CN106751295B - A kind of moulding laser holographic recording materials and preparation method thereof - Google Patents
A kind of moulding laser holographic recording materials and preparation method thereof Download PDFInfo
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- CN106751295B CN106751295B CN201611072261.XA CN201611072261A CN106751295B CN 106751295 B CN106751295 B CN 106751295B CN 201611072261 A CN201611072261 A CN 201611072261A CN 106751295 B CN106751295 B CN 106751295B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
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- C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
- C08F259/08—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing fluorine
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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Abstract
The invention discloses a kind of moulding laser holographic recording materials and preparation method thereof, wherein the moulding laser holographic recording materials, including imaging resin and for the irradiation grafting modified Teflon micro mist of the composite modified imaging resin；The mass ratio of irradiation grafting modified Teflon micro mist and both imaging resins is 1/20~1/200.The present invention is by improving the crucial microcosmic composition of material and structure, it can effectively solve the problem that resin used in existing moulding laser holographic information recording layer easily occurs viscous version in mold process, falls a little the problem of the defects of even defect compared with prior art, obtain the moulding laser holographic recording materials that internal uniformity is good, stability is high.
Description
Technical field
The invention belongs to laser hologram information-recording material fields, record more particularly, to a kind of moulding laser holographic
Material and preparation method thereof, the moulding laser holographic recording materials are micro- by imaging resin and irradiation grafting modified Teflon
Powder composition, be kind of the composite material for being particularly suitable for moulding laser holographic record.
Background technique
Counterfeit and shoddy goods not only damage the interests of businessman and consumer, influence social economic order, also give state tax revenue
Massive losses are brought, anti-counterfeiting technology becomes one of the effective means of strike counterfeit and shoddy goods.In existing anti-counterfeiting technology, laser is complete
Cease mould pressing technology because its not transreplication, recognition methods multiplicity, not reproducible use the advantages that, be widely used.The technology be by
The holographic grating being formed in nickel version is transferred on contour forging anti-fake material under certain temperature, pressure, realizes hologram
Batch duplicating.Wherein, hologram recording material is the important component of contour forging anti-fake material, and realizes laser hologram mould
The key of pressure technology.Moulding laser holographic recording materials need the high grade of transparency, glossiness and flatness, good wearability, heat-resisting
Property, anti-sticking version performance and cutting performance.The imaging resin of moulding laser holographic recording materials is mainly thermoplastic acrylic at present
The coating of ester resin or polyurethane resin, preparation is flat and smooth.However imaging resin and the interaction of nickel version are stronger, molding
Shi Buyi is separated with nickel version, viscous version, peeling is occurred, is fallen a little the phenomenon that even defect, is unfavorable for the transfer of hologram, reduces life
Finished product rate.
Ptfe surface energy is low, lubricity is good, and abrasion resistance, heat resistance and chemical stability are good, frequently as not snearing
Material or wear-resistant material are applied to space flight, chemical industry, electronics, machinery, medicine and other fields.These advantages of polytetrafluoroethylene (PTFE) make its micro mist
Surface property for improving imaging resin is possibly realized.But the hydrophobicity of ptfe micropowder is compared with plate or membranaceous polytetrafluoro
Ethylene is higher, is practically insoluble in water or any organic solvent.Existing ptfe micropowder and the compound of resin mainly pass through
Exhibiting high surface activating agent is added to change micro mist surface characteristic, of short duration can be scattered in resin solution.But this method is not
Have and fundamentally solve the problems, such as ptfe micropowder bad dispersibility in resin, and the density of ptfe micropowder with
Resin difference is larger, and after the long period places, ptfe micropowder must be settled；And the surfactant price used is high
Expensive, residual is difficult to remove, and will have a negative impact to the performance of material.Similarly, because of the imaging tree with contour forging anti-fake material
The poor compatibility of rouge, ptfe micropowder imaging resin in be easy to reunite, be difficult to it is evenly dispersed.Therefore, complete for laser
Imaging resin/ptfe micropowder composite material stability of breath mould pressing technology is poor, comprehensive performance is undesirable.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the purpose of the present invention is to provide a kind of moulding laser holographics
Recording materials and preparation method thereof, wherein by the crucial microcosmic composition of material and structure (the especially table of polytetrafluoroethylene (PTFE)
Surface treatment etc.) it improves, it can effectively solve the problem that existing moulding laser holographic information recording layer tree used compared with prior art
Rouge easily occurs viscous version in mold process, falls a little the problem of the defects of even defect, and the present invention is modified poly- using irradiation grafting
Tetrafluoroethene micro mist and imaging resin compounded, while by electron beam irradiation ptfe micropowder surface grafting polymerization object simultaneously
Grafting rate is controlled, ptfe micropowder can be improved and the compatibility of resin is imaged, obtains that internal uniformity is good, stability is high
Moulding laser holographic recording materials；Also, the present invention is by controlling in the composite material recorded for moulding laser holographic
The proportion of both resin and irradiation grafting modified Teflon micro mist is imaged, so that the moulding laser holographic recording materials have
Good wearability, anti-sticking version performance can greatly improve the efficiency of molding working process.
