CN1903921A - Bicomponent platinum catalyst vulcanizer and its preparation method - Google Patents
Bicomponent platinum catalyst vulcanizer and its preparation method Download PDFInfo
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- CN1903921A CN1903921A CN 200610062031 CN200610062031A CN1903921A CN 1903921 A CN1903921 A CN 1903921A CN 200610062031 CN200610062031 CN 200610062031 CN 200610062031 A CN200610062031 A CN 200610062031A CN 1903921 A CN1903921 A CN 1903921A
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Abstract
The present invention relates to a double-component platinum catalyst curing agent. It includes agent A and agent B which can be uniformly mixed when they are used, in which the agent A is mixture of vinyl raw rubber, gas phase white carbon black and platinum complex, and the agent B is mixture of vinyl raw rubber, gas phase white carbon black, silicon oil whose end contains hydrogen and inhibitor. When the agent A and agent B are mixed, their mass ratio is agent A: agent B = (0.8-1.0)(1.0-1.5). Said invention also provides the preparation method of said double-component platinum catalyst curing agent.
Description
Technical field
The present invention relates to a kind of vulcanizing agent and preparation method thereof, refer in particular to a kind of bicomponent platinum catalyst vulcanizer and preparation method thereof.
Background technology
In recent years, silicon rubber is very extensive in sector applications such as electronics, medical treatment, aerospace, food sanitations, and along with the requirement of these industries improves constantly, special more harsh for the requirement of bio-medical food grade macromolecular material, all securities of lay special stress on silastic material, harmless, and meet the food rank.The vulcanizing agent that uses in the silastic material production process at present mostly is traditional peroxide vulcanizing agent, for example 2,4-dichlorobenzoperoxide (DCBP, commodity " two 24 " by name), 2,5-dimethyl-2,5-di-t-butyl hexane peroxide (DBPMH, trade(brand)name claims " two 25 " again) etc., this peroxide vulcanizing agent in use easily produces peculiar smell, and curing temperature, vulcanization rate are all not fully up to expectations, the silicone rubber products performance of producing is also undesirable, all is restricted in the application of a lot of industries.
Summary of the invention
Technical problem to be solved by this invention is: a kind of bicomponent platinum catalyst vulcanizer is provided, and its cure efficiency is good, and nonpoisonous and tasteless, and security is good, can also effectively reduce production costs.
The further technical problem to be solved of the present invention is: the preparation method that a kind of bicomponent platinum catalyst vulcanizer is provided.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of bicomponent platinum catalyst vulcanizer comprises and is mixed the A agent and the B agent of mixing well in use again.Wherein, described A agent is the mixture of vinyl rubber, the white carbon black of gas phase and platinum complex compound; The B agent is the mixture of vinyl rubber, the white carbon black of gas phase, end containing hydrogen silicone oil and inhibitor.
Further improvement in the technical proposal is: the mass ratio of described A agent, B agent is during hybrid modulation: the A agent: B agent=(0.8～1.0): (1.0～1.5).
Further improvement in the technical proposal is: the mass parts content of described each composition of A agent is: 20～40 parts of vinyl rubbers, 20 parts of the white carbon blacks of gas phase, 40～60 parts in platinum complex compound.
Further improvement in the technical proposal is: the mass parts content of described each composition of B agent is: 30～40 parts of vinyl rubbers, 15 parts of the white carbon blacks of gas phase, 47～53 parts in platinum complex compound, 2～3 parts in inhibitor.
