CN108752580B - A kind of double anti-forge material, antifalsification label and preparation method and false-proof detection method - Google Patents
A kind of double anti-forge material, antifalsification label and preparation method and false-proof detection method Download PDFInfo
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- CN108752580B CN108752580B CN201810504858.XA CN201810504858A CN108752580B CN 108752580 B CN108752580 B CN 108752580B CN 201810504858 A CN201810504858 A CN 201810504858A CN 108752580 B CN108752580 B CN 108752580B
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- 239000000463 material Substances 0.000 title claims abstract description 88
- 238000001514 detection method Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 16
- 230000009477 glass transition Effects 0.000 claims abstract description 13
- 238000003490 calendering Methods 0.000 claims abstract description 11
- 230000003446 memory effect Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 22
- -1 dimethyl ester compound Chemical class 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 230000015556 catabolic process Effects 0.000 claims description 9
- 238000006731 degradation reaction Methods 0.000 claims description 9
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229940095054 ammoniac Drugs 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 125000001118 alkylidene group Chemical group 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- VXJPCEOTZNHHOA-UHFFFAOYSA-N [K].OC Chemical compound [K].OC VXJPCEOTZNHHOA-UHFFFAOYSA-N 0.000 claims description 2
- 125000000732 arylene group Chemical group 0.000 claims description 2
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical class C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 abstract description 4
- 125000003342 alkenyl group Chemical group 0.000 abstract 1
- 230000001678 irradiating effect Effects 0.000 description 7
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- ALOUNLDAKADEEB-UHFFFAOYSA-N dimethyl sebacate Chemical compound COC(=O)CCCCCCCCC(=O)OC ALOUNLDAKADEEB-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- PVRATXCXJDHJJN-UHFFFAOYSA-N dimethyl 2,3-dihydroxybutanedioate Chemical compound COC(=O)C(O)C(O)C(=O)OC PVRATXCXJDHJJN-UHFFFAOYSA-N 0.000 description 1
- UNYPJOQXQWCISC-UHFFFAOYSA-N dimethyl 2-nonylpropanedioate Chemical compound CCCCCCCCCC(C(=O)OC)C(=O)OC UNYPJOQXQWCISC-UHFFFAOYSA-N 0.000 description 1
- FXJUUMGKLWHCNZ-UHFFFAOYSA-N dimethyl furan-2,3-dicarboxylate Chemical compound COC(=O)C=1C=COC=1C(=O)OC FXJUUMGKLWHCNZ-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940014772 dimethyl sebacate Drugs 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012781 shape memory material Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
- G09F3/02—Forms or constructions
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Theoretical Computer Science (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Luminescent Compositions (AREA)
- Examining Or Testing Airtightness (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The present invention relates to a kind of double anti-forge material, antifalsification label and preparation method and false-proof detection methods.The material has fluorescent effect under ultraviolet light, has shape memory effect under the conditions of 50~120 DEG C, structural formula:R is any one or more of combination of alkyl, alkyl, naphthenic base, aromatic radical；R1For any one or more of combination of alkyl, alkenyl, aromatic radical；5≤n≤1000, and n is integer.There is the pattern of setting protrusion or the plate of text vacuumizing and material is pressed into surface under the conditions of 180~240 DEG C by tablet press machine, plate is rolled in the environment of slightly above material glass transition temperature later, forms surfacing and the antifalsification label with a thickness of 0.1~1.5mm after calendering.Double anti-forge material of the present invention and antifalsification label have fluorescence falsification preventing and the anti-fake double anti-forge effect of shape memory, and antifalse effect is more preferable.In addition preparation method and detection method of the present invention are simple.
Description
Technical field
The invention belongs to anti-fake material technical field, it is specifically related to a kind of double anti-forge material, antifalsification label and preparation
Method and false-proof detection method.
Background technique
With being constantly progressive for society, the development of industrial or agricultural, the commodity that class is different, dazzling are promoting commodity economy
While high speed development, the needs of the living standard of people's continuous improvement are also met.However, unpleasant adulterant
Dragons and snakes jumbled together enters circulation market.Counterfeit money, forged bill, the adulterant under counterfeit trade-mark shielding and pseudo- certificate etc. often make one to be deceived,
It sustains a loss.Anti-fake material starts to be widely used in certificate, currency, label and vital document, the marrow of anti-fake material
It is difficult mimetism and property easy to identify, the deep favor by many people.Nowadays, anti-fake material has become most important and most popular
One of research field.Scientist has been successfully prepared various anti-fake materials, such as fluorescence falsification preventing material, laser anti-counterfeit material,
Shape memory anti-fake material etc..
