CN1446856A - High strength condensed type combination of organosilicon die glue - Google Patents
High strength condensed type combination of organosilicon die glue Download PDFInfo
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Abstract
A condensed high-adhesion organosilicon composition used as mould adhesive PTV-2 is composed of components A and B. The said component A consists of silica rubber 107, pretreated silica rubber, plasticizer, filler, TiO2 and solidifying promoter. The said component B comprises one or more of tetramethoxy silane, tetraethoxy silane and hydrolytic tetraethoxy silane and dibutyl tin bilaurate. Its advantages are high tension strength and high tear strength.
Description
Technical field
High-strength condensed type silicone mold glue composition of the present invention relates to a kind of two component condensed room temperature vulcanized silicone rubbers (hereinafter to be referred as RTV-2 glue) prescription and manufacturing process thereof of high mechanical strength.Main as mold glue.
Background technology
RTV-2 glue has excellent release property, thereby can be used as the soft mode material and be used for historical relic, artwork, toy, electrical equipment, instrument and mechanical component etc. in a large number and duplicate and make.But silicon rubber is a kind of noncrystalline structure, and intermolecular gravitation is very low, so tensile strength, tearing strength are very low, has no value for use, and must meet the requirements of application target by suitable technology, prescription.
Summary of the invention
The objective of the invention is to: prescription and manufacturing process thereof that a kind of two component condensed room temperature vulcanized silicone rubbers of the high mechanical strength that use value arranged are provided.
The object of the invention can be achieved through the following technical solutions: high-strength condensed type silicone mold glue composition, with silicon rubber is main raw material, being equipped with linking agent, catalyzer and stopping composition makes, be with the two components of A, B, carry out crosslinking reaction as catalyzer and obtain two component condensed room temperature vulcanized silicone rubbers through dibutyl tin laurate, reaction expression is:
The A component is by 107 silicon rubber, basic glue, softening agent, stopping composition, TiO
2, the deep layer curing catalyst forms, wherein, 107 silicon rubber/basic glue is 30/70-50/50, the B component is made up of one or more and dibutyl tin laurate in tetramethoxy-silicane, tetraethoxysilane, the tetraethoxysilane hydrolyzate, and described basic glue is through pretreated 107 silicon rubber.
On the technique scheme basis, described basic glue is that the constitution controller hexamethyldisilazane is added in 107 silicon rubber, add the white carbon black of handling with hexamethyldisilazane after mixing well again, mediate, mixing after, the sizing material that obtains is mediated at normal temperatures, at 160-180 ℃ of following vacuum kneading, can obtain basic glue after the cooling then.
Described stopping composition is one or more the mixture in white carbon black, silica powder, diatomite, the kaolin; Described softening agent is a low viscosity silicone, as the silicone oil of 100cps; Described deep layer curing catalyst is one or more in water, phosphoric acid salt and the magnesium oxide.
The manufacture craft of A component is: after 107 glue, basic glue, softening agent are stirred at normal temperatures, add stopping composition, whipping temp more than 80 ℃ to mixing, the cooling back adds the deep layer curing catalyst, can obtain the A component.
The manufacture craft of B component is: one or more in tetramethoxy-silicane, tetraethoxysilane, the tetraethoxysilane hydrolyzate with can use after dibutyl tin laurate mixes.
Because the RTV-2 glue that uses as mold glue will have good flowability, so that better processing property is arranged, so the viscosity of A component should be lower than 70000cps, generally selects 107 silicon rubber of 2700--70000cps range of viscosities for use, preferably 107 silicon rubber of 5000--50000cps range of viscosities.Each substance weight part of A component is:
Base glue/107 silicon rubber 100
Softening agent 5-15
Stopping composition 0-10
Deep layer curing catalyst 0.1-1.
Superiority of the present invention is: owing to adopted this prescription and process system, make the stretching of RTV-2 glue and tearing strength can reach 3.5MPa, 28KN/m respectively.