The present invention also provides a kind of preparation method of bicomponent platinum catalyst vulcanizer, comprises the steps:
A1, synthetic platinum complex compound, the aqueous solution and the ethene double-seal head of a certain amount of Platinic chloride are dissolved in the dehydrated alcohol, being heated to 120 ℃ refluxed 2～3 hours, add sodium bicarbonate again, under 6.66KPa, 45 ℃ of conditions, steam then except that dehydrated alcohol and moisture content, filter the black solid thing, promptly obtain a kind of vinylsiloxane co-ordination complex of platinum;
A2, be mixed with the A agent, platinum complex compound, the white carbon black of gas phase and vinyl rubber are put into stirrer, be warming up to 100 ℃～120 ℃, vacuum～0.06mPa thermal treatment 2 hours promptly obtains the A agent;
B1, preparation end containing hydrogen silicone oil, with D4, hold hydrogeneous double-seal head, KF-99, acidic cationic resin to drop in the reaction vessel in proportion and be controlled at 65 ℃～700 ℃ following stirring and refluxing 2～3 hours, then be warming up to 115 ℃～120 ℃ again and continue stirred polymerizations 2～3 hours, reaction finishes after-filtration gained liquid and drops into and remove low molecule 120 ℃ of decompressions in the reaction vessel and obtain molecular formula end containing hydrogen silicone oil as follows:
B2, preparation inhibitor add a certain amount of methylbutynol and picoline in the reaction vessel, at N
2Protection is stirring at room down, slowly drips (CH
3)
2SiCl
2, reaction heating in the dropping process, temperature rises, and drips off the back and continues reaction 2 hours at 60 ℃, filters then, washes, and product layer is moved in the reaction vessel through dried over sodium sulfate, refilters, and distillation obtains structural formula inhibitor as follows:
B3, be mixed with the B agent, will synthetic end containing hydrogen silicone oil, the white carbon black of gas phase, vinyl rubber, inhibitor drop in the stirrer and be warming up to 100 ℃～120 ℃, vacuum～0.06mPa thermal treatment 2～3 hours promptly obtains the B agent.
The invention has the beneficial effects as follows: compare with traditional peroxide vulcanizing agent, the present invention has following advantage:
1, once sulfuration is finished, technology such as need not post cure and boil;
2, do not produce any new recruit, free from extraneous odour in the sulfidation;
3, health rank height meets Valuation Standards such as FDA, SGS, and is more safer than import " two 24 ", " two 25 ";
4, the power saving that saves time provides high efficiency to reduce production costs simultaneously;
5, dimensional stability is good, and shrinking percentage is low;
When 6, utilizing bicomponent platinum catalyst vulcanizer of the present invention to vulcanize, sulfurized silicon rubber generation addition reaction, be different from original polyreaction, the intermolecular combination of silicon rubber is better, the tensile strength of product, do tear strength, rebound performance improves greatly, good physicals and biochemical properties such as that the add-on type rubber unvulcanizate of addition has is nonpoisonous and tasteless, good springiness, volatility, curing temperature that transparency is good, extremely low are low, physiology inertia, good biocompatibility can be widely used in medical treatment and food sanitation, field such as electric.
Adopt preparation method of the present invention, can prepare the A agent and the B agent of bicomponent platinum catalyst vulcanizer fast, and the good stability of A agent, B agent.
Embodiment
The invention provides a kind of bicomponent platinum catalyst vulcanizer, comprise and mixed the A agent and the B agent of mixing well in use again.
Wherein, described A agent is the mixture of vinyl rubber, the white carbon black of gas phase and platinum complex compound, and the mass parts content of each composition of A agent is: 20～40 parts of vinyl rubbers, 20 parts of the white carbon blacks of gas phase, 40～60 parts in platinum complex compound; The B agent is the mixture of vinyl rubber, the white carbon black of gas phase, end containing hydrogen silicone oil and inhibitor, and the mass parts content of each composition of B agent is: 30～40 parts of vinyl rubbers, 15 parts of the white carbon blacks of gas phase, 47～53 parts of containing hydrogen silicone oils of end, 2～3 parts in inhibitor.
The invention provides three prescriptions as shown in the table:
| Composition | Prescription one | Prescription two | Prescription three | |
| The A agent | The vinyl rubber | 20 parts | 40 parts | 30 parts |
| The white carbon black of gas phase | 20 parts | 20 parts | 20 parts | |
| The platinum complex compound | 40 parts | 60 parts | 50 parts | |
| The B agent | The vinyl rubber | 30 parts | 40 parts | 35 parts |
| The white carbon black of gas phase | 15 parts | 15 parts | 15 parts | |
| The end containing hydrogen silicone oil | 47 parts | 53 parts | 50 parts | |
| Inhibitor | 2 parts | 3 parts | 2 parts | |
A agent, B agent be good and difference packaging and storing by manufacturer's prepared beforehand, before use, just with A agent and B agent hybrid modulation, and promptly joins promptly and uses.During hybrid modulation, synthetic vulcanizing agent consumption is to treat 1.8%～2.5% of vulcanized rubber total amount, wherein, the mass ratio of described A agent, B agent is: the A agent: B agent=(0.8～1.0): (1.0～1.5), i.e. A agent, B agent account for respectively treats 0.8%～1.0%, 1.0%～1.5% of vulcanized rubber total amount.Concrete ratio is then looked and is applied to the different vulcanizations of rubber and difference to some extent, for example:
When being used for the sulfuration of common precipitation glue, A agent consumption is to treat 0.8%～1.0% of vulcanized rubber gross weight, and B agent consumption is 1.0%～1.2%, adds 75 ℃～85 ℃ of sulphur temperature, and corresponding to add the sulphur time be 10～15 minutes;
When being used for the sulfuration of high-grade gas phase glue, A agent consumption is 1.0%, and B agent consumption is 1.2%～1.5%, adds 110 ℃～130 ℃ of sulphur temperature, and corresponding to add the sulphur time be 5～8 minutes;
When being used for the oil pressure type and adding sulphur, A agent consumption is 1.0%, and B agent consumption is 1.2%～1.5%, 85 ℃～110 ℃ of mould temperature, and adding the sulphur time is 75 seconds～100 seconds;
In the above-mentioned various sulfuration, it is high more to add the sulphur temperature, and it is short more to add the sulphur time.
