CN107829302A - A kind of method that ultraviolet light irradiation prepares improved polyalkene non-woven membrane - Google Patents
A kind of method that ultraviolet light irradiation prepares improved polyalkene non-woven membrane Download PDFInfo
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- CN107829302A CN107829302A CN201711106052.7A CN201711106052A CN107829302A CN 107829302 A CN107829302 A CN 107829302A CN 201711106052 A CN201711106052 A CN 201711106052A CN 107829302 A CN107829302 A CN 107829302A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/28—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
Abstract
The present invention relates to a kind of method that ultraviolet light irradiation prepares improved polyalkene non-woven membrane, belong to field of high polymer material modification.This method comprises the following steps：Vinyl silicane coupling agent is stirred in water and obtains the vinyl nano SiO 2 particle hydrosol, adds hydrophilic graft monomer and initiator thereto, it is standby to lead to nitrogen；Polyolefm non-woven barrier film is cleaned using acetone, is put into after drying in the above-mentioned vinyl nano SiO 2 particle hydrosol and soaks 10min；Polyolefm non-woven barrier film after immersion is subjected to graft modification under ultraviolet light irradiation and nitrogen protection, takes out, clean after reaction, being dried to obtain improved polyalkene non-woven membrane.Improved polyalkene non-woven membrane prepared by the present invention has the advantages that good hydrophilic property, rate of liquid aspiration are high, alkalis suction quantity is big, heat endurance is high.
Description
Technical field
The present invention relates to a kind of field of high polymer material modification, more particularly to a kind of prepared using ultraviolet light irradiation is changed
The method of property polyolefm non-woven barrier film.
Background technology
Ni-MH battery (MH-Ni batteries) has many good qualities, such as bigger than energy, and specific power is high, can high-multiplying power discharge, circulation
Long lifespan, memory-less effect is pollution-free, non-maintaining, securely and reliably, non-environmental-pollution etc., thus receive significant attention, turn into generation
One of focus of various countries of boundary secondary cell development.Battery diaphragm is one of stock for forming battery, is except positive and negative in battery
Another important part outside electrode and electrolyte, " the 3rd electrode " of battery of being known as.Nickel-hydrogen battery separator is more
Selection Fypro barrier film, polyester fiber barrier film, polyvinyl chloride flexible plastic barrier film, semipermeable membrane and new type polyolefin is non-knits
Barrier film is made, wherein it is polyolefm non-woven barrier film that research application is more.
Polyolefine fiber molecular structure quite stable, the polyolefm non-woven cloth produced with it have the chemistry of height steady
Qualitative (such as alkaline-resisting, resistance to oxidation), almost without weight loss in highly basic, and can higher temperature (>100 DEG C) under use, also have
Have preferable mechanical strength and toughness, proportion is small, ratio resistance is small, good permeability, the series of advantages such as cheap, be more to manage
The battery diaphragm base material thought.But due to not having hydrophilic radical in polyolefin macromolecular structure, and crystallinity is high, while fiber is cut
Face is rounded, compact structure, lacks micropore and gap, so the hydrophily extreme difference of polyolefin.Therefore the polyolefin produced is non-
Woven cloths battery diaphragm alkalis suction quantity is low, and it is slow to inhale alkali speed, causes infiltration to electrolyte and holding capacity poor, turn into restriction its
The basic reason applied in Ni-MH battery.
For the shortcomings of polyolefine fiber, its hydrophilicity, Jin Erke are improved using the method for graft modification mostly
To improve the suction alkali speed of polyolefm non-woven barrier film and alkalis suction quantity, infiltration and holding capacity of its barrier film to electrolyte are lifted.
Monomer for graft modification be some one end with can be formed with other polymers or inorganic filler, fiber surface active force compared with
Strong chemical bond or the polar group of hydrogen bond, the other end carry low point of the vinyl that can be grafted on polyolefin or unsaturated bond
Sub- organic compound, mainly there are maleic anhydride, acrylicacidandesters, methacrylic acid and its ester, styrene, methacrylic acid contracting
Water glyceride etc..
