CN1693363A - Process for synthesizing nano barium titanate/polyurethane elastic composite - Google Patents
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- CN1693363A CN1693363A CN 200510040280 CN200510040280A CN1693363A CN 1693363 A CN1693363 A CN 1693363A CN 200510040280 CN200510040280 CN 200510040280 CN 200510040280 A CN200510040280 A CN 200510040280A CN 1693363 A CN1693363 A CN 1693363A
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Abstract
A process for synthesizing the electrostrictive nano-barium carbonate/polyurethane elastomer compound includes such steps as proportionally mixing nano-barium carbonate, solvent and coupling agent, adding it to polyester polyol, adding isocyanate and cross-linking agent, polymerizing and high-temp solidifying.
Description
Technical field
The present invention relates to the synthetic method of the nano barium phthalate/polyurethane elastic composite of tool electrostrictive property.
Background technology
Polyurethane(s) (being called for short urethane Polyurethane) because of the carbamate groups-NH-COO-in its macromolecular main chain gains the name, is a kind of superpolymer with special performance and many-sided purposes.A kind of as urethane resin, polyurethane elastomer is a kind of high molecular polymer between General Purpose Rubber and rigid plastic.It had both had the high strength of plastics, the elasticity and the toughness that have rubber again, under high rigidity, still keep elasticity, under the soft state, also has higher physical strength, and have abrasion performance, oil resistant, tear-resistant, resistance to chemical attack, anti-x radiation x,, snappiness good with other material cementabilities, excellent properties such as the strong and good biocompatibility of vibration absorption ability.
People (J.Appl.Sci. such as Newman in 1994, Part B:Polym.Phys., 1994,32:2721-2731) find first, under powerful extra electric field effect, polyurethane elastomer can produce very large electric field and induce strain, and the quadratic term of this strain ratio and external electric field intensity.Find that through the research back Electrostrictive Response in Polyurethane Elastomers is to cause the main factor of this strained.Compared to inorganic piezoelectric ceramics and other piezopolymers, the specific acoustic resistance that polyurethane elastomer is lower, good mechanical flexibility, good processing properties and cheap tooling cost make it can be applied to acoustical device and transverter especially; And its strain-responsive characteristics greatly very fast, at manufacture of intraocular muscle with control and also can well be used with aspects such as driving mechanisms.But the specific inductivity of comparing polyurethane elastomer with piezoelectric ceramics is lower, and is dynamo-electric active in piezoceramic material, makes it in application facet some restrictions arranged.
Inorganic nano-organic polymer composite material not only can have the feature and the character of inorganic materials and organic polymer concurrently, as toughness, ductility and the workability of thermotolerance, high-temperature stability, low thermal coefficient of expansion and the organic polymer of inorganic materials; And, often can also promptly strengthen and toughness reinforcing because the disperse phase of nanoscale has increased interfacial interaction greatly.Compound on nanometer and molecular level of organic polymer and inorganics will make separately advantage obtain the embodiment of fullest.Nano composite material be after single component material, matrix material, function-graded material the 4th generation material.Piezoelectric ceramics has very big specific inductivity, if carry out nano level piezoceramic material and polyurethane elastomer compound, just can improve the dielectric properties of polyurethane elastomer, make the matrix material of excellent combination property, and can improve the electrostrictive property of material.Liu Chunxiao, people such as Zhu Guozhen utilize two rollers to prepare a series of Pb-based lanthanumdoped zirconate titanatess (PZT)/polyurethane elastomer (PU) mixture (functional polymer journal, 2001,14 (3): 311-314).The Young's modulus of mixture and specific inductivity increase and increase along with PZT content.When low PZT content, the Young's modulus of mixture increases very fast, increases more remarkable when high PZT content.In the mixture, PZT has limited the recoverable deformation of PU, makes mixture have higher mechanical property.The electricity of pure PU and 2vol%PZT mixture causes stress and follows the relation that simply equals strength of electric field square, and electric field induced strain presents shrinkage phenomenon.
In existing dielectric materials, the barium titanate with perovskite structure is one of dielectric ceramic that has high-k.And nano barium phthalate ratio nano PZT is easier to preparation, and also has similar ferroelectric, piezoelectric property.Therefore, as a kind of electrostriction material nano barium phthalate/polyurethane elastic composite bright development prospect is arranged.
