CN110229353A - A method of improving organic powder-compound polyurethane material interface performance and mechanical property - Google Patents
A method of improving organic powder-compound polyurethane material interface performance and mechanical property Download PDFInfo
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
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Abstract
The invention discloses a kind of improvement organic powder-compound polyurethane material interface performance and the method for mechanical property, preparation process includes the preparation of polyurethane composite solution, coagulating bath preparation, polyurethane composite solution blade coating, inversion of phases molding and is dried;This method is not under the premise of changing organic powder-compound polyurethane material preparation process, using the poor solvent by polyurethane, N, dinethylformamide and polarity are lower than N, the ternary mixed solvent of the solvent compounding of dinethylformamide, enable unmodified organic powder preferably it is evenly dispersed in polyurethane solution, both the original characteristic of organic powder particle had been retained, improve the mechanical property of composite material again, organic powder-compound polyurethane material obtained has good intensity and strain property, and preparation process is simple, it is bionical weaving, taking in equal fields has extensive market demand prospect.
Description
Technical field
The present invention relates to technical field of composite materials, more particularly to a kind of improvement organic powder-compound polyurethane material
The method of interface performance and mechanical property.
Background technique
Polyurethane is the high molecular material being combined by soft segment and rigid chain segment block, and elasticity is between rubber and modeling
Expect between material.Contain a large amount of carbamate groups, ester group and urea groups isopolarity group in polyurethane structural, imparts poly- ammonia
The characteristics such as the excellent wearability of ester elastomer, higher intensity, good elasticity, lower temperature resistance and heat resistance, while polyurethane
Material also has excellent biocompatibility, so that polyurethane becomes one of the new material being widely noticed, what is prepared is organic
Powder-compound polyurethane material is widely used in thin polymer film field.
With the development of science and technology, thin polymer film in national economy using more and more extensive, to thin-film material
Service performance, the requirement of especially mechanical property and hydrophilic moisture-inhibiting comfort is also higher and higher.Currently, single molten using tradition
Organic powder-compound polyurethane material prepared by agent and single forming method has under the conditions of organic powder proportion is higher
Interface interaction between machine powder and polyurethane is poor, so that the intensity of compound polyurethane material and strain are poor;In organic powder
Under the conditions of body proportion is lower, compound polyurethane material is only capable of embodying the performance of polyurethane body material, good cannot show
The excellent surface characteristic of natural organic powder.In addition, by being modified to organic powder surface, such as plasma modification, surface
The methods of graft modification can improve the interface binding power between organic powder and polyurethane material, and then improve polyurethane composite
The mechanical property of material, still, the surface modification of organic powder can destroy the surface characteristic of organic powder, cannot realize well pair
The effective use of powder.For current organic powder-compound polyurethane material poor interface performance and tensile mechanical properties
Defect, by changing organic powder-compound polyurethane material forming process, so as to improve the boundary between organic powder and polyurethane
Face performance, prepare it is a kind of it is high filling, strong mechanical performance organic powder-polyurethane composite membrane have very important significance.
The patent application of Publication No. CN105111490A discloses a kind of preparation side of high-strength and high-modulus highly-elastic urethane film
Method, the method use ammonium salt as coagulating bath, so that without fixed in the ammonium salt molecule and polyurethane in the polyurethane film after film forming
Shape distinguishes the micro- cross-linked structure formed in the form of hydrogen bond between son, or nano whiskers structure is formed in the hole of polyurethane film
And nano-spherical structure, the tensile stress and strain of polyurethane film, but disadvantage is that the composite membrane can be increased simultaneously
Do not have good hydrophilic water vapour permeability.
Open the 8th phase of magazine " fabrics for industrial use " October in 2006 is entitled, and " extra-fine wool powders are anti-to polyurethane film
The influence of water penetrability " article in have studied different content wool powder to the mechanical property and waterproof and moisture permeability of polyurethane film
The influence of energy, for the solvent that this article uses for single n,N-Dimethylformamide, the film build method of use is immersion precipitation
Method, prepared polyurethane/wool powder composite membrane has certain water vapour permeability, but disadvantage is that composite membrane breaks
Resistance to spalling and elongation at break are lower.