Chinese invention patent 201010589184.1 discloses a kind of novel nickel-hydrogen battery diaphragm, including barrier film base fabric and sulphur
Acidic group, sulfonic group are equably grafted on the surface of barrier film base fabric by sulfonation processing, and acrylic monomer is anti-by chemical graft
The surface of barrier film base fabric should be equably grafted on, barrier film base fabric is made up of polyolefin sheath core fiber or by polypropylene fibre system
It is made into or by the collocation of polyolefin sheath core fiber and polypropylene fibre, by wet papermaking or dry carding technological forming,
Spun lacing is reinforced and is made.The novel nickel-hydrogen battery diaphragm of the disclosure of the invention, chemical stability is good, oxidation resistance is strong, intensity is big
The characteristics of.But the invention carries out sulfonation processing using gaseous sulfur trioxide to polyalkene diaphragm, and the requirement to sulfonation equipment is higher,
And a large amount of acid waste waters can be produced, processing cost is big and cost is higher.
Chinese invention patent 201610954848.7 disclose a kind of modified polyolefin hydro carbons barrier film for covering silicon dioxide layer and
Its preparation method.After ammoniacal liquor, water, ethanol and Tween 80 are well mixed, then tetraethyl orthosilicate is added thereto, stir,
TPO barrier film is added, after soaking a period of time, takes out and cleans, dries, that is, product is made.But the dioxy prepared using the method
Silica dioxide coating on SiClx coating polyalkene diaphragm easily comes off, and performance is unstable, and service life is shorter.
The modification technology of existing polyolefm non-woven barrier film, which is concentrated mainly on, carries out hydrophilic modifying aspect to it, to improve it
With the compatibility and imbibition ability of Ni-MH battery electrolyte, but complex process, the damage to barrier film are larger.In addition, a small amount of research
Polyolefm non-woven barrier film is modified using inorganic nanoparticles and improves its heat endurance, but inorganic nanoparticles and barrier film
Connect insecure, easily fall off, on the one hand cause modified diaphragm performance unstable, on the other hand can influence the property of Ni-MH battery
Energy and safety.
The content of the invention
The purpose of the present invention is to avoid above-mentioned the deficiencies in the prior art part and provide a kind of ultraviolet light irradiation preparation and change
The method of property polyolefm non-woven barrier film.To achieve these goals, the present invention adopts the following technical scheme that：
A kind of method that ultraviolet light irradiation prepares improved polyalkene non-woven membrane, specifically include following process and step
Suddenly：A) 12~18h will be stirred at room temperature in vinyl silicane coupling agent addition deionized water obtain the vinyl of transparent and homogeneous
The nano SiO 2 particle hydrosol, grafted monomers and initiator are then added into the vinyl nano SiO 2 particle hydrosol
In, stir, be passed through high pure nitrogen 30min, it is standby；
B) after polyolefm non-woven barrier film being cleaned using acetone, spontaneously drying, immerse above-mentioned added with grafted monomers and drawing
In the vinyl nano SiO 2 particle hydrosol for sending out agent, 10min is soaked；
C) the polyolefm non-woven barrier film after immersion is transferred to 5~20mm under uviol lamp, under nitrogen protection irradiate 2~
30min carries out graft modification；
D) polyolefm non-woven barrier film is taken out after reaction terminates, 2~4h is cleaned with hot deionized water, to remove membrane surface
Homopolymer；It is then placed in baking oven and is dried at 50 DEG C, obtains improved polyalkene non-woven membrane.
In above-mentioned preparation method, described vinyl silicane coupling agent is vinyltrimethoxy silane, the second of vinyl three
In TMOS, the tert-butoxy silane of vinyl three, vinyl silane tri-butyl peroxy and vinyltriacetoxy silane
One or more, the quality of step c medium vinyl silane couplers is the 2%~15% of deionized water quality.
In above-mentioned preparation method, described grafted monomers be acrylic acid, methacrylic acid and acrylamide in one kind or
Several, initiator is ammonium persulfate or ammonium ceric nitrate.
In above-mentioned preparation method, mass concentration of the grafted monomers in the hydrosol is 2%~20%, and initiator is in water
Mass concentration in colloidal sol is 0.05%~0.3%.
In above-mentioned preparation method, described polyolefm non-woven barrier film is polyethylene nonwoven barrier film, polypropylene nonwoven
One kind in barrier film and ES non-woven membranes.
In above-mentioned preparation method, described exposure time is preferably 5~20min.