To achieve the above object, according to one aspect of the present invention, a kind of moulding laser holographic recording materials are provided,
It is characterized in that, including imaging resin and for the irradiation grafting modified Teflon micro mist of the composite modified imaging resin；
Wherein, the irradiation grafting modified Teflon micro mist and the mass ratio that both resins are imaged are 1/20~1/200.
As present invention further optimization, the surface grafting object of the irradiation grafting modified Teflon micro mist is third
Polymerizate, acrylic amide of the olefin(e) acid class containing double bond monomer polymerizate and esters of acrylic acid containing double bond monomer are containing double
At least one of the polymerizate of key monomer.
As present invention further optimization, the imaging resin is acrylate or polyurethane resin.
As present invention further optimization, the irradiation grafting modified Teflon micro mist is micron order, and partial size is
0.2 micron~4 microns.
It is another aspect of this invention to provide that the present invention provides a kind of preparation method of moulding laser holographic recording materials,
Characterized by comprising the following steps:
(1) it disperses ptfe micropowder in monomer solution, then, using monomer solution described in electron beam irradiation,
Cause monomer ptfe micropowder surface grafting polymerization to get arrive graft modification ptfe micropowder；
The mass fraction of monomer described in the monomer solution is 4wt.%~40wt.%, the ptfe micropowder
Mass ratio with both monomers is 1/0.5~1/3；
The irradiation dose of the electron beam irradiation is 20kGy~90kGy, and dosage rate is preferably 4kGy/pass~30kGy/
pass；
(2) the graft modification ptfe micropowder for obtaining the step (1) is scattered in solvent, is grafted
Modified Teflon micro mist dispersion liquid；
(3) imaging resin is dissolved in solvent and forms imaging resin solution；Then, the step (2) is obtained described
Graft modification ptfe micropowder dispersion liquid is mixed with the imaging resin solution, is carried out ultrasonic wave auxiliary and is dispersed with stirring, obtains
To finely dispersed imaging resin/irradiation grafting modified Teflon micro mist composite dispersion liquid；
(4) the imaging resin for obtaining the step (3)/irradiation grafting modified Teflon micro mist composite diffusion
Liquid is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Another aspect according to the invention, the present invention provides a kind of preparation method of moulding laser holographic recording materials,
Characterized by comprising the following steps:
(1) ptfe micropowder is irradiated using electron beam, it is micro- obtains polytetrafluoroethylene (PTFE) of the surface containing free radical
Powder；Then, the ptfe micropowder by the surface containing free radical is distributed in monomer solution, is placed in inert gas environment
Under, 1 hour~8 hours are reacted at 50 DEG C~80 DEG C to get graft modification ptfe micropowder is arrived；
The mass fraction of monomer described in the monomer solution is 30wt.%~70wt.%, the ptfe micropowder
Mass ratio with the monomer is 1/1.2~1/12；
The irradiation dose of the electron beam is 30kGy~270kGy；Radiation dose rate be preferably 30kGy/pass~
90kGy/pass；
(2) the graft modification ptfe micropowder for obtaining the step (1) is scattered in solvent, is grafted
Modified Teflon micro mist dispersion liquid；
(3) imaging resin is dissolved in solvent and forms imaging resin solution；Then, the step (2) is obtained described
Graft modification ptfe micropowder dispersion liquid is mixed with the imaging resin solution, is carried out ultrasonic wave auxiliary and is dispersed with stirring, obtains
To finely dispersed imaging resin/irradiation grafting modified Teflon micro mist composite dispersion liquid；
(4) the imaging resin for obtaining the step (3)/irradiation grafting modified Teflon micro mist composite diffusion
Liquid is uniformly coated on basement membrane, up to moulding laser holographic recording materials after drying.
As present invention further optimization, in the step (1), the monomer is that acrylic compounds contain double bond monomer, third
Acrylamide is containing double bond monomer and esters of acrylic acid containing at least one of double bond monomer；Used by the monomer solution
Solvent is deionized water；
Preferably, the acrylic compounds are at least one of acrylic acid and methacrylic acid containing double bond monomer；It is described
Acrylic amide is acrylamide, Methacrylamide, N-isopropylacrylamide and hydroxymethyl acrylamide containing double bond monomer
At least one of；The esters of acrylic acid is methyl methacrylate, glycidyl methacrylate, first containing double bond monomer
Base hydroxy-ethyl acrylate, methacrylate, ethyl acrylate, hydroxy-ethyl acrylate, butyl methacrylate and methyl-prop
At least one of olefin(e) acid isobornyl thiocyanoacetate.
