appear in excellent storage stability during encapsulating, be convenient to increase filler, better tensile strength is arranged, and elasticity and binding property are good, the catalytic curing system that price is lower.
The present invention is achieved through the following technical solutions.
The catalytic curing system of single-component room curing silicon rubber of the present invention, it is made up of solidifying agent and curing catalysts, and its solidifying agent is ortho-silicate or phenyl trialkoxy silane, and curing catalysts is with general formula R ' NR " CH
2Si (OR )
3Be the alpha-substitution amino methyl trialkoxy silane of representative, R ' can be H, alkyl or aryl in the formula, R, and " can be alkyl, aryl, aralkyl, substituted alkyl, substituted aryl, R be methyl or ethyl.
The catalytic curing system of single-component room curing silicon rubber of the present invention can also can be used two or more alpha-substitution amino methyl trialkoxy silane simultaneously with a kind of alpha-substitution amino methyl trialkoxy silane.
The catalytic curing system of single-component room curing silicon rubber of the present invention can add simultaneously with general formula R ' NR " CH
2Si (CH
3) (OR )
2, being the amino dimethyl dialkoxy silicane of alpha-substitution of representative, it also can be with one or more alpha-substitution amino dimethyl dialkoxy silicane.
The consumption of the catalytic curing system of single-component room curing silicon rubber of the present invention is: 100 parts in basic glue, add ortho-silicate or phenyl trialkoxy silane 3-10 part, add the amino dimethyl dialkoxy silicane of alpha-substitution amino methyl trialkoxy silane 1-5 part and alpha-substitution 0-3 part.
The catalytic curing system of one-component room curing silicon rubber of the present invention can with (C
2H
5)
2NCH
2Si (OC
2H
5)
3And Cl
2CHSi (OC
2H
5)
3Or (C
2H
5)
2NCH
2Si (OC
2H
5)
3And C
6H
5NHCH
2Si (OC
2H
5)
3Be used.
Adopt the catalytic curing system of single-component room curing silicon rubber of the present invention to make the single-component room curing silicon rubber following advantage arranged:
Hardening time short, and adjustable, silastic surface hardening time from below 5 minutes to adjustable more than 12 minutes.
2. excellent storage stability stores that performance does not change more than six months.
3. do not occur the tackify peak during encapsulating, therefore can increase the reinforcer consumption, preparation high strength room curing silicon rubber perhaps increases filler to reduce cost.
4. the tensile strength height can reach 1.2-1.5Mpa.
5. good springiness, elongation can reach 300%.
6. the binding property with metal is good, and aluminium-aluminium slip resistance can reach 1.6Mpa.
7. the amino dimethyl dialkoxy silicane of ortho-silicate and alpha-substitution amino methyl trialkoxy silane and alpha-substitution price is all cheaper, so cost is low.
Further specify the present invention by the following examples.
Embodiment 1. is 100 parts of hydroxyl-terminated injecting two methyl siloxanes (molecular weight 3-6 ten thousand), 1 part of aerosil, and 10 parts of precipitated silicas, 3 parts in zinc oxide carries out mixingly on three roller rubber mixing machines, and it is dry that the rubber unvulcanizate that obtains is put into vacuum drying oven, obtains basic glue.
In dry nitrogen atmosphere, take by weighing 100 parts in above-mentioned basic glue, add n-C
4H
9NHCH
2Si (OC
2H
5)
33 parts, n-C
4H
9NHCH
2Si (CH
3) (OC
2H
5)
21 part, Si (OCH
3)
46 parts, pour into sealing preservation in the metal hose after mixing well, the tackify peak does not appear during impregnation.
Extrude from metallic hose when placing air when glue, observing the surface cure time is 7 minutes, and the mechanical property that records after the curing is: tensile strength: 1.5Mpa; Elongation 300%; Shore hardness: 40A; Aluminium under the room temperature-aluminium slip resistance: 1.6Mpa.
Store not change of performance more than six months.
Embodiment 2. takes by weighing 100 parts in the basic glue of embodiment 1 in dry nitrogen atmosphere, add n-C
4H
9NHCH
2Si (OC
2H
5)
23 parts, Si (OCH
3)
4Part, pour into sealing preservation in the metal hose after mixing well.The tackify peak does not appear during impregnation.
Extrude from metallic hose when placing air when glue, observing the surface cure time is 5 minutes, and the mechanical property that records after the curing is: tensile strength: 1.2Mpa; Elongation 200%; Shore hardness 40A; Aluminium under the room temperature-aluminium slip resistance: 1.2Mpa.
Store not change of performance more than six months.
Embodiment 3. takes by weighing 100 parts in the basic glue of embodiment 1 in the blanket of nitrogen of drying, add (C
2H
5)
2NCH
2Si (OC
2H
5)
32.5 part, n-C
4H
9NHCH
2Si (CH
3) (OC
2H
5)
21.5 part, C
6H
5Si (OC
2H
5)
36 parts, pour into sealing preservation in the metal hose after mixing well, the tackify peak does not appear during impregnation.
