CN102942667B - Polysiloxane-polyurethane gel material and preparation method thereof - Google Patents
Polysiloxane-polyurethane gel material and preparation method thereof Download PDFInfo
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- CN102942667B CN102942667B CN201210403073.6A CN201210403073A CN102942667B CN 102942667 B CN102942667 B CN 102942667B CN 201210403073 A CN201210403073 A CN 201210403073A CN 102942667 B CN102942667 B CN 102942667B
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- polysiloxane
- polyurethane
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- semi prepolymer
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Abstract
The invention relates to a polysiloxane-polyurethane gel material and a preparation method thereof. The material is the polysiloxane-polyurethane gel material capable of being used as a vibration and noise reduction buffering agent of an underwater acoustic device. The material has good environmental friendliness and good buffering capacity, has no migration or exudation of plasticizer when being used for a long time, and has small compressive deformation. The material has no plasticizer, and enhances buffering capacity by introducing short-chain polysiloxane. Besides, organic compound participates in the chemical reaction of the gel formation, to form a crosslinked macro-molecule gel. No migration or exudation of plasticizer when the material is used for a long time. The material has good environmental friendliness.
Description
Technical field
The invention belongs to organic polymer material preparation field, specifically a kind of polysiloxane-polyurethane(s) gel material and preparation method thereof.
Background technology
Polysiloxane-polyurethane(s) gel material can be used as the vibration and noise reducing buffer reagent of underwater sound device, and buffer reagent is mainly used light wax oil and plasticizer-containing polyurethane gle at present.It is low that polysiloxane-polyurethane(s) gel material has overcome light wax oil visco-elasticity, the shortcoming that easily breakage is run off, overcome again plasticizer-containing polyurethane gle and added in a large number softening agent, after using in for some time, gel property is oozed out, loses in plasticizer migration, compressive set is large, buffering resilience reduces, the same easily damaged shortcoming running off is oozed out in plasticizer migration.No matter be that light wax oil or plasticizer-containing polyurethane gle all can cause underwater environment in various degree to pollute after breakage is run off.
Polysiloxane molecule is the chain-like structure that is repeated to form by Si-O key unit, and its bond energy is 443.5kJ/mol, high more a lot of than C-C bond energy 355kJ/mol.Polysiloxane has volution molecular configuration, and its intermolecular forces is less, thereby has good resiliency and shape restorability, and the introducing of polysiloxane molecule segment can improve the shock-absorbing capacity of material and reduce compressive set.
Because polysiloxane molecule segment and polyurethane(s) segment solubility parameters differ greatly, consistency is poor, directly adopts physical blending mode to have serious being separated.In order to improve both consistencies, can make polysiloxane be incorporated in polyurethane(s) macromole by chemical bonded refractory.Polysiloxane and polyester or polyether glycol can be used as to soft section jointly participates in polyurethane(s) chemical reaction.But the low surface energy of polysiloxane makes its segment easily migrate to the interface of air-polymkeric substance, causes the degree of being separated serious, surperficial organosilicon segment number is increased, surface free energy lowers.Polysiloxane molecule chain is longer, and polysiloxane silicon segment is more easily to surface transport, and the degree that is separated is larger, and surperficial silicon segment number is increased.Otherwise polysiloxane molecule chain is shorter, the degree that is separated is less, and polysiloxane silicon segment is difficult for to surface transport.
Summary of the invention
In order to overcome the deficiencies in the prior art, a kind of polysiloxane-polyurethane(s) gel material and preparation method thereof is proposed, described material is the polysiloxane-polyurethane(s) gel material that can be used for the vibration and noise reducing buffer reagent of underwater sound device, this material has good environment friendly, there is good resiliency, life-time service is without plasticizer migration and ooze out, and compressed shape diminishes.