The present invention also provides a kind of preparation method of bicomponent platinum catalyst vulcanizer, comprises the steps:
A1, synthetic platinum complex compound, the aqueous solution of 1 mass parts Platinic chloride and the ethene double-seal head of 16 mass parts are dissolved in the 35 mass parts dehydrated alcohols, being heated to 120 ℃ refluxed 2～3 hours, add 10 mass parts sodium bicarbonates again, under 6.66KPa, 45 ℃ of conditions, steam then except that dehydrated alcohol and moisture content, filter the black solid thing, promptly obtain the vinylsiloxane co-ordination complex of two kinds of platinum;
A2, be mixed with the A agent, platinum complex compound, the white carbon black of gas phase and vinyl rubber are put into stirrer, be warming up to 100 ℃～120 ℃, vacuum～0.06mPa thermal treatment 2 hours promptly obtains the A agent, and wherein, the stirrer that is adopted preferably adopts planetary mixer;
B1, preparation end containing hydrogen silicone oil, with D4 (octamethylcyclotetrasiloxane), hold hydrogeneous double-seal head, KF-99 (molecular formula is:
), acidic cationic resin (adopting perfluorinated sulfonic resin usually) drops in the reaction vessel in proportion and be controlled at 65 ℃～700 ℃ following stirring and refluxing 2～3 hours, then be warming up to 115 ℃～120 ℃ again and continue stirred polymerizations 2～3 hours, reaction finishes after-filtration gained liquid and drops into and remove low molecule 120 ℃ of decompressions in the reaction vessel and obtain molecular formula end containing hydrogen silicone oil as follows:
B2, preparation inhibitor add 200 parts of methylbutynols and 145 parts of picolines in the reaction vessel, at N
2Protection is stirring at room down, slowly drips (CH
3)
2SiCl
2, reaction heating in the dropping process, temperature rises, and drips off the back and continues reaction 2 hours at 60 ℃, filters then, washes, and product layer is moved in the reaction vessel through dried over sodium sulfate, refilters, and distillation obtains structural formula inhibitor as follows:
B3, be mixed with the B agent, will synthetic end containing hydrogen silicone oil, the white carbon black of gas phase, vinyl rubber drop in the stirrer and be warming up to 100 ℃～120 ℃, vacuum～0.06mPa thermal treatment 2～3 hours promptly obtains the B agent, wherein, the stirrer that is adopted preferably adopts planetary mixer.
Wherein, in the A1 step, Platinic chloride itself is the tetravalence hexa-coordinate, will be reduced to divalence earlier at the beginning of the reaction, and what often use is its aqueous isopropanol, proves that Platinic chloride can be reduced to divalence by Virahol.
Above-mentioned dimer can be used as pure compound and separates after draining solvent, showing has two propylene molecules and platinum complex coordination.When having excessive Virahol and chlorion to exist, this dimer is dissociable again to be unit molecule, the compound of divalence four-coordination.
Ethene on the platinum or propylene ligand can quantitatively replaced by the silico ethylene compound more than 50 ℃, so addition the time, silico ethylene and platinum complexing.In the reaction, si-h bond separately was added to respectively on the pt atom of four of divalence it was oxidized to the tetravalence hexa-coordinate before this, then hydrogen row is added on the vinyl coordination of ethene is changed into platinum-carbon coordination, and is later under the effect of new vinyl, the intermediate cancellation of this tetravalence hexa-coordinate
Again recover the state of divalence four-coordination.
