CN105885005A - Preparation method of polyurethane elastomer material - Google Patents
Preparation method of polyurethane elastomer material Download PDFInfo
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- CN105885005A CN105885005A CN201610459034.6A CN201610459034A CN105885005A CN 105885005 A CN105885005 A CN 105885005A CN 201610459034 A CN201610459034 A CN 201610459034A CN 105885005 A CN105885005 A CN 105885005A
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- CN
- China
- Prior art keywords
- polyurethane elastomer
- preparation
- elastomer material
- chain extender
- room temperature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/69—Polymers of conjugated dienes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
Abstract
The invention discloses a preparation method of a polyurethane elastomer material. The preparation method includes placing a HTBN (hydroxyl-terminated butadiene-acrylonitrile copolymer) into a four-neck flask, and removing water for 2-3 hours at 100-110 DEG C under vacuum; decreasing the temperature to the room temperature, adding isocyanate and reacting for 2-3 hours in the atmosphere of nitrogen; adding a chain extender when the temperature is decreased to the room temperature again, and reacting for 1-2 hours at 60-70 DEG C; placing all the materials into a mould after reaction is terminated, conducting hot press molding and curing in a drying oven at 90-100 DEG C for 20-24 hours so as to obtain the polyurethane elastomer material. The polyurethane elastomer material prepared by the preparation method is high in permittivity and excellent in mechanical property.
Description
Technical field
The present invention relates to polyurethane material technical field, particularly relate to the preparation method of a kind of polyurethane elastomer material.
Background technology
At the electroactive polymer (electroactive polymer, EAP) that the nineties in 20th century progressively grows up,
Its characteristic is that big change of shape occurs under electricity irritation, and this makes many scientists and research worker be devoted to transform EAP
Material, and expand the range of application of macromolecular material.The behavioral pattern of EAP material is similar to biological muscles, has high disconnected
The features such as fragility, intrinsic vibration damping, big actuation performance, therefore, often as the synonym of " artificial-muscle ".
EAP material can provide bigger strain than Conventional piezoelectric pottery, can be usually reached the strain deformation of 380%, and domestic also have
The similar experimental verification large strain deformation of this degree, under same strained condition, EAP is applicable to more apply to be needed
Ask.
In general, EAP material can be divided into electron type EAP and ion-type EAP, has different behavioral pattern.Such as electronics
The driving of type EAP is to utilize electric field or Coulomb force, can be divided into electrostriction elastomer, dielectric elastomer, ferroelectric polymers；
The driving principle of ion-type EAP is to utilize diffusion or the migration of ion, has CNT, conducting polymer, polymer solidifying
The kind such as glue, ion polymer-metal composite material, different types of EAP material has different excellent, shortcomings, thus
Apply in different occasions.Wherein, belong to electron type EAP dielectric elastomer material (dielectric elastomer,
DE) it is widely used in actuator, sensor, electromotor etc., there is good application performance.
The method improving elastomer dielectric constant in prior art mainly has two kinds: one to be normal by filling high consumption high dielectric
The ceramic packing of number, such as lead magnesio-niobate (PMN), lanthanum zirconium titanium acid lead.But fill ceramic body filler in a large number and make elasticity
The modulus of body improves, and reduces pliability and the mechanical deformation ability of elastomer, and composite material shaping process also compares
Difficulty, it is difficult to being prepared as micron-sized thin film, fault in material also compares many, is easily caused electrical breakdown.All these defects
Processing with the elastomer of ceramic filler and serviceability are reduced；One is to fill conductor or semiconductor fills.
Such as: nano-silver thread, Graphene, CNT etc..When the content of conducting particles reaches percolation threshold, material meeting
There is transformation from insulator to conductor, but when conducting particles content is close to excess effusion value but when being not reaching to excess effusion value, be situated between
Electric constant can reach maximum, and this is caused by electron displacement polarization；When conducting particles content oozes up to or over exceeding
During value, the spacing of conducting particles diminishes, and migrates between particle, forms conductive path, thus causes bigger dielectric to be damaged
Consumption, electric breakdown strength reduces, and material is destroyed.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of polyurethane elastomer material, elastic polyurethane prepared by the method
Body material has the highest dielectric constant and mechanical property.