When glue was extruded from metallic hose, observing the surface cure time was 12 minutes.The mechanical property that records after the curing is: tensile strength: 1.2Mpa; Elongation 200%; Shore hardness: 32A; Room temperature aluminium-aluminium slip resistance: 1.3Mpa.
Store not change of performance more than six months.
Embodiment 4. takes by weighing 100 parts in the basic glue of embodiment 1 in dry nitrogen atmosphere, add (C
2H
5)
2-NCH
2Si (OC
2H
5)
33 parts, Si (OCH
3)
43 parts, NH
2CH
2CH
2NHCH
2Si (CH
3) (OC
2H
5)
21 part of Cl
2CHSi (OC
2H
5)
33 parts, pour into sealing preservation in the metal hose after mixing well.The tackify peak does not appear during impregnation.
Extrude from flexible pipe when placing air when glue, observing the surface cure time is 10 minutes.The mechanical property that records after the curing is: tensile strength: 1.2Mpa; Elongation 200%; Shore hardness 38A; Room temperature aluminium-aluminium slip resistance: 1.2Mpa.
Store more than 1 year, performance finds no variation.
Embodiment 5 takes by weighing 100 parts in the basic glue of embodiment 1 in dry nitrogen atmosphere, add (C
2H
5)
2-NCH
2Si (OC
2H
5)
33 parts, Si (OCH
3)
43 parts, NH
2(CH
2)
6NHCH
2Si (CH
3)-(OC
2H
5)
21 part of C
6H
5NHCH
2Si (OC
2H
5)
33 parts, pour into sealing preservation in the metal hose after mixing well.The tackify peak does not appear during impregnation.
Extrude from flexible pipe when placing air when glue, observing the surface cure time is 10 minutes.The mechanical property that records after the curing is: tensile strength 1.2Mpa; Elongation 250%; Shore hardness 36A; Room temperature aluminium-aluminium slip resistance: 1.4Mpa.
Store more than 1 year, performance finds no variation.
Claims (5)
1. the catalytic curing system of a single-component room curing silicon rubber, it is made up of solidifying agent and curing catalysts, it is characterized in that solidifying agent is ortho-silicate or phenyl trialkoxy silane, and curing catalysts is with general formula R ' NR " CH
2Si (OR )
3Alpha-substitution amino methyl trialkoxy silane for representative, R ' in the general formula is H, alkyl or aryl, " be alkyl, aryl, aralkyl, substituted alkyl, substituted aryl; R is methyl or ethyl; the consumption of catalytic curing system is: 100 parts in basic glue (quality; down together) adds ortho-silicate or phenyl trialkoxy silane 3-10 part, R ' NR " CH to R
2Si (OR )
31-5 part and R ' NR " CH
2Si (CH
3) (OR )
30-3 part.
2. catalytic curing system according to claim 1 is characterized in that adding simultaneously R ' NR " CH
2Si (CH
3) (OR )
2Be the amino dimethyl dialkoxy silicane of the alpha-substitution of representative.
3. catalytic curing system according to claim 1 and 2 is characterized in that curing catalysts is one or more alpha-substitution amino methyl trialkoxy silane, or the amino dimethyl dialkoxy silicane of one or more alpha-substitution.
4. catalytic curing system according to claim 1 and 2, it is characterized in that can with (C
2H
5)
2-NCH
2Si (OC
2H
5)
3And C1
2CHSi (OC
2H
5)
3Be used.
5. catalytic curing system according to claim 1 and 2, it is characterized in that can with (C
2H
5)
2-NCH
2Si (OC
2H
5)
3And C
6H
5NHCH
2Si (OC
2H
5)
3Be used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116911.7A CN1058735C (en) | 1996-04-30 | 1996-04-30 | Single-component catalytic curing system for curing silastic at atmospheric temp. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116911.7A CN1058735C (en) | 1996-04-30 | 1996-04-30 | Single-component catalytic curing system for curing silastic at atmospheric temp. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1163905A CN1163905A (en) | 1997-11-05 |
| CN1058735C true CN1058735C (en) | 2000-11-22 |
Family
ID=5123864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96116911.7A Expired - Fee Related CN1058735C (en) | 1996-04-30 | 1996-04-30 | Single-component catalytic curing system for curing silastic at atmospheric temp. |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1058735C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303143C (en) * | 2004-09-14 | 2007-03-07 | 刘兴宏 | Colorless transparent silicone rubber crosslinking curing agent |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1629209B (en) * | 2003-12-17 | 2010-04-28 | 北京三辰化工有限公司 | Method for preparing electronic-grade single-component dealcoholizing-type room temperature cured silicon rubber by non-high-temperature vacuum dewatering method |
-
1996
- 1996-04-30 CN CN96116911.7A patent/CN1058735C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303143C (en) * | 2004-09-14 | 2007-03-07 | 刘兴宏 | Colorless transparent silicone rubber crosslinking curing agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1163905A (en) | 1997-11-05 |
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