1), contain organism such as N, P, S bicomponent platinum catalyst vulcanizer of the present invention in use notes and can not contact:; 2), Sn, Hg, As plasma compound; 3), contain alkynes and vinyl group compound.Do not solidify or solidify slowly in order to avoid make the Pt poisoning of catalyst.And some pigment dyestuff can cause solidifying and slowly or not solidify, and needs test earlier before using.
Claims (9)
1, a kind of bicomponent platinum catalyst vulcanizer is characterized in that, comprises being mixed the A agent and the B agent of mixing well in use again, and wherein, described A agent is the mixture of vinyl rubber, the white carbon black of gas phase and platinum complex compound; The B agent is the mixture of vinyl rubber, the white carbon black of gas phase, end containing hydrogen silicone oil and inhibitor.
2, bicomponent platinum catalyst vulcanizer as claimed in claim 1 is characterized in that: the mass ratio of described A agent, B agent is during hybrid modulation: the A agent: B agent=(0.8～1.0): (1.0～1.5).
3, bicomponent platinum catalyst vulcanizer as claimed in claim 1 or 2 is characterized in that: the mass parts content of described each composition of A agent is: 20～40 parts of vinyl rubbers, 20 parts of the white carbon blacks of gas phase, 40～60 parts in platinum complex compound.
4, bicomponent platinum catalyst vulcanizer as claimed in claim 1 or 2 is characterized in that: the mass parts content of described each composition of B agent is: vinyl rubber 30-40 part, 15 parts of the white carbon blacks of gas phase, 47～53 parts of containing hydrogen silicone oils of end, 2～3 parts in inhibitor.
5, a kind of preparation method of bicomponent platinum catalyst vulcanizer as claimed in claim 1 comprises the steps:
A1, synthetic platinum complex compound, the aqueous solution and the ethene double-seal head of a certain amount of Platinic chloride are dissolved in the dehydrated alcohol, being heated to 120 ℃ refluxed 2～3 hours, add sodium bicarbonate again, under 6.66KPa, 45 ℃ of conditions, steam then except that dehydrated alcohol and moisture content, filter the black solid thing, promptly obtain a kind of vinylsiloxane co-ordination complex of platinum;
A2, be mixed with the A agent, platinum complex compound, the white carbon black of gas phase and vinyl rubber are put into stirrer, be warming up to 100 ℃～120 ℃, vacuum～0.06mPa thermal treatment 2 hours promptly obtains the A agent;
B1, preparation end containing hydrogen silicone oil, with D4, hold hydrogeneous double-seal head, KF-99, acidic cationic resin to drop in the reaction vessel in proportion and be controlled at 65 ℃～700 ℃ following stirring and refluxing 2～3 hours, then be warming up to 115 ℃～120 ℃ again and continue stirred polymerizations 2～3 hours, reaction finishes after-filtration gained liquid and drops into and remove low molecule 120 ℃ of decompressions in the reaction vessel and obtain molecular formula end containing hydrogen silicone oil as follows:
B2, preparation inhibitor add a certain amount of methylbutynol and picoline in the reaction vessel, at N
2Protection is stirring at room down, slowly drips (CH
3)
2SiCl
2, reaction heating in the dropping process, temperature rises, and drips off the back and continues reaction 2 hours at 60 ℃, filters then, washes, and product layer is moved in the reaction vessel through dried over sodium sulfate, refilters, and distillation obtains structural formula inhibitor as follows:
B3, be mixed with the B agent, will synthetic end containing hydrogen silicone oil, the white carbon black of gas phase, vinyl rubber, inhibitor drop in the stirrer and be warming up to 100 ℃～120 ℃, vacuum～0.06mPa thermal treatment 2～3 hours promptly obtains the B agent.
6, the preparation method of a kind of bicomponent platinum catalyst vulcanizer as claimed in claim 5, it is characterized in that: in the described A1 step, the consumption of the aqueous solution of Platinic chloride, ethene double-seal head, dehydrated alcohol, sodium bicarbonate is respectively 1 mass parts, 16 mass parts, 35 mass parts, 10 mass parts.
7, the preparation method of a kind of pair of component platinum catalyst vulcanizer as claimed in claim 5 is characterized in that: in the described B2 step, the consumption of methylbutynol, picoline is respectively 200 mass parts, 145 mass parts.