Summary of the invention
The objective of the invention is to propose a kind of method that can synthesize nano barium phthalate/polyurethane elastic composite that a kind of technology is simple, preparation process is convenient to operate with excellent dielectric properties and electrostrictive property.By the directly synthetic nano barium phthalate/polyurethane elastic composite of providing electrostrictive property of the synthetic method commonly used of using polyurethane elastomer.
For achieving the above object, the present invention proposes a kind of method of synthetic tool electrostrictive property nano barium phthalate/polyurethane elastic composite, this method forms suspension liquid by nano barium phthalate is mixed with solvent, coupling machine, directly add in the polyurethane elastomer synthesis material polyester polyol, add isocyanic ester and linking agent direct polymerization, at high temperature solidify and get.Its processing step is as follows:
(1) nano level metatitanic acid barium powder is joined in the good solvent of solubilized polyester and be made into suspension, the mass ratio of barium carbonate powder and solvent is 1/20～1/4;
(2) mass ratio in nano barium carbonate powder in the nano barium carbonate powder suspension and hexanodioic acid kind polyester polyvalent alcohol is the ratio of (0～3/2), the suspension of nano barium carbonate powder is added in the hexanodioic acid kind polyester polyvalent alcohol, be heated to 150 ℃～170 ℃, under the vacuum condition of 100Pa～300Pa, remove solvent;
(3) be cooled to 60 ℃～80 ℃, the linking agent that adding is mixed by glycols chainextender and the agent of trifunctional alcohols side chain, the mol ratio of chainextender and side chain agent is 1/1～1/4 in the mixed cross-linker, and the mol ratio of mixed cross-linker and polyester polyol is 1/2～2/3;
(4) add isocyanic ester, the mol ratio of isocyanic ester and polyester polyol is 3/2～5/2;
(5) all materials are stirred, solidify 4h～10h down, promptly get nano barium phthalate/polyurethane elastic composite at 100 ℃～120 ℃.
Compared with prior art, the present invention has following advantage:
Technology of the present invention is simple, the nano barium carbonate powder that will be dispersed in the building-up process in the solvent directly adds in the reaction raw materials, thereby just nano barium carbonate powder has been dispersed in the elastomerics in the elastomeric while of synthesis of polyurethane, has obtained nano barium phthalate/polyurethane elastic composite.In building-up process, only need the ordinary laboratory instrument to get final product, and need not to adopt complicated experiment equipment such as two roller injection moulding machines etc.In addition, the temperature and pressure conditional request in present method is not high, and need not the free NCO% value at reaction later stage assaying reaction thing.Utilize synthetic method of the present invention can prepare nano barium phthalate/polyurethane elastic composite with more excellent dielectric properties and electrostrictive property.The specific inductivity of material increases than conventional polyurethanes elastomerics (specific inductivity is about 5) more than 7.5, and can adjust the dielectric properties of matrix material by the content of adjusting nano barium phthalate.In addition, the electrostrictive property of material also makes moderate progress than the conventional polyurethanes elastomerics, and its shortens time of response, strain keeps stable, maximum strain can reach 1%～3% under the high pressure.
Description of drawings
Fig. 1 is the specific inductivity of example 1 matrix material and the graph of relation of frequency, and specific inductivity has a peak value (8.3) at about 500Hz place, and the increase specific inductivity along with frequency descends subsequently, can see that its downcurve is level and smooth, linear approximate relationship.
Fig. 2 is the electric field induced strain and the time relation graphic representation of example 1 matrix material, has added the voltage of 5000V among the figure at 60s, 180s and 300s place; Removed impressed voltage at 120s, 240s and 360s place.