Embodiment
Embodiment 1, and the A component is mixed, vulcanized by 107 silicon rubber and basic glue, the stopping composition of appropriate process, 20000cps viscosity, and the component of silicon rubber (weight part) is:
62 parts in base glue
38 parts in 107 silicon rubber
10 parts of 100cps silicone oil
10 parts of the white carbon blacks of nano white carbon black+vapor phase process
TiO
20.5 part
0.8 part in water is prepared 107 glue, basic glue, softening agent in proportion, is mixed, after stirring at normal temperatures, add composite stopping composition again, whipping temp must be more than 80 ℃: kept 10 hours, the cooling back adds the deep layer curing catalyst, can obtain the A component.
The manufacture craft of base glue: the constitution controller hexamethyldisilazane is added in 107 glue, add the white carbon black of handling with hexamethyldisilazane after mixing well again, and in kneader, mediate 1-2h, take out the back on three roller rubber mixing machines mixing for 3 times, the sizing material that obtains is mediated 1h at normal temperatures, at 160-180 ℃ of following vacuum kneading 2-4h, can obtain basic glue after the cooling then.
The B component is 1 part of a methyl silicate, tetraethyl silicate I part, 2 parts of dibutyl tin laurates.To can use after above-mentioned three kinds of materials mixing.
Present embodiment makes the physical strength of cross-linked rubber be significantly improved, and tension and tearing strength are greater than 3.5MPa, 28KN/m.
It below is the contrast of each component consumption
(1) contrast of various viscosity 107 silicon rubber
Use 107 glue of various viscosity separately, prescription: 60 parts in basic glue, 40 parts in 107 glue, 10 parts of 100cps silicone oil, 10 parts of CG-25 powders.
Shown in the performance table 1, when the viscosity of 107 glue increased, the physical strength of cross-linked rubber was significantly improved, and can select 107 glue of 20000cps and 50000cps viscosity separately for use as can be seen from Table 1.
The physical mechanical of different viscosity 107 silicon rubber compares:
Table 1
| 107 glue kinds (cps) | 2700 | ?5000 | ?20000 | ?50000 |
| 25 ℃ of viscosity (cps) | 16000 | ?18000 | ?43000 | ?76000 |
| Solidifying agent 3# | 3％ | ?3％ | ?3％ | ?3％ |
| Presetting period (min) | 53 | ?47 | ?38 | ?28 |
| Hardness (ShoreA) | 24 | ?22 | ?21 | ?15 |
| Elongation (%) | 361 | ?407 | ?531 | ?629 |
| Tensile strength (MPa) | 2.30 | ?2.63 | ?2.90 | ?3.12 |
| Tearing toughness (KN/m) | 17.8 | ?19.0 | ?24.5 | ?27.0 |
The comparison of the composite data of 107 glue of two kinds of different viscosity sees Table 2, shown in the table 3.Prescription: 60 parts in basic glue, 40 parts in 107 glue, 10 parts of 100cps silicone oil, CG-25 powder 10 parts of (a) 50000cps, 107 glue and the composite table 2 of 5000cps 107 glue