Fluorescence falsification preventing material can respond different fluorescent effects after environmental stimuli, and scientific and technological content is higher, color concealment
It is good, there is certain aesthetics.Laser anti-counterfeit reflects different color or pattern by different angle observation, and antifalse effect is good
Good, color is beautiful.Shape-memory material is a kind of current novel anti-fake material, and shape can occur certain after environmental stimuli
Variation, and the process of change in shape be it is controllable, can be to be edited.The antifalsification label inspection made of shape memory anti-fake material
Proved recipe formula is simple, reliable, and shape memory anti-fake material is then easy with identification, copies the difficult and moderate depth of price by business and consumer
Favor.But with the rapid development of science and technology, fake and forged bring high profit makes forgery technology also can more mix the spurious with the genuine,
Huge challenge is brought to anti-fake material.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of double anti-forge material, antifalsification label and preparation method with
False-proof detection method.
In order to achieve the object of the present invention, the invention adopts the following technical scheme:
A kind of double anti-forge material, the material have fluorescent effect under ultraviolet light, and the material is in 50~120 DEG C of items
There is shape memory effect under part, the structural formula of the material is as follows:
Wherein, R is the combination of alkylidene, cycloalkylidene, any group in arylene or a variety of groups；R1For Asia
Alkyl；5≤n≤1000, and n is integer.
Further technical solution: for the glass transition temperature of the material at 45~120 DEG C, degradation temperature is 260~300
℃；The breaking strength of the material is 30~110MPa, and elongation at break is 5~15%, 36~52MJ/m of toughness after moisture absorption3。
Antifalsification label made of double anti-forge material described in a kind of, the label are obtained by following procedure of processing:
Step 1, by tablet press machine vacuumizing and the material is pressed into surface by 180~240 DEG C of under the conditions ofs has
Set the pattern of protrusion or the plate of text, the 0.1~2mm of plate thickness, the pattern or text height 0.1 of the protrusion~
1mm；
Step 2 rolls the plate in the environment of the slightly above material glass transition temperature, is formed after calendering
Surfacing and film with a thickness of 0.1~1.5mm, the film constitute the antifalsification label.
A kind of preparation method of the double anti-forge material, comprising the following steps:
Step 1, by 35~156 parts by weight dimethyl ester compounds and the alcohol ammoniac compounds of 28~87 parts by weight heating it is molten
It solves and stirs evenly to form reaction solution；The structural formula of the dimethyl ester compound isThe alcohol Ammonia
Close object structural formula be
Be added 0.1~0.3 parts by weight basic catalyst in step 2, Xiang Suoshu reaction solution, heated sealed to 60~80 DEG C it is anti-
Answer 2~for 24 hours；
Reaction solution described in step 2 is heated to 95~105 DEG C by step 3, and water pump vacuumizes reaction 1~3 hour；
Reaction solution described in step 3 is heated to 145~155 DEG C by step 4, and oil pump vacuumizes reaction 0.5~1.5 hour；
Reaction solution described in step 4 is heated to 210~230 DEG C by step 5, and oil pump vacuumizes reaction 0.5~1.5 hour,
Obtain the double anti-forge material.
Further technical solution: the catalyst is sodium methoxide solution, methanol potassium solution, any in alcohol sodium solution
Kind.
The antifalsification label is heated 10 under the conditions of 50~120 DEG C by a kind of false-proof detection method of the antifalsification label
~30 seconds, the antifalsification label is placed under ultraviolet light later, observes the shape and color change of antifalsification label；When described anti-
There is the pattern of setting protrusion on pseudo label surface or text and issues expected fluorescent effect, then it represents that the antifalsification label be it is true, it is no
It is then false.
Further technical solution: the antifalsification label heating directlys adopt hot wind or hot-water soak.
The beneficial effects of the present invention are:
(1) double anti-forge material of the present invention has good thermal stability and excellent mechanical performance.The present invention
The double anti-forge material and the antifalsification label made of the double anti-forge material are shunk after the heating, and surface shape occurs
Variation, while apparent fluorescence color is generated under ultraviolet irradiation, so that strong tactile and vision difference are generated to people, it is anti-fake
Significant effect, and detect simple to operate.Due to different group R and R1The double anti-forge material of composition can issue difference
Fluorescence color so that copy difficulty it is big, i.e., the antifalse effect of double anti-forge material of the present invention is more preferable.