Compared with prior art, the advantage of the invention is that being carried out by above-mentioned preparation method to polyolefm non-woven barrier film
Hydrophilic modifying is grafted, the hydrophily of improved polyalkene non-woven membrane is efficiently improved, inhales alkali speed and alkalis suction quantity；The present invention adopts
Graft reaction is participated in the vinyl nano SiO 2 particle hydrosol, nano SiO 2 particle is connected to grafting segment
On, and tridimensional network is constituted as " bridged bond " of the intersegmental crosslinking of different grafted chains, on the one hand further increase modification
The hydrophily of polyolefm non-woven barrier film, inhale alkali speed and alkalis suction quantity, another aspect nano SiO 2 particle are connected firmly, made
Do not fallen off during, significantly improve the heat endurance and cyclical stability on improved polyalkene non-woven membrane surface.
Brief description of the drawings
Fig. 1 is the stereoscan photograph on improved polyalkene non-woven fabrics membrane fibers surface.
Embodiment
The present invention is described in further detail with reference to embodiment and accompanying drawing, but the invention is not limited in following
Embodiment.
Embodiment 1：
Transparent and homogeneous are obtained by 12h is stirred at room temperature in 5g vinyltrimethoxy silanes addition 95g deionized waters
The vinyl nano SiO 2 particle hydrosol, 10g acrylic acid and 0.2g ammonium persulfates are then added into vinyl silica
In the nano particle hydrosol, stir, be passed through high pure nitrogen 30min, it is standby；Polypropylene nonwoven barrier film is washed using acetone
Only after, spontaneously drying, immersion is above-mentioned added with the vinyl nano SiO 2 particle hydrosol of acrylic acid and ammonium persulfate, soaks
10min is steeped, is then transferred under uviol lamp at 10mm, 8min is irradiated under nitrogen protection and carries out graft modification；After reaction terminates
Polypropylene nonwoven barrier film is taken out, 2h is cleaned with hot deionized water, is then placed in baking oven and is dried at 50 DEG C, is obtained modified poly-
Polypropylene nonwoven barrier film.
Embodiment 2：
Transparent and homogeneous are obtained by 15h is stirred at room temperature in 2g VTESs addition 100g deionized waters
The vinyl nano SiO 2 particle hydrosol, 15g methacrylic acids and 0.08g ammonium ceric nitrates are then added into vinyl dioxy
In the SiClx nano particle hydrosol, stir, be passed through high pure nitrogen 30min, it is standby；Polyethylene nonwoven barrier film is used third
Ketone is cleaned, after natural drying, is immersed above-mentioned added with methacrylic acid and the vinyl nano SiO 2 particle water of ammonium ceric nitrate
In colloidal sol, 10min is soaked, is then transferred under uviol lamp at 5mm, irradiated 20min under nitrogen protection and carry out graft modification；Instead
Polyethylene nonwoven barrier film is taken out after should terminating, 2h is cleaned with hot deionized water, is then placed in baking oven and is dried at 50 DEG C, obtained
To modified poly ethylene non-woven membrane.Fig. 1 is the scanning of modified poly ethylene non-woven membrane fiber surface made from the present embodiment
Electromicroscopic photograph.
Embodiment 3
Will 15g vinyltriacetoxy silanes add 100g deionized waters in stir at room temperature 18h obtain it is homogeneous
The bright vinyl nano SiO 2 particle hydrosol, 4g acrylamides and 0.3g ammonium persulfates are then added into vinyl dioxy
In the SiClx nano particle hydrosol, stir, be passed through high pure nitrogen 30min, it is standby；Polypropylene nonwoven barrier film is used third
Ketone is cleaned, after natural drying, and it is water-soluble to immerse the above-mentioned vinyl nano SiO 2 particle added with acrylamide and ammonium persulfate
In glue, 10min is soaked, is then transferred under uviol lamp at 20mm, irradiated 12min under nitrogen protection and carry out graft modification；Instead
Polypropylene nonwoven barrier film is taken out after should terminating, 4h is cleaned with hot deionized water, is then placed in baking oven and is dried at 50 DEG C, obtained
To modified polypropene non-woven membrane.
Embodiment 4
Will the tert-butoxy silane of 10g vinyl three add 100g deionized waters in stir at room temperature 16h obtain it is homogeneous
The bright vinyl nano SiO 2 particle hydrosol, 10g acrylamides and 0.2g ammonium ceric nitrates are then added into vinyl two
In the silica nano particle hydrosol, stir, be passed through high pure nitrogen 30min, it is standby；ES non-woven membranes are used into acetone
Clean, after natural drying, immerse above-mentioned added with acrylamide and the vinyl nano SiO 2 particle hydrosol of ammonium ceric nitrate
In, 10min is soaked, is then transferred under uviol lamp at 9mm, 15min is irradiated under nitrogen protection and carries out graft modification；Reaction knot
ES non-woven membranes are taken out after beam, 4h is cleaned with hot deionized water, is then placed in baking oven and is dried at 50 DEG C, obtain being modified ES
Non-woven membrane.
