CN1280920A - Reversible thermosensitive display material and its preparing process - Google Patents
Reversible thermosensitive display material and its preparing process Download PDFInfo
- Publication number
- CN1280920A CN1280920A CN 00119587 CN00119587A CN1280920A CN 1280920 A CN1280920 A CN 1280920A CN 00119587 CN00119587 CN 00119587 CN 00119587 A CN00119587 A CN 00119587A CN 1280920 A CN1280920 A CN 1280920A
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- microcapsules
- reversible thermosensitive
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- thermosensitive display
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Abstract
A reversible thermosensitive indication material is made up by coating a kind of reversible thermosensitive allochroic microcapsules on paper or film. Said microcapsule is composed of the colouring material including electronic colour-masking dye, electronic compatible developer, crystallization promoter and solvent, and the wall film of microcapsule uses amino resin or epoxy resin. It can be used for antiforge purpose.
Description
The present invention is display material of being made into of a kind of reversible heat-sensible electrochromic substance and preparation method thereof.
Present existing thermosensitive display material is thermal fax paper and thermal printing paper mostly, but their weak point is that the information of putting down in writing up can not be hidden wipes, some purposes that specific use is arranged can't be realized, for example anti-fake mark, special bill, certificate etc.For many years people seeking always a kind of easy to make and the record the erasable under certain condition material of information.
The objective of the invention is to invent a kind of reversible thermosensitive display material and preparation method thereof.
Reversible thermosensitive display material of the present invention mainly is made up of reversible heat-sensible variable color emblem capsule pigment and base material thereof, the microcapsules that are enclosed with chromophoric dyestuffs are made dispersion emulsion to be coated on base material such as paper, the macromolecule membrane, for reducing cost, therefore only need be coated with very thin one deck is changeable colour.The composition of chromophoric dyestuffs is (wt%) in the microcapsules:
The sub-property leuco dye of powering: 0.1～35%
Electronics compatibility developer: 0.1～40%
Crystallization promoter: 0.02～25%
Solvent: 2～80%
The wall membrane material of microcapsules can be amino resins or epoxy resin, as: melamine, E51 epoxy resin etc.
The base material of above-mentioned reversible heat-sensible color development microcapsules can be paper, macromolecule membrane etc., reversible heat-sensible variable color microcapsules are coated on paper or the film, make picture and text, can make paper, polyethylene, the polyester film that just can show recorded information under certain condition.
Select different chromonic material and color development temperature thereof, can obtain the display material that under different temperatures, develops the color or hide.
To power when material of the present invention is made sub-property leuco dye, electronics compatibility developer, crystallization promoter and four kinds of materials of solvent are formed the interior chromonic material of microcapsules, the wall membrane material of microcapsules is amino resins or epoxy resin, and the composition of chromophoric dyestuffs material is as described above in the microcapsules.The preparation method and the prior art of microcapsules are same, are to make the disclosed routine techniques of microcapsules at present.The microcapsule emulsion that is inclusive with the reversible heat-sensible chromotropic dye is coated on the base material gets final product.
The sub-property of power supply of the present invention leuco dye can be the triphenylmenthane phthalide compound, spiropyran compounds, fluoran compound etc.Specifically can exemplify out 3-chloro-6 phenylamino fluoranes, 3-lignocaine-6-methyl-7-chlorine fluorane, 3.3.3-three (to dimethylamino phenyl) phthalein, 3,3-dibutoxy fluorane, 3-lignocaine-7-phenylamino fluorane, 3-dimethyl-7,8-phenyl fluorane etc.Also wherein two or more can be used.
The electronics compatibility developer that the present invention matches with leuco dye can be a benzotriazole, phenols, thiourea derivative, aromatic carboxylic acid etc., object lesson such as 5-butyl BTA, nonyl phenol, bisphenol-A, Bisphenol F, 1, the two hydroxyl naphthalenes of 5-, alkyl paraben, allylthiourea, phthalic acid, trimesic acid, salicylic acid and slaine thereof.Also wherein two or more can be used.
