CN102030992A - Liquid silicon rubber platinum catalyst taking polyethylene glycol as ligand and preparation method thereof - Google Patents
Liquid silicon rubber platinum catalyst taking polyethylene glycol as ligand and preparation method thereof Download PDFInfo
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- CN102030992A CN102030992A CN 201010559336 CN201010559336A CN102030992A CN 102030992 A CN102030992 A CN 102030992A CN 201010559336 CN201010559336 CN 201010559336 CN 201010559336 A CN201010559336 A CN 201010559336A CN 102030992 A CN102030992 A CN 102030992A
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- polyoxyethylene glycol
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- polyethylene glycol
- silicon rubber
- platinic chloride
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Abstract
The invention provides a liquid silicon rubber platinum catalyst taking polyethylene glycol as ligand. The catalyst is a composition generated by dissolving chloroplatinic acid (H2PtCl6) in the polyethylene glycol with the molecular weight of 200-800. In the liquid silicon rubber platinum catalyst, the catalytic activity is good, the storage and use are easy, and cavities and bulbs can not be generated in the heating and crosslinking processes. The invention also provides a preparation method of the catalyst, which is as follows: 1) dissolving chloroplatinic acid (H2PtCl6) in the polyethylene glycol with the molecular weight of 200-800; 2) heating the polyethylene glycol in the step 1), and accelerating the composition of the chloroplatinic acid and the polyethylene glycol; and 3) adding sodium bicarbonate in the polyethylene glycol in the step 2) so as to remove acid in the polyethylene glycol. By utilizing the preparation method, the catalyst can be rapidly and stably prepared.
Description
Technical field
The invention belongs to the crosslinking catalyst field of add-on type liquid silicon rubber.
Background technology
Since the invention of add-on type liquid silicon rubber, selection of catalysts is exactly a very important problem
[1]Especially for the single-component add-on type liquid silicon rubber, selection of catalysts is crucial especially, wish that it has lower activity so that transport and store when low temperature, and when high temperature, higher activity can be arranged so that rapid crosslinking curing should not produce bad influence to rubber itself simultaneously.The catalyzer that generally uses is the platiniferous title complex now, as platinum-vinyl siloxane complex (Karstedt catalyzer)
[2] [3], Platinic chloride-aqueous isopropanol
[4] [5]Deng.Wherein Karstedt catalyzer and derivative thereof have very high catalytic activity, can at room temperature make silicon rubber matrix generation cross-linking and curing reaction, thereby are applied in widely in the bi-component addition type liquid silastic
[6]But because its activity is too high, may make raw material before processing is finished, can't not continue to process, cause loss, even can damage machine with regard to crosslinking curing.In order to reduce catalyst activity, must add some reaction suppressors, as alkynol etc.This makes that on the one hand system is complicated, and micromolecular on the other hand alkynol volatilizees easily, has caused the unstable of product.In the single-component add-on type liquid silicon rubber, this problem is more serious, much adopt the product of such catalyzer must remain on subzero 20 degree deposit could make do not take place in the storage process crosslinked, for the storage and the transportation of product brought many inconvenience.And adopt Platinic chloride-aqueous isopropanol activity of such catalysts less, and can place for some time in room temperature, do not need very cryopreservation yet.But use such catalyzer must heat to improve rate of crosslinking.Because the boiling point of Virahol has only about 82 ℃,, limited this Application of Catalyst scope so after the heat cross-linking temperature surpasses 82 ℃, can reduce product performance (comprising intensity, transparency and elasticity etc.) at a large amount of bubbles of the inner generation of rubber.
Reference:
[1] add-on type organo-silicone rubber progress, Tan Bien etc., China Synthetic Rubber Industry, the 3rd volume, 1999
【2】Platinum?Complexes?of?Unsaturated?Siloxanes?and?Platinum?Containing?Organopolysiloxanes, Karstedt USP?3?775?452,1973
【3】Catalysts?for?The?Reaction?of?SiH?with?Organic?Compounds?Containing?Aliphatic?Unsaturation, Willing?USP?3?419?593，1968
[4] preparation of addition-type silicon rubber platinum catalyst and activity research thereof, Tan Bien etc., Chinese glue paste, the 10th volume, the 4th phase, 2000
[5] market of organosilicon material and product development (continuous eight), Huang Wenrun etc., organosilicon material and application, the 1st volume, the 1st phase, 1994
[6] the liquid embedding composition and the preparation of bi-component addition type silicon rubber, Wang Wei etc., Chinese patent, 200810162462
Summary of the invention
The objective of the invention is to overcome the difficult problem that single component add-on type liquid silicon rubber catalyzer selects and provide a kind of and have medium catalytic activity, be easy to store and use, what can not produce hole and bubble in the heat cross-linking process again is the liquid silastic platinum catalyst of part with the polyoxyethylene glycol.
In order to reach above technical purpose, the present invention adopts following technical scheme:
Described catalyzer is: Platinic chloride (H
2PtCl
6) to be dissolved in molecular weight be the title complex that is produced in the polyoxyethylene glycol of 200-800.
By above technical scheme, catalytic activity of the present invention is good, is easy to store and use, and can not produce hole and bubble in the heat cross-linking process.
The present invention also provides above Preparation of catalysts method, 1), with Platinic chloride (H
2PtCl
6) be dissolved in the polyoxyethylene glycol that molecular weight is 200-800; 2), the polyoxyethylene glycol in the step 1) is heated, quickening Platinic chloride and polyoxyethylene glycol cooperates; 3), in step 2) in polyoxyethylene glycol in add sodium bicarbonate, in order to remove acid wherein.
By above preparation method, can stably prepare aforementioned catalyzer rapidly.
Description of drawings
Fig. 1 is the single-component add-on type liquid silicon rubber performance table of different catalysts preparation;
Fig. 2 is the catalyst performance comparison sheet of the several embodiment preparations of the present invention.
Embodiment
The present invention is for being the single-component add-on type liquid silicon rubber platinum catalyst of part with the polyoxyethylene glycol, and described catalyzer is: Platinic chloride (H
2PtCl
6) to be dissolved in molecular weight be the title complex that is produced in the polyoxyethylene glycol of 200-800.Described molecular weight is that the polyoxyethylene glycol of 200-800 is high boiling polyoxyethylene glycol, and after the Platinic chloride dissolving, wherein activeconstituents is the title complex of Platinic chloride and polyoxyethylene glycol.
The single-component add-on type liquid silicon rubber catalyzer that the present invention is prepared has good cryopreservation and higher high-temperature catalytic activity.The present invention and Karstedt catalyzer are contrasted, use the single-component add-on type liquid silicon rubber of catalyzer of the present invention, can be 0 ℃ of left and right sides prolonged preservation, and the product needed of using the Karstedt catalyzer is-20 ℃ of preservations, will very fast crosslinking curing in case surpass-20 ℃.And than Platinic chloride-Virahol catalyzer, the boiling point of the polyoxyethylene glycol that uses among the present invention is more than 250 ℃, even still can not produce hole or bubble in rubber inside so the heat cross-linking temperature reaches 100-150 ℃, the product performance that obtain are better than the product performance of use Platinic chloride-Virahol catalyzer.In addition, this Preparation of catalysts process is fairly simple, compares with preparation Karstedt catalyzer, does not need through complicated reaction and vacuum distillation process, and raw material is also more cheap to be easy to get, so cost is lower.In sum, the present invention is more suitable for doing the catalyzer of single component add-on type liquid silicon rubber product.Can be widely used in the preparation of single-component add-on type liquid silicon rubber mould, goods, glue paste, perfusion material etc., wide application prospect all be arranged in industries such as electronics, biology, the energy and chemical industry.
Illustrate the preparation of the single-component add-on type liquid silicon rubber that uses catalyzer of the present invention: with the α of 100 parts of viscosity 1000mPa.s, ω-divinyl polydimethylsiloxane and 5 parts of H massfractions are that 0.5% silicon oil of low hydrogen content mixes the back and adds 20 parts of white carbon blacks that apparent density is 70g/L, add 0.5 part of above-mentioned catalyzer (being equivalent to platinum massfraction 30ppm) again.After thorough mixing is even, vacuum removal of air bubbles.Specimen is in the shelf time of room temperature operable time and 0 ℃, and the silicon rubber appearance property that obtains after crosslinked of 150 ℃ of heating 10 minutes, and contrast Karstedt catalyzer and Platinic chloride-Virahol catalyzer the results are shown in Figure 1.
The present invention is mainly used in the production of single-component add-on type liquid silicon rubber, belongs to the crosslinking catalyst field of add-on type liquid silicon rubber.Be mainly used in the problem that solves existing single component add-on type liquid silicon rubber product needed utmost point low-temperature storage.This catalyzer is obtained through heat treated by the solution of polyoxyethylene glycol and Platinic chloride.Catalyst consumption is the 1-100ppm of single-component add-on type liquid silicon rubber.This catalyzer is mainly used in the preparation of single-component add-on type liquid silicon rubber, has good cryopreservation and higher high-temperature catalytic ability, and does not produce bubble in the heat cross-linking process.Can be used for the making of products such as single-component add-on type liquid silica gel mould, goods, tackiness agent, perfusion material.
The present invention also provides with the polyoxyethylene glycol preparation method of the single-component add-on type liquid silicon rubber platinum catalyst that is part, and it comprises the steps: 1), with Platinic chloride (H
2PtCl
6) be dissolved in the polyoxyethylene glycol that molecular weight is 200-800; 2), the polyoxyethylene glycol in the step 1) is heated, quickening Platinic chloride and polyoxyethylene glycol cooperates; 3), in step 2) in polyoxyethylene glycol in add sodium bicarbonate, in order to remove acid wherein, obtain orange moderately viscous liquid catalyst.
Described Platinic chloride (H
2PtCl
6) be Platinic chloride solid (H
2PtCl
66H
2O).
In the described step 1), the mass ratio of Platinic chloride and polyoxyethylene glycol is 1:10-1:1000.
Described step 2) in, 30-40 ℃ of heating 0.5-3 hour.
Among the present invention, Platinic chloride (H
2PtCl
6) and molecular weight be that the high boiling polyoxyethylene glycol of 200-800 is analytical pure, do not pass through special purification process.
Present method is to adopt high boiling polyoxyethylene glycol as part, obtains a kind of novel single-component add-on type liquid silicon rubber catalyzer thereby carry out coordination with Platinic chloride.Concrete measure is as follows: at first, Platinic chloride is dissolved in the high boiling polyoxyethylene glycol, the molecular weight of polyoxyethylene glycol is between 200-800, the mass ratio of Platinic chloride and polyoxyethylene glycol is between 1:10-1:1000, in fact, because the solubleness of Platinic chloride in polyoxyethylene glycol is lower, even if it fully dissolves, the amount of employed Platinic chloride is also also little, the restriction of described mass ratio is in order more to help controlling final catalyst concentration, to make the convenient artificial amount that adds catalyzer be unlikely to too big or too little.Then, with this solution heating, temperature heated 0.5-3 hour at 30-40 ℃, so that fully cooperate.The purpose that is heated is in order to add fast response and to make sufficient reacting, if do not heat, speed of response can be slower.At last, with this solution cooling, the adding solid sodium bicarbonate is removed the sour after-filtration in this solution, the acid that the adding sodium bicarbonate is removed in this solution is the use of catalyzer for convenience, because when this catalyzer uses, residual acid may the catalyzed polymerization product decomposition reaction, influence result of use, finally obtain orange polyoxyethylene glycol-Platinic chloride complex solution.During use, this catalyst by proportion directly added get final product uniform mixing in the matrix.
Below preparation example of the present invention:
Embodiment 1:
It is in 400 the polyoxyethylene glycol, at N that 0.2g Platinic chloride crystal is dissolved in the 10g molecular weight
2Protect following 35 ℃ of heating 0.5 hour, the cooling back adds 0.2g NaHCO
3After-filtration obtains orange medium-viscosity liquid, platiniferous 0.74%.
Embodiment 2:
It is in 300 the polyoxyethylene glycol, at N that 0.2g Platinic chloride crystal is dissolved in the 2g molecular weight
2Protect following 40 ℃ of heating 3 hours, the cooling back adds 0.2g NaHCO
3After-filtration obtains orange medium-viscosity liquid, platiniferous 3.4%.
Embodiment 3:
It is in 600 the polyoxyethylene glycol, at N that 0.2g Platinic chloride crystal is dissolved in the 200g molecular weight
2Protect following 30 ℃ of heating 1 hour, the cooling back adds 0.2g NaHCO
3After-filtration obtains orange medium-viscosity liquid, platiniferous 0.037%.