Embodiment
The present invention is further described below in conjunction with example:
Embodiment 1
Nano level metatitanic acid barium powder is joined the N that contains coupling agent (coupling dosage be barium titanate powder body weight 1.6%), be made into the suspension liquid of 10% (wt/wt) in the N-dimethylacetamide solution, stir under the room temperature and take out 1ml after 4 hours and join in poly-(hexylene glycol-neopentyl glycol) adipic acid ester polyvalent alcohol (hydroxyl value is 74) of 6.2g, the powerful stirring is heated to 160 ℃ and vacuumizes with the solvent in the system of purifying.Keep breaking of vacuum temperature to 75 ℃, add 0.2728g1,1,1-TriMethylolPropane(TMP) and 0.046ml 1,4-butyleneglycol (the linking agent proportioning is 80%) continues fully to stir.Add the 1.17ml tolylene diisocyanate again, all materials are fully stirred rapidly, pour in the mould, in baking oven, solidify 10h down, slowly reduce to room temperature, promptly get nano barium phthalate/polyurethane elastic composite in 110 ℃.As can be seen from Figure 1 the specific inductivity of gained material and frequency relation are stable, and the specific inductivity maximum value increases, and the maximum dielectric constant is 8.3.From electric field induced strain and time chart, the response of the electric field induced strain of material is fast, and recovery is good, strain stable, and maximum strain is-0.0176 (5000V impressed voltage).
To gather the poly-hexanodioic acid butyleneglycol neopentyl glycol ester polyol that hexanodioic acid hexylene glycol neopentyl glycol ester polyol more has identical relative molecular mass among the embodiment 1, all the other conditions are constant.Gained material maximum dielectric constant is 8.1, and maximum strain is-0.021 (5000V impressed voltage).
With the 1.5ml more of nano barium carbonate powder suspension liquid add-on among the embodiment 1, all the other conditions are constant.The maximum dielectric constant is 8.6, and maximum strain is-0.0152 (5000V impressed voltage).
With tolylene diisocyanate among the embodiment 1 more 4,4 '-diphenylmethanediisocyanate, all the other conditions are constant.The maximum dielectric constant is 8.0, and maximum strain is-0.0186 (5000V impressed voltage).
With among the embodiment 11,4-butyleneglycol more 1, the 6-hexylene glycol, all the other conditions are constant.The maximum dielectric constant is 8.7, and maximum strain is-0.0158 (5000V impressed voltage).
Embodiment 6
With among the embodiment 11,1, the 1-TriMethylolPropane(TMP) is glycerine more, and all the other conditions are constant.The maximum dielectric constant is 8.6, and maximum strain is-0.0108 (5000V impressed voltage).
Embodiment 7
With the poly-more poly-hexanodioic acid hexylene glycol neopentyl glycol ester polyol of hexanodioic acid hexylene glycol neopentyl glycol ester polyol (hydroxyl value is 74) (hydroxyl value is 56) among the embodiment 1, all the other conditions are constant.Gained material maximum dielectric constant is 8.1, and maximum strain is-0.02 (5000V impressed voltage).
Embodiment 8
With the proportioning of mixed cross-linker among the embodiment 1 more 60%, all the other conditions are constant.The maximum dielectric constant is 8.6, and maximum strain is-0.0184 (5000V impressed voltage)
As can be seen, content, the relative molecular mass that changes polyester polyol, the kind that changes polyester polyol that the dielectric properties of matrix material and electrostrictive property can be by changing barium titanate, change the kind of isocyanic ester and change elastomeric cross-linking system and adjust among the above embodiment.
Embodiment 9
A kind of synthetic method with electrostrictive property nano barium phthalate/polyurethane elastic composite:
(1) nano level metatitanic acid barium powder is joined in the good solvent of solubilized polyester and be made into suspension, the mass ratio of barium carbonate powder and solvent is 1/20～1/4, as: can adopt 1/20,1/4,1/7,1/12 or 1/18 mass ratio;
(2) mass ratio in nano barium carbonate powder in the nano barium carbonate powder suspension and hexanodioic acid kind polyester polyvalent alcohol is the ratio of (0～3/2), the suspension of nano barium carbonate powder is added in the hexanodioic acid kind polyester polyvalent alcohol, be heated to 150 ℃～170 ℃ (as: 150 ℃, 170 ℃ or 161 ℃), under the vacuum condition of 100Pa～300Pa (as: 100Pa, 300Pa, 130Pa, 240Pa), remove solvent;
(3) be cooled to 60 ℃～80 ℃, present embodiment adds the linking agent that is mixed by glycols chainextender and the agent of trifunctional alcohols side chain down at 60 ℃, 80 ℃, 70 ℃ or 75 ℃, the mol ratio of chainextender and side chain agent is 1/1～1/4 in the mixed cross-linker, specifically can select 1/1,1/4,1/2 or 1/3, the mol ratio of mixed cross-linker and polyester polyol is 1/2～2/3, specifically can select 1/2,2/3 or 11/20;
(4) add isocyanic ester, the mol ratio of isocyanic ester and polyester polyol is 3/2～5/2, as: 3/2,5/2 or 4/2;
(5) all materials are stirred, solidify 4h～10h down at 100 ℃～120 ℃, promptly get nano barium phthalate/polyurethane elastic composite, concrete set time and temperature can be selected: 100 ℃ solidify 4h down, and 120 ℃ solidify 10h down, and 108 ℃ solidify 7h down.