Open magazine " polymer material science and engineering " the 8th phase of August in 2011 entitled " fibroin powder and medical poly- ammonia
Ester colloidal sol blending-hot pressing blend film preparation and performance " article in different fibroins from pressure sintering are prepared for using solution blending
The polyurethane composite membrane of powder content, prepared polyurethane composite membrane has certain breaking strength, but its shortcoming exists
In: when fibroin powder content is larger, polyurethane/silk fibroin composite membrane coating elongation at break is limited well below polyurethane film
The application of polyurethane/silk fibroin composite membrane coating.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of improvement organic powder-compound polyurethane material interface performance and power
Learn performance method, under the premise of not changing organic powder-compound polyurethane material preparation process, using by polyurethane not
Good solvent, n,N-Dimethylformamide and polarity make lower than the ternary mixed solvent that the solvent of n,N-Dimethylformamide is compounded
Unmodified organic powder can preferably it is evenly dispersed in polyurethane solution, both retained the original spy of organic powder particle
Property, and improving the mechanical property of composite material, organic powder-compound polyurethane material obtained has good intensity and strain
Performance.
To achieve the above object, the present invention provides a kind of improvement organic powder-compound polyurethane material interface performance and
The method of mechanical property, includes the following steps:
(1) polyurethane composite solution is prepared: the poor solvent, N,N-dimethylformamide and polarity of polyurethane are lower than N,
The solvent compounding of dinethylformamide is ternary mixed solvent, then base polyurethane prepolymer for use as and unmodified organic powder are placed in
In ternary mixed solvent, generating polyurethane composite solution is prepared in vacuum defoamation after mechanical stirring is uniform;
(2) coagulating bath is prepared: deionized water being mixed with alcohol organic solvent, is configured to solidify after mixing evenly
Bath;
(3) polyurethane composite solution scratches: by polyurethane composite solution blade coating on mold;
(4) inversion of phases molding and drying process: the mold containing polyurethane composite solution is immersed in coagulating bath immediately and is soaked
Bubble, puts in a drying box again after taking-up and is heat-treated.
Further, the mass fraction of the poor solvent of polyurethane described in step (1) is 5%~45%;The N, N-
The mass fraction of dimethylformamide is 30%~90%;Quality point of the polarity lower than the solvent of N,N-dimethylformamide
Number is 5%~30%.
Further, the mass percent of base polyurethane prepolymer for use as described in step (1) is 5%~33.25%;It is described not change
Property organic powder mass percent be 0.5%~17.5%;The mass percent of the ternary mixed solvent be 65%~
90%.
Further, the poor solvent of polyurethane described in step (1) is total for one or both of toluene or dimethylbenzene
Mixed object;The solvent that the polarity is lower than N,N-dimethylformamide is one of acetone, dioxane or tetrahydrofuran or more
Kind mixture.
Further, base polyurethane prepolymer for use as described in step (1) is Polyether-Polyol Polyurethane Prepolymer or polyester polyurethane
One of performed polymer or polyester-polyether Type Polyurethane Prepolymer.
Further, unmodified organic powder described in step (1) is the protein fibre powder or fine of fine
Wool fiber powder or one or both of leather powder or a variety of.
Further, churned mechanically whipping temp described in step (1) be 20~45 DEG C, stirring rate be 500~
3000 revs/min, mixing time is 1.5~5h.
Further, the mass fraction ratio of deionized water described in step (2) and alcohol organic solvent be 99%:1%~
80%:20%;The conductivity of the deionized water is 16M Ω cm;The alcohol organic solvent is ethyl alcohol or 1- propyl alcohol or 1-
Butanol or one of 2- propyl alcohol or ethylene glycol;The solution temperature of the coagulating bath is 10~50 DEG C.
