CN101735472A - Porous membrane material continuous radiation grafting method and support equipment therefor - Google Patents
Porous membrane material continuous radiation grafting method and support equipment therefor Download PDFInfo
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- CN101735472A CN101735472A CN200910227534A CN200910227534A CN101735472A CN 101735472 A CN101735472 A CN 101735472A CN 200910227534 A CN200910227534 A CN 200910227534A CN 200910227534 A CN200910227534 A CN 200910227534A CN 101735472 A CN101735472 A CN 101735472A
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Abstract
The invention relates to a porous membrane material continuous radiation grafting method and support equipment therefor, belonging to the technical field of graft copolymerization. The method comprises the following steps: a macromolecule porous membrane material with absorbed allyl monomer aqueous solution or aqueous emulsion passed through an electron beam irradiation chamber for carrying out electron beam electron beam in an expansion mode. The method features simple process, can be used to overcome the defect of discontinuous pre-irradiation and copolymerization irradiation in the prior art and is conducive to industrialized application of the radiation grafting technology. Meanwhile, according to the characteristics that the porous membrane material is porous and easy to be continuously transmitted, electron beam irradiation is directional and absorption dose is large, the invention further provides the support equipment for carrying out the porous membrane material continuous radiation grafting method; the equipment comprises an electron accelerator, an irradiation chamber connected with the electron accelerator, a coating device and a guidance device for guiding the coated macromolecule porous membrane material to pass through the irradiation chamber. The equipment features high automation degree, high pertinence and excellent application prospect.
Description
Technical field
The invention belongs to the graft copolymerization technical field, relate to the serialization radiation graft process of porous film material, also relate to a kind of equipment that matches with this serialization radiation graft process simultaneously.
Background technology
Utilizing radiation grafting technology to introduce functional groups on porous film material, is a kind of effective way of preparation functional membrane material.So far, the researchist has carried out a large amount of explorations in this field, for example utilizes radiation grafting technology to prepare battery diaphragm, ion-exchange membrane, metal ion huge legendary turtle condensation material, filtering material and anti-biotic material etc.
In non-patent literature 1, Xiang Zhengyu, all ages Rong utilizes electron beam irradiation to be soaked with the silk of methacryloyl amine aqueous solution, has obtained the silk fabric through the Methacrylamide graft modification, sample wrinkle resistance after the grafting obviously improves, anxious bullet improves 30%, and slow bullet improves 12%, and wet bullet improves 40; Dyeing behavioies such as dye uptake, vividness and colour fastness also all increase.Dong Yuan, Lanzhou-Xinjiang wise man etc. disclose the grafting graft reaction with pre-irradiation PP non-woven fabrics such as vinylformic acid, methyl methacrylate, methyl acrylate, 4-vinylpridine respectively in non-patent literature 2-5, and the influence of parameters such as temperature of reaction, reaction times, stopper, monomer concentration and linking agent to percentage of grafting has been discussed.In non-patent literature 6, Geng Jiannuan, enemy agronomy etc. have been studied vinyl cyanide and the cografting reaction of vinylformic acid on the pre-irradiation polypropylene non-woven fabric in the air, and the influence to percentage of grafting of pre-irradiation absorption dose, graft reaction temperature, reaction times, monomer concentration and ratio and molar salt concentration has been discussed.Patent CN98123916.1 then discloses a kind of grafting method for preparing antiseptic material of pyridine salt type polymer, this method is a matrix with the PP non-woven fabrics, adopt pre-radiation or be total to the radiation initiation grafting, make functional group be combined in the polymer-based carbon surface, obtain to contain antiseptic material of pyridine salt type polymer by quaterisation then by chemical bonded refractory with anti-microbial activity.This technical costs is low, antimicrobial efficiency is high, antibiotic security and persistence are good, and various bacteria virus is all had removal effect, and is applied widely.Patent CN200410066999.6 provides a kind of hydrogel wound dressing that contains radiosensitizing agent, and provide the preparation method: with component wiring solution-formings such as polyvinylpyrrolidone, polyvinyl alcohol, radiation sensitive agent, softening agent, pH regulator agent, water, be cast on the non-woven fabrics after the deaeration, freezing curing molding and cover separate-type paper after cut out encapsulation, carry out irradiation with cobalt-60 then and obtain hydrogel wound dressing.This method is compared with conventional art has low, the simple technological process and other advantages of irradiation dose.