Crystallization promoter can be an organic dyestuff as Vetaflavin, auramine, anthraquinone etc.,
The solvent that uses in the above-mentioned system can be the ester class, wax class or alcohols.As dodecoic acid 14 esters, tetradecylic acid ten diester, tetradecylic acid 14 esters, hexadecylic acid monooctyl ester, hexadecylic acid heptyl ester, hexadecylic acid ten diester, hexadecylic acid octadecyl ester, p-tert-butyl benzoic acid hexadecyl ester, the two hexadecyl esters of thio-2 acid.Ka Naba wax, palm wax, insect wax, microwax.Lauryl alcohol, tetradecyl alchohol, hexadecanol, 18 alcohol, docosanol etc.Also wherein two or more can be used.
In the above-mentioned preparation: the weight ratio of power sub-property leuco dye and electronics compatibility developer is 1: 0.5～1: 15;
The weight ratio of sub-property leuco dye and crystallization promoter of powering is: 1: 0.2～1: 2;
The weight ratio of sub-property leuco dye and solvent of powering is 1: 5～1: 50.
If reversible heat-sensible variable color microcapsules of the present invention are mixed with printing ink, promptly, then can be advantageously used in trade mark with the base material of printing ink as microcapsules, various needs such as certificate prevent the printing figure message palmed off.
The present invention relates to a kind of reversible thermosensitive display material.Its essence is a kind of reversible heat-sensible variable color microcapsules pigment with memory effect.It is coated paper or surperficial thermal fax paper and the thermal printing paper and the erasable information recording carrier that can show repeatedly of just can making of macromolecule membrane.This reversible heat-sensible variable color microcapsules pigment with memory effect also can be used for modulating anti-forgery ink, is used for various needs such as trade mark or certificate and prevents the picture and text printing palmed off.This printing figure message is hidden colourless at normal temperatures, changes coloured picture and text into after temperature is higher than a specified temp and cooling, if be placed under the specific low temperature, it can be returned to hidden colourless state again.By changing prescription, can obtain and the corresponding state of above-mentioned this change color process: printing figure message is coloured at normal temperatures, change hidden colourless state after temperature is higher than a specified temp into, if be placed under the specific low temperature, it can be returned to colored state again.
This reversible heat-sensible variable color microcapsules pigment with memory effect can be made various different colours and discoloring temperature, therefore can wiping information record and anti-counterfeit printing aspect be with a wide range of applications.
Example 1
The preparation of A component:
Get 150 part 4% EMA anhydride copolymer (trade name: aqueous solution EMA-31 MONSANTOCHEMICAL CO), sodium hydroxide solution adjusting PH=3.5 with 10%.Add 9 parts in urea, 1 part of resorcinol is warming up to 65 ℃ and makes it form homogeneous solution.
The preparation of B component:
With following each composition heating and melting, make it become even melt, keep 75 ℃ of temperature.
4 parts of 3-lignocaines-6-methyl-7-chlorine fluorane
8 parts of bisphenol-As
0.05 part of Vetaflavin
67 parts of hexadecylic acid heptyl esters
8 parts of UV-326 (ultraviolet absorber)
The B component is added in the A component, stir fast and make it to form emulsion, in system, add 22 part 37% formalin then.Be incubated 60 ℃ and also continue to stir 4 hours, obtain the microcapsules aqueous dispersions after the cooling.In this dispersion liquid, add paper with 30 parts in glue, mix.On paper, be coated with, promptly obtain repeatedly used electrothermal sensitive recording paper after the drying.This paper is a reddish orange in the time of 24 ℃, and heating surpasses 35 ℃ and becomes colorless, and still keeps colourless state when being cooled to 24 ℃, reverts to reddish orange after continuing to be cooled to 0 ℃.
Example 2
A component preparation: with example 1
The preparation of B component:
With following each composition heating and melting, make it become even melt, keep 75 ℃ of temperature.