Further, mold described in step (3) is polytetrafluoroethylene (PTFE).
Further, the time impregnated in coagulating bath described in step (4) is 1.5~6h;Temperature in the drying box
It is 30~80 DEG C;The time of the heat treatment is 12~48h.
The beneficial effects of the present invention are:
1, technical solution of the present invention is adopted under the premise of not changing organic powder-compound polyurethane material preparation process
Three be compounded with the poor solvent, N,N-dimethylformamide and polarity by polyurethane lower than the solvent of N,N-dimethylformamide
First mixed solvent, compared to the single good solvent of tradition, organic powder can preferably it is evenly dispersed in polyurethane solution, both
Retain the original characteristic of organic powder particle, and improve the mechanical property of composite material, organic powder-polyurethane obtained is compound
Material has good intensity and strain property;
2, the ternary mixed solvent that the present invention uses is during preparing organic powder-compound polyurethane material, poly- ammonia
The arrangement that metastable state system can drive polyurethane molecular chain more orderly caused by the poor solvent of ester, to improve polyurethane
The intensity and strain property of material;In film forming procedure, the self-adjusting process of polyurethane molecular chain be conducive to polyurethane with it is organic
Good interface binding power is formed between powder, to improve organic powder-compound polyurethane material mechanical property;
3, increase the interface performance of composite material compared to traditional organic powder improving particle surface, the present invention is not to having
Machine powder particle carries out surface and is modified, and can retain organic powder particle on the basis of keeping composite material excellent mechanical performances
Original characteristic, so that compound polyurethane material has specific functional features possessed by organic powder;
4, organic powder provided by the invention-compound polyurethane material preparation process is simple, and prepared organic powder-is poly-
Urethane composite material has excellent mechanical performances, weave it is bionical, take etc. there is extensive market demand prospect in fields.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated;It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The fixed present invention;Unless stated otherwise, the present invention uses reagent, method and apparatus for the art conventional reagent, method and
Equipment.
Embodiment 1
The present embodiment provides it is a kind of improvement organic powder-compound polyurethane material interface performance and mechanical property method,
Include the following steps:
(1) polyurethane composite solution is prepared: by mass fraction than toluene, the N for 5%:90%:5%, N- dimethyl formyl
Amine and dioxane compounding be ternary mixed solvent, then by mass fraction than for the polyester polyurethane of 15%:15%:70% it is pre-
Aggressiveness, unmodified superfine wool powder are mixed with ternary mixed solvent, and vacuum defoamation is configured to gather after mechanical stirring 2.5h
Urethane composite solution;Wherein, whipping temp is 25 DEG C, and stirring rate is 700 revs/min;
(2) coagulating bath is prepared: by mass fraction than the deionized water and ethylene glycol compounding for 95%:5%, after mixing evenly
It is configured to coagulating bath;Wherein, the temperature of coagulating bath solution is 40 DEG C, and the conductivity of deionized water is 16M Ω cm;
(3) polyurethane composite solution scratches: configured polyurethane composite solution glass bar is scratched in polytetrafluoroethyl-ne
On alkene mold;
(4) inversion of phases molding and drying process: the mold containing polyurethane composite solution is immersed in coagulating bath immediately and is soaked
It is taken out after bubble 1.5h, then is placed in 30 DEG C of drying boxes and is heat-treated 48h.
Comparative example
This comparative example provides a kind of side for improving organic powder-compound polyurethane material interface performance and mechanical property
Method, compared with Example 1, the difference is that the single n,N-Dimethylformamide solvent of solvent for use, other and 1 phase of embodiment
Together.
Embodiment 2~7
Embodiment 2~7 provides a kind of side for improving organic powder-compound polyurethane material interface performance and mechanical property
Method, compared with Example 1, the difference is that changing toluene in step (1), n,N-Dimethylformamide and dioxane
Mass fraction ratio, Examples 1 to 7 and the corresponding each specific mass fraction ratio of solvent of comparative example and its organic powder-obtained are poly-
The mechanical property of urethane composite material is as shown in table 1.