Comparative example 1
10g acrylic acid and 0.2g ammonium persulfates are added in 95g deionized waters and stirred at room temperature, is passed through High Purity Nitrogen
Gas 30min, it is standby；Polypropylene nonwoven barrier film is cleaned using acetone, after natural drying, immersed above-mentioned added with acrylic acid and mistake
In the aqueous solution of ammonium sulfate, 10min is soaked, is then transferred under uviol lamp at 10mm, irradiated 8min under nitrogen protection and carry out
Graft modification；Reaction takes out polypropylene nonwoven barrier film after terminating, and cleans 2h with hot deionized water, is then placed in baking oven 50
Dried at DEG C, obtain modified polypropene non-woven membrane.
Comparative example 2
2g VTESs, 15g methacrylic acids and 0.08g ammonium ceric nitrates are added in 100g deionized waters
Stir at room temperature, be passed through high pure nitrogen 30min, it is standby；Polyethylene nonwoven barrier film is cleaned using acetone, be naturally dry
After dry, immerse in the above-mentioned aqueous solution added with VTES, methacrylic acid and ammonium ceric nitrate, soak 10min,
It is then transferred under uviol lamp at 5mm, irradiates 20min under nitrogen protection and carry out graft modification；Reaction takes out poly- second after terminating
Alkene non-woven membrane, 2h is cleaned with hot deionized water, be then placed in baking oven and dried at 50 DEG C, obtain that modified poly ethylene is non-to be knitted
Make barrier film.
Comparative example 3
6g nano SiO 2 particles, 10g acrylamides and 0.2g ammonium ceric nitrates are added in 100g deionized waters in room
Stirred under temperature, be passed through high pure nitrogen 30min, it is standby；ES non-woven membranes are cleaned using acetone, after natural drying, leaching
Enter in the above-mentioned aqueous solution added with nano SiO 2 particle, acrylamide and ammonium ceric nitrate, soak 10min, be then transferred into
Under uviol lamp at 9mm, 15min is irradiated under nitrogen protection and carries out graft modification；Reaction takes out ES non-woven membranes after terminating, and uses
Hot deionized water cleans 4h, is then placed in baking oven and is dried at 50 DEG C, obtains being modified ES non-woven membranes.
Table 1 is before polyolefm non-woven diagram modification and 1~embodiment of the embodiment of the present invention 4,1~comparative example of comparative example 3
The property of obtained improved polyalkene non-woven membrane.
Property before and after the polyolefm non-woven diagram modification of table 1
Understood according to the property contrast before and after polyolefm non-woven diagram modification in table 1, modified polyolefin prepared by the present invention
Hydrocarbon non-woven membrane has the advantages that good hydrophilic property, rate of liquid aspiration are high, alkalis suction quantity is big, heat endurance is high.
In the preparation process of the present invention, vinyl silicane coupling agent is made by sol method has the two of multiple vinyl
The silica nano particle hydrosol, then add grafted monomers thereto and initiator participates in polyolefm non-woven barrier film together
Graft modification is reacted, and nano SiO 2 particle is connected on grafting segment, and as the " bridge of the intersegmental crosslinking of different grafted chains
Key " constitutes tridimensional network, on the one hand further increases the hydrophily of improved polyalkene non-woven membrane, inhales alkali speed
And alkalis suction quantity, another aspect nano SiO 2 particle are connected firmly, not fallen off during use, significantly improve modified polyolefin
The heat endurance and cyclical stability of hydrocarbon non-woven membrane.And nano SiO 2 particle is directly added into reaction system, or
Vinyl silicane coupling agent is directly added graft modification reaction system by person, can not realize above beneficial effect.
