CN103435836A - Preparation method of polymer foam material in open pore structure - Google Patents
Preparation method of polymer foam material in open pore structure Download PDFInfo
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Abstract
The invention discloses a preparation method of a polymer foam material in an open pore structure. The preparation method comprises the steps of blending two or more polymers by a melt blending method to form a blend of the polymer, preparing a green body in a definite shape by vacuum mold pressing, putting the green body in a high-pressure reaction kettle, supplying gas, rising temperature and pressure above a supercritical point of the gas to allow the gas to be converted to supercritical fluid, allowing the green body of the blend of the polymers to be foamed by a quick pressure reduction method after the supercritical fluid is saturated in the green body, immersing an obtained polymer foaming material in an appropriate etchant, allowing the etchant and the polymer foaming material to perform physical or chemical reaction, allowing at least one polymer in the polymer foaming material to be dissolved or degraded so as to form channels connecting cells in cell walls, taking out after a certain time, and obtaining the polymer foam material in the open pore structure.
Description
Technical field
The invention belongs to the polymer foams field, say more specifically as existing open-cell foam materials field provides a kind of new preparation process, there is the preparation method of the polymer foams of open-celled structure.
Background technology
Open cell polymer foams, refer between the abscess in foam and be interconnected, and the gas phase in foam and polymkeric substance are all the foam materialss of external phase.Because the foam structure in polymeric matrix is open, between abscess, be interconnected, can form complicated passage, allow micro-molecular gas or fluid flow by material.If can accurately control size and the form of abscess in open-cell foam materials, just can determine the particle size through material, make it play centrifugation.Open cell polymer foams can be used as separation and sorbing material, support of the catalyst, Thermosensitive Material Used for Controlled Releasing of Medicine, liquid separation mould material, advanced low-k materials etc.
The common preparation method of open cell polymer foams has three kinds: phase separation method, radiation exposure method, stretching method.Phase separation method is that the above mixture system of two-phase or two-phase (polymkeric substance, additive and solvent) produces phase-splitting under the effects such as temperature or solvent, thereby form the method for specific microvoid structure in polymeric matrix, prepared material can be perforate or unicellular structure.But its main drawback is to need to use a large amount of expensive, harmful solvents, and production process is very complicated.The charged particle irradiate base material that the radiation exposure method utilizes nuclear reactor to produce, charged particle penetrates film and leaves a trace, and then film is placed in to chemical reagent and corrodes, and can obtain microporous membrane, and the hole on film is straight circular hole mostly.Within 1972, the U.S. adopts stretching method to produce the polypropylene micropore filtering film, process is: polypropylene is film extrusion under higher than its fusing point at first, then in tension-free situation, be placed on the polypropylene fusing point following cooling, time is no more than 5 s, then the film punching is then controlled to certain stretch ratio and stretched, then by film thermoforming under certain temperature and tension force, thereby make required perforated film.The product that stretching method and rays method make is soft thin products, and certain difficulty is arranged when producing hard or thick article.
Adopt the foam materials of the standby thermoplastic polymer of supercutical fluid reduction of blood pressure in high-speed legal system, what generally obtain is the foam materials with unicellular structure, independent of one another between abscess and abscess.Summer broad sense (summer broad sense, Master's thesis, Dalian University of Technology, Dalian, 2010) adopt gas injection continuous warming of improved supercritical co step-down foaming repeatedly the treating processes of release prepare polymethylmethacrylate (PMMA) porous material, the sample interior abscess has connectedness to a certain degree.But the experiment complex disposal process, foam structure is wayward, and the size of sample interior abscess is larger, not in the scope of cellular plastic.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with polymer foams of open-celled structure, described method technique is simple, and the product distribution of cells prepared according to the method for the invention is even and the foam material inclusion-free is residual.
A kind of preparation method with polymer foams of open-celled structure, processing step is as follows:
(1) adopt scorification that two or more polymkeric substance is carried out to blend, obtain the blend of polymkeric substance;
(2) the blend vacuum mold of the resulting polymkeric substance of step (1) is pressed into to base substrate the cooling and shaping of design shape;
(3) the blend base substrate of the resulting polymkeric substance of step (2) is placed in to autoclave, be converted into supercutical fluid more than passing into gas and heating up, be forced into the super critical point of described gas, when supercutical fluid, in base substrate, reach capacity after state, adopt the reduction of blood pressure in high-speed method to make the base substrate foaming, obtain the polymer foaming material after cooling and shaping;
(4) the resulting polymer foaming material of step (3) is immersed in suitable etching liquid, certain hour obtains having the polymer foams of open-celled structure after taking out;
(5) by the resulting polymer foams with open-celled structure of step (4) successively with ethanol, distilled water repetitive scrubbing to remove the impurity in the polymer foams with open-celled structure.