In the present embodiment, described solvent is N, N-N,N-DIMETHYLACETAMIDE or N-Methyl pyrrolidone, described polyester polyol is poly-hexanodioic acid hexylene glycol neopentyl glycol ester polyol, poly-hexanodioic acid butyleneglycol neopentyl glycol ester polyol, the polyneopentyl glycol adipate polyvalent alcohol, poly-adipate glycol neopentyl glycol ester polyol or poly-hexanodioic acid hexylene glycol ester polyol, described glycols chainextender is an ethylene glycol, propylene glycol, 1,4-butyleneglycol or hexylene glycol, the agent of described trifunctional alcohols side chain is glycerine or 1,1, the 1-TriMethylolPropane(TMP), described mixed cross-linker mixes for any one glycols chainextender and any one trifunctional alcohols side chain agent, described isocyanic ester is 2, the 4-tolylene diisocyanate, 2, the 6-tolylene diisocyanate, 4,4 '-diphenylmethanediisocyanate or hexamethylene diisocyanate, the temperature of described adding mixed cross-linker is 70 ℃～80 ℃, optimum temps is 70 ℃～75 ℃, best curing temperature is 110 ℃, optimum curing time is 6h, and the typical case mole proportioning of polyester polyol in the described system and isocyanic ester is 1/2, and total in the system-NCO is 1.05/1 with the typical ratio of-OH.
Claims (8)
1. synthetic method with electrostrictive property nano barium phthalate/polyurethane elastic composite is characterized in that:
(1) nano level metatitanic acid barium powder is joined in the good solvent of solubilized polyester and be made into suspension, the mass ratio of barium carbonate powder and solvent is 1/20～1/4;
(2) mass ratio in nano barium carbonate powder in the nano barium carbonate powder suspension and hexanodioic acid kind polyester polyvalent alcohol is the ratio of (0～3/2), the suspension of nano barium carbonate powder is added in the hexanodioic acid kind polyester polyvalent alcohol, be heated to 150 ℃～170 ℃, under the vacuum condition of 100Pa～300Pa, remove solvent;
(3) be cooled to 60 ℃～80 ℃, the linking agent that adding is mixed by glycols chainextender and the agent of trifunctional alcohols side chain, the mol ratio of chainextender and side chain agent is 1/1～1/4 in the mixed cross-linker, and the mol ratio of mixed cross-linker and polyester polyol is 1/2～2/3;
(4) add isocyanic ester, the mol ratio of isocyanic ester and polyester polyol is 3/2～5/2;
(5) all materials are stirred, solidify 4h～10h down, promptly get nano barium phthalate/polyurethane elastic composite at 100 ℃～120 ℃.
2. according to the synthetic method of the described nano barium phthalate/polyurethane elastic composite of claim 1, it is characterized in that: described solvent is N,N-dimethylacetamide or N-Methyl pyrrolidone.
3. according to the synthetic method of the described nano barium phthalate/polyurethane elastic composite of claim 1, it is characterized in that: described polyester polyol is poly-hexanodioic acid hexylene glycol neopentyl glycol ester polyol, poly-hexanodioic acid butyleneglycol neopentyl glycol ester polyol, polyneopentyl glycol adipate polyvalent alcohol, poly-adipate glycol neopentyl glycol ester polyol or poly-hexanodioic acid hexylene glycol ester polyol.