Claims (6)
1. a kind of method that ultraviolet light irradiation prepares improved polyalkene non-woven membrane, it is characterised in that have following process and
Step：
A) 12~18h will be stirred at room temperature in vinyl silicane coupling agent addition deionized water obtain the vinyl of transparent and homogeneous
The nano SiO 2 particle hydrosol, grafted monomers and initiator are then added into the vinyl nano SiO 2 particle hydrosol
In, stir, be passed through high pure nitrogen 30min, it is standby；
B) polyolefm non-woven barrier film is cleaned using acetone, after natural drying, immersed above-mentioned added with grafted monomers and initiator
The vinyl nano SiO 2 particle hydrosol in, soak 10min；
C) the polyolefm non-woven barrier film after immersion is transferred to 5~20mm under uviol lamp, under nitrogen protection irradiate 2~
30min carries out graft modification；
D) polyolefm non-woven barrier film is taken out after reaction terminates, 2~4h is cleaned with hot deionized water, to remove the equal of membrane surface
Polymers；It is then placed in baking oven and is dried at 50 DEG C, obtains improved polyalkene non-woven membrane.
2. the method that a kind of ultraviolet light irradiation according to claim 1 prepares improved polyalkene non-woven membrane, its feature
It is described vinyl silicane coupling agent for vinyltrimethoxy silane, VTES, the uncle of vinyl three
One or more in butoxy silane, vinyl silane tri-butyl peroxy and vinyltriacetoxy silane, in step c
The quality of vinyl silicane coupling agent is the 2%~15% of deionized water quality.
3. the method that a kind of ultraviolet light irradiation according to claim 1 prepares improved polyalkene non-woven membrane, its feature
One or more in being acrylic acid, methacrylic acid and acrylamide in described grafted monomers, initiator is persulfuric acid
Ammonium or ammonium ceric nitrate.
4. the method that a kind of ultraviolet light irradiation according to claim 1 prepares improved polyalkene non-woven membrane, its feature
It is 2%~20% in the mass concentration in the grafted monomers in the hydrosol, mass concentration of the initiator in the hydrosol is
0.05%~0.3%.
5. the method that a kind of ultraviolet light irradiation according to claim 1 prepares improved polyalkene non-woven membrane, its feature
In being polyethylene nonwoven barrier film, polypropylene nonwoven barrier film and ES non-woven membranes in described polyolefm non-woven barrier film
One kind.
6. the method that a kind of ultraviolet light irradiation according to claim 1 prepares improved polyalkene non-woven membrane, its feature
It is that described exposure time is preferably 5~20min.
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| CN112133871A (en) * | 2020-09-24 | 2020-12-25 | 湖南省凯纳方科技有限公司 | Surface grafting method of mh-ni battery diaphragm |
| CN112133870A (en) * | 2020-09-24 | 2020-12-25 | 湖南省凯纳方科技有限公司 | Preparation process of battery diaphragm for increasing ion exchange capacity |
| CN112553880A (en) * | 2020-11-24 | 2021-03-26 | 东华大学 | Method for depositing metal oxide on surface of limited-time protective product based on polyolefin non-woven fabric and protective product prepared by method |
| CN112735862A (en) * | 2020-12-23 | 2021-04-30 | 天津大学 | Surface grafting-based polypropylene film insulation property optimization system and use method |
| CN114645457A (en) * | 2022-03-25 | 2022-06-21 | 广州俊麒无纺布企业有限公司 | Non-woven fabric easy to color and resistant to aging and preparation method thereof |
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| CN112133870A (en) * | 2020-09-24 | 2020-12-25 | 湖南省凯纳方科技有限公司 | Preparation process of battery diaphragm for increasing ion exchange capacity |
| CN112553880A (en) * | 2020-11-24 | 2021-03-26 | 东华大学 | Method for depositing metal oxide on surface of limited-time protective product based on polyolefin non-woven fabric and protective product prepared by method |
| CN112553880B (en) * | 2020-11-24 | 2022-03-01 | 东华大学 | Method for depositing metal oxide on surface of limited-time protective product based on polyolefin non-woven fabric and protective product prepared by method |
| CN112735862A (en) * | 2020-12-23 | 2021-04-30 | 天津大学 | Surface grafting-based polypropylene film insulation property optimization system and use method |
| CN114645457A (en) * | 2022-03-25 | 2022-06-21 | 广州俊麒无纺布企业有限公司 | Non-woven fabric easy to color and resistant to aging and preparation method thereof |
| CN114645457B (en) * | 2022-03-25 | 2023-01-06 | 广州俊麒无纺布企业有限公司 | Non-woven fabric easy to color and resistant to aging and preparation method thereof |
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