As seen use the composite physical strength of mold glue that do not make of 50000cps 107 glue and 5000cps 107 glue to be significantly improved.(b) the composite table 3 of 20000cps107 glue and 5000cps107 glue
As seen use the composite physical strength of mold glue that do not make of 20000cps107 glue and 5000cps107 glue to be significantly improved.The different ratios of (2) 107 glue and basic glue is selected, and physicals sees Table 4 and selects viscosity 20000cps107 glue for use, fills a prescription to be (basic glue+20000cps107 glue): 100cps silicone oil: CG-25 powder=100: 10: 10 tables 4
It is very poor that "/" expression mixes the back levelling property, is difficult to measure its mechanical property.Select 107 glue of viscosity 50000cps for use, filling a prescription is (basic glue+50000cps107 glue): 100cps silicone oil: CG-25 powder=100: 10: 10 performance such as following table 5: table 5
The viscosity of the mold glue that 107 glue of use 50000cps are done is bigger, be awkward, and physical strength is unlike the physical strength height that uses 20000cps107 glue, so the proportioning of selecting 107 glue of viscosity 20000cps and basic glue for use has very high physical strength near 40: 60 the time.So near the ratio of basic glue and 20000cps 107 glue was 60: 40, seek optimum proportion.107 glue=50/50-70/30 table 6 of base glue: 20000cps
This shows basic glue: 20000cps107 glue=62: 38 o'clock, physical strength maximum, this ratio are optimum proportion.(3) selection of softening agent 100cps silicone oil ratio: consider and the intermiscibility of room temperature vulcanized silicone rubber, select low viscosity silicone for use, as 100cps silicone oil.Its physical and mechanical properties sees Table 7.Base glue: 20000cps107 glue: CG-25=60: 40: 10 tables 7
So softening agent 100cps silicone oil be chosen as 5-15 part.(4) stopping composition is composite
| Two kind of 107 glue proportioning | 20∶80 | ?40∶60 | ?50∶50 | ??60∶40 | ?80∶20 |
| 25 ℃ of viscosity (cps) | 25000 | ?30000 | ?32000 | ??54000 | ?66000 |
| Solidifying agent 3# | 3％ | ?3％ | ?3％ | ??3％ | ?3％ |
| Presetting period (min) | 49 | ?36 | ?34 | ??41 | ?35 |
| Hardness (ShoreA) | 21 | ?19 | ?20 | ??20 | ?19 |
| Elongation (%) | 473 | ?516 | ?524 | ??540 | ?553 |
| Tensile strength (MPa) | 2.80 | ?2.80 | ?2.60 | ??2.80 | ?2.70 |
| Tearing toughness (KN/m) | 22.8 | ?23.1 | ?23.0 | ??24.7 | ?25.4 |
| Two kind of 107 glue proportioning | 20∶80 | ?40∶60 | ?50∶50 | ?60∶40 | ?80∶20 |
| 25 ℃ of viscosity (cps) | 24000 | ?29000 | ?32000 | ?33000 | ?39000 |
| Solidifying agent 3# | 3％ | ?3％ | ?3％ | ?3％ | ?3％ |
| Presetting period (min) | 53 | ?45 | ?47 | ?42 | ?38 |
| Hardness (ShoreA) | 23 | ?23 | ?21 | ?21 | ?21 |
| Elongation (%) | 425 | ?432 | ?480 | ?506 | ?563 |
| Tensile strength (MPa) | 2.60 | ?2.60 | ?2.72 | ?2.78 | ?2.80 |