Though the method for utilizing radiation grafting technology to introduce functional groups on porous film material was carried out application test in a plurality of fields, how to realize that it still is the technical barrier that makes us perplexing so far that radiation grafted serialization is produced.Existing radiation grafting technology mainly is common radiation grafting and pre-irradiation grafting.Radiation grafting is that the grafted monomer solution that will be soaked with base material places radiation field to carry out irradiation altogether, bath raio is big in the radiation grafting technological process, the homopolymerization product is many, aftertreatment is difficult, not only wasting grafted monomer improves cost, and only be suitable in the gamma-radiation radiation field, carrying out, the industrializing implementation difficulty is very big.Need in the pre-irradiation grafting to place radiation field to carry out radiation base material earlier, take out base material then and immerse in the grafted monomer solution, utilize trapped radical residual on the base material and the copolymerization of peroxidation group initiation grafting.The graft reaction of monomer and base material needs the higher temperature and the protection of inert atmosphere usually after the pre-radiation, and the reaction times is also long.In addition, the radiation absorbed dose of pre-irradiation grafting processing requirement base material is big, and is also relatively more serious to the damage of base material.These factors have all been brought very big difficulty to the industrializing implementation of pre-irradiation grafting technology.
Citing document:
Non-patent literature 1: radiation research and radiation process journal, the 15th the 3rd phase of volume of August in 1997, P155～158;
Non-patent literature 2: use chemical industry, the 35th the 5th phase of volume of May in 2006, P332～334;
Non-patent literature 3: use chemical industry, the 35th the 8th phase of volume of August in 2006, P569～571;
Non-patent literature 4: Guangdong chemical industry, 2006 the 8th phases the 33rd volume (total the 160th phase), P20～22;
Non-patent literature 5: use chemical industry, the 35th the 9th phase of volume of September in 2006, P653～655;
Non-patent literature 6: radiation research and radiation process journal, the 23rd the 4th phase of volume of August in 2005, P237～240.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art part, a kind of porous membrane material continuous radiation graft process is provided, the production technique of serialization is that the industrial applications of radiation graft process is laid a good foundation.In addition, according to the porous film material porous, be easy to continuously transmission and electron beam irradiation orientation, characteristic that absorbed dose rate is big, the equipment that provides a kind of and porous membrane material continuous radiation graft process to match then is another object of the present invention.
Porous membrane material continuous radiation graft process comprises the steps: to make the high-molecular porous mould material that is adsorbed with the vinyl monomer aqueous solution or water miscible liquid to move through the electron beam irradiation chamber with deployed condition and carries out electron beam irradiation grafting.High-molecular porous mould material is long paper or less sheet (preferably long paper); When moving through the electron beam irradiation chamber, long paper can utilize the guidance device guiding of guiding roller and so on, and the device such as travelling belt that then can utilize of small pieces transmits.
In massfraction, contain vinyl monomer 5～50%, tackifier 0～5%, wetting agent 0.1～2% in the described vinyl monomer aqueous solution, water surplus; As preferred version, contain vinyl monomer 10～30%, tackifier 0.1～3%, wetting agent 0.1～0.5% in the vinyl monomer aqueous solution, water surplus.
In massfraction, contain vinyl monomer 5～50%, tackifier 0～5%, emulsifying agent 0.1～5% in the described vinyl monomer water miscible liquid, water surplus; As preferred version, contain vinyl monomer 10～30%, tackifier 0.1～3%, emulsifying agent 0.5～3% in the vinyl monomer aqueous solution, water surplus.
Described vinyl monomer is a kind of or composition wherein in the following compound: vinylformic acid, sodium acrylate, potassium acrylate, acrylate, acrylamide, methacrylic acid, sodium methacrylate, methacrylic acid potassium, methacrylic ester, toxilic acid, fumaric acid, Sodium styrene sulfonate, sodium allyl sulfonate, vinyl acetate, vinylbenzene, vinyl pyridine, methylene-succinic acid.
Described tackifier are a kind of or mixture wherein in the following compound: Xylo-Mucine, Natvosol, hydroxypropylcellulose, polyacrylamide, polyoxyethylene, polyvinyl alcohol, polyethylene pyrrole Lopa Nationality alkane ketone.Add tackifier, the vinyl monomer aqueous solution or water miscible liquid are adjusted to proper viscosity, be beneficial to coating and transmission, guarantee the stop that the preceding monomer of radiation grafting is necessary on porous film material.
Described wetting agent/emulsifying agent is a kind of or mixture wherein in the following compound: sodium alkyl sulfate, sodium alkyl benzene sulfonate, alkyl alcohol Soxylat A 25-7, alkylphenol polyoxyethylene, laurylene base sulfonate.Though wetting agent and emulsifying agent belong to tensio-active agent together, and all can from above several tensio-active agents of enumerating, choose arbitrarily, but both effects are also incomplete same: wetting agent is at the vinyl monomer water solution system, it mainly acts on is in order to increase the wetting capacity of grafted monomer and grafting base material, to make the grafted monomer rapid osmotic among the porous film material as the grafting base material.