(2) double anti-forge material of the present invention by dimethyl ester compound and alcohol ammoniac compounds do not need to add it is molten
Synthesis obtains in the case where agent, and synthetic method is simple, no pollution to the environment, and product does not need clarification, and recycling is easy.
The chemical equation of dimethyl ester compound and alcohol ammoniac compounds of the present invention is as follows:
During the preparation process, the effect that the water pump vacuumizes is double anti-forge material of the present invention: removing reactant
Impurity in system；The effect that oil pump vacuumizes is to prevent reaction system to be oxidized, and molecular weight of product is gradually increased, whole
Performance is more preferable.
(3) during the preparation process, the shape of the plate is permanent memory shape to antifalsification label of the present invention, after calendering
The shape of the film of formation is interim shape memory, after the antifalsification label passes through the detection of false-proof detection method, Jiu Huicong
Interim shape memory switchs to permanent memory shape, and the pattern or text of antifalsification label surface bulge display again at this time,
To be more conducive to realize shape memory antiforge function.
Detailed description of the invention
Fig. 1 is the schematic diagram that double anti-forge material generates shape memory effect in example 1.Example 1 pair as can be seen from Figure 1
The smooth interim shape memory of weight anti-fake material slightly above glass transition temperature at a temperature of heating after be gradually restored to roll over
Folded permanent memory shape.
Fig. 2 is the schematic diagram that double anti-forge material generates fluorescent effect in example 1,2,3.As can be seen from Figure 2 example 1,
2, the fluorescent effect of different colours is generated under the ultraviolet light of the 365nm of 3 double anti-forge materials, example 1 generates blue-fluorescence,
Example 2 generates green fluorescence, and example 3 generates yellow fluorescence.
Fig. 3 is the false-proof detection method schematic diagram of double anti-forge label in example 1.Example 1 is dual as can be seen from Figure 3
The false-proof detection method of antifalsification label: blue-fluorescence can be issued under heating and ultraviolet irradiation and surface shows certified products two
The text of protrusion.
Fig. 4 is that double anti-forge material generates the fluorescence pattern that fluorescent effect obtains in example 1.Example 1 as can be seen from Figure 4
The fluorescence spectra of double anti-forge material, the peak of fluorescence mainly in the spectral range of blue light, show 1 material of example ultraviolet
Blue-fluorescence is issued after light excitation.
Specific embodiment
More specific detail is made to technical solution of the present invention below with reference to embodiment:
Example 1
It takes dimethyl sebacate 9.5g, 1,3 diamino -2- propyl alcohol 3.7g to be uniformly mixed at 70 DEG C, 250 μ L sodium methoxides is added
Solution (concentration 5mol/L) seals 70 DEG C of heating 12h.Water pump vacuumize and be heated to 100 DEG C of reaction 2h to reaction system without
Liquid exists, and water pump is changed to oil pump and vacuumizes and be heated to 150 DEG C of reaction 1h, last oil pump, which vacuumizes, is heated to 220 DEG C
1h is reacted, double anti-forge material is obtained.
For the glass transition temperature of the double anti-forge material at 50 DEG C, degradation temperature is 280 DEG C；The fracture of the material is strong
Degree is 70MPa, elongation at break 8%, toughness 45MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
0.1mm, shape or text protrusion 0.1mm.Plate is heated, it is smooth that the plate of heating is pressed into 0.1mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Reveal pattern or text, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue obvious
Blue-fluorescence, obtain double anti-forge label.
Example 2
It takes dimethyl malenate 13.5g, 1,3 diamino -2- propyl alcohol 9.3g to be uniformly mixed at 70 DEG C, 650 μ L methanol is added
Sodium solution (concentration 5mol/L) seals 70 DEG C of heating 10h.Water pump vacuumizes and is heated to 100 DEG C of reaction 1h to reaction system
No liquid exists, and water pump is changed to oil pump and vacuumizes and be heated to 150 DEG C of reaction 0.8h, last oil pump, which vacuumizes, to be heated to
220 DEG C of reaction 1h, are prepared double anti-forge material.
For the glass transition temperature of the double anti-forge material at 120 DEG C, degradation temperature is 300 DEG C；The fracture of the material
Intensity is 110MPa, elongation at break 5%, toughness 52MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
1mm, shape or text protrusion 0.5mm.Plate is heated, it is smooth that the plate of heating is pressed into 0.8mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Pattern or text out, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue apparent
Green fluorescence obtains double anti-forge label.
Example 3
It takes dimethyl terephthalate (DMT) 5.9g, 1,3 diamino -2- propyl alcohol 2.8g to be uniformly mixed at 70 DEG C, 190 μ L first is added
Alcohol sodium solution (concentration 5mol/L) seals 70 DEG C of heating 10h.Water pump vacuumizes and is heated to 100 DEG C of reaction 1.5h to reaction
System no liquid exists, and water pump is changed to oil pump and vacuumizes and is heated to 150 DEG C of reaction 0.5h, last oil pump vacuumizes heating
To 220 DEG C of reaction 0.8h, double anti-forge material is prepared.
For the glass transition temperature of the double anti-forge material at 90 DEG C, degradation temperature is 290 DEG C；The fracture of the material is strong
Degree is 100MPa, elongation at break 7%, toughness 43MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
2mm shape or text protrusion 1mm.Plate is heated, the plate of heating is pressed into smooth thin of 1.5mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Pattern or text, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue apparent yellow
Color fluorescence obtains double anti-forge label.
Example 4
It takes and decane dicarboxylic dimethyl ester 2.6g, 1,3 diamino -2- propyl alcohol 1.9g is uniformly mixed at 60 DEG C, 100 μ L are added
Sodium methoxide solution (concentration 5mol/L) seals 60 DEG C of heating for 24 hours.Water pump vacuumizes and is heated to 95 DEG C of reaction 3h to reactant
It is that no liquid exists, water pump is changed to oil pump and vacuumizes and be heated to 155 DEG C of reaction 0.5h, last oil pump, which vacuumizes, to be heated to
210 DEG C of reaction 1.5h, are prepared double anti-forge material.
For the glass transition temperature of the double anti-forge material at 45 DEG C, degradation temperature is 260 DEG C；The fracture of the material is strong
Degree is 30MPa, elongation at break 15%, toughness 36MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
2mm, shape or text protrusion 1mm.Plate is heated, the plate of heating is pressed into smooth thin of 1.5mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Pattern or text, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue apparent bright
Blue color fluorescence, obtains double anti-forge label.
Example 5
It takes and dimethyl adipate 7.0g, 1,3 diamino -2- propyl alcohol 3.7g is uniformly mixed at 60 DEG C, 250 μ L methanol are added
Sodium solution (concentration 5mol/L) seals 65 DEG C of heating 14h.Water pump vacuumizes and is heated to 100 DEG C of reaction 1.5h to reactant
It is that no liquid exists, water pump is changed to oil pump and vacuumizes and be heated to 155 DEG C of reaction 0.8h, last oil pump, which vacuumizes, to be heated to
215 DEG C of reaction 1.2h, are prepared double anti-forge material.
For the glass transition temperature of the double anti-forge material at 82 DEG C, degradation temperature is 287 DEG C；The fracture of the material is strong
Degree is 85MPa, elongation at break 7%, toughness 46MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
2mm, shape or text protrusion 1mm.Plate is heated, the plate of heating is pressed into smooth thin of 1.5mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Pattern or text, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue apparent light
Blue color fluorescence, obtains double anti-forge label.
Example 6
It takes dimethyl tartrate 3.7g, 1,3 diamino -2- propyl alcohol 1.9g to be uniformly mixed at 65 DEG C, 130 μ L sodium methoxides is added
Solution (concentration 5mol/L) seals 75 DEG C of heating 12h.Water pump vacuumize and be heated to 105 DEG C of reaction 2h to reaction system without
Liquid exists, and water pump is changed to oil pump and vacuumizes and be heated to 150 DEG C of reaction 1.2h, last oil pump, which vacuumizes, is heated to 220
DEG C reaction 1h, double anti-forge material is prepared.
For the glass transition temperature of the double anti-forge material at 92 DEG C, degradation temperature is 285 DEG C；The fracture of the material is strong
Degree is 105MPa, elongation at break 5%, toughness 39MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
2mm, shape or text protrusion 1mm.Plate is heated, the plate of heating is pressed into smooth thin of 1.5mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Pattern or text, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue apparent shallow
Yellow fluorescence obtains double anti-forge label.
Example 7
It takes furan dicarboxylic acid dimethyl ester 7.4g, 1,3 diamino -2- propyl alcohol 3.7g to be uniformly mixed at 65 DEG C, 260 μ L first is added
Alcohol sodium solution (concentration 5mol/L) seals 70 DEG C of heating 15h.Water pump vacuumizes and is heated to 110 DEG C of reaction 2.5h to reaction
System no liquid exists, and water pump is changed to oil pump and vacuumizes and be heated to 150 DEG C of reaction 1h, last oil pump, which vacuumizes, to be heated to
225 DEG C of reaction 1.5h, are prepared double anti-forge material.
For the glass transition temperature of the double anti-forge material at 95 DEG C, degradation temperature is 295 DEG C；The fracture of the material is strong
Degree is 107MPa, elongation at break 6%, toughness 49MJ/m after moisture absorption3。
Using tablet press machine, which designs various shapes or text, a certain distance is arranged between shape or text
(distance is rolled thinning degree according to plate and is arranged, and plate is calendered thinner, then distance is bigger).Mold is selected to take out in high temperature
Above-mentioned double anti-forge material is pressed into surface with the plate with mold corresponding pattern or text under vacuum condition, plate thickness is
2mm, shape or text protrusion 1mm.Plate is heated, the plate of heating is pressed into smooth thin of 1.5mm using three-roller calendar
Film.It when smooth film is made antifalsification label, with heat gun or is immersed in boiled water, film will shrink and show
Pattern or text, when separately irradiating film ultraviolet light pen or be placed under cash inspecting machine, irradiated area will issue apparent deep
Green fluorescence obtains double anti-forge label.
The above example is merely to illustrate implementation of the invention, is not intended to limit the scope of the invention.?
The modifications and adaptations that technical staff makes according to the present invention in practical application, still fall within protection scope of the present invention.
Claims (7)
1. a kind of double anti-forge material, it is characterised in that: the material has fluorescent effect under ultraviolet light, and the material is 50
There is shape memory effect under the conditions of~120 DEG C, the structural formula of the material is as follows:
Wherein, R is the combination of alkylidene, cycloalkylidene, any group in arylene or a variety of groups；R1For alkylidene；
5≤n≤1000, and n is integer.
2. double anti-forge material as described in claim 1, it is characterised in that: the glass transition temperature of the material 45~
120 DEG C, degradation temperature is 260~300 DEG C；The breaking strength of the material is 30~110MPa, and elongation at break is 5~15%,
36~52MJ/m of toughness after moisture absorption3。
3. a kind of antifalsification label made of double anti-forge material of any of claims 1 or 2: it is characterized in that the label passes through
Following procedure of processing obtains:
Step 1 has setting vacuumizing and the material is pressed into surface under the conditions of 180~240 DEG C by tablet press machine
The pattern of protrusion or the plate of text, the 0.1~2mm of plate thickness, 0.1~1mm of pattern or text height of the protrusion；
Step 2 rolls the plate in the environment of the slightly above material glass transition temperature, and surface is formed after calendering
Film smooth and with a thickness of 0.1~1.5mm, the film constitute the antifalsification label.
4. a kind of preparation method of double anti-forge material as claimed in claim 1 or 2, it is characterised in that the following steps are included:
Step 1 dissolves by heating 35~156 parts by weight dimethyl ester compounds and the alcohol ammoniac compounds of 28~87 parts by weight simultaneously
It stirs evenly to form reaction solution；The structural formula of the dimethyl ester compound isThe alcohol ammoniac compounds
Structural formula be
0.1~0.3 parts by weight basic catalyst, heated sealed to 60~80 DEG C of reactions 2 are added in step 2, Xiang Suoshu reaction solution
~for 24 hours；
Reaction solution described in step 2 is heated to 95~105 DEG C by step 3, and water pump vacuumizes reaction 1~3 hour；
Reaction solution described in step 3 is heated to 145~155 DEG C by step 4, and oil pump vacuumizes reaction 0.5~1.5 hour；
Reaction solution described in step 4 is heated to 210~230 DEG C by step 5, and oil pump vacuumizes reaction 0.5~1.5 hour, obtains
The double anti-forge material.
5. the preparation method of double anti-forge material as claimed in claim 4, it is characterised in that: the catalyst is that sodium methoxide is molten
Any one of liquid, methanol potassium solution, alcohol sodium solution.
6. a kind of false-proof detection method of antifalsification label as claimed in claim 3, it is characterised in that: by the antifalsification label 50
It is heated under the conditions of~120 DEG C 10~30 seconds, the antifalsification label is placed under ultraviolet light later, observes the shape of antifalsification label
And color change；When there are the pattern for setting protrusion or text in the antifalsification label surface and issues expected fluorescent effect, then it represents that
The antifalsification label is true, is otherwise false.
7. the false-proof detection method of antifalsification label as claimed in claim 6, it is characterised in that: the antifalsification label heating is direct
Using hot wind or hot-water soak.
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| CN102968928A (en) * | 2012-11-23 | 2013-03-13 | 黄为民 | Multi-layered anti-counterfeit label and production method and multi-layered anti-counterfeit indication method thereof |
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