Technical scheme of the present invention is: a kind of polysiloxane-polyurethane(s) gel material and preparation method thereof, polysiloxane-polyurethane(s) gel material is comprised of semi prepolymer A, hydroxyl polymer-containing, catalyzer and the auxiliary agent containing short chain polysiloxane, the preparation method of polysiloxane-polyurethane(s) gel material comprises two steps, first step is that semi prepolymer A is synthetic, and second step is material preparation; In the polysiloxane-polyurethane(s) gel material making, each components in mass portion number is; Semi prepolymer A 30-60 part, hydroxyl polymer-containing 200-600 part, semi prepolymer A is 1.08-1.3 with the ratio of the functionality of hydroxyl polymer-containing, is preferably 1.1-1.2; Described catalyzer and the consumption of auxiliary agent are respectively 0.01-1% and the 0.5-2% of hydroxyl polymer-containing quality;
Described first step semi prepolymer A is synthetic is by the polysiloxane containing following general formula (1)
With the di-isocyanate reaction of following general formula (2),
OCN-X-NCO (2)
Make the semi prepolymer A containing isocyanate groups containing following general formula (3).
Concrete preparation method is, in the reaction vessel that can heat and stir, as general formula (1) polysiloxane 30-60 part, under 60 ℃ of-90 ℃ of conditions and as vulcabond 70-160 part of general formula (2), stirring reaction 1-3h, the isocyanate terminated base semi prepolymer A that to prepare isocyanate group relative mass percentage composition be 15%-25%.
Wherein, R
1for CH
3, CH
2cH
3, CH
2cH
2cH
3, CH (CH
3)
2in a kind of;
R
2for CH
3, CH
2cH
3, CH
2cH
2cH
3, CH (CH
3)
2in a kind of;
R
1and R
2can be the same or different;
R
3for CH
2cH
2, CH
2cH
2cH
2, CH
2cH (CH
3), CH
2cH
2cH
2cH
2, CH
2cH (CH
3) CH
2in a kind of;
R
4for CH
2cH
2, CH
2cH
2cH
2, CH
2cH (CH
3), CH
2cH
2cH
2cH
2, CH
2cH (CH
3) CH
2in a kind of;
R
3and R
4can be the same or different;
N is more than or equal to 1 to be less than or equal to 8 integer;
In semi prepolymer A, the quality percentage composition of isocyanic ester is 15%-25%;
Vulcabond is one or more of tolylene diisocyanate, diphenylmethanediisocyanate, isophorone diisocyanate, dicyclohexyl methane diisocyanate, carbodiimide-uretonimine-modified diphenylmethanediisocyanate, urethane-modified diphenylmethanediisocyanate, Methylcyclohexyl diisocyanate, tetramethyl-mphenylenedimethylim-vulcabond, xylylene diisocyanate, hexamethylene diisocyanate, PPDI.
The preparation of described second step material be the semi prepolymer A containing isocyanic ester that synthesizes of first step and hydroxyl polymer-containing under the effect of catalyzer and auxiliary agent, high-speed stirring mixes, pours into a mould and prepare polysiloxane-polyurethane(s) gel material.
Wherein in the polysiloxane-polyurethane(s) gel material making, each components in mass portion number is: semi prepolymer A30-60 part, hydroxyl polymer-containing 200-600 part, be mass fraction, and the ratio of the functionality of semi prepolymer A, hydroxyl polymer-containing is 1.08-1.3, be preferably 1.1-1.2.Described catalyzer and the consumption of auxiliary agent are respectively 0.01-1% and the 0.5-2% of hydroxyl polymer-containing quality.
Hydroxyl polymer-containing is the mixture of relative molecular mass scope 600～8000, functionality 2～5, the polyether glycol that contains two or more, polyester polyol, polyolefin polyhydric alcohol.Described polyether glycol is preferably one or more of polyoxypropyleneglycol, polyoxytrimethylene triol, polyoxytrimethylene tetrol, Polyoxyethylene glycol, polytetrahydrofuran diol, diethylenetriamine polyethers pentol, Xylitol polyethers pentol.Described polyester polyol is preferably one or more of hexylene glycol polyester glycol, poly-phthalic acid glycol ether esterdiol, polycaprolactone glycol, polycaprolactonetriol.Described polyolefin polyhydric alcohol is preferably one or more of hydroxy-terminated polybutadienes, terminal hydroxy group epoxidized polybutadiene.
Catalyzer is two or more the mixture in amine, organic tin, organo-bismuth class, organic zinc class.Described amine is preferably one or more of triethylenediamine, cyclohexyl methyl tertiary amine, tetramethyl-Alkylenediamine, trimethylammonium hydroxyethylethylene diamine, dimethylcyclohexylamine, and described organic tin is preferably one or more of dibutyl tin laurate, two (dodecyl sulphur) dibutyl tin, dibutyltin diacetate, two (1-oxygen iso-octyl oxygen) dibutyl tin, two tetradecanoic acid dibutyl tins.Described organo-bismuth class is preferably isocaprylic acid bismuth.Described organic zinc class is preferably isocaprylic acid zinc.
Auxiliary agent is defoamer, flow agent and water-removal agent.Described defoamer is preferably organosilicon and modified polyorganosiloxane defoamer.Described flow agent is preferably polyacrylate flow agent.Described water-removal agent is preferably molecular sieve desiccant.
Beneficial effect of the present invention is:
1) polysiloxane-polyurethane(s) gel material is not containing any softening agent, introduce short chain polysiloxane, strengthened resiliency, compressed shape change is little, and organic compound all participates in the chemical reaction of gelinite formation, form cross-linked macromolecular gelinite, after long-time use, can not ooze out and move, there is environment friendly well.
2) technical process of the present invention is clear, and preparation method is practical.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.The umber of following component is mass fraction.
Embodiment mono-
Get 50 parts of the polydimethylsiloxanes of molecular weight 730,116 parts of diphenylmethanediisocyanates, 80 ℃ of stirring reaction 2h, preparing isocyanate content is 20% semi prepolymer A.
Get 10 parts of 40 parts of semi prepolymer A, 550 parts of polyoxypropyleneglycols that relative molecular mass is 8000, polyoxytrimethylene tetrols that relative molecular mass is 1200,0.8 part of dibutyl tin laurate, isocaprylic acid bismuth 0.4,1.0 parts of trimethylammonium hydroxyethylethylene diamine, 2.2 parts of modified polyorganosiloxane defoamers, 3.1 parts of polyacrylate flow agents.Be uniformly mixed casting.
After 7 days, reach optimum performance, without oozing out, VLRH hardness is 40, and permanent compression set is 4.1%, and falling-rebounding ball is 22.
Embodiment bis-
Get in embodiment mono-16 parts of semi prepolymer A40 part of preparation, 310 parts of polyoxypropyleneglycols that relative molecular mass is 6000,20 parts of polytetrahydrofuran diols that relative molecular mass is 2000, polyoxytrimethylene triols that relative molecular mass is 600,1.0 parts of two tetradecanoic acid dibutyl tins, triethylenediamine 0.6,1.5 parts of silicone antifoam agents, 3 parts of molecular sieve desiccants, 1.3 parts of polyacrylate flow agents.Be uniformly mixed casting.
After 7 days, reach optimum performance, without oozing out, VLRH hardness is 33, and permanent compression set is 5.1%, and falling-rebounding ball is 18.
Embodiment tri-
Get 40 parts of the polydiethylsiloxanes of molecular weight 540,40 parts of diphenylmethanediisocyanates, 60 parts of tolylene diisocyanates, 90 ℃ of stirring reaction 2h, preparing isocyanate content is 25% semi prepolymer A.
Get 410 parts of the polyoxypropyleneglycols of 50 parts of semi prepolymer A, relative molecular mass 5000,30 parts of the polycaprolactonetriols of relative molecular mass 1000,8 parts of the Xylitol polyethers pentols of relative molecular mass 1000,1.4 parts of two (dodecyl sulphur) dibutyl tins, 1.0 parts of cyclohexyl methyl tertiary amines, 1.8 parts of modified polyorganosiloxane defoamers, 2.2 parts of molecular sieve desiccants, 1.6 parts of polyacrylate flow agents.Be uniformly mixed casting.
After 7 days, reach optimum performance, without oozing out, VLRH hardness is 42, and permanent compression set is 3.9%, and falling-rebounding ball is 28.
Embodiment tetra-
Get 60 parts of the polydimethylsiloxanes of molecular weight 288,15 parts of diphenylmethanediisocyanates, 38 parts of hexamethylene diisocyanates, 28 parts of PPDI, 80 ℃ of stirring reaction 2h, preparing isocyanate content is 15% semi prepolymer A.