In aforesaid method, polymkeric substance is thermoplastic polymer, can be unformed thermoplastic polymer, or the crystalline thermoplastic polymkeric substance.
In aforesaid method, the operation of scorification is as follows: by the blend of polymkeric substance, in the congruent melting of normal pressure, blend polymer, melt at temperature mixing even to mixed with polymers.
In aforesaid method, for the gas foamed, be carbonic acid gas, nitrogen or air.
In aforesaid method, the rate of pressure reduction (mean rate) of reduction of blood pressure in high-speed foaming is 5 ~ 60 MPa/s.
In aforesaid method, the etching liquid that the polymer foaming material immerses can be a kind of solution, a kind of solvent or its mixed solution.Requirement to etching liquid is: etching liquid can with polymer foaming material production physics or chemical reaction, make in the polymer foaming material to have at least a kind of polymkeric substance dissolved or the degraded, form the passage that connects abscess on cell wall, the final polymer foams with open-celled structure that forms.
In aforesaid method, the time that the polymer foaming material is immersed in etching liquid is 30 min ~ 4 h, and the etching liquid temperature is 15 ~ 65 ℃.
The invention has the beneficial effects as follows: first, polymer foams with open-celled structure prepared by the method for the invention, abscess is Open architecture, between abscess, can form complicated passage, be suitable as sound-absorbing, absorption and special separation material, also be applicable to Thermosensitive Material Used for Controlled Releasing of Medicine; The second, the present invention forms for polymer foams the novel method that open-celled structure provides a kind of different designs; The 3rd, polymer foams with open-celled structure prepared by the method for the invention, the experiment conditions such as time that can be immersed in etching liquid by control saturation pressure, temperature of saturation, rate of pressure reduction, polymer foaming material are controlled its cell morphology, to meet different needs; The 4th, the conventional gas under the method for the invention employing supercritical state is as whipping agent, with low cost, is conducive to environment protection; The 5th, the method for the invention technique is simple, adopts conventional equipment processing, is easy to realize suitability for industrialized production.
The accompanying drawing explanation
Accompanying drawing 1 is the scanning electron microscope (SEM) photograph of the prepared polymer foams section with open-celled structure of embodiment 1.
Accompanying drawing 2 is scanning electron microscope (SEM) photographs of the prepared polymer foams section with open-celled structure of embodiment 2.
Embodiment
Below in conjunction with embodiment, technology bill of the present invention is further described, but it is important to point out, embodiment can not be interpreted as to limitation of the present invention.
Below in each embodiment, polymethylmethacrylate (PMMA) is by sumitomo chemical company production, model LG2; Poly(lactic acid) (PLA) is produced by NatureWorks company, model 2002D; General Purpose Polystyrenre (PS), the Ningbo platform, the trade mark is 5250; Polycaprolactone (PCL) is produced by Sigma-Aldrich; Polycarbonate (PC) changes into company by Japanese Supreme Being people and produces, model K-1300.
embodiment 1
(1) by polymethylmethacrylate and polystyrene mass ratio, be 80:20 batching, under normal pressure, 200 ℃ in torque rheometer mixing 8 min, obtain the blend of polymkeric substance;
(2) blend of the resulting polymkeric substance of step (1) is carried out to vacuum compression molding, molding temperature is 200 ℃, and dwell pressure is 10 MPa, and the dwell time is 7 min, sheet blend base substrate the cooling and shaping of the polymkeric substance that to obtain thickness be 0.8 mm;
(3) the sheet blend base substrate of the resulting polymkeric substance of step (2) is placed in to autoclave, pass into carbonic acid gas, pressure-controlling in reactor is at 20 MPa, temperature is controlled at 90 ℃, when supercritical co, in base substrate, reach capacity after state, with the release speed of about 15 MPa/s by the Pressure Drop in reactor to normal pressure, obtain the polymer foaming material after cooling and shaping;
(4) the resulting polymer foaming material of step (3) is immersed in the hexanaphthene under room temperature, the immersion time is 2 h, obtains having the polymer foams of open-celled structure;
(5) by the resulting polymer foams with open-celled structure of step (4) successively with ethanol, distilled water repetitive scrubbing to remove the impurity in the polymer foaming material with open-celled structure.
The product with liquid nitrogen prepared by the present embodiment carries out brittle failure, adopt scanning electron microscope (SEM) to be observed its section, Fig. 1 is the scanning electron microscope (SEM) photograph of the prepared polymer foams section with open-celled structure of embodiment 1, many apertures are as can be seen from the figure arranged on cell wall, illustrate that this is the polymer foams with open-celled structure.
The percentage of open area that utilizes the true density instrument to record the present embodiment products obtained therefrom is 68%.
embodiment 2
(1) by polymethylmethacrylate and poly(lactic acid) mass ratio, be 80:20 batching, under normal pressure, 180 ℃ in torque rheometer mixing 8 min, obtain the blend of polymkeric substance;
(2) blend of the resulting polymkeric substance of step (1) is carried out to vacuum compression molding, molding temperature is 180 ℃, and dwell pressure is 5 MPa, and the dwell time is 5 min, sheet blend base substrate the cooling and shaping of the polymkeric substance that to obtain thickness be 0.8 mm;
(3) the sheet blend base substrate of the resulting polymkeric substance of step (2) is placed in to autoclave, pass into carbonic acid gas, pressure-controlling in reactor is at 20 MPa, temperature is controlled at 90 ℃, when supercritical co, in base substrate, reach capacity after state, with the release speed of about 15 MPa/s by the Pressure Drop in reactor to normal pressure, obtain the polymer foaming material after cooling and shaping;
(4) the resulting polymer foaming material of step (3) is immersed in the mixed solution of phosphate buffered saline buffer (PH=8.2) that volume ratio is 1:1 and ethanol, mixeding liquid temperature is 60 ℃, the immersion time is 30 min, obtains having the polymer foams of open-celled structure;
(5) by the resulting polymer foams with open-celled structure of step (4) successively with ethanol, distilled water repetitive scrubbing to remove the impurity in the polymer foams with open-celled structure.
The product with liquid nitrogen prepared by the present embodiment carries out brittle failure, adopts scanning electron microscope (SEM) to be observed its section.Fig. 2 is the scanning electron microscope (SEM) photograph of the prepared polymer foams section with open-celled structure of embodiment 2, the mutual UNICOM of abscess as we can see from the figure.
The percentage of open area that utilizes the true density instrument to record the present embodiment products obtained therefrom is 60%.
embodiment 3
(1) by polymethylmethacrylate and polystyrene mass ratio, be 20:80 batching, under normal pressure, 200 ℃ in torque rheometer mixing 8 min, obtain the blend of polymkeric substance;
(2) identical with embodiment 1 step (2);
(3) the sheet blend base substrate of the resulting polymkeric substance of step (2) is placed in to autoclave, pass into carbonic acid gas, pressure-controlling in reactor is at 20 MPa, temperature is controlled at 90 ℃, when supercritical co, in base substrate, reach capacity after state, with the release speed of about 20 MPa/s by the Pressure Drop in reactor to normal pressure, obtain the polymer foaming material after cooling and shaping;
(4) the resulting polymer foaming material of step (3) is immersed in acetic acid, the immersion time is 3 h, obtains having the polymer foams of open-celled structure;
(5) identical with embodiment 1 step (5).
The percentage of open area that utilizes the true density instrument to record the present embodiment products obtained therefrom is 63%.
embodiment 4
(1) by polycaprolactone and polystyrene mass ratio, be 80:20 batching, under normal pressure, 180 ℃ in torque rheometer mixing 8 min, obtain the blend of polymkeric substance;
(2) identical with embodiment 2 steps (2);
(3) identical with embodiment 1 step (3);
(4) identical with embodiment 1 step (4);
(5) identical with embodiment 1 step (5).
The percentage of open area that utilizes the true density instrument to record the present embodiment products obtained therefrom is 65%.
embodiment 5
(1) by polycarbonate and polystyrene mass ratio, be 80:20 batching, under normal pressure, 200 ℃ in torque rheometer mixing 8 min, obtain the blend of polymkeric substance;
(2) identical with embodiment 1 step (2);
(3) the sheet blend base substrate of the resulting polymkeric substance of step (2) is placed in to autoclave, pass into carbonic acid gas, pressure-controlling in reactor is at 20 MPa, temperature is controlled at 180 ℃, when supercritical co, in base substrate, reach capacity after state, with the release speed of about 15 MPa/s by the Pressure Drop in reactor to normal pressure, obtain the polymer foaming material after cooling and shaping;
(4) identical with embodiment 1 step (4);
(5) identical with embodiment 1 step (5).