| Tearing toughness (KN/m) | 20.3 | ?20.0 | ?23.1 | ?23.6 | ?24.6 |
| Base glue and 107 glue proportionings | 10∶90 | ?20∶80 | ?30∶70 | ?40∶60 | ?50∶50 | ?60∶40 | ?70∶30 | ?80∶20 | ?90∶10 |
| 25 ℃ of viscosity (cps) | 30000 | ?31000 | ?33000 | ?36000 | ?40000 | ?56000 | ?73000 | ?89000 | ?≥00000 |
| Solidifying agent 3# | 3％ | ?3％ | ?3％ | ?3％ | ?3％ | ?3％ | ?3％ | ?3％ | ?3％ |
| Presetting period (min) | 40 | ?40 | ?38 | ?39 | ?39 | ?37 | ?36 | ?32 | ?27 |
| Hardness (ShoreA) | 19 | ?18 | ?19 | ?20 | ?22 | ?23 | ?27 | ?/ | ?/ |
| Elongation (%) | 244 | ?321 | ?384 | ?435 | ?492 | ?542 | ?433 | ?/ | ?/ |
| Tensile strength (MPa) | 0.30 | ?0.71 | ?1.50 | ?2.16 | ?2.90 | ?2.95 | ?2.84 | ?/ | ?/ |
| Tearing toughness (KN/m) | 3.00 | ?4.23 | ?7.96 | ?15.6 | ?21.3 | ?24.5 | ?23.2 | ?/ | ?/ |
| Base glue and 107 glue proportionings | 10∶90 | ?20∶80 | ?30∶70 | ?40∶60 | ?50∶50 | ?60∶40 | 70∶30 | 80∶20 | 90∶10 |
| 25 ℃ of viscosity (cps) | 42000 | ?44000 | ?49000 | ?77000 | ≥ 100000 | ≥ 100000 | ≥ 100000 | ||
| Solidifying agent 3# | 3％ | ?3％ | ?3％ | ?3％ | ?3％ | ?3％ | 3％ | 3％ | 3％ |
| Presetting period (min) | 45 | ?38 | ?35 | ?33 | ?33 | ?30 | 25 | 21 | 15 |
| Hardness (ShoreA) | 19 | ?19 | ?20 | ?19 | ?20 | ?22 | / | / | / |
| Elongation (%) | 216 | ?322 | ?351 | ?473 | ?539 | ?564 | / | / | / |
| Tensile strength (MPa) | 0.40 | ?0.91 | ?1.32 | ?1.79 | ?2.50 | ?2.96 | / | / | / |
| Tearing toughness (KN/m) | 1.8 | ?5.4 | ?8.4 | ?15.3 | ?23.6 | ?27.6 | / | / | / |
| Base glue and 107 glue proportionings | ??50∶50 | ??55∶45 | ??58∶42 | ??60∶40 | ??62∶38 | ??65∶35 | ??70∶30 |
| Solidifying agent 1# | ??3％ | ??3％ | ??3％ | ??3％ | ??3％ | ??3％ | ??3％ |
| Presetting period (min) | ??50 | ??59 | ??54 | ??50 | ??48 | ??48 | ??47 |
| Hardness (ShoreA) | ??13 | ??13 | ??12 | ??15 | ??13 | ??13 | ??12 |
| Elongation (%) | ??768 | ??804 | ??926 | ??817 | ??827 | ??798 | ??783 |
| Tensile strength (MPa) | ??2.87 | ??3.06 | ??2.93 | ??3.25 | ??3.57 | ??2.87 | ??2.84 |
| Tearing toughness (KN/m) | ??20.5 | ??24.9 | ??25.6 | ??27.9 | ??29.8 | ??27.9 | ??27.1 |
| The silicone oil weight part | 5 | 10 | ?15 | ?20 |
| 25 ℃ of viscosity (cps) | 49000 | 37000 | ?31000 | ?25000 |
| Solidifying agent 3# | 3％ | 3％ | ?3％ | ?3％ |
| Presetting period (min) | 34 | 30 | ?35 | ?33 |
| Hardness (ShoreA) | 22 | 18 | ?17 | ?16 |
| Elongation (%) | 437 | 467 | ?496 | ?513 |
| Tensile strength (MPa) | 2.30 | 2.50 | ?2.42 | ?2.2 |
| Tearing toughness (KN/m) | 21.7 | 21.6 | ?20.5 | ?17.2 |
What preferentially be used as the silicon rubber filling material mainly is synthetic fine silica powder (white carbon black of vapor phase process and the white carbon black of the precipitator method): the natural quartz powder: diatomite and kaolin (through purification, grinding and processing) can be used as half reinforcement stopping composition or increment stopping composition.