Described porous membrane material continuous radiation graft process, comprise to the high-molecular porous mould material behind the electron beam irradiation wash, the exsiccant step.
In the described porous membrane material continuous radiation graft process, by coating the aqueous solution of vinyl monomer or water miscible liquid (grafting liquid) are adsorbed onto on the high-molecular porous mould material, and adsorptive capacity is quantitatively controlled.
With the supporting equipment of porous membrane material continuous radiation graft process, comprise rumbatron, the radiation chamber that links to each other with rumbatron, the high-molecular porous mould material after also comprising apparatus for coating and guiding coating is by the guidance device of radiation chamber.Apparatus for coating can adopt any one in the coating forms such as dip-coating, blade coating, roller coating, cylinder coating, spraying, choose quantitative accuracy higher coating device as far as possible, as the apparatus for coating that adopts the dip-coating form generally includes steeping vat and evenness calender, and porous film material is by going up evenness calender homogenize, quantitatively behind the steeping vat.
With the supporting equipment of porous membrane material continuous radiation graft process, comprise water washing device and drying installation, and the high-molecular porous mould material behind the guiding irradiation passes through the guidance device of water washing device and drying installation successively.Water washing device can be selected dyeing open width rinsing machine commonly used for use; Drying installation can adopt cylinder oven dry or tunnel oven dry.
Among the present invention, can be made or natural formation by natural polymer or synthesized polymer material as the porous film material of grafting base material, the industry that is suitable for is used is mainly textiles (comprising woven fabrics, knitted fabrics and non-woven fabrics).Vinyl monomer wherein then be a class contain unsaturated double-bond, can be by the compound or the composition of radiation-initiated polymerization, in the technical scheme of the present invention vinyl monomer is distributed to and makes the aqueous solution or water miscible liquid in the water.The porous film material that evenly is adsorbed with vinyl monomer is during continuously by the electron beam irradiation chamber, porous film material and vinyl monomer generation radiation cografting; Because monomer system is the aqueous solution or water miscible liquid, simple easily wash-out homopolymer and the unreacted monomer just washed gets product behind the drying and dehydrating.Porous membrane material continuous radiation graft process provided by the present invention, substituted the conventional container that is total in the radiation grafting process with the hole in the porous film material, be equivalent to dwindle the bath raio in the conventional radiation grafting technology altogether, increased substantially the utilization ratio of grafted monomer, reduce the generation of homopolymer, reduced the comprehensive cost of radiation grafting technology.Because grafting liquid has certain viscosity, be adsorbed in equably that the back has temporarily formed one with the grafting base material in the hole of porous film material, thereby for next step radiation grafting and continuously transmission basis of reality is provided.And percentage of grafting can be controlled the adsorptive capacity of grafting liquid by monomeric concentration and base material in the adjusting grafting liquid.
In addition, electron beam irradiation has directional property, and dose rate is tens of times to hundreds of times of common gamma-radiation radiation dose rate, and the required absorption dose of radiation grafting can reach in moment, therefore graft reaction also can be finished moment, and this radiation grafting for serialization provides another guarantee.In addition, the dose rate of electron beam irradiation can help the automatization control of implementing process by the line amount of adjusting electron beam and the transmission speed control of base material.
Support equipment can be made up of uncoiling machine, apparatus for coating, rumbatron and the radiation chamber that links to each other with rumbatron, water washing device, drying unit, winder and guidance device on the whole, the porous film material of rolling is emitted from the uncoiling machine that is located at front equipment end, after passing through coating, irradiation, washing, oven dry workshop section under the guiding of guidance device successively by the winder rolling.General uncoiling machine has constant tension control device and display unit, in order to the tension force (selection of tension force size is limited by the strength of materials) in the control porous film material operational process.Can also set up the sealing protection tunnel between apparatus for coating and the radiation chamber, to prevent to react the volatilization of preceding grafted monomer and moisture, the shielding scattered electrons.
For the heat and the ozone that produce in the electron beam irradiation process are in time discharged, air exhausting device also is equipped with in the radiation chamber below, but produced simultaneously wind can make porous film material that violent shake takes place, and influences the irradiation effect.For addressing this problem, have additional the capsule of band titanium window in the radiation chamber, electron beam penetrates and titanium window on being located at capsule is injected in the capsule from rumbatron, and the porous film material that is soaked with grafted monomer is subjected to electron irradiation when passing capsule radiation-induced graft copolymerization takes place.The sealing protection tunnel then can shield scattered electrons well.This complete equipment does not limit the specific form of rumbatron, but owing to be film irradiation, does not need very high energy, and the accelerator of the following energy of 1MeV gets final product usually, as 0.15～1MeV; Uniformity requirement to radiation dose is higher: compare with set(ting)value, require escalation rate≤± 5% of lateral radiation dosage, radiation dose escalation rate≤± 5% in time.
Description of drawings
Fig. 1 is the structural representation of support equipment of the present invention;
Fig. 2 is the sectional view of capsule.
Embodiment
As depicted in figs. 1 and 2, the guidance device (forming by a series of guiding rollers in the present embodiment) that mainly comprises uncoiling machine 1, apparatus for coating 2, the radiation chamber 4 that links to each other with rumbatron 6, water washing device 9, drying installation 10, winder 11 and various piece is run through successively with the supporting equipment of porous membrane material continuous radiation graft process.Be provided with the capsule 8 of band titanium window 14 in the radiation chamber 4, electronics is injected radiation chamber 4 after rumbatron 6 quickens, and in titanium window 14 was injected capsule 8, capsule 8 can pass from its inside for porous film material 12.Air exhausting device 5 is equipped with in the bottom of radiation chamber 4, so that in time remove ozone and heat that radiation produces.Apparatus for coating 2 relies on storage tank 7 and charging pump 13 to supply with grafting liquid (aqueous solution of vinyl monomer or water miscible liquid) for it; For the volatilization that prevents monomer, moisture and the scattering of electronics, also be provided with sealing protection tunnel 3 between apparatus for coating 2 and the radiation chamber 4.
Porous membrane material continuous radiation graft process, step is:
1) the preparation vinyl monomer aqueous solution or water miscible liquid (concrete proportioning see Table 1, table 2) injected storage tank 7, and squeezed in the apparatus for coating 2 by charging pump 13;
2) start rumbatron 6, transfer to required voltage and line amount, passed titanium window 14 by the electron beam of its acceleration and inject in the capsule 8;
2) with high-molecular porous mould material 12 long paper framves on uncoiling machine 1, and utilize leading-in device to guide it successively by apparatus for coating 2, sealing protection tunnel 3 and radiation chamber 4, be adsorbed with the vinyl monomer aqueous solution or water miscible liquid on the high-molecular porous mould material 12 after applied, be subjected to electron beam irradiation when moving through capsule 8 in the electron beam irradiation chamber 4, radiation-induced graft copolymerization takes place with deployed condition.High-molecular porous mould material 12 behind the graft reaction takes place be led to water washing device 9 and wash, removing unreacted monomer and homopolymer, after drying installation 10 is dry and by winder 11 rollings, promptly get the high-molecular porous mould material of via radiation grafting modification.
Claims (10)
1. porous membrane material continuous radiation graft process is characterized in that, this method comprises the steps: to make the high-molecular porous mould material that is adsorbed with the vinyl monomer aqueous solution or water miscible liquid to move through the electron beam irradiation chamber with deployed condition to carry out electron beam irradiation grafting.
2. porous membrane material continuous radiation graft process as claimed in claim 1 is characterized in that, in massfraction, contains vinyl monomer 5～50%, tackifier 0～5%, wetting agent 0.1～2% in the described vinyl monomer aqueous solution, water surplus.
3. porous membrane material continuous radiation graft process as claimed in claim 1 is characterized in that, in massfraction, contains vinyl monomer 5～50%, tackifier 0～5%, emulsifying agent 0.1～5% in the described vinyl monomer water miscible liquid, water surplus.
4. as the arbitrary described porous membrane material continuous radiation graft process of claim 1～3, it is characterized in that described vinyl monomer is a kind of or composition wherein in the following compound: vinylformic acid, sodium acrylate, potassium acrylate, acrylate, acrylamide, methacrylic acid, sodium methacrylate, methacrylic acid potassium, methacrylic ester, toxilic acid, fumaric acid, Sodium styrene sulfonate, sodium allyl sulfonate, vinyl acetate, vinylbenzene, vinyl pyridine, methylene-succinic acid.
5. as claim 2 or 3 described porous membrane material continuous radiation graft process, it is characterized in that described tackifier are a kind of or mixture wherein in the following compound: Xylo-Mucine, Natvosol, hydroxypropylcellulose, polyacrylamide, polyoxyethylene, polyvinyl alcohol, polyethylene pyrrole Lopa Nationality alkane ketone.
6. as claim 2 or 3 described porous membrane material continuous radiation graft process, it is characterized in that described wetting agent/emulsifying agent is a kind of or mixture wherein in the following compound: sodium alkyl sulfate, sodium alkyl benzene sulfonate, alkyl alcohol Soxylat A 25-7, alkylphenol polyoxyethylene, laurylene base sulfonate.
7. as claim 1 or 2 or 3 described porous membrane material continuous radiation graft process, it is characterized in that, this method comprise to the high-molecular porous mould material behind the electron beam irradiation wash, the exsiccant step.
8. as claim 1 or 2 or 3 described porous membrane material continuous radiation graft process, it is characterized in that, by coating the aqueous solution of vinyl monomer or water miscible liquid are adsorbed onto on the high-molecular porous mould material, and adsorptive capacity is quantitatively controlled.
9. with the supporting equipment of the arbitrary described porous membrane material continuous radiation graft process of claim 1-3, comprise rumbatron, the radiation chamber that links to each other with rumbatron, it is characterized in that the high-molecular porous mould material after described equipment also comprises apparatus for coating and guides coating is by the guidance device of radiation chamber.
As described in the claim 9 with the supporting equipment of porous membrane material continuous radiation graft process, it is characterized in that, this equipment comprises water washing device, drying installation, and the high-molecular porous mould material behind the guiding irradiation passes through the guidance device of water washing device and drying installation successively.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009534A (en) * | 2010-09-07 | 2011-04-13 | 淄博兰雁集团有限责任公司 | Fabric printing and dyeing device with electron accelerator mechanism |
| CN103319747A (en) * | 2013-07-16 | 2013-09-25 | 莱州联友金浩新型材料有限公司 | Grafting treatment apparatus and grafting treatment method for battery diaphragm material |
| US9212238B2 (en) | 2012-12-28 | 2015-12-15 | Industrial Technology Research Institute | Microparticle, addition agent and filtering membrane |
| CN105879826A (en) * | 2016-06-08 | 2016-08-24 | 河南科高辐射化工科技有限公司 | Post-heating solid liquid reaction device for radiation grafting |
| CN106229450A (en) * | 2016-09-29 | 2016-12-14 | 河南科高辐射化工科技有限公司 | A kind of high-capacity nickel-hydrogen battery barrier film |
| CN108822250A (en) * | 2018-09-03 | 2018-11-16 | 安徽联合辐化有限公司 | The synthetic method and equipment of aqueous high molecular lotion |
| CN109482114A (en) * | 2018-10-12 | 2019-03-19 | 河南科高辐射化工科技有限公司 | A kind of dynamic solid-liquid reaction device for web-like perforated membrane pre-irradiation grafting |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5318866A (en) * | 1993-04-23 | 1994-06-07 | Pall Corporation | Battery separators |
| FR2911883B1 (en) * | 2007-01-29 | 2009-05-01 | Intissel Soc Par Actions Simpl | IONIZING RADIATION GRAFTING PROCESS USING REACTIVE SURFACE MOLECULE, TEXTILE SUBSTRATE AND BATTERY SEPARATOR OBTAINED BY GRAFTING |
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2009
- 2009-12-18 CN CN2009102275347A patent/CN101735472B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009534A (en) * | 2010-09-07 | 2011-04-13 | 淄博兰雁集团有限责任公司 | Fabric printing and dyeing device with electron accelerator mechanism |
| US9212238B2 (en) | 2012-12-28 | 2015-12-15 | Industrial Technology Research Institute | Microparticle, addition agent and filtering membrane |
| CN103319747A (en) * | 2013-07-16 | 2013-09-25 | 莱州联友金浩新型材料有限公司 | Grafting treatment apparatus and grafting treatment method for battery diaphragm material |
| CN105879826A (en) * | 2016-06-08 | 2016-08-24 | 河南科高辐射化工科技有限公司 | Post-heating solid liquid reaction device for radiation grafting |
| CN106229450A (en) * | 2016-09-29 | 2016-12-14 | 河南科高辐射化工科技有限公司 | A kind of high-capacity nickel-hydrogen battery barrier film |
| CN108822250A (en) * | 2018-09-03 | 2018-11-16 | 安徽联合辐化有限公司 | The synthetic method and equipment of aqueous high molecular lotion |
| CN109482114A (en) * | 2018-10-12 | 2019-03-19 | 河南科高辐射化工科技有限公司 | A kind of dynamic solid-liquid reaction device for web-like perforated membrane pre-irradiation grafting |
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