Get 160 parts of the polyoxypropyleneglycols of 50 parts of semi prepolymer A, relative molecular mass 4000,30 parts of the polyoxytrimethylene triols of relative molecular mass 3000,30 parts of the polytetrahydrofuran diols of relative molecular mass 2000,15 parts of the polyoxytrimethylene triols of relative molecular mass 1200,0.9 part of two (dodecyl sulphur) dibutyl tin, 0.7 part of cyclohexyl methyl tertiary amine, 1.5 parts of modified polyorganosiloxane defoamers, 2.0 parts of molecular sieve desiccants, 1.5 parts of polyacrylate flow agents.Be uniformly mixed casting.
After 7 days, reach optimum performance, without oozing out, VLRH hardness is 37, and permanent compression set is 3.6%, and falling-rebounding ball is 25.
Although very described the described in the text invention of protecting with claim in detail with reference to some embodiment; but it will be understood by those skilled in the art that the present invention who protects with claim described in literary composition can realize by other embodiment those embodiment except for illustration purpose.The description of the embodiment that the spirit and scope of claims should not be limited to comprise in literary composition.
Claims (6)
1. the preparation method of polysiloxane-polyurethane(s) gelinite, it is characterized in that: polysiloxane-polyurethane(s) gel material is comprised of semi prepolymer A, hydroxyl polymer-containing, catalyzer and the auxiliary agent containing short chain polysiloxane, the preparation method of polysiloxane-polyurethane(s) gel material comprises two steps, first step is that semi prepolymer A is synthetic, and second step is material preparation; In the polysiloxane-polyurethane(s) gel material making, each components in mass portion number is: semi prepolymer A 30-60 part, hydroxyl polymer-containing 200-600 part, semi prepolymer A is 1.08-1.3 with the ratio of the functionality of hydroxyl polymer-containing, and described catalyzer and the consumption of auxiliary agent are respectively 0.01-1% and the 0.5-2% of hydroxyl polymer-containing quality;
Described first step semi prepolymer A is synthetic is by the polysiloxane containing following general formula
React with the vulcabond containing following general formula,
OCN-X-NCO
Make the semi prepolymer A containing isocyanate groups containing following general formula;
Wherein, R
1for CH
3, CH
2cH
3, CH
2cH
2cH
3, CH (CH
3)
2in a kind of;
R
2for CH
3, CH
2cH
3, CH
2cH
2cH
3, CH (CH
3)
2in a kind of;
R
3for CH
2cH
2, CH
2cH
2cH
2, CH
2cH (CH
3), CH
2cH
2cH
2cH
2, CH
2cH (CH
3) CH
2in a kind of;
R
4for CH
2cH
2, CH
2cH
2cH
2, CH
2cH (CH
3), CH
2cH
2cH
2cH
2, CH
2cH (CH
3) CH
2in a kind of;
N is more than or equal to 1 to be less than or equal to 8 integer;
Vulcabond is a kind of of tolylene diisocyanate, diphenylmethanediisocyanate, isophorone diisocyanate, dicyclohexyl methane diisocyanate, carbodiimide-uretonimine-modified diphenylmethanediisocyanate, urethane-modified diphenylmethanediisocyanate, Methylcyclohexyl diisocyanate, tetramethyl-mphenylenedimethylim-vulcabond, xylylene diisocyanate, hexamethylene diisocyanate, PPDI;
The concrete preparation method of this step is, in the reaction vessel that can heat and stir, by described polysiloxane 30-60 part, under 60 ℃ of-90 ℃ of conditions with described vulcabond 70-160 part, stirring reaction 1-3 hour, preparing relative mass percentage composition is the isocyanate group semi prepolymer A of 15%-25%;
Second step: the semi prepolymer A containing isocyanic ester that first step is synthesized and hydroxyl polymer-containing are under the effect of catalyzer and auxiliary agent, and high-speed stirring mixes, pours into a mould and prepare polysiloxane-polyurethane(s) gel material;
Wherein in the polysiloxane-polyurethane(s) gel material making, each components in mass portion number is: semi prepolymer A 30-60 part, hydroxyl polymer-containing 200-600 part, and the ratio of the functionality of semi prepolymer A, hydroxyl polymer-containing is 1.1-1.2, described catalyzer and the consumption of auxiliary agent are respectively 0.01-1% and the 0.5-2% of hydroxyl polymer-containing quality in hydroxyl polymer-containing;
Hydroxyl polymer-containing is relative molecular mass scope 600 ~ 8000, functionality 2 ~ 5, the polyether glycol that contains two or more, polyester polyol, the mixture of polyolefin polyhydric alcohol, described polyether glycol is preferably polyoxypropyleneglycol, polyoxytrimethylene triol, polyoxytrimethylene tetrol, Polyoxyethylene glycol, polytetrahydrofuran diol, diethylenetriamine polyethers pentol, Xylitol polyethers pentol a kind of, described polyester polyol is hexylene glycol polyester glycol, poly-phthalic acid glycol ether esterdiol, polycaprolactone glycol, polycaprolactonetriol a kind of, described polyolefin polyhydric alcohol is hydroxy-terminated polybutadienes, terminal hydroxy group epoxidized polybutadiene a kind of,
Catalyzer is two or more the mixture in amine, organic tin, organo-bismuth class, organic zinc class, described amine is a kind of of triethylenediamine, cyclohexyl methyl tertiary amine, tetramethyl-Alkylenediamine, trimethylammonium hydroxyethylethylene diamine, dimethylcyclohexylamine, and described organic tin is a kind of of dibutyl tin laurate, dibutyltin diacetate, two dibutyl tins, dibutyl tin bis, two tetradecanoic acid dibutyl tins; Auxiliary agent is defoamer, flow agent and water-removal agent.
2. the preparation method of polysiloxane-polyurethane(s) gelinite according to claim 1, is characterized in that: described defoamer is modified polyorganosiloxane defoamer.
3. the preparation method of polysiloxane-polyurethane(s) gelinite according to claim 1 and 2, is characterized in that: described flow agent is polyacrylate flow agent.
4. the preparation method of polysiloxane-polyurethane(s) gelinite according to claim 1 and 2, is characterized in that: described water-removal agent is molecular sieve desiccant.
5. the preparation method of polysiloxane-polyurethane(s) gelinite according to claim 1 and 2, is characterized in that: described organic zinc class is isocaprylic acid zinc.
6. the preparation method of polysiloxane-polyurethane(s) gelinite according to claim 1 and 2, is characterized in that: described organo-bismuth class is isocaprylic acid bismuth.
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| CN103360562B (en) * | 2013-03-21 | 2015-09-30 | 哈尔滨工程大学 | A kind of Polysiloxane-polyuregelolyurethane gelolyurethane material and preparation method thereof |
| CN103709412B (en) * | 2013-12-27 | 2016-04-20 | 成都硅宝科技股份有限公司 | Hybrid organosilicon thermoplastic elastomer and preparation method thereof |
| CN105017496B (en) * | 2014-04-28 | 2017-10-10 | 北京化工大学 | A kind of gradient polymeric organic silicon nano gel, preparation method and the usage |
| CN105482053B (en) * | 2015-12-18 | 2017-11-17 | 安徽优特公路养护科技有限公司 | A kind of airfield runway basic unit damage repair high polymer grouting material |
| FR3055899B1 (en) * | 2016-09-13 | 2020-09-11 | Valeo Systemes De Controle Moteur | SOLVENT FREE SYNTHESIS OF SILICONE / POLYURETHANE MATERIALS |
| CN108610466B (en) * | 2018-05-17 | 2021-04-06 | 山东大学 | Polyurea elastomer with polysiloxane completely replacing polyether and preparation method thereof |
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| EP1338615A2 (en) * | 2002-02-23 | 2003-08-27 | Goldschmidt AG | Branched polyurethane, formulations containing these and their use in thickening aqueous systems |
| CN101280104A (en) * | 2008-05-07 | 2008-10-08 | 北京理工大学 | Polymer electrolyte |
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Denomination of invention: Polysiloxane-polyurethane gel material and preparation method thereof Effective date of registration: 20141127 Granted publication date: 20140813 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: Qingdao Advanced Marine Material Technology Co., Ltd. Registration number: 2014990000998 |
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Address after: 266000 Qingdao science and technology, Huangdao District, Shandong, No. two road, No. 167 Patentee after: Qingdao Advanced Marine Material Technology Co., Ltd. Address before: 266101 No. 143, Zhuzhou Road, Laoshan District, Shandong, Qingdao Patentee before: Qingdao Advanced Marine Material Technology Co., Ltd. |