Below be the physical and mechanical properties that various stopping composition are filled postcure glue, see Table 8.Base glue: 20000cps107 glue: 100cps silicone oil: stopping composition=62: 38: 10: 10 tables 8
This shows: (a) select for use nano-calcium carbonate, nano silicon micronization, JL-958, P820 can make the A component viscosity of mold glue very big separately from viscosity.(b) preferentially select the composite stopping composition of nano silicon micronization, JL-958 and JL-958 and silicon powder for use from tension and tearing strength, but the price of nano silicon micronization and JL-958 is too high, but can affirm that major ingredient is that physical strength is significantly increased silica-filled material along with reducing of particle diameter.The consumption of half reinforcement stopping composition is 0-10 part.See Table 9, basic glue: 20000cps107 glue: 100cps silicone oil: CG-05=62: 38: 10: (0-10) table 9
There is by product (as methyl alcohol, ethanol etc.) to produce when (5) the selection RTV-2 glue of deep layer curing catalyst vulcanizes, they need to overflow to the surface from the cross-linked rubber internal divergence, because by product is difficult for emitting, will have influence on inner sulfuration, in order to address this problem, on technology, adopt the layering perfusion.We adopt and add a small amount of vulcanization accelerator, as water, phosphoric acid salt and magnesium oxide etc.(6) selection of solidifying agent
| Project | Viscosity (cps) | Hardness (ShoreA) | Elongation (%) | Tensile strength (MPa) | Tearing toughness (KN/m) |
| Nano-calcium carbonate | ?80000 | ?13 | ?720 | ?2.71 | ?19.9 |
| Silicon powder | ?53000 | ?22 | ?638 | ?2.73 | ?21.2 |
| Nano silicon micronization | ?93000 | ?13 | ?823 | ?3.49 | ?30.6 |
| M500 | ?52000 | ?21 | ?532 | ?2.84 | ?24.8 |
| JL-958 | ?72000 | ?12 | ?847 | ?4.07 | ?32.3 |
| JL-958: silicon powder | ?68000 | ?17 | ?817 | ?3.64 | ?32.4 |
| P820 |
| The CG-05 weight part | 5 | ?10 |
| 25 ℃ of viscosity (cps) | 52000 | ?54000 |
| Solidifying agent 3# | 3％ | ?3％ |
| Presetting period (min) | 40 | ?44 |
| Hardness (ShoreA) | 15 | ?16 |
| Elongation (%) | 789 | ?723 |
| Tensile strength (MPa) | 3.35 | ?3.37 |
| Tearing toughness (KN/m) | 29.9 | ?30.7 |
The requirement of duplicating according to artwork is sought and is solidified early stage slow and the later stage is solidified solidifying agent faster.Quanmethyl silicate mainly is a control sulfurized curing speed in early stage, the curing speed in early stage of tetraethyl orthosilicate is slower, it is subjected to the influence of envrionment temperature more much smaller than quanmethyl silicate when solidifying, so use the mixture of tetraethyl orthosilicate, quanmethyl silicate, is catalyzer with the organotin.
So the prescription of solidifying agent is: quanmethyl silicate: tetraethyl orthosilicate: organotin catalysts=1: 1: 2.
Claims (9)
1, high-strength condensed type silicone mold glue composition, with silicon rubber is main raw material, being equipped with linking agent, catalyzer and stopping composition makes, it is characterized in that two components with A, B, carry out crosslinking reaction as catalyzer and obtain two component condensed room temperature vulcanized silicone rubbers through dibutyl tin laurate, reaction expression is:
A component (weight part) is by 107 silicon rubber, basic glue, softening agent, stopping composition, TiO
2, the deep layer curing catalyst forms, wherein, 107 rubber/basic glue is 30/70-50/50, and the B component is made up of one or more and dibutyl tin laurate in tetramethoxy-silicane, tetraethoxysilane, the tetraethoxysilane hydrolyzate, and described basic glue is through pretreated 107 silicon rubber.
2, high-strength condensed type silicone mold glue composition according to claim 1, it is characterized in that: described basic glue is that the constitution controller hexamethyldisilazane is added in 107 glue, add the white carbon black of handling with hexamethyldisilazane after mixing well again, mediate, mixing after, the sizing material that obtains is mediated at normal temperatures, at 160-180 ℃ of following vacuum kneading, can obtain basic glue after the cooling then.
3, high-strength condensed type silicone mold glue composition according to claim 1 is characterized in that: described stopping composition be in white carbon black, silica powder, diatomite, the kaolin one or more.
4, high-strength condensed type silicone mold glue composition according to claim 1 is characterized in that described deep layer curing catalyst is one or more in water, phosphoric acid salt and the magnesium oxide.
5, high-strength condensed type silicone mold glue composition according to claim 1 is characterized in that described softening agent is a silicone oil with low viscosity, comprises 100cps silicone oil.
6, high-strength condensed type silicone mold glue composition according to claim 1 and 2, the manufacture craft that it is characterized in that described A component is: after 107 glue, basic glue, softening agent are stirred at normal temperatures, add stopping composition, whipping temp more than 80 ℃ to mixing, the cooling back adds the deep layer curing catalyst, can obtain the A component.
