CN109867891A - A kind of mixing prepares the clean method for preparing of high-melting-point porous material - Google Patents
A kind of mixing prepares the clean method for preparing of high-melting-point porous material Download PDFInfo
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- CN109867891A CN109867891A CN201910095919.6A CN201910095919A CN109867891A CN 109867891 A CN109867891 A CN 109867891A CN 201910095919 A CN201910095919 A CN 201910095919A CN 109867891 A CN109867891 A CN 109867891A
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Abstract
The present invention provides the clean method for preparing that a kind of mixing prepares high-melting-point porous material, step includes: S1, prepares mould material and packing material；Two kinds of S2, mixing materials: ultrasonic drying mode after grinding or dissolution can be used；S3, mixing and molding: heating pressurization forms mixing material；S4, high-temperature calcination: the mould material removed in material obtains porous structure.The present invention is based on mixing and moldings, suitable for preparing high-melting-point porous material, the porous material of this method preparation is with a wide range of applications, the material controls the main indicators such as porosity, aperture, the hole shape of finished product by the form and ratio that change mould material, and harmful substance is not generated in process of production, belongs to a kind of clean manufacturing method.
Description
Technical field
The invention belongs to polymer material molding technical field, in particular to a kind of mixing prepares high-melting-point porous material
Clean method for preparing.
Background technique
Porous material is the material that network structure is made of the hole closed or penetrated through, and there is branch on the boundary or surface of hole
Column or flat support.Porous material typical structure has two-dimensional structure and three-dimensional structure: two-dimensional structure is existed by a large amount of polygonal holes
Aggregation is formed in plane；Three-dimensional structure is then to be formed by a large amount of polyhedron-shaped holes in space clustering.
For opposite continuous media material, porous material generally have specific surface area is high, relative density is low, specific strength is high,
The advantages that light-weight, heat-insulated, good penetrability, sound insulation.Specifically, porous material generally power, heat, sound, light, in terms of all
There are excellent performance and high consistency.Porous material can improve the mechanical performances such as strength and stiffness, while can change raising punching
Hit toughness；Porous material can have unique optical property since two kinds of material dielectric constants or refractive index are different.Micropore
Porous silica material can issue visible light under the irradiation of laser, will become the ideal material of manufacture novel photoelectric subcomponent.
A kind of preparation method of multistage (micrometer/nanometer) pore structure material, describes one disclosed in CN201210185031
Kind realizes 150-800 μm of gradient through hole, lacking using mixing using selective laser (spot diameter is micro-meter scale) sintering
Oxygenolysis forms 10-100 μm of random spherical pore, obtains tens of receive using etching process amount high polymer micro balloons during the sintering process
The method in rice surface imperfection hole, finally obtains a kind of three-dimensional multistage pore structure with this method, due to the randomness of pore structure, no
The performance of systematicness, material cannot be guaranteed.
CN108641118A discloses one kind using cellulose as substrate, by being freeze-dried its internal liquid gas
Method instead of obtaining three-dimensional material.The porous material that this kind of method obtains has preferable performance, but this kind of mode obtains
The mechanical property of materials is poor.
Summary of the invention
In view of this, being directed to the deficiencies in the prior art, the present invention provides a kind of mixing, to prepare high-melting-point porous
The clean method for preparing of material, this method have simple process, pore shape and the easily controllable advantage of pore size.
The present invention provides the clean method for preparing that a kind of mixing prepares high-melting-point porous material, step includes:
S1, prepare mould material and packing material: using natural macromolecular material as mould material, being with heat-resistant polymer
The decomposition temperature of packing material, the heat-resistant polymer is higher than 350 DEG C；
S2, mould material and packing material are uniformly mixed, obtain mixing material；
S3, mixing and molding: form mixing material by open mill heating pressurization；
S4, high-temperature calcination: material at high temperature after molding is calcined, and the calcination temperature is higher than mould material decomposition temperature.
For this method using natural macromolecular material as mould material, such material can be decomposed into water and two under high temperature environment
The harmless products such as carbonoxide can be extracted largely in the natural environment, can also buy corresponding dusty material, source in market
It is easily obtained extensively.The pore morphology of obtained porous material is identical as template molecule shape, can pass through the ratio of mixing material
Adjustment is to realize the controllable of porosity of porous material.
Preferably, in step S1, the mould material includes one in cellulose, hemicellulose, chitosan or lignin
Kind；The packing material includes polytetrafluoroethylene (PTFE) (400 degrees Celsius or more are decomposed), (decomposition temperature 400-500 is Celsius for polyimides
One or more of degree) or polyphenylene sulfide (500 degrees Celsius of decomposition temperature or more).
More preferred, in step S1, the scale of the mould material is 1-10000nm.The shape of the mould material
Can decide for uniform spherical, rodlike, sheet, block etc., the size and shape of mould material the aperture of porous material with
Hole shape.
Preferably, in step S2, by percentage to the quality, the mould material accounts for the 10-50% of mixing material.Template material
Material accounts for that mass ratio is too high to be not easy to be kneaded molding, and too low to be unfavorable for performance optimization, while the ratio of mould material is desired product
Porosity.
More preferred, in step S2, it is mixed that the hybrid mode dried after suspension is obtained using dispersion in grinding or solvent
It closes uniform.
It is described to be ground to be ground to sample in 5000 times of observed under electron microscope it is further preferred that in step S2, depending on
Material is evenly distributed in open country, without obvious agglomeration, agglomeration, that is, can be considered that reaching mixing requires；Dispersion obtains in the solvent
The step of suspension includes: to disperse the powder of packing material in a solvent, and mould material is uniformly added in ultrasonic mixing afterwards, is continued
Ultrasound is stablized until obtained emulsion without deposited phenomenon.Since natural polymer is practically insoluble in any solvent, mould material
Shape and structure will not be destroyed, and can be realized aperture, porosity, hole shape are precisely controlled.
Specifically, the solvent is ethyl alcohol, DMF etc..
Specifically, the drying mode can be rotary evaporation or vacuum drying.
Preferably, in step S3, the time of the mixing is 25-35min, decomposition temperature of the melting temperature than mould material
Low 30-50 DEG C.
Preferably, in step S4, the calcination temperature is 10-30 DEG C higher than the decomposition temperature of mould material, when the calcining
Between be 1.5-2.5h.
More preferred, it is 150-170 DEG C by the corresponding calcination temperature of mould material of cellulose, with wood in step S4
Quality is that the corresponding calcination temperature of mould material is 220-240 DEG C, is by the corresponding calcination temperature of mould material of chitosan
180-200℃。
Compared with the prior art, the invention has the following advantages that
Present invention utilizes packing material tolerance high temperature and cellulose, chitosan, lignin, hemicellulose etc. are natural high
Molecular material pyrolytic does not generate the property of pernicious gas.The aperture of porous material determines by the size of mould material, template
The size of material is within the scope of 1~10000nm；The form in hole is identical by template molecule shape, can for it is spherical, linear, rodlike,
Sheet, block etc.；Porosity is determined by the ratio of mixing material.Using the porous material of the method for the invention preparation in each side
Face all there is performance outstanding and can be controlled by the form and ratio for changing mould material the porosity of finished product, aperture,
The main indicators such as hole shape, furthermore do not generate harmful substance in process of production, belong to a kind of clean manufacturing method, have good
Application prospect.
Detailed description of the invention
Fig. 1 is the process flow for the clean method for preparing that a kind of mixing provided by the invention prepares high-melting-point porous material
Figure.
Specific embodiment
Below in conjunction with specific embodiment and embodiment, it is specifically described the present invention, advantages of the present invention and various effects
It thus will clearly present.It will be understood by those skilled in the art that these specific embodiments and embodiment are for illustrating
The present invention is not intended to limit the present invention.
Throughout the specification, unless otherwise specified, terms used herein are interpreted as usual in this field
Used meaning.Therefore, unless otherwise defined, all technical and scientific terms used herein has leads with belonging to the present invention
The identical meaning of the general understanding of field technique personnel.Contradiction if it exists, this specification are preferential.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention, can pass through
Market is commercially available or can be prepared by existing method.For example, natural polymer used in the examples and resistance to height
Warm polymer is that market is commercially available.
Embodiment 1
The clean method for preparing that a kind of mixing prepares high-melting-point porous material is present embodiments provided, using cellulose as mould
For plate molecule, polytetrafluoroethylene (PTFE) are as packing material, mixing and molding high-melting-point porous material, step includes:
1) template molecule and packing material are prepared: purchase shape, size cellulosic material appropriate and ultra-fine (100nm
Within) polytetrafluorethylepowder powder；
2) mixed-powder: cellulose and polytetrafluoroethylene (PTFE) are weighed with mass ratio 3:7 ratio, two kinds of materials are made using grinding method
Material uniformly mixing, and sample and see whether under an electron microscope uniformly, sample is added in 5000 × observed under electron microscope
Material is evenly distributed in the visual field, without obvious agglomeration, agglomeration, is considered as and reaches mixing requirement；
3) mixing and molding: open mill is added in the cellulose mixed and polytetrafluorethylepowder powder, open mill temperature 80 is set
DEG C, it is kneaded 30min, obtains the composite sheet of cellulose and polytetrafluoroethylene (PTFE)；
4) high-temperature calcination: moulding material is calcined 2 hours for 150 degrees Celsius in small-sized calcining furnace, gas shield is not necessarily to, obtains
To porous material.
Embodiment 2
The clean method for preparing that a kind of mixing prepares high-melting-point porous material is present embodiments provided, using chitosan as mould
For plate molecule, polyimides are as packing material, mixing and molding high-melting-point porous material, step includes:
1) template molecule and packing material are prepared: purchase shape, size chitosan material appropriate and ultra-fine (100nm
Within) polyimide powder；
2) mixed-powder: chitosan and polyimides are weighed with mass ratio 4:6 ratio, polyimide powder is dispersed in
In DMF, chitosan is uniformly added in ultrasonic mixing afterwards, since natural polymer is practically insoluble in any solvent, mould material shape
It will not be destroyed with structure, continuation ultrasound is stablized until obtained emulsion without deposited phenomenon, is considered as and reaches mixing requirement；
3) mixing and molding: open mill is added in the chitosan mixed and polyimide powder, open mill temperature 110 is set
DEG C, it is kneaded 30min, obtains the composite sheet of chitosan and polyimides；
4) high-temperature calcination: moulding material is calcined 2 hours for 180 degrees Celsius in small-sized calcining furnace, gas shield is not necessarily to, obtains
To porous material.
Embodiment 3
The clean method for preparing that a kind of mixing prepares high-melting-point porous material is present embodiments provided, using lignin as mould
For plate molecule, polyphenylene sulfide are as packing material, mixing and molding high-melting-point porous material, step includes:
1) template molecule and packing material are prepared: purchase shape, size lignin material appropriate and ultra-fine (100nm
Within) pps powder；
2) mixed-powder: lignin and polyphenylene sulfide are weighed with mass ratio 2:8 ratio, two kinds of materials are made using grinding method
Uniformly mixing, and sample and see whether under an electron microscope uniformly, view is added in 5000 × observed under electron microscope in sample
Material is evenly distributed in open country, without obvious agglomeration, agglomeration, is considered as and reaches mixing requirement；
3) mixing and molding: open mill is added in the lignin mixed and pps powder, open mill temperature 150 is set
DEG C, it is kneaded 30min, obtains the composite sheet of lignin and polyphenylene sulfide；
4) high-temperature calcination: moulding material is calcined 2 hours for 230 degrees Celsius in small-sized calcining furnace, gas shield is not necessarily to, obtains
To porous material.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (9)
1. a kind of mixing prepares the clean method for preparing of high-melting-point porous material, step includes:
S1, prepare mould material and packing material: being filling with heat-resistant polymer using natural macromolecular material as mould material
The decomposition temperature of material, the heat-resistant polymer is higher than 350 DEG C；
S2, mould material and packing material are uniformly mixed, obtain mixing material；
S3, mixing and molding: form mixing material by open mill heating pressurization；
S4, high-temperature calcination: material at high temperature after molding is calcined, and the calcination temperature is higher than mould material decomposition temperature.
2. the clean method for preparing that mixing as described in claim 1 prepares high-melting-point porous material, it is characterised in that: step S1
In, the mould material includes one of cellulose, hemicellulose, chitosan or lignin；The packing material includes poly-
One or more of tetrafluoroethene, polyimides or polyphenylene sulfide.
3. the clean method for preparing that mixing as claimed in claim 1 or 2 prepares high-melting-point porous material, it is characterised in that: step
In rapid S1, the scale of the mould material is 1-10000nm.
4. the clean method for preparing that mixing as described in claim 1 prepares high-melting-point porous material, it is characterised in that: step S2
In, by percentage to the quality, the mould material accounts for the 10-50% of mixing material.
5. the clean method for preparing that mixing as claimed in claim 4 prepares high-melting-point porous material, it is characterised in that: step S2
In, it is uniformly mixed using the hybrid mode that dispersion in grinding or solvent obtains drying after suspension.
6. the clean method for preparing that mixing as claimed in claim 5 prepares high-melting-point porous material, it is characterised in that: step S2
In, it is described be ground to be ground to sample material in 5000 times of observed under electron microscope, the visual field be evenly distributed, without obvious knot
Block, agglomeration；The step of dispersion obtains suspension in the solvent includes: to disperse the powder of packing material in a solvent,
Mould material is uniformly added in ultrasonic mixing afterwards, continues ultrasound until obtained emulsion is stablized without deposited phenomenon.
7. the clean method for preparing that mixing as described in claim 1 prepares high-melting-point porous material, it is characterised in that: step S3
In, the time of the mixing is 25-35min, and melting temperature is 30-50 DEG C lower than the decomposition temperature of mould material.
8. the clean method for preparing that mixing as described in claim 1 prepares high-melting-point porous material, it is characterised in that: step S4
In, the calcination temperature is 10-30 DEG C higher than the decomposition temperature of mould material, and the calcination time is 1.5-2.5h.
9. the clean method for preparing that mixing as claimed in claim 8 prepares high-melting-point porous material, it is characterised in that: step S4
In, it is 150-170 DEG C by the corresponding calcination temperature of mould material of cellulose, using lignin as the corresponding calcining temperature of mould material
Degree is 220-240 DEG C, is 180-200 DEG C by the corresponding calcination temperature of mould material of chitosan.
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Citations (6)
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| JPS6166730A (en) * | 1984-09-07 | 1986-04-05 | Chuko Kasei Kogyo Kk | Production of porous material of polytetrafluoroethylene resin |
| US20050163924A1 (en) * | 2002-09-17 | 2005-07-28 | 3M Innovative Properties Company | Porous surfactant mediated metal oxide films |
| CN1807510A (en) * | 2006-02-07 | 2006-07-26 | 南京工业大学 | Thermoplastic polyimide microporous material and its preparation process |
| CN101528824A (en) * | 2006-08-18 | 2009-09-09 | 珀雷克斯公司 | Sintered polymeric materials and applications thereof |
| CN102504478A (en) * | 2011-11-24 | 2012-06-20 | 东北石油大学 | Porous-grade polyether-ether-ketone self-lubricating wear-resistant composite material and preparation method thereof |
| CN106062038A (en) * | 2014-03-18 | 2016-10-26 | 东丽株式会社 | Polyphenylene sulfide porous body and production method thereof, polyphenylene sulfide-thermoplastic resin block copolymer and production method thereof |
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2019
- 2019-01-31 CN CN201910095919.6A patent/CN109867891A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6166730A (en) * | 1984-09-07 | 1986-04-05 | Chuko Kasei Kogyo Kk | Production of porous material of polytetrafluoroethylene resin |
| US20050163924A1 (en) * | 2002-09-17 | 2005-07-28 | 3M Innovative Properties Company | Porous surfactant mediated metal oxide films |
| CN1807510A (en) * | 2006-02-07 | 2006-07-26 | 南京工业大学 | Thermoplastic polyimide microporous material and its preparation process |
| CN101528824A (en) * | 2006-08-18 | 2009-09-09 | 珀雷克斯公司 | Sintered polymeric materials and applications thereof |
| CN102504478A (en) * | 2011-11-24 | 2012-06-20 | 东北石油大学 | Porous-grade polyether-ether-ketone self-lubricating wear-resistant composite material and preparation method thereof |
| CN106062038A (en) * | 2014-03-18 | 2016-10-26 | 东丽株式会社 | Polyphenylene sulfide porous body and production method thereof, polyphenylene sulfide-thermoplastic resin block copolymer and production method thereof |
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