As present invention further optimization, in the step (1), the ptfe micropowder is micron order, preferably
, partial size is 0.2 micron~4 microns；The graft modification ptfe micropowder is to be filtered, washed and be dried
It obtains afterwards.
As present invention further optimization, in the step (2), the solvent is ethyl acetate or butyl acetate.
As present invention further optimization, in the step (3), the imaging resin is acrylate or poly- ammonia
Ester resin, the solvent are toluene, butanone, any one in ethyl acetate.
Contemplated above technical scheme through the invention, compared with prior art, since irradiation grafting is modified poly- four
Vinyl fluoride micro mist is dispersed into imaging resin, and in ptfe micropowder surface grafting polymerization object and is controlled by electron beam irradiation
Grafting rate processed can improve ptfe micropowder and the compatibility of resin is imaged, obtain that internal uniformity is good, stability is high
Moulding laser holographic recording materials.The present invention is generated free radicals by electron beam irradiation on ptfe micropowder surface, and is drawn
Monomer polymerization is sent out, the ptfe micropowder of polymer graft modification is obtained；Modified ptfe micropowder has been dispersed in
In solvent, ptfe micropowder dispersion liquid is obtained；Dispersion liquid and imaging resin alloy are coated and dried up to the laser
Hologram recording material.The preparation method is simple, easy to operate, and gained laser holographic recording material is low with surface energy, wearability is good
The advantages of, it can be applied to high-end anti-counterfeit field.
Moulding laser holographic recording materials produced by the present invention, irradiation grafting modified Teflon micro mist therein at
As the mass ratio of both resins is 1/20~1/200；The partial size of ptfe micropowder is that (partial size is preferably 0.2 micro- to micron order
Rice~4 microns), by carrying out electron beam irradiation to the ptfe micropowder, and the dosage of electron beam irradiation is controlled, caused single
Body ptfe micropowder surface grafting polymerization (such case is first to disperse ptfe micropowder in monomer solution,
Electron beam irradiation monomer solution is used again, causes monomer in ptfe micropowder surface grafting polymerization, gained is mutual radiation
It is grafted ptfe micropowder；It is of course also possible to be first to irradiate using electron beam to ptfe micropowder, surface is obtained
Ptfe micropowder containing free radical, then add it in monomer solution and reacted, gained is that pre-irradiation grafting is poly-
Tetrafluoroethene).By the dosage (such as dosage rate condition, irradiation dose condition) and other conditions that control electron beam irradiation
(proportion of both concentration, monomer and ptfe micropowder of such as monomer solution) passes through the whole of each response parameter condition
Body cooperation, can control the grafting rate of ptfe micropowder surface grafting polymerization object, so that polytetrafluoroethylgranule granule is keeping low
It while the energy of surface, is also not susceptible to reunite, greatly improves the uniformity that polytetrafluoroethylgranule granule disperses in imaging resin, by
This improves ptfe micropowder and the compatibility that resin is imaged, to improve final moulding laser holographic recording materials obtained
Uniformity and stability.
Specifically, the composite material and preparation method in the present invention for moulding laser holographic record has following excellent
Point and obvious progress:
(1) the surface energy that moulding laser holographic recording materials are reduced using ptfe micropowder, is reduced in mold process
Interaction between coating and nickel version reduces viscous version phenomenon, improves yield rate and quality.
(2) ptfe micropowder is improved using electron beam irradiation grafting and the compatibility of resin is imaged, and then improve it
Storage stability, while also improving dispersion concentration of the ptfe micropowder in imaging resin solution.
(3) the irradiation grafting ptfe micropowder of the achievable higher grafting rate of the present invention.
(4) preparation method of modified Teflon micro mist of the present invention is simple, avoids introducing other auxiliary agents, clean without dirt
Dye, is easy to heavy industrialization.
Detailed description of the invention
Fig. 1 is the infrared spectrum for the irradiation grafting modified Teflon micro mist being prepared in embodiment 1 and 10；Fig. 1
Original polytetrafluoroethylene (PTFE), co-irradiation grafting polytetrafluoroethylene (PTFE), pre-irradiation grafting polytetrafluoroethylene (PTFE) are respectively corresponded from top to bottom；
Fig. 2 is prepared in imaging resin/original ptfe micropowder composite dispersion liquid (a) and imaging resin/embodiment 11
Photo after obtained irradiation grafting modified Teflon micro mist composite dispersion liquid (b) storage 72 hours；
Fig. 3 is the water contact angle photo for the moulding laser holographic recording materials being prepared in embodiment 2.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Moulding laser holographic recording materials in the present invention are micro- by imaging resin and irradiation grafting modified Teflon
The composite material of powder composition；Wherein, the mass ratio of the irradiation grafting modified Teflon micro mist and imaging resin is 1/
20~1/200.
Wherein, the surface grafting object of the irradiation grafting modified Teflon micro mist be acrylic compounds, acrylic amide,
Or polymerizate of the esters of acrylic acid containing double bond monomer.
The imaging resin is acrylate or polyurethane resin.
The irradiation grafting modified Teflon micro mist is micron order, and partial size is 0.2~4 micron.
Correspondingly, in the present invention moulding laser holographic recording materials preparation method, specifically includes the following steps:
1. dispersing ptfe micropowder in monomer solution, monomer is caused in polytetrafluoroethylene (PTFE) using electron beam irradiation
Micro mist surface grafting polymerization is filtered, is washed, being dried to obtain graft modification ptfe micropowder after the completion of irradiation；The monomer
The mass fraction of solution is 4wt.%~40wt.%, and the mass ratio of ptfe micropowder and monomer is 1/0.5~1/3；It is described
The dosage rate of electron beam irradiation be 4kGy/pass~30kGy/pass (due to sample can by under conveyer belt to electronic beam current,
Dosage rate unit kGy/pass is the dosage for indicating every one way), irradiation dose is 20kGy~90kGy；
2. irradiating using electron beam to ptfe micropowder, it is micro- to obtain polytetrafluoroethylene (PTFE) of the surface containing free radical
Powder, the ptfe micropowder by surface containing free radical are distributed in monomer solution, are placed in inert gas environment, 50 DEG C~
It is reacted 1~8 hour at 80 DEG C, filters, washs after reaction, being dried to obtain graft modification ptfe micropowder；The list
The mass fraction of liquid solution is 30wt.%~70wt.%, and the mass ratio of ptfe micropowder and monomer is 1/1.2~1/12；
The dosage rate of the irradiation is 30kGy/pass~90kGy/pass, and irradiation dose is 30kGy~270kGy；
3. 1. or 2. resulting graft modification ptfe micropowder is scattered in solvent by step, it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid；
4. imaging resin is dissolved in solvent, 3. graft modification ptfe micropowder dispersion liquid that step is obtained is added
Into imaging resin solution, ultrasonic wave auxiliary is dispersed with stirring, and obtains the modified polytetrafluoro of finely dispersed imaging resin/irradiation grafting
Ethylene micro mist composite dispersion liquid；
5. by step, 4. resulting imaging resin/irradiation grafting modified Teflon micro mist composite dispersion liquid is equably applied
(basement membrane can be polyethylene terephthalate film, polychloroethylene film, simple tension polypropylene screen, two-way to cloth on basement membrane
The common basement membrane such as stretched polypropylene films), up to moulding laser holographic recording materials after drying.
Wherein:
Step 1. or step 2. in, the monomer be acrylic compounds, acrylic amide or esters of acrylic acid list containing double bond
Body, the solvent of the monomer solution are deionized water.
Step 3. in, the solvent be ethyl acetate or butyl acetate.
Step 4. in, the imaging resin be acrylate or polyurethane resin；It is organic used in resin solution
Solvent is toluene, butanone, ethyl acetate.
The following are specific embodiments
Embodiment 1
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
The ester modified ptfe micropowder of acid glycidyl, wherein the partial size of irradiation grafting modified Teflon micro mist is 0.2 micro-
Rice, the mass ratio with acrylate are 1/20.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. dispersing ptfe micropowder in the glycidyl methacrylate aqueous solution of 4wt.%, using electronics
Beam irradiates mixed solution, filters, washs after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder
Mass ratio with glycidyl methacrylate is 1/0.5, radiation dose rate 4kGy/pass, irradiation dose 20kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate is dissolved in butanone, 2. graft modification ptfe micropowder dispersion liquid that step is obtained
It is added in resin solution, ultrasonic wave auxiliary is dispersed with stirring, and it is modified poly- to obtain finely dispersed acrylate/irradiation grafting
Tetrafluoroethene micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 2:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polyacrylic acid change
Property ptfe micropowder, wherein the partial size of irradiation grafting modified Teflon micro mist be 0.2 micron, with acrylate
Mass ratio be 3/100.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. dispersing ptfe micropowder in the acrylic acid aqueous solution of 12wt.%, mixed using electron beam irradiation molten
Liquid is filtered after the completion, is washed, being dried to obtain graft modification ptfe micropowder.The matter of ptfe micropowder and acrylic acid
Amount is than being 1/1, radiation dose rate 20kGy/pass, irradiation dose 60kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of butanone and toluene, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 3:
Moulding laser holographic recording materials in the present embodiment, including polyurethane resin and the poly- methylol propylene of irradiation grafting
Amide modifications ptfe micropowder, wherein the partial size of irradiation grafting modified Teflon micro mist is 2 microns, with polyurethane tree
The mass ratio of rouge is 1/100.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. dispersing ptfe micropowder in the hydroxymethylacrylamwater water solution of 6wt.%, using electron beam irradiation
Mixed solution is filtered after the completion, is washed, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder and hydroxyl first
The mass ratio of base acrylamide is 1/0.8, radiation dose rate 20kGy/pass, irradiation dose 40kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. polyurethane resin to be dissolved in the in the mixed solvent of ethyl acetate and toluene, 2. graft modification that step is obtained gathers
Tetrafluoroethene micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed polyurethane tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting polyurethane resin/irradiation grafting modified Teflon micro mist composite dispersion liquid is equably
It is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 4:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polyacrylic acid second
Ester modified ptfe micropowder, wherein the partial size of irradiation grafting modified Teflon micro mist is 0.2 micron, with acrylate
The mass ratio of resin is 1/25.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. it disperses ptfe micropowder in the ethyl acrylate aqueous solution of 20wt.%, it is mixed using electron beam irradiation
Solution is closed, filters, wash after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder and acrylic acid
The mass ratio of ethyl ester is 1/1.5, radiation dose rate 10kGy/pass, irradiation dose 20kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in ethyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate is dissolved in toluene, 2. graft modification ptfe micropowder dispersion liquid that step is obtained
It is added in resin solution, ultrasonic wave auxiliary is dispersed with stirring, and it is modified poly- to obtain finely dispersed acrylate/irradiation grafting
Tetrafluoroethene micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 5:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
Sour modified Teflon micro mist, wherein the partial size of irradiation grafting modified Teflon micro mist is 4 microns, with acrylate tree
The mass ratio of rouge is 1/200.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. it disperses ptfe micropowder in the metering system aqueous acid of 40wt.%, it is mixed using electron beam irradiation
Solution is closed, filters, wash after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder and acrylic acid
Mass ratio be 1/3, radiation dose rate 30kGy/pass, irradiation dose 90kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in ethyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of butanone and toluene, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 6:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
The hydroxy ethyl ester modified ptfe micropowder of acid, wherein the partial size of irradiation grafting modified Teflon micro mist is 0.2 micron, with third
The mass ratio of alkene acid ester resin is 1/50.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. dispersing ptfe micropowder in the hydroxyethyl methacrylate aqueous solution of 15wt.%, using electron beam
Mixed solution is irradiated, filters, wash after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder with
The mass ratio of hydroxyethyl methacrylate is 1/2, radiation dose rate 30kGy/pass, irradiation dose 60kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of butanone and toluene, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 7:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
Acid butyl ester modified Teflon micro mist, wherein the partial size of irradiation grafting modified Teflon micro mist is 4 microns, with acrylic acid
The mass ratio of ester resin is 1/100.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. dispersing ptfe micropowder in the butyl methacrylate aqueous solution of 10wt.%, using electron beam spoke
According to mixed solution, filters, washs after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder and first
The mass ratio of base butyl acrylate is 1/1, radiation dose rate 20kGy/pass, irradiation dose 60kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of ethyl acetate and toluene, 2. graft modification that step is obtained
Ptfe micropowder dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylic acid
Ester resin/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 8:
Moulding laser holographic recording materials in the present embodiment, including polyurethane resin and irradiation grafting polymethylacrylic acid
Isobornyl thiocyanoacetate modified Teflon micro mist, wherein the partial size of irradiation grafting modified Teflon micro mist is 0.2 micron, and poly-
The mass ratio of urethane resin is 3/100.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. dispersing ptfe micropowder in the isobornyl methacrylate aqueous solution of 15wt.%, using electronics
Beam irradiates mixed solution, filters, washs after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder
Mass ratio with isobornyl methacrylate is 1/3, radiation dose rate 30kGy/pass, irradiation dose 60kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in ethyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. polyurethane resin to be dissolved in the in the mixed solvent of ethyl acetate and toluene, 2. graft modification that step is obtained gathers
Tetrafluoroethene micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed polyurethane tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting polyurethane resin/irradiation grafting modified Teflon micro mist composite dispersion liquid is equably
It is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 9:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
Amide modifications ptfe micropowder, wherein the partial size of irradiation grafting modified Teflon micro mist is 0.2 micron, with acrylic acid
The mass ratio of ester resin is 3/100.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. it disperses ptfe micropowder in the methacryl amine aqueous solution of 8wt.%, it is mixed using electron beam irradiation
Solution is closed, filters, wash after the completion, being dried to obtain graft modification ptfe micropowder.Ptfe micropowder and methyl-prop
The mass ratio of acrylamide is 1/0.5, radiation dose rate 10kGy/pass, irradiation dose 20kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate is dissolved in toluene, 2. graft modification ptfe micropowder dispersion liquid that step is obtained
It is added in resin solution, ultrasonic wave auxiliary is dispersed with stirring, and it is modified poly- to obtain finely dispersed acrylate/irradiation grafting
Tetrafluoroethene micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 10:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
Acid glycidyl ester modified Teflon micro mist, wherein irradiation grafting modified Teflon grain size of micropowder is 0.2 micron, with
The mass ratio of acrylate is 1/150.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. irradiating using electron beam to ptfe micropowder, obtained ptfe micropowder is distributed to methyl
It in glycidyl acrylate aqueous solution, is placed in inert gas environment, is reacted at 80 DEG C 2 hours, filter after reaction,
It washs, be dried to obtain graft modification ptfe micropowder.The mass fraction of glycidyl methacrylate solution is
The mass ratio of 30wt.%, ptfe micropowder and glycidyl methacrylate is 1/2.Radiation dose rate is 30kGy/
Pass, irradiation dose 30kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of toluene and butanone, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 11:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
Sour methyl esters modified Teflon micro mist, wherein the partial size of irradiation grafting modified Teflon micro mist is 4 microns, with acrylic acid
The mass ratio of ester resin is 7/200.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. irradiating using electron beam to ptfe micropowder, obtained ptfe micropowder is distributed to methyl
It in methyl acrylate aqueous solution, is placed in inert gas environment, is reacted at 65 DEG C 1 hour, filter, wash after reaction,
It is dried to obtain graft modification ptfe micropowder.The mass fraction of methyl methacrylate solution is 35wt.%, polytetrafluoroethyl-ne
The mass ratio of alkene micro mist and methyl methacrylate is 1/12.Radiation dose rate is 30kGy/pass, irradiation dose 60kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate is dissolved in toluene, 2. graft modification ptfe micropowder dispersion liquid that step is obtained
It is added in resin solution, ultrasonic wave auxiliary is dispersed with stirring, and it is modified poly- to obtain finely dispersed acrylate/irradiation grafting
Tetrafluoroethene micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 12:
Moulding laser holographic recording materials in the present embodiment, including polyurethane resin and irradiation grafting polyacrylamide change
Property ptfe micropowder, the partial size of the irradiation grafting modified Teflon micro mist is 2 microns, with polyurethane resin
Mass ratio is 1/40.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. irradiating using electron beam to ptfe micropowder, obtained ptfe micropowder is distributed to propylene
It in amide aqueous solution, is placed in inert gas environment, reacts 8 hours at 50 DEG C, filter, wash after reaction, is dry
To graft modification ptfe micropowder.The mass fraction of acrylamide solution is 70wt.%, ptfe micropowder and propylene
The mass ratio of amide is 1/1.2.Radiation dose rate is 90kGy/pass, irradiation dose 270kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. polyurethane resin to be dissolved in the in the mixed solvent of toluene and ethyl acetate, 2. graft modification that step is obtained gathers
Tetrafluoroethene micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed polyurethane tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting polyurethane resin/irradiation grafting modified Teflon micro mist composite dispersion liquid is equably
It is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 13:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polymethyl
Acid esters modified Teflon micro mist, the partial size of the irradiation grafting modified Teflon micro mist is 0.2 micron, with propylene
The mass ratio of acid ester resin is 1/20.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. irradiating using electron beam to ptfe micropowder, obtained ptfe micropowder is distributed to methyl
It in acrylate aqueous solution, is placed in inert gas environment, is reacted at 70 DEG C 3 hours, filter, wash after reaction, is dry
It is dry to obtain graft modification ptfe micropowder.The mass fraction of methacrylic acid ester solution is 60wt.%, and polytetrafluoroethylene (PTFE) is micro-
The mass ratio of powder and methacrylate is 1/1.5.Radiation dose rate is 50kGy/pass, irradiation dose 150kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in ethyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of toluene and butanone, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 14:
Moulding laser holographic recording materials in the present embodiment, including acrylate and irradiation grafting polyacrylic acid hydroxyl
Ethyl ester modified ptfe micropowder, the partial size of the irradiation grafting modified Teflon micro mist is 2 microns, with acrylic acid
The mass ratio of ester resin is 3/200.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. irradiating using electron beam to ptfe micropowder, obtained ptfe micropowder is distributed to propylene
It in sour hydroxyl ethyl ester aqueous solution, is placed in inert gas environment, is reacted at 55 DEG C 1.5 hours, filter, wash after reaction,
It is dried to obtain graft modification ptfe micropowder.The mass fraction of hydroxy-ethyl acrylate solution is 50wt.%, polytetrafluoroethylene (PTFE)
The mass ratio of micro mist and hydroxy-ethyl acrylate is 1/1.2.Radiation dose rate is 50kGy/pass, irradiation dose 200kGy.
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of toluene and butanone, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step, 3. resulting acrylate/irradiation grafting modified Teflon micro mist composite dispersion liquid is uniform
Ground is coated on basement membrane, up to moulding laser holographic recording materials after drying.
Embodiment 15:
Moulding laser holographic recording materials in the present embodiment, including acrylate and the poly- isopropyl third of irradiation grafting
Acrylamide modified Teflon micro mist, the partial size of the irradiation grafting modified Teflon micro mist is 2 microns, with propylene
The mass ratio of acid ester resin is 3/200.
This moulding laser holographic recording materials are prepared according to the following steps and obtain:
1. irradiating using electron beam to ptfe micropowder, obtained ptfe micropowder is distributed to isopropyl
It in base acrylamide aqueous solution, is placed in inert gas environment, is reacted 2.5 hours at 60 DEG C, filter, wash after reaction
It washs, be dried to obtain graft modification ptfe micropowder.The mass fraction of N-isopropylacrylamide solution be 40wt.%, poly- four
The mass ratio of vinyl fluoride micro mist and N-isopropylacrylamide is 1/4.Radiation dose rate is 50kGy/pass, and irradiation dose is
250kGy。
2. by step, 1. resulting graft modification ptfe micropowder is scattered in butyl acetate, and it is poly- to obtain graft modification
Tetrafluoroethene micro mist dispersion liquid.
3. acrylate to be dissolved in the in the mixed solvent of toluene and butanone, 2. graft modification that step is obtained poly- four
Vinyl fluoride micro mist dispersion liquid is added in resin solution, and ultrasonic wave auxiliary is dispersed with stirring, and obtains finely dispersed acrylate tree
Rouge/irradiation grafting modified Teflon micro mist composite dispersion liquid.
4. by step 3. resulting acrylate/compound point of irradiation grafting modified Teflon micro mist
Dispersion liquid is uniformly coated on basement membrane, up to moulding laser holographic recording materials after drying.
The preparation condition of preparation method and the visible the following table 1 of parameter comparison in above-described embodiment 1-15.
1 embodiment 1-15 material ratio relationship of table and preparation condition
Imaging resin in the present invention can be the moulds commonly used in the prior art such as acrylate or polyurethane resin
Press laser holographic recording material.
Acrylic compounds can be acrylic acid, methacrylic acid, acrylic amide list containing double bond containing double bond monomer in the present invention
Body can be acrylamide, Methacrylamide, N-isopropylacrylamide, hydroxymethyl acrylamide, and esters of acrylic acid contains double bond
Monomer can be methyl methacrylate, glycidyl methacrylate, hydroxyethyl methacrylate, methacrylate,
Ethyl acrylate, hydroxy-ethyl acrylate, butyl methacrylate, isobornyl methacrylate.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of moulding laser holographic recording materials, which comprises the following steps:
(1) it disperses ptfe micropowder in monomer solution, then, using monomer solution described in electron beam irradiation, causes
Monomer ptfe micropowder surface grafting polymerization to get arrive graft modification ptfe micropowder；The monomer is propylene
Acids is containing double bond monomer, acrylic amide containing double bond monomer and esters of acrylic acid containing at least one of double bond monomer；It is described
Solvent used by monomer solution is deionized water；
The mass fraction of monomer described in the monomer solution is the wt.% of 4 wt.%~40, the ptfe micropowder and institute
The mass ratio for stating both monomers is 1/0.5~1/3；
The irradiation dose of the electron beam irradiation is 20kGy~90kGy, and dosage rate is 4kGy/pass~30kGy/pass；
The graft modification ptfe micropowder is obtained after being filtered, washed and being dried；
(2) the graft modification ptfe micropowder for obtaining the step (1) is scattered in solvent, obtains graft modification
Ptfe micropowder dispersion liquid；
(3) imaging resin is dissolved in solvent and forms imaging resin solution；Then, the grafting step (2) obtained
Modified Teflon micro mist dispersion liquid is mixed with the imaging resin solution, is carried out ultrasonic wave auxiliary and is dispersed with stirring, is divided
Dissipate uniform imaging resin/irradiation grafting modified Teflon micro mist composite dispersion liquid；
(4) the imaging resin for obtaining the step (3)/irradiation grafting modified Teflon micro mist composite dispersion liquid applies
Cloth on basement membrane, it is dry after up to moulding laser holographic recording materials, irradiation grafting changes in the moulding laser holographic recording materials
Property ptfe micropowder and the mass ratio of imaging both resin be 1/20~1/200.
2. a kind of preparation method of moulding laser holographic recording materials, which comprises the following steps:
(1) ptfe micropowder is irradiated using electron beam, obtains ptfe micropowder of the surface containing free radical；It connects
, the ptfe micropowder by the surface containing free radical is distributed in monomer solution, it is placed under inert gas environment,
1 hour~8 hours are reacted at 50 DEG C~80 DEG C to get graft modification ptfe micropowder is arrived；The monomer is acrylic compounds
Containing double bond monomer, acrylic amide containing double bond monomer and esters of acrylic acid containing at least one of double bond monomer；The monomer
Solvent used by solution is deionized water；
The mass fraction of monomer described in the monomer solution is the wt.% of 30 wt.% ~ 70, the ptfe micropowder and institute
The mass ratio for stating monomer is 1/1.2~1/12；
The irradiation dose of the electron beam is 30kGy~270kGy；Radiation dose rate is 30kGy/pass~90kGy/pass；
The graft modification ptfe micropowder is obtained after being filtered, washed and being dried；
(2) the graft modification ptfe micropowder for obtaining the step (1) is scattered in solvent, obtains graft modification
Ptfe micropowder dispersion liquid；
(3) imaging resin is dissolved in solvent and forms imaging resin solution；Then, the grafting step (2) obtained
Modified Teflon micro mist dispersion liquid is mixed with the imaging resin solution, is carried out ultrasonic wave auxiliary and is dispersed with stirring, is divided
Dissipate uniform imaging resin/irradiation grafting modified Teflon micro mist composite dispersion liquid；
(4) the imaging resin/irradiation grafting modified Teflon micro mist composite dispersion liquid obtained the step (3) is equal
Be coated on basement membrane evenly, it is dry after up to moulding laser holographic recording materials, irradiated in the moulding laser holographic recording materials
The mass ratio of graft modification ptfe micropowder and both imaging resins is 1/20~1/200.
3. the preparation method of moulding laser holographic recording materials as claimed in claim 1 or 2, which is characterized in that the step (1)
In, the acrylic compounds are at least one of acrylic acid and methacrylic acid containing double bond monomer；The acrylic amide contains
Double bond monomer is at least one in acrylamide, Methacrylamide, N-isopropylacrylamide and hydroxymethyl acrylamide
Kind；The esters of acrylic acid is methyl methacrylate, glycidyl methacrylate, hydroxyethyl methacrylate containing double bond monomer
At least one in ethyl ester, ethyl acrylate, hydroxy-ethyl acrylate, butyl methacrylate and isobornyl methacrylate
Kind.
4. the preparation method of moulding laser holographic recording materials as claimed in claim 1 or 2, which is characterized in that the step (1)
In, the ptfe micropowder is micron order, and partial size is 0.2 micron~4 microns.
5. the preparation method of moulding laser holographic recording materials as claimed in claim 1 or 2, which is characterized in that the step (2)
In, the solvent is ethyl acetate or butyl acetate；
In the step (3), the imaging resin be acrylate or polyurethane resin, the solvent be toluene, butanone,
Any one in ethyl acetate.
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| CN102020751A (en) * | 2009-09-21 | 2011-04-20 | 浙江中科辐射高分子材料研发中心 | Method for preparing anti-dripping agent |
| CN102933619A (en) * | 2011-05-25 | 2013-02-13 | 泰国Abs有限公司 | Compositions including polytetrafluoroethylene and processes for preparation thereof |
| CN102977276A (en) * | 2012-09-20 | 2013-03-20 | 中国科学院上海应用物理研究所 | Aqueous polytetrafluoroethylene material, preparation method and uses thereof |
| CN103923264A (en) * | 2014-03-19 | 2014-07-16 | 浙江歌瑞新材料有限公司 | Hydrophilic and oleophilic polytetrafluoroethylene micro-powder and preparation method thereof |
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| CN102020751A (en) * | 2009-09-21 | 2011-04-20 | 浙江中科辐射高分子材料研发中心 | Method for preparing anti-dripping agent |
| CN102933619A (en) * | 2011-05-25 | 2013-02-13 | 泰国Abs有限公司 | Compositions including polytetrafluoroethylene and processes for preparation thereof |
| CN102977276A (en) * | 2012-09-20 | 2013-03-20 | 中国科学院上海应用物理研究所 | Aqueous polytetrafluoroethylene material, preparation method and uses thereof |
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