7, high-strength condensed type silicone mold glue composition according to claim 1 is characterized in that B component manufacture craft is: one or more in tetramethoxy-silicane, tetraethoxysilane, the tetraethoxysilane hydrolyzate with can use after dibutyl tin laurate mixes.
8, high-strength condensed type silicone mold glue composition according to claim 1 and 2 is characterized in that described 107 silicon rubber are the 5000--50000cps range of viscosities.
9, high-strength condensed type silicone mold glue composition according to claim 8 is characterized in that each substance weight part of A component is:
Base glue/107 silicon rubber 100
Softening agent 5-15
Stopping composition 0-10
Deep layer curing catalyst 0.1-1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701106B (en) * | 2009-11-27 | 2011-11-23 | 合肥凯蒙新材料有限公司 | Two-component addition type room temperature vulcanized silicone rubber for manufacturing handprint mold and footprint mold |
| CN101544881B (en) * | 2009-05-12 | 2012-07-11 | 成都硅宝科技股份有限公司 | Bi-component silicone pouring sealant for LED photoelectric display device and method for manufacturing same |
| CN101724377B (en) * | 2008-10-28 | 2013-02-13 | 上海回天化工新材料有限公司 | High-strength condensed type double-component organosilicon acid-resisting sealant and preparation method thereof |
| CN103497518A (en) * | 2013-09-12 | 2014-01-08 | 上海工程技术大学 | Novel mold rubber and preparation method thereof |
| CN103980835A (en) * | 2014-04-22 | 2014-08-13 | 太原市泰派斯特电子有限公司 | Dealcoholization-type single-component RTV conducting silicone adhesive and preparation method thereof |
| CN106609038A (en) * | 2016-11-28 | 2017-05-03 | 湖北航天化学技术研究所 | Silicone rubber coating layer deeply cured in closed environment |
| CN107868466A (en) * | 2017-12-15 | 2018-04-03 | 深圳市红叶杰科技有限公司 | A kind of double-component condensed type high-temperature-resisting silicon rubber and preparation method |
| CN111117253A (en) * | 2019-12-31 | 2020-05-08 | 郑州国之正生物科技有限公司 | Blood vessel casting agent and casting mold specimen prepared by adopting blood vessel casting agent |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101724377B (en) * | 2008-10-28 | 2013-02-13 | 上海回天化工新材料有限公司 | High-strength condensed type double-component organosilicon acid-resisting sealant and preparation method thereof |
| CN101544881B (en) * | 2009-05-12 | 2012-07-11 | 成都硅宝科技股份有限公司 | Bi-component silicone pouring sealant for LED photoelectric display device and method for manufacturing same |
| CN101701106B (en) * | 2009-11-27 | 2011-11-23 | 合肥凯蒙新材料有限公司 | Two-component addition type room temperature vulcanized silicone rubber for manufacturing handprint mold and footprint mold |
| CN103497518A (en) * | 2013-09-12 | 2014-01-08 | 上海工程技术大学 | Novel mold rubber and preparation method thereof |
| CN103497518B (en) * | 2013-09-12 | 2016-01-20 | 上海工程技术大学 | A kind of Novel mold rubber and preparation method thereof |
| CN103980835A (en) * | 2014-04-22 | 2014-08-13 | 太原市泰派斯特电子有限公司 | Dealcoholization-type single-component RTV conducting silicone adhesive and preparation method thereof |
| CN106609038A (en) * | 2016-11-28 | 2017-05-03 | 湖北航天化学技术研究所 | Silicone rubber coating layer deeply cured in closed environment |
| CN106609038B (en) * | 2016-11-28 | 2020-04-10 | 湖北航天化学技术研究所 | Silicone rubber coating layer deeply cured in closed environment |
| CN107868466A (en) * | 2017-12-15 | 2018-04-03 | 深圳市红叶杰科技有限公司 | A kind of double-component condensed type high-temperature-resisting silicon rubber and preparation method |
| CN111117253A (en) * | 2019-12-31 | 2020-05-08 | 郑州国之正生物科技有限公司 | Blood vessel casting agent and casting mold specimen prepared by adopting blood vessel casting agent |
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