Colourless fluoran dyes (trade name; Green DCF Japan hodogaya chemical)
4 parts
20 parts of nonyl phenols
0.06 part of anthraquinone
60 parts of stearyl alcohols
8 parts of UV-326 (ultraviolet absorber)
6 parts of antioxidant 1010s
The B component is added in the A component, stir fast and make it to form emulsion, in system, add 22 part 37% formalin then.Be incubated 60 ℃ and also continue to stir 4 hours, obtain the microcapsules aqueous dispersions after the cooling.In this dispersion liquid, add paper with 30 parts in glue, mix.On paper, be coated with, promptly obtain repeatedly used electrothermal sensitive recording paper after the drying.This paper is colourless at normal temperatures, and heating shows green when surpassing 65 ℃ and cool to room temperature, continues to be cooled to 0 ℃ and keep recovering after two hours colourless state.
Claims (7)
1. a reversible thermosensitive display material is made up of reversible heat-sensible variable color microcapsules and base material thereof, it is characterized in that reversible heat-sensible variable color microcapsules are applied on base material, and wherein the composition of chromophoric dyestuffs is (wt%) in the reversible heat-sensible variable color microcapsules:
Sub-property leuco dye 0.1-35% powers
Electronics compatibility developer 0.1-40%
Crystallization promoter 0.02-25%
Solvent 2-80%
2. reversible thermosensitive display material according to claim 1, the base material that it is characterized in that scribbling reversible heat-sensible color development microcapsules is paper or macromolecular material.
3. the preparation method of a reversible thermosensitive display material, it is characterized in that the sub-property of power supply leuco dye, electronics compatibility developer, crystallization promoter and solvent chromonic material are contained within the microcapsules, the wall membrane material of microcapsules is amino resins or epoxy resin, and the composition of the chromonic material in the microcapsules is (wt%):
Sub-property leuco dye 0.1-35% powers
Electronics compatibility developer 0.1-40%
Crystallization promoter 0.02-25%
Solvent 2-80%
The above-mentioned reversible heat-sensible variable color microcapsule emulsion of making coated on the base material get final product.
4. according to the preparation method of the reversible thermosensitive display material described in the claim 3, the weight ratio of it is characterized in that powering sub-property leuco dye and electronics compatibility developer is: 1: 0.5-1: 15.
5. according to the preparation method of the reversible thermosensitive display material described in the claim 3, it is characterized in that powering sub-property leuco dye and crystallization promoter weight ratio are: 1: 0.2-1: 5.
6. according to the preparation method of the reversible thermosensitive display material described in the claim 3, the sub-property leuco dye that it is characterized in that powering with the weight of solvent ratio is: 1: 5-1: 50.
7. according to the reversible thermosensitive display material described in claim 1 or 3, it is characterized in that reversible heat-sensible variable color microcapsules are mixed with printing ink, be used for anti-fake mark and make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00119587 CN1280920A (en) | 2000-08-10 | 2000-08-10 | Reversible thermosensitive display material and its preparing process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00119587 CN1280920A (en) | 2000-08-10 | 2000-08-10 | Reversible thermosensitive display material and its preparing process |
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| CN1280920A true CN1280920A (en) | 2001-01-24 |
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| CN 00119587 Pending CN1280920A (en) | 2000-08-10 | 2000-08-10 | Reversible thermosensitive display material and its preparing process |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1989015B (en) * | 2004-07-15 | 2011-06-15 | 惠普开发有限公司 | Compositions, systems and methods for imaging |
| CN102863949A (en) * | 2012-08-31 | 2013-01-09 | 上海俊彩文具用品有限公司 | Developing temperature control agent with memory and temperature variation synthesis particle using developing temperature control agent |
| CN102987663A (en) * | 2012-12-19 | 2013-03-27 | 邹勇 | Silica gel ring and making method thereof |
| CN103205250A (en) * | 2013-03-05 | 2013-07-17 | 上海市电力公司 | Reversible thermochromic material and application thereof |
| CN105324445A (en) * | 2013-05-13 | 2016-02-10 | 法斯维尔公司 | Thermochromic ink composition |
| CN108366617A (en) * | 2015-12-31 | 2018-08-03 | 菲利普莫里斯生产公司 | Aerosol including heat indicator generates product |
| CN109154528A (en) * | 2016-05-24 | 2019-01-04 | 株式会社日立制作所 | Temperature history display body and article quality management method using same |
| CN110114647A (en) * | 2016-12-14 | 2019-08-09 | 株式会社日立产机系统 | Temperature detection material, temperature detection ink using same, temperature indicator, method for manufacturing temperature detection material, and article management system |
| CN110770035A (en) * | 2017-06-20 | 2020-02-07 | 索尼公司 | Reversible recording medium |
| CN112339467A (en) * | 2021-01-07 | 2021-02-09 | 虎丘影像（苏州）有限公司 | Fluorine-containing thermosensitive dye microcapsule, preparation method thereof and film |
| CN113429420A (en) * | 2021-06-09 | 2021-09-24 | 江南大学 | Preparation method of high-sensitivity temperature-sensing reversible color-changing microcapsule |
-
2000
- 2000-08-10 CN CN 00119587 patent/CN1280920A/en active Pending
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1989015B (en) * | 2004-07-15 | 2011-06-15 | 惠普开发有限公司 | Compositions, systems and methods for imaging |
| CN102863949A (en) * | 2012-08-31 | 2013-01-09 | 上海俊彩文具用品有限公司 | Developing temperature control agent with memory and temperature variation synthesis particle using developing temperature control agent |
| CN102863949B (en) * | 2012-08-31 | 2014-10-15 | 上海俊彩文具用品有限公司 | Developing temperature control agent with memory and temperature variation synthesis particle using developing temperature control agent |
| CN102987663B (en) * | 2012-12-19 | 2015-01-28 | 深圳市利勇安硅橡胶制品有限公司 | Silica gel ring and making method thereof |
| CN102987663A (en) * | 2012-12-19 | 2013-03-27 | 邹勇 | Silica gel ring and making method thereof |
| CN103205250B (en) * | 2013-03-05 | 2015-04-29 | 上海市电力公司 | Reversible thermochromic material and application thereof |
| CN103205250A (en) * | 2013-03-05 | 2013-07-17 | 上海市电力公司 | Reversible thermochromic material and application thereof |
| CN105324445A (en) * | 2013-05-13 | 2016-02-10 | 法斯维尔公司 | Thermochromic ink composition |
| CN105324445B (en) * | 2013-05-13 | 2018-06-01 | 法斯维尔公司 | Thermochromatic inks composition |
| US10239336B2 (en) | 2013-05-13 | 2019-03-26 | Fasver | Method and device for the secure protection of an official document and official document thus protected |
| CN108366617B (en) * | 2015-12-31 | 2021-08-03 | 菲利普莫里斯生产公司 | Aerosol-generating article comprising a thermal indicator and method of use thereof |
| CN108366617A (en) * | 2015-12-31 | 2018-08-03 | 菲利普莫里斯生产公司 | Aerosol including heat indicator generates product |
| US11330835B2 (en) | 2015-12-31 | 2022-05-17 | Philip Morris Products S.A. | Aerosol-generating article comprising a thermal indicator |
| CN109154528A (en) * | 2016-05-24 | 2019-01-04 | 株式会社日立制作所 | Temperature history display body and article quality management method using same |
| CN109154528B (en) * | 2016-05-24 | 2020-06-30 | 株式会社日立制作所 | Temperature history display body and article quality management method using same |
| CN110114647B (en) * | 2016-12-14 | 2022-04-22 | 株式会社日立产机系统 | Temperature detection material, manufacturing method thereof and application of temperature detection material |
| CN110114647A (en) * | 2016-12-14 | 2019-08-09 | 株式会社日立产机系统 | Temperature detection material, temperature detection ink using same, temperature indicator, method for manufacturing temperature detection material, and article management system |
| US11572486B2 (en) | 2016-12-14 | 2023-02-07 | Hitachi Industrial Equipment Systems Co., Ltd. | Temperature detection material, temperