CN109860485A - A kind of polyimide nano-fiber diaphragm and its manufacturing method - Google Patents
A kind of polyimide nano-fiber diaphragm and its manufacturing method Download PDFInfo
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Abstract
The present invention relates to a kind of polyimide nano-fiber diaphragm and its manufacturing methods, which is characterized in that comprises the following steps: S1, preparing modifying agent, S2, spinning solution is prepared, S3, electrostatic spinning diaphragm is prepared, S4, prepares nano fiber diaphragm, S5, prepares polyimide diaphragm.The present invention reaches the intensity for not only increasing substantially nano fiber diaphragm using the method for adding a kind of homemade modifying agent and polyamic acid co-spun yarn, but also reduces the purpose in nano fiber diaphragm aperture；Method of the invention also has technical effect below: so that the mechanical property of polyimide nano-fiber diaphragm has been obtained significant raising polyimide resin structure applicatory extensive, and can improve the heat resistance of polyimide resin；Modifying agent can form good connection with polyimide fiber, improve the stability and mechanical property of fibre diaphragm by surface chemical structure and itself melting deformation during the preparation process.
Description
Technical field
The present invention relates to the methods of Preparation of Polyimide Nanofibers by Electrospinning diaphragm, and in particular to has high-strength
Degree, high temperature tolerance, a kind of polyimide nano-fiber diaphragm of high puncture-resistant intensity and its manufacturing method.
Background technique
Polyimides is a kind of ring chain compound in molecular structure containing imide structure, has high-strength and high-modulus, resistance to
The excellent performances such as high temperature, low temperature resistant and radiation hardness and excellent solvent resistance and dimensional stability, in addition its good biology
Compatibility and dielectric properties.By the polyimide nano-fiber diaphragm of method of electrostatic spinning preparation due in combination with fibre diaphragm
Large specific surface area, porosity height and polyimide high temperature-resistant and chemically stable characteristic, become present polymer nanofiber
The material that diaphragm is concerned.Currently, the polyimide nano-fiber diaphragm prepared by existing method of electrostatic spinning is due to ultra-fine fibre
Dimension arrangement is unordered, and volume is fluffy, is also simple physics accumulation between fiber, there is no very strong interactions, so receiving
The mechanical property of rice fibre diaphragm is generally poor, and aperture is larger, greatly limits its practical application.There are mainly two types of methods to solve
Above-mentioned problem, first is that, by be physically or chemically crosslinked improve nano fiber diaphragm intensity, as base extraction polyamic acid fiber every
Heat-treating methods have been made the polyimide fiber diaphragm with cross-linked structure after film, but this method will via base extraction and
The process of washing, technique are slightly complicated；Or using heat-fusible type resin and polyimide resin co-spun yarn, dependence is heat-fusible
The characteristics of type resin can be with high-temperature fusion, by heat treatment bring it about it is molten cause it is micro- be crosslinked, this method is because needing to have polyamides
The compatibility of imide resin is good, and the feature that temperature tolerance is high, and selectable resin is extremely limited, in addition heat-fusible type resin plus
Enter so that the viscosity of spinning solution increases considerably, is unfavorable for electrostatic spinning process.Another method is by surface coated ceramic
Slurry improves nano fiber diaphragm intensity, reduces aperture, but raising of this method to polyimide nano-fiber diaphragm intensity
It is extremely limited, and the cementability of ceramic particle and diaphragm is poor, is easy to cause " picking " phenomenon, durability is poor.
Summary of the invention
The present invention for the polyimide nano-fiber diaphragm of the preparation of method of electrostatic spinning in the prior art, tensile strength is low,
The disadvantage that punctured resistance is low, aperture is excessive, provides that a kind of simple process, applied widely, intensity is high, temperature tolerance is good, endurable
Pierce the polyimide nano-fiber diaphragm and preparation method thereof the features such as intensity is high and the high aperture of porosity is small.
To realize the technical purpose, the present invention provides a kind of preparation methods of polyimide nano-fiber diaphragm, include
Following steps:
S1, modifying agent is prepared, modifying agent is made in the modification of glass powder surface；
S2, spinning solution is prepared, spinning solution is made in modifying agent and polyamic acid (PAA) solution blending；
S3, electrostatic spinning diaphragm is prepared, (loosely) electrostatic spinning diaphragm is made by electrostatic spinning in spinning solution；
S4, prepare nano fiber diaphragm, will (loose) electrostatic spinning diaphragm by hot pressing be processed into nanofiber every
Film；
S5, polyimide diaphragm is prepared, nano fiber diaphragm is obtained into polyimide diaphragm using Fractional Heat-treatment.
Preferably, the glass powder is glass powder with low melting point.
Preferably, glass powder with low melting point melting temperature is 300 DEG C -500 DEG C, and granularity is -2000 mesh of 100 mesh.
Specifically, the modification method that the glass powder surface is modified to modifying agent includes: to be added to glass powder to contain
Have in the coupling agent solution of 5wt%-50wt%, under conditions of temperature is 5 DEG C -80 DEG C, turns in 100r/min-8000r/min
Speed is lower to stir 0.5h-10h, and modifying agent is made in filtering, drying.
Preferably, the coupling agent is selected from containing amino, vinyl, epoxy group, acrylate-based, acryloxy silane
One of coupling agent is a variety of, and solvent used in the coupling agent solution is selected from: water, ethyl alcohol, methanol, acetone, normal propyl alcohol,
Isopropanol, ethylene glycol, propylene glycol, N, N '-dimethyl formamide, N, one of N '-dimethyl acetamide and dimethyl sulfoxide
Or a variety of mixed solution.
Specifically, the preparation method of the modifying agent and polyamic acid (PAA) blend solution includes: in -5 DEG C of -20 DEG C of temperature
0.5h-2h is stirred under the conditions of degree is made spinning solution, the weight ratio of modifying agent and polyamic acid (PAA) is (1:20)-(1:1),
It is further preferred that being (1:20)-(1:10).The weight ratio of modifying agent and polyamic acid is between 1:20 to 1:1, additive amount mistake
It will affect the performance of diaphragm greatly, additive amount is too small, does not have corresponding effect.
Preferably, the polyamic acid (PAA) solution concentration is 5wt%-18wt%, solvent N, N '-dimethyl first
Amide, N, one of N '-dimethyl acetamide, N-Methyl pyrrolidone, tetrahydrofuran, methanol, ethyl alcohol, isopropanol or more
Kind.
Specifically, the electrostatic spinning process condition is spinning flow 0.01mL/min-1mL/min, needle point to receiver board
Or the distance of receiving roll is 100mm-500mm, spinning voltage 10KV-30KV.
Specifically, the hot pressing fabrication process condition is 100 DEG C -150 DEG C of hot pressing temperature, hot pressing pressure 10KG-30KG, heat
Press the time: 0.1s-2s.
Specifically, it includes the first stage that the use Fractional Heat-treatment, which obtains polyimide diaphragm specific steps: heating speed
1 DEG C/min-10 DEG C/min of rate, 80 DEG C -120 DEG C of stage last heat treatment temperature are warming up to heat treatment temperature, keep 30min；The
Two-stage: 1 DEG C/min-10 DEG C/min of heating rate, is warming up to heat treatment temperature by 220 DEG C -450 DEG C of final heat treatment temperature, protects
Hold 30min-60min.
It is another object of the present invention to provide a kind of polyimide nano-fiber diaphragm, it includes polyimides and low
Melting glass frit.
Further, glass powder with low melting point melting temperature is 300 DEG C -500 DEG C.
Further, which is now that diaphragm is prepared using above-mentioned method.
Technical solution of the present invention has the advantage that
Using the method for adding a kind of homemade modifying agent and polyamic acid co-spun yarn, reaches and both increase substantially Nanowire
Dimension reduces the purpose in nano fiber diaphragm aperture every film strength；
Compared with prior art, method of the invention also has technical effect below:
1, polyimide nano-fiber diaphragm produced by the present invention has physical crosslinking structure, and the introducing of crosslinking points makes to gather
The mechanical property of acid imide nano fiber diaphragm has obtained significant raising；
2, the present invention is applicatory poly- compared with conventional organic resin blending and modifying polyimide nano-fiber diaphragm method
Imide resin structure is extensive, and can improve the heat resistance of polyimide resin；
3, the present invention is compared with general inorganic/polyimides blending and modifying polyimide nano-fiber diaphragm method, this hair
Bright modifying agent can be formed good by surface chemical structure and itself melting deformation during the preparation process with polyimide fiber
Good connection, improves the stability and mechanical property of fibre diaphragm.
4, present invention process route is simple, and polyimide nano-fiber membrane properties obtained are excellent, has preferable produce
Industry prospect.
Specific embodiment
Below based on embodiment, present invention is described, it should be understood by one skilled in the art that provided herein
Embodiment is provided to the purpose of explanation, and the protection scope of invention is not limited to following embodiments.
For not specifically specified technological parameter, routine techniques progress can refer to.
Embodiment 1
A kind of preparation method of polyimide nano-fiber diaphragm, specific steps are as follows:
S1, modifying agent is prepared
It is 350 DEG C by fusing point, granularity is that the glass powder of 1000 mesh is added to the 3- aminopropyl triethoxysilicane of 10wt%
In the ethanol solution of alkane, under conditions of temperature is 30 DEG C, 2h is stirred under 2000r/min revolving speed, then by filtering, drying system
Obtain modifying agent；
S2, spinning solution is prepared
To with 4,4'- biphenyl ether dianhydride (ODPA) and 4,4- diphenyldiamine (ODA) is the polyamic acid of raw material preparation
(PAA) above-mentioned modifying agent is added in solution, stirs 0.5h under the conditions of 0 DEG C, spinning solution is made.The weight ratio of modifying agent and PAA is
1:20；The concentration of PAA solution: the solution of 10wt%；Solvent are as follows: N, N '-dimethyl formamide；
S3, electrostatic spinning diaphragm is prepared
Electrostatic spinning diaphragm loosely, Static Spinning is made using method of electrostatic spinning in spinning solution obtained in step S2
Silk process conditions: spinning flow are as follows: the distance of 0.5mL/min, needle point to receiver board or receiving roll is 300mm, spinning voltage are as follows:
25KV；
S4, nano fiber diaphragm is prepared
Electrostatic spinning diaphragm obtained in step S3 is passed through into hot pressing processing technology, obtains nano fiber diaphragm, hot pressing work
Skill condition: hot pressing temperature: 110 DEG C, hot pressing pressure are as follows: 25KG, hot pressing time: 0.5s；
S5, polyimide diaphragm is prepared
Nano fiber diaphragm obtained in step S4 is placed in high temperature oven, is prepared using piecewise heat treatment method poly-
The first stage: heating rate: acid imide diaphragm 5 DEG C/min, is warming up to 80 DEG C, keeps 30min, second stage: heating rate: 5
DEG C/min, final heat treatment temperature: 350 DEG C, keep 60min.
Embodiment 2
S1, modifying agent is prepared
It is 400 DEG C by fusing point, granularity is that the glass powder of 1200 mesh is added to the γ-(2,3- the third oxygen of epoxy) third of 12wt%
In ethanol/water (95v/5v) solution of base trimethoxy silane, under conditions of temperature is 25 DEG C, stirred under 5000r/min revolving speed
4h is mixed, modifying agent then is made by filtering, drying；
S2, spinning solution is prepared
To with pyromellitic acid anhydride (PMDA) and 4,4- diphenyldiamine (ODA) is the polyamic acid of raw material preparation
(PAA) above-mentioned modifying agent is added in solution, stirs 1h under the conditions of 5 DEG C, spinning solution is made.The weight ratio of modifying agent and PAA are as follows: 1:
15.The concentration of PAA solution: the solution of 12wt%；Solvent are as follows: N, N '-dimethyl formamide/tetrahydrofuran (80v/20v)；
S3, electrostatic spinning diaphragm is prepared
Electrostatic spinning diaphragm loosely, Static Spinning is made using method of electrostatic spinning in spinning solution obtained in step S2
Silk process conditions: spinning flow are as follows: the distance of 0.3mL/min, needle point to receiver board or receiving roll is 300mm, spinning voltage are as follows:
25KV；
S4, nano fiber diaphragm is prepared
Electrostatic spinning diaphragm obtained in step S3 is passed through into hot pressing processing technology, obtains nano fiber diaphragm, hot pressing work
Skill condition: hot pressing temperature: 110 DEG C, hot pressing pressure are as follows: 25KG, hot pressing time: 1s；
S5, polyimide diaphragm is prepared
Nano fiber diaphragm obtained in step S4 is placed in high temperature oven, is prepared using piecewise heat treatment method poly-
The first stage: heating rate: acid imide diaphragm 5 DEG C/min, is warming up to 80 DEG C, keeps 30min, second stage: heating rate: 5
DEG C/min, final heat treatment temperature: 400 DEG C, keep 45min.
Embodiment 3
S1, modifying agent is prepared
It is 450 DEG C by fusing point, granularity is that the glass powder of 2000 mesh is added to γ-(methacryloxypropyl) propyl of 12wt%
In ethyl alcohol/normal propyl alcohol (60v/40v) solution of trimethoxy silane, under conditions of temperature is 50 DEG C, under 8000r/min revolving speed
4h is stirred, modifying agent then is made by filtering, drying.
S2, spinning solution is prepared
It is poly- to being prepared using 4,4'- biphenyl ether dianhydride (ODPA) and bis- (the trifluoromethoxy)-benzidines of 2,2'- as raw material
Above-mentioned modifying agent is added in amic acid (PAA) solution, stirs 2h under the conditions of 0 DEG C, spinning solution is made.The weight of modifying agent and PAA
Than are as follows: 1:12.The concentration of PAA solution: the solution of 8wt%；Solvent are as follows: N-Methyl pyrrolidone/ethyl alcohol (90v/10v).
S3, electrostatic spinning diaphragm is prepared
Electrostatic spinning diaphragm loosely, Static Spinning is made using method of electrostatic spinning in spinning solution obtained in step S2
Silk process conditions: spinning flow are as follows: the distance of 0.1mL/min, needle point to receiver board or receiving roll is 250mm, spinning voltage are as follows:
30KV；
S4, nano fiber diaphragm is prepared
Electrostatic spinning diaphragm obtained in step S3 is passed through into hot pressing processing technology, obtains nano fiber diaphragm, hot pressing work
Skill condition: hot pressing temperature: 110 DEG C, hot pressing pressure are as follows: 25KG, hot pressing time: 1s；
S5, polyimide diaphragm is prepared
Nano fiber diaphragm obtained in step S4 is placed in high temperature oven, is prepared using piecewise heat treatment method poly-
The first stage: heating rate: acid imide diaphragm 5 DEG C/min, is warming up to 100 DEG C, keeps 30min, second stage: heating rate:
5 DEG C/min, final heat treatment temperature: 450 DEG C, keep 40min.
Comparative example:
The preparation of S1, electrostatic spinning diaphragm
By 4,4'- biphenyl ether dianhydride (ODPA) and 4,4- diphenyldiamine (ODA) is the polyamic acid (PAA) of raw material preparation
Electrostatic spinning diaphragm loosely is made using method of electrostatic spinning in solution, in which: the concentration of PAA solution: the solution of 16wt%；It is molten
Agent are as follows: N, N '-dimethyl acetamide.Electrostatic spinning process condition: spinning flow are as follows: 0.1mL/min or connects needle point to receiver board
The distance for receiving roller is 300mm, spinning voltage are as follows: 20KV；
The preparation of S2, nano fiber diaphragm
Electrostatic spinning diaphragm obtained in step S1 is passed through into hot pressing processing technology, obtains nano fiber diaphragm, hot pressing work
Skill condition: hot pressing temperature: 105 DEG C, hot pressing pressure are as follows: 20KG, hot pressing time: 0.3s；
The preparation of S3, polyimide diaphragm
Nano fiber diaphragm obtained in step S2 is placed in high temperature oven, is prepared using piecewise heat treatment method poly-
The first stage: heating rate: acid imide diaphragm 5 DEG C/min, is warming up to 80 DEG C, keeps 30min, second stage: heating rate: 5
DEG C/min, final heat treatment temperature: 300 DEG C, it is warming up to heat treatment temperature, keeps 20min.
Relative to the pure polyimide nanofiber membrane of method of electrostatic spinning preparation, the present invention adds a kind of homemade low melting point
The modifying agent that glass powder surface is modified to, using the method for itself and polyamic acid co-spun yarn, in stringent technological parameter and condition
Control under, the modified polyimide nano fiber diaphragm prepared has that simple process, applied widely, intensity is high, heatproof
Property good, puncture-resistant intensity it is high and the features such as the high aperture of porosity is small, advantageously account for the safety of power battery and use the longevity
Life, widens the application field of polyimide nano-fiber diaphragm.Specific performance comparison see the table below 1.
The comparison of 1 polyimide nano-fiber membrane properties of table
Claims (10)
1. a kind of preparation method of polyimide nano-fiber diaphragm, which is characterized in that comprise the following steps:
S1, modifying agent is prepared, modifying agent is made in the modification of glass powder surface；
S2, spinning solution is prepared, spinning solution is made in modifying agent and polyamic acid PAA solution blending；
S3, electrostatic spinning diaphragm is prepared, electrostatic spinning diaphragm is made by electrostatic spinning in spinning solution；
S4, nano fiber diaphragm is prepared, electrostatic spinning diaphragm is processed into nano fiber diaphragm by hot pressing；
S5, polyimide diaphragm is prepared, nano fiber diaphragm is obtained into polyimide diaphragm using Fractional Heat-treatment.
2. preparation method according to claim 1, which is characterized in that the glass powder melting temperature is 300 DEG C -500 DEG C,
Granularity is -2000 mesh of 100 mesh.
3. preparation method according to claim 1, which is characterized in that the glass powder surface is modified to the modification of modifying agent
Method and step includes: that glass powder is added in the coupling agent solution containing 5wt%-50wt%, is 5 DEG C -80 DEG C in temperature
Under the conditions of, 0.5h-10h is stirred under 100r/min-8000r/min revolving speed, obtained modifying agent is dried in filtering.
4. preparation method according to claim 3, which is characterized in that the coupling agent, which is selected from, contains amino, vinyl, epoxy
One of base, acrylate-based, acryloxy silane coupling agent or a variety of, solvent used in the coupling agent solution
It is selected from: water, ethyl alcohol, methanol, acetone, normal propyl alcohol, isopropanol, ethylene glycol, propylene glycol, N, N '-dimethyl formamide, N, N '-two
One of methylacetamide and dimethyl sulfoxide or a variety of mixed solutions.
5. preparation method according to claim 1, which is characterized in that the modifying agent and polyamic acid PAA blend solution
Preparation method include: under the conditions of -5 DEG C of -20 DEG C of temperature stir 0.5h-2h spinning solution, modifying agent and polyamic acid is made
The weight ratio of PAA is (1:20)-(1:1).
6. preparation method according to claim 1, which is characterized in that the polyamic acid PAA solution concentration is
5wt%-18wt%, solvent N, N '-dimethyl formamide, N, N '-dimethyl acetamide, N-Methyl pyrrolidone, tetrahydro furan
It mutters, one of methanol, ethyl alcohol, isopropanol or a variety of.
7. preparation method according to claim 1, which is characterized in that the electrostatic spinning process condition is spinning flow
The distance of 0.01mL/min-1mL/min, needle point to receiver board or receiving roll is 100mm-500mm, spinning voltage 10KV-
30KV。
8. preparation method according to claim 1, which is characterized in that the hot pressing fabrication process condition is hot pressing temperature
100 DEG C -150 DEG C, hot pressing pressure 10KG-30KG, hot pressing time: 0.1s-2s；It is described that polyimides is obtained using Fractional Heat-treatment
Diaphragm specific steps include the first stage: 1 DEG C/min-10 DEG C/min of heating rate, 80 DEG C -120 of stage last heat treatment temperature
DEG C, it is warming up to heat treatment temperature, keeps 30min；Second stage: 1 DEG C/min-10 DEG C/min of heating rate, final heat treatment temperature
220 DEG C -450 DEG C of degree is warming up to heat treatment temperature, keeps 30min-60min.
9. a kind of polyimide nano-fiber diaphragm, it is characterised in that include polyimides and glass powder, wherein glass powder is molten
Melting temperature is 300 DEG C -500 DEG C.
10. polyimide nano-fiber diaphragm according to claim 9, it is characterised in that appoint using in claim 1-8
Method described in one is prepared.
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| CN113604014A (en) * | 2021-08-24 | 2021-11-05 | 江阴市宏丰塑业有限公司 | High-weather-resistance high-rigidity glass fiber reinforced PBT (polybutylene terephthalate) -PET (polyethylene terephthalate) alloy modified material |
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| CN111640902A (en) * | 2020-06-08 | 2020-09-08 | 淮北市吉耐新材料科技有限公司 | Preparation process of lithium battery diaphragm |
| CN113604014A (en) * | 2021-08-24 | 2021-11-05 | 江阴市宏丰塑业有限公司 | High-weather-resistance high-rigidity glass fiber reinforced PBT (polybutylene terephthalate) -PET (polyethylene terephthalate) alloy modified material |
| CN114635230A (en) * | 2022-04-02 | 2022-06-17 | 天津工业大学 | Bulk phase super-hydrophobic nanofiber membrane for membrane distillation and preparation method thereof |
| CN114635230B (en) * | 2022-04-02 | 2024-03-26 | 天津工业大学 | Bulk super-hydrophobic nanofiber membrane for membrane distillation and preparation method thereof |
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