The mechanical property of the different toluene of table 1, n,N-Dimethylformamide and the lower gained composite material of dioxane proportion
As can be seen from Table 1, with the increase of poor solvent toluene in ternary solvent system, polyurethane composite obtained
The trend risen is presented in tensile strength, elongation at break and the toughness of material, when toluene, n,N-Dimethylformamide and dioxane
Mass fraction ratio 45%:45%:10% when, prepared organic powder-compound polyurethane material mechanical property is best.And
Every mechanical property of compound polyurethane material obtained by Examples 1 to 7 is significantly better than that composite material prepared by comparative example,
Show that the present invention is substantially better than tradition using organic powder-compound polyurethane material mechanical property of ternary solvent system preparation
The composite material of single solvent immersion precipitation preparation.
Embodiment 8~11
Embodiment 8~11 provides a kind of improvement organic powder-compound polyurethane material interface performance and mechanical property
Method, compared with Example 7, the difference is that the solvent type in ternary mixed solvent is changed, the quality between each solvent
Score ratio is still 45%:45%:10%, each corresponding specific solvent composition of embodiment and its organic powder-polyurethane obtained
The mechanical property of composite material is as shown in table 2.
The mechanical property of the lower gained composite material of 2 different solvents of table composition
As can be seen from Table 2, the solvent type in ternary mixed solvent is larger to the Effect on Mechanical Properties of composite material,
The weaker solvent of middle polarity is added with the mechanical property for being conducive to improve compound polyurethane material, therefore, the corresponding first of embodiment 9
Organic powder-compound polyurethane material power obtained by benzene, n,N-Dimethylformamide and tetrahydrofuran ternary mixed solvent
Learn performance relatively more preferably.
Embodiment 12~13
Embodiment 12~13 provides a kind of improvement organic powder-compound polyurethane material interface performance and mechanical property
Method, compared with Example 9, the difference is that changing toluene in ternary mixed solvent, n,N-Dimethylformamide and four
The mass fraction ratio of hydrogen furans, the corresponding specific mass fraction ratio of embodiment 12 and 13 and its organic powder-polyurethane obtained
The mechanical property of composite material is as shown in table 3.
The mechanical property of the different toluene of table 3, n,N-Dimethylformamide and the lower gained composite material of tetrahydrofuran proportion
As can be seen from Table 3, in ternary mixed solvent polarity be lower than, the solvent quality score pair of n,N-Dimethylformamide
The Effect on Mechanical Properties of compound polyurethane material is larger, and with the increase of the solvent quality score, compound polyurethane material
The trend risen is presented in tensile strength, elongation at break and toughness, when the matter of toluene, n,N-Dimethylformamide and tetrahydrofuran
It is preferable to measure organic powder-compound polyurethane material mechanical property obtained when score ratio is 40%:30%:30%.
Embodiment 14~17
Embodiment 14~17 provides a kind of improvement organic powder-compound polyurethane material interface performance and mechanical property
Method, compared with embodiment 13, the difference is that changing polyester polyurethane performed polymer, unmodified superfine wool powder
The mass fraction of body and ternary mixed solvent ratio, the corresponding specific mass fraction ratio of embodiment 14~17 and its organic powder obtained
Body-compound polyurethane material mechanical property is as shown in table 4.
Under the different polyester polyurethane performed polymers of table 4, unmodified superfine wool powder and ternary mixed solvent proportion
The mechanical property of gained composite material
As can be seen from Table 4, the ratio of base polyurethane prepolymer for use as, unmodified superfine wool powder and ternary mixed solvent
It is larger to the Effect on Mechanical Properties of compound polyurethane material, higher polyester polyurethane performed polymer content and lower unmodified
Superfine wool powder content is more advantageous to the mechanical property for improving gained compound polyurethane material.When polyester polyurethane is pre-
The mass fraction ratio of aggressiveness, unmodified superfine wool powder and ternary mixed solvent is 33.25%:0.5%:66.25%
When obtained organic powder-compound polyurethane material mechanical property it is preferable.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes
It also should be regarded as protection scope of the present invention into supplement;Meanwhile all substantial technologicals according to the present invention do above-described embodiment
Any equivalent variations change, modification and differentiation, still fall within protection scope of the present invention.
Claims (10)
1. a kind of method for improving organic powder-compound polyurethane material interface performance and mechanical property, which is characterized in that including
Following steps:
(1) polyurethane composite solution is prepared: the poor solvent, N,N-dimethylformamide and polarity of polyurethane are lower than N, N- bis-
The solvent compounding of methylformamide is ternary mixed solvent, then base polyurethane prepolymer for use as and unmodified organic powder are placed in ternary
In the mixed solvent, generating polyurethane composite solution is prepared in vacuum defoamation after mechanical stirring is uniform;
(2) coagulating bath is prepared: deionized water being mixed with alcohol organic solvent, is configured to coagulating bath after mixing evenly;
(3) polyurethane composite solution scratches: by polyurethane composite solution blade coating on mold;
(4) inversion of phases molding and drying process: the mold containing polyurethane composite solution is immersed in coagulating bath immediately and is impregnated, is taken
It puts in a drying box and is heat-treated again after out.
2. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: the mass fraction of the poor solvent of polyurethane described in step (1) is 5%~45%;The N, N- bis-
The mass fraction of methylformamide is 30%~90%;Mass fraction of the polarity lower than the solvent of N,N-dimethylformamide
It is 5%~30%.
3. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: the mass percent of base polyurethane prepolymer for use as described in step (1) is 5%~33.25%;It is described not change
Property organic powder mass percent be 0.5%~17.5%;The mass percent of the ternary mixed solvent be 65%~
90%.
4. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: the poor solvent of polyurethane described in step (1) is the blending of one or both of toluene or dimethylbenzene
Object;The solvent that the polarity is lower than N,N-dimethylformamide is one of acetone, dioxane or tetrahydrofuran or a variety of
Mixture.
5. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: base polyurethane prepolymer for use as described in step (1) is that Polyether-Polyol Polyurethane Prepolymer or polyester polyurethane are pre-
One of aggressiveness or polyester-polyether Type Polyurethane Prepolymer.
6. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: unmodified organic powder described in step (1) is the protein fibre powder or fine of fine
One or both of wool fiber powder or leather powder are a variety of.
7. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: churned mechanically whipping temp described in step (1) is 20~45 DEG C, and stirring rate is 500~3000
Rev/min, mixing time is 1.5~5h.
8. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: the mass fraction ratio of deionized water described in step (2) and alcohol organic solvent be 99%:1%~
80%:20%;The conductivity of the deionized water is 16M Ω cm;The alcohol organic solvent is ethyl alcohol or 1- propyl alcohol or 1-
Butanol or one of 2- propyl alcohol or ethylene glycol;The solution temperature of the coagulating bath is 10~50 DEG C.
9. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: mold described in step (3) is polytetrafluoroethylene (PTFE).
10. a kind of organic powder-compound polyurethane material interface performance and mechanical property of improving according to claim 1
Method, it is characterised in that: the time impregnated in coagulating bath described in step (4) is 1.5~6h;Temperature in the drying box is
30~80 DEG C;The time of the heat treatment is 12~48h.
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CN113863023A (en) * | 2021-10-18 | 2021-12-31 | 武汉纺织大学 | Lasting antibacterial leather and preparation method thereof |
CN114716720A (en) * | 2022-03-10 | 2022-07-08 | 陕西科技大学 | Preparation method of vertical ordered polyurethane microporous membrane |
CN115125737A (en) * | 2022-07-06 | 2022-09-30 | 河南步锐实业有限公司 | Flexible container bag applying polyurethane coating |
CN115785770A (en) * | 2022-11-25 | 2023-03-14 | 武汉纺织大学 | Paint doped with wool powder and preparation method thereof |
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