8, the preparation method of a kind of pair of component platinum catalyst vulcanizer as claimed in claim 5 is characterized in that: the stirrer that is adopted in A2, the B3 step is a planetary mixer.
9, the preparation method of a kind of pair of component platinum catalyst vulcanizer as claimed in claim 5 is characterized in that: in the B1 step, acidic cationic resin is a perfluorinated sulfonic resin.
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| CN101407635B (en) * | 2008-11-14 | 2011-04-06 | 成都硅宝科技股份有限公司 | Addition type heat conducting silicon rubber and manufacturing method thereof |
| CN101514260B (en) * | 2009-03-13 | 2011-06-29 | 东莞市贝特利新材料有限公司 | Silastic composition and preparation method thereof |
| CN101314642B (en) * | 2008-06-24 | 2012-04-04 | 江苏强盛功能化学股份有限公司 | Method for removing foreign flavor of silicon rubber products |
| CN103319903A (en) * | 2013-07-01 | 2013-09-25 | 江苏天辰硅材料有限公司 | Double-component addition type room-temperature vulcanizing silicone rubber and preparation method thereof |
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| CN105255195A (en) * | 2015-11-03 | 2016-01-20 | 东莞劲胜精密组件股份有限公司 | Low-temperature rapidly-vulcanized solid silicon rubber raw material and production method thereof |
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| CN101407635B (en) * | 2008-11-14 | 2011-04-06 | 成都硅宝科技股份有限公司 | Addition type heat conducting silicon rubber and manufacturing method thereof |
| CN101514260B (en) * | 2009-03-13 | 2011-06-29 | 东莞市贝特利新材料有限公司 | Silastic composition and preparation method thereof |
| CN103540135B (en) * | 2012-12-28 | 2016-04-06 | 江苏兴缘高温线缆有限公司 | A kind of environment-friendly type silica gel insulating sheath material |
| CN103540134A (en) * | 2012-12-28 | 2014-01-29 | 江苏兴缘高温线缆有限公司 | Preparation method of environment-friendly silica gel insulating sheathing material |
| CN103540135A (en) * | 2012-12-28 | 2014-01-29 | 江苏兴缘高温线缆有限公司 | Environment-friendly silica gel insulating sheathing material |
| CN103540134B (en) * | 2012-12-28 | 2016-04-06 | 江苏兴缘高温线缆有限公司 | A kind of preparation method of environment-friendly type silica gel insulating sheath material |
| CN103319903A (en) * | 2013-07-01 | 2013-09-25 | 江苏天辰硅材料有限公司 | Double-component addition type room-temperature vulcanizing silicone rubber and preparation method thereof |
| CN103319903B (en) * | 2013-07-01 | 2015-08-12 | 江苏天辰硅材料有限公司 | A kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method |
| CN104927363A (en) * | 2015-06-30 | 2015-09-23 | 东莞市圣力堡有机硅科技有限公司 | Novel platinum vulcanizing agent and preparation technology thereof |
| CN105255195A (en) * | 2015-11-03 | 2016-01-20 | 东莞劲胜精密组件股份有限公司 | Low-temperature rapidly-vulcanized solid silicon rubber raw material and production method thereof |
| CN105255195B (en) * | 2015-11-03 | 2018-08-31 | 广东劲胜智能集团股份有限公司 | A kind of low temperature short vulcanization solid-state silica gel materials and preparation method thereof |
| CN107619605A (en) * | 2017-01-21 | 2018-01-23 | 田志强 | Preparation method for the two-component room temperature fast-curing silica gel of DIY toys |
| CN111875971A (en) * | 2020-08-18 | 2020-11-03 | 东莞市众展有机硅材料有限公司 | Double-component platinum vulcanizing agent for promoting adhesion of silica gel and PC material |
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| CN112251165A (en) * | 2020-10-27 | 2021-01-22 | 东莞市众展有机硅材料有限公司 | Special prime coat-free platinum vulcanizing agent for combination of metal substrate and silica gel and preparation method thereof |
| CN112280469A (en) * | 2020-10-27 | 2021-01-29 | 东莞市众展有机硅材料有限公司 | Special bottom-coating-free platinum vulcanizing agent for combination of PA (polyamide) substrate and silica gel and preparation method thereof |
| CN112280469B (en) * | 2020-10-27 | 2022-03-25 | 东莞市众展有机硅材料有限公司 | Special bottom-coating-free platinum vulcanizing agent for combination of PA (polyamide) substrate and silica gel and preparation method thereof |
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