The percentage of open area that utilizes the true density instrument to record the present embodiment products obtained therefrom is 62%.
Claims (7)
1. the preparation method with polymer foams of open-celled structure is characterized in that processing step is as follows:
(1) adopt melt-blending process that two or more polymkeric substance is carried out to blend, obtain the blend of polymkeric substance;
(2) the blend vacuum mold of the resulting polymkeric substance of step (1) is pressed into to base substrate the cooling and shaping of design shape;
(3) the blend base substrate of the resulting polymkeric substance of step (2) is placed in to autoclave, be converted into supercutical fluid more than passing into gas and heating up, be forced into the super critical point of described gas, when supercutical fluid, in base substrate, reach capacity after state, adopt the reduction of blood pressure in high-speed method to make the base substrate foaming, obtain the polymer foaming material after cooling and shaping;
(4) the resulting polymer foaming material of step (3) is immersed in suitable etching liquid, certain hour obtains having the polymer foams of open-celled structure after taking out.
2. a kind of preparation method with polymer foams of open-celled structure according to claim 1, is characterized in that described polymkeric substance is thermoplastic polymer.
3. a kind of preparation method with polymer foams of open-celled structure according to claim 1, is characterized in that the described gas for foaming is carbonic acid gas, nitrogen or air.
4. a kind of preparation method with polymer foams of open-celled structure according to claim 1, is characterized in that the etching liquid that described polymer foaming material immerses can be a kind of solution, a kind of solvent or its mixed solution; Requirement to etching liquid is: etching liquid can with polymer foaming material production physics or chemical reaction, make in the polymer foaming material to have at least a kind of polymkeric substance dissolved or the degraded, form the passage that connects abscess on cell wall, the final polymer foams with open-celled structure that forms.
5. a kind of preparation method with polymer foams of open-celled structure according to claim 1, is characterized in that the time that described polymer foaming material is immersed in etching liquid is 30 min ~ 4 h, and the etching liquid temperature is 15 ~ 65 ℃.
6. a kind of preparation method with polymer foams of open-celled structure according to claim 1, is characterized in that the operation of described scorification is as follows: melt at temperature mixing even to mixed with polymers by the blend of polymkeric substance in the congruent melting of normal pressure, blend polymer.
7. according to the described a kind of preparation method with polymer foams of open-celled structure of one of claim 1 to 6, it is characterized in that the blend base substrate of polymkeric substance adopts the foaming of reduction of blood pressure in high-speed method, the rate of pressure reduction of described reduction of blood pressure in high-speed is 5 ~ 60 MPa/s.
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| CN104592543A (en) * | 2015-02-02 | 2015-05-06 | 四川大学 | Porous polymer material with dual-peak pore structure and preparation method thereof |
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| CN104877245A (en) * | 2015-05-26 | 2015-09-02 | 华南理工大学 | Method for preparing rubber-toughened PS foam material through extrusion of supercritical fluid |
| CN105001512A (en) * | 2015-07-01 | 2015-10-28 | 中国科学院宁波材料技术与工程研究所 | Open-cell polymer foam material and preparation method therefor |
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| CN104629078A (en) * | 2015-02-02 | 2015-05-20 | 四川大学 | Preparation method of gradient porous polymer material |
| CN104592543A (en) * | 2015-02-02 | 2015-05-06 | 四川大学 | Porous polymer material with dual-peak pore structure and preparation method thereof |
| CN104877245A (en) * | 2015-05-26 | 2015-09-02 | 华南理工大学 | Method for preparing rubber-toughened PS foam material through extrusion of supercritical fluid |
| CN105001512B (en) * | 2015-07-01 | 2017-06-27 | 中国科学院宁波材料技术与工程研究所 | A kind of open cell polymer foams and preparation method thereof |
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| CN106798945B (en) * | 2016-12-05 | 2019-11-12 | 四川大学 | Polymer tissue engineering rack porous material and preparation method thereof with good hole connectivity |
| CN106798945A (en) * | 2016-12-05 | 2017-06-06 | 四川大学 | With connective polymer tissue engineering rack porous material of good hole and preparation method thereof |
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| CN109082049A (en) * | 2018-06-19 | 2018-12-25 | 嘉兴南洋职业技术学院 | A kind of supercritical fluid foamed fluoropolymer material and preparation method thereof |
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