By this catalyzer of synthetic different platinum contents, can control catalytic activity.For the silicone rubber crosslinking reaction of catalysis equal in quality, the amount that the higher catalyzer of platinum containing amount adds can reduce accordingly, but is not easy to mix; The catalyzer that platinum containing amount is lower need add more more, but is easy to mix.Adopt the less polyoxyethylene glycol of molecular weight (be as molecular weight 300 polyoxyethylene glycol) because its boiling point is low, and temperature tolerance is less better, but the viscosity ratio of catalyzer is lower; And adopt the temperature tolerance of the bigger polyoxyethylene glycol of molecular weight (be as molecular weight 600 polyoxyethylene glycol) can be better, but viscosity is big, and it is not very convenient using.After the molecular weight of polyoxyethylene glycol surpasses 800, become waxy solid, just be not suitable for having prepared this catalyzer.
Adopt the catalyzer of above method preparation, have moderate catalysis speed and excellent catalytic performance, can be widely used in the crosslinked field of addition-type silicon rubber.
Claims (5)
1. be the liquid silastic platinum catalyst of part with the polyoxyethylene glycol, it is characterized in that described catalyzer is: Platinic chloride (H
2PtCl
6) to be dissolved in molecular weight be the title complex that is produced in the polyoxyethylene glycol of 200-800.
2. as claimed in claim 1 is the preparation method of the liquid silastic platinum catalyst of part with the polyoxyethylene glycol, it is characterized in that described method comprises the steps: 1), with Platinic chloride (H
2PtCl
6) be dissolved in the polyoxyethylene glycol that molecular weight is 200-800; 2), the polyoxyethylene glycol in the step 1) is heated, quickening Platinic chloride and polyoxyethylene glycol cooperates; 3), in step 2) in polyoxyethylene glycol in add sodium bicarbonate, in order to remove acid wherein.
3. as claimed in claim 2 is the preparation method of the liquid silastic platinum catalyst of part with the polyoxyethylene glycol, it is characterized in that described Platinic chloride (H
2PtCl
6) be Platinic chloride solid (H
2PtCl
66H
2O).
4. as claimed in claim 2 is the preparation method of the liquid silastic platinum catalyst of part with the polyoxyethylene glycol, it is characterized in that in the described step 1), the mass ratio of Platinic chloride and polyoxyethylene glycol is 1:10-1:1000.
5. as claimed in claim 2 is the preparation method of the liquid silastic platinum catalyst of part with the polyoxyethylene glycol, it is characterized in that described step 2) in, 30-40 ℃ of heating 0.5-3 hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374899A (en) * | 2014-11-14 | 2015-02-25 | 东莞兆舜有机硅新材料科技有限公司 | Method for testing anti-poisoning effect of additional liquid silicone rubber |
| CN104672453A (en) * | 2015-02-05 | 2015-06-03 | 烟台德邦先进硅材料有限公司 | Synthesis method of special addition type catalyst for high-refractive index LED packaging resin |
| CN114214028A (en) * | 2021-12-23 | 2022-03-22 | 绵阳惠利电子材料有限公司 | Organosilicon packaging material for network transformer |
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| GB1041028A (en) * | 1964-01-20 | 1966-09-01 | Ici Ltd | Veterinary compositions comprising paraquat salts |
| WO2005033116A1 (en) * | 2003-10-02 | 2005-04-14 | Dow Corning Toray Co., Ltd. | Preparation of a halosilylated chain hydrocarbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104374899A (en) * | 2014-11-14 | 2015-02-25 | 东莞兆舜有机硅新材料科技有限公司 | Method for testing anti-poisoning effect of additional liquid silicone rubber |
| CN104672453A (en) * | 2015-02-05 | 2015-06-03 | 烟台德邦先进硅材料有限公司 | Synthesis method of special addition type catalyst for high-refractive index LED packaging resin |
| CN104672453B (en) * | 2015-02-05 | 2017-06-13 | 烟台德邦先进硅材料有限公司 | The synthetic method of add-on type high index of refraction LED potting resin special-purpose catalysts |
| CN114214028A (en) * | 2021-12-23 | 2022-03-22 | 绵阳惠利电子材料有限公司 | Organosilicon packaging material for network transformer |
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