A kind of preparation method of polyurethane elastomer material, described method includes:
The hycar (HTBN) of terminal hydroxy group is put in four-hole boiling flask, at 100-under vacuum condition
110 DEG C are removed water 2-3h；
Treat that temperature drops to room temperature, add carbimide, and react 2-3h in a nitrogen atmosphere；
When temperature drops to room temperature again, add chain extender, and at 60-70 DEG C, react 1～2h；
After the completion of reaction resulting materials is put in mould, hot-forming after be put in the baking oven of 90-100 DEG C solidification 20-
24h, obtains described polyurethane elastomer material.
Each raw-material mass fraction is used to be respectively as follows:
The carbimide of the HTBN of 80-88 part, 6-10 part, and the chain extender of 6-10 part, and above-mentioned each raw-material total part
Number is 100.
Described carbimide includes: hexamethylene diisocyanate (HDI), liquefaction 4,4 '-diphenyl methane two isocyanide
Acid esters (L-MDI) or toluene di-isocyanate(TDI) (TDI).
Described chain extender is 1,4-butanediol BDO.
As seen from the above technical solution provided by the invention, the polyurethane elastomer material prepared by said method has
The highest dielectric constant and mechanical property.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, required use in embodiment being described below
Accompanying drawing is briefly described, it should be apparent that, the accompanying drawing in describing below is only some embodiments of the present invention, for
From the point of view of those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain according to these accompanying drawings
Other accompanying drawings.
Fig. 1 is the preparation method schematic flow sheet of polyurethane elastomer material described in the embodiment of the present invention；
Fig. 2 is lifted the relation schematic diagram of three example test gained dielectric constants and frequency by the present invention；
Fig. 3 is lifted the relation between three example test gained stress and strains by the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly and completely
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on
Embodiments of the invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise
Embodiment, broadly falls into protection scope of the present invention.
Method described in the embodiment of the present invention is by being modified nitrile rubber so that it is strand two ends are hydroxyl, with isocyanide
Acid esters and dihydroxylic alcohols generation chemical reaction, the synthesis polyurethane elastomeric materials containing polar group, the addition of polar group,
The motor capacity and the polarizability that make strand are greatly enhanced, it is possible to the effective dielectric constant improving polyurethane material.
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail, is illustrated in figure 1 described in the embodiment of the present invention poly-
The preparation method schematic flow sheet of urethane elastomeric material, described method includes:
Step 11: the hycar (HTBN) of terminal hydroxy group is put in four-hole boiling flask, under vacuum condition
At 100-110 DEG C except water 2-3h；
In this step, in above-mentioned HTBN, acrylonitrile content is 10.4%.
Step 12: treat that temperature drops to room temperature, adds carbimide, and reacts 2-3h in a nitrogen atmosphere；
Step 13: when temperature drops to room temperature again, adds chain extender, and reacts 1～2h at 60-70 DEG C；
Step 14: after the completion of reaction resulting materials is put in mould, hot-forming after be put in the baking oven of 90-100 DEG C
Solidification 20-24h, obtains described polyurethane elastomer material.
In implementing, above-mentioned used each raw-material mass fraction is respectively as follows:
The carbimide of the HTBN of 80-88 part, 6-10 part, and the chain extender of 6-10 part, and above-mentioned each raw-material total part
Number is 100.
It addition, above-mentioned carbimide may include that hexamethylene diisocyanate (HDI), liquefaction 4,4 '-diphenyl
Methane diisocyanate (L-MDI) or toluene di-isocyanate(TDI) (TDI).
Described chain extender can be 1,4-butanediol (BDO).
With concrete example, the performance of above-mentioned preparation method and obtained polyurethane elastomer material is carried out in detail the most again
Illustrate:
Example 1, synthesis gained HTBN is put in four-hole boiling flask, at 100～110 DEG C except water 2h under vacuum condition；
Treat that temperature drops to room temperature, add the hexamethylene diisocyanate HDI measured, react 3h in a nitrogen atmosphere；
Treat that temperature drops to room temperature again, add BDO, at 60 DEG C, react 1-2h；
Material is put in mould after terminating by reaction, hot-forming, is put in the baking oven of 100 DEG C solidification 24h subsequently, obtains
Described polyurethane elastomer material.
Example 2, preparation method are identical with example 1, except for the difference that the HDI of 6-10 part is changed into the liquefaction 4,4 ' of 6-10 part-
Methyl diphenylene diisocyanate (L-MDI).
Example 3, preparation method are identical with example 1, and the HDI of 6-10 part except for the difference that changes into the toluene diisocynate of 6-10 part
Ester TDI.
Normal to mechanical property, specific insulation and the dielectric of the polyurethane elastomer material obtained by above three example below
Number is measured:
First polyurethane elastomer material is cut into a length of 20mm in working area, the dumbbell shape tensile bars of a width of 4mm.Use
The tensilon of Mei Tesi industrial system (Chinese) company limited.Draw speed is 50mm/min.
It is 1mm that polyurethane elastomer material is cut into thickness again, the disk of a diameter of 10mm, and upper and lower surface covers upper electrode,
Put in instrument.Use the wideband dielectric electric impedance analyzer of Novocontrol company of Germany.Dielectric electric impedance analyzer is surveyed
Try its at room temperature 101-107Frequency range in dielectric constant.
Above-mentioned specific insulation uses EST121 type numeral ultra-high resistance, micro current instrument to measure.
Final testing result, is illustrated in figure 2 the present invention and is lifted the relation of three examples test gained dielectric constants and frequency and show
Being intended to, be illustrated in figure 3 the present invention and lifted the relation between three example test gained stress and strains, table 1 below is three
The specific insulation contrast of example test gained:
Table 1
| Specific insulation Ω mm | |
| Embodiment 1 | 5.41×1012 |
| Embodiment 2 | 2.66×1012 |
| Embodiment 3 | 4.07×1012 |
As can be seen here: according to the dielectric constant of the polyurethane elastomer material obtained by preparation method of the present invention relative to tradition
Polyurethane material can improve 1.5-2 times, there is the highest dielectric constant and mechanical property.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, the change that can readily occur in or replace
Change, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be with claims
Protection domain is as the criterion.
Claims (4)
1. the preparation method of a polyurethane elastomer material, it is characterised in that described method includes:
The hycar (HTBN) of terminal hydroxy group is put in four-hole boiling flask, at 100-under vacuum condition
110 DEG C are removed water 2-3h；
Treat that temperature drops to room temperature, add carbimide, and react 2-3h in a nitrogen atmosphere；
When temperature drops to room temperature again, add chain extender, and at 60-70 DEG C, react 1～2h；
After the completion of reaction resulting materials is put in mould, hot-forming after be put in the baking oven of 90-100 DEG C solidification 20-
24h, obtains described polyurethane elastomer material.
The preparation method of polyurethane elastomer material the most according to claim 1, it is characterised in that used each former material
The mass fraction of material is respectively as follows:
The carbimide of the HTBN of 80-88 part, 6-10 part, and the chain extender of 6-10 part, and above-mentioned each raw-material total part
Number is 100.
The preparation method of polyurethane elastomer material the most according to claim 1 or claim 2, it is characterised in that
Described carbimide includes: hexamethylene diisocyanate (HDI), liquefaction 4,4 '-diphenyl methane two isocyanide
Acid esters (L-MDI) or toluene di-isocyanate(TDI) (TDI).
The preparation method of polyurethane elastomer material the most according to claim 1, it is characterised in that
Described chain extender is 1,4-butanediol (BDO).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610459034.6A CN105885005A (en) | 2016-06-22 | 2016-06-22 | Preparation method of polyurethane elastomer material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610459034.6A CN105885005A (en) | 2016-06-22 | 2016-06-22 | Preparation method of polyurethane elastomer material |
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| CN201610459034.6A Pending CN105885005A (en) | 2016-06-22 | 2016-06-22 | Preparation method of polyurethane elastomer material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488254A (en) * | 2017-08-29 | 2017-12-19 | 北京石油化工学院 | Dielectric elastomer material and preparation method thereof |
| CN109535380A (en) * | 2018-12-19 | 2019-03-29 | 广州机械科学研究院有限公司 | A kind of heat cross-linked type thermoplastic polyurethane elastomer and its preparation method and application |
| WO2019213948A1 (en) * | 2018-05-10 | 2019-11-14 | 北京化工大学 | Butadiene rubber-polyurethane elastomer material having ultra-low rolling resistance and preparation method therefor |
| CN112661924A (en) * | 2020-12-18 | 2021-04-16 | 宝胜科技创新股份有限公司 | Preparation method and application of thermal-oxidative-aging-resistant polyurethane elastomer material |
| CN113307927A (en) * | 2021-05-21 | 2021-08-27 | 苏州市雄林新材料科技有限公司 | Soft high-elasticity TPU film and preparation method thereof |
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| JPS6114222A (en) * | 1984-06-29 | 1986-01-22 | Asahi Chem Ind Co Ltd | Novel urethane prepolymer and its resin and production thereof |
| CN1919890A (en) * | 2006-08-11 | 2007-02-28 | 中国石油天然气集团公司 | Synthesis method of high-performance multipurpose urethane elastomer |
| CN101108889A (en) * | 2007-06-05 | 2008-01-23 | 北京化工大学 | Polyurethane/vinyl polymer IPN bi-component damping material |
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| JPS6114222A (en) * | 1984-06-29 | 1986-01-22 | Asahi Chem Ind Co Ltd | Novel urethane prepolymer and its resin and production thereof |
| CN1919890A (en) * | 2006-08-11 | 2007-02-28 | 中国石油天然气集团公司 | Synthesis method of high-performance multipurpose urethane elastomer |
| CN101108889A (en) * | 2007-06-05 | 2008-01-23 | 北京化工大学 | Polyurethane/vinyl polymer IPN bi-component damping material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488254A (en) * | 2017-08-29 | 2017-12-19 | 北京石油化工学院 | Dielectric elastomer material and preparation method thereof |
| CN107488254B (en) * | 2017-08-29 | 2019-12-20 | 北京石油化工学院 | Dielectric elastomer material and preparation method thereof |
| WO2019213948A1 (en) * | 2018-05-10 | 2019-11-14 | 北京化工大学 | Butadiene rubber-polyurethane elastomer material having ultra-low rolling resistance and preparation method therefor |
| CN109535380A (en) * | 2018-12-19 | 2019-03-29 | 广州机械科学研究院有限公司 | A kind of heat cross-linked type thermoplastic polyurethane elastomer and its preparation method and application |
| CN109535380B (en) * | 2018-12-19 | 2021-01-26 | 广州机械科学研究院有限公司 | Heat-crosslinking thermoplastic polyurethane elastomer and preparation method and application thereof |
| CN112661924A (en) * | 2020-12-18 | 2021-04-16 | 宝胜科技创新股份有限公司 | Preparation method and application of thermal-oxidative-aging-resistant polyurethane elastomer material |
| CN112661924B (en) * | 2020-12-18 | 2022-05-17 | 宝胜科技创新股份有限公司 | Preparation method and application of thermal-oxidative-aging-resistant polyurethane elastomer material |
| CN113307927A (en) * | 2021-05-21 | 2021-08-27 | 苏州市雄林新材料科技有限公司 | Soft high-elasticity TPU film and preparation method thereof |
| CN113307927B (en) * | 2021-05-21 | 2022-08-23 | 苏州市雄林新材料科技有限公司 | Soft high-elasticity TPU film and preparation method thereof |
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Application publication date: 20160824 |
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