4. according to the synthetic method of the described nano barium phthalate/polyurethane elastic composite of claim 1, it is characterized in that: described glycols chainextender is ethylene glycol, propylene glycol, 1,4-butyleneglycol or hexylene glycol, the agent of described trifunctional alcohols side chain is glycerine or 1,1, the 1-TriMethylolPropane(TMP), described mixed cross-linker mixes for any one glycols chainextender and any one trifunctional alcohols side chain agent.
5. according to the synthetic method of the described nano barium phthalate/polyurethane elastic composite of claim 1, it is characterized in that: described isocyanic ester is a 2,4 toluene diisocyanate, 2, the 6-tolylene diisocyanate, 4,4 '-diphenylmethanediisocyanate or hexamethylene diisocyanate.
6. according to the synthetic method of the described barium titanate/polyurethane elastic composite of claim 1, it is characterized in that: the temperature of described adding mixed cross-linker is 70 ℃～80 ℃, and optimum temps is 70 ℃～75 ℃.
7. according to the synthetic method of the described nano barium phthalate/polyurethane elastic composite of claim 1, it is characterized in that: best curing temperature is 110 ℃, and optimum curing time is 6h.
8. according to the synthetic method of the described nano barium phthalate/polyurethane elastic composite of claim 1, it is characterized in that: the typical case mole proportioning of polyester polyol in the described system and isocyanic ester is 1/2, and total in the system-NCO is 1.05/1 with the typical ratio of-OH.
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| CN103146179A (en) * | 2013-04-01 | 2013-06-12 | 北京化工大学 | Polyurethane elastomer composite material with low modulus and high dielectric constant, and preparation method of composite material |
| CN103547548A (en) * | 2011-03-23 | 2014-01-29 | 密苏里大学学监 | High dielectric constant composite materials and methods of manufacture |
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| CN105061713A (en) * | 2015-07-22 | 2015-11-18 | 东莞市吉鑫高分子科技有限公司 | Thermoplastic polyurethane elastomer with electrostrictive property, preparation method therefor and application thereof |
| CN107141770A (en) * | 2017-06-26 | 2017-09-08 | 俞秀英 | A kind of electrostrictive composite and its preparation method and application |
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| CN103547548A (en) * | 2011-03-23 | 2014-01-29 | 密苏里大学学监 | High dielectric constant composite materials and methods of manufacture |
| CN103146179A (en) * | 2013-04-01 | 2013-06-12 | 北京化工大学 | Polyurethane elastomer composite material with low modulus and high dielectric constant, and preparation method of composite material |
| CN104987701A (en) * | 2015-07-22 | 2015-10-21 | 东莞市雄林新材料科技股份有限公司 | Electrostrictive TPU film and preparation method and application thereof |
| CN105061713A (en) * | 2015-07-22 | 2015-11-18 | 东莞市吉鑫高分子科技有限公司 | Thermoplastic polyurethane elastomer with electrostrictive property, preparation method therefor and application thereof |
| CN108084696A (en) * | 2016-11-22 | 2018-05-29 | 阿托姆公开有限公司 | For the composite material with electrostrictive property of mechanical energy retracting device |
| CN107141770A (en) * | 2017-06-26 | 2017-09-08 | 俞秀英 | A kind of electrostrictive composite and its preparation method and application |
| US20210093232A1 (en) * | 2019-09-30 | 2021-04-01 | University-Industry Foundation (Uif), Yonsei University | Liquid information sensor and method of driving the same |
| US11696709B2 (en) * | 2019-09-30 | 2023-07-11 | University-Industry Foundation (Uif), Yonsei University | Liquid information sensor and method of driving the same |
| CN110819103A (en) * | 2019-11-01 | 2020-02-21 | 李昌龙 | TPU acoustic film and preparation method thereof |
| CN111410748A (en) * | 2020-01-08 | 2020-07-14 | 苏州星烁纳米科技有限公司 | Perovskite quantum dot composition and preparation method thereof, perovskite quantum dot film and preparation method thereof |
| CN111410748B (en) * | 2020-01-08 | 2022-10-18 | 苏州星烁纳米科技有限公司 | Perovskite quantum dot composition and preparation method thereof, perovskite quantum dot film and preparation method thereof |
| CN115368534A (en) * | 2022-09-26 | 2022-11-22 | 四川大学 | High-electrostriction polyurethane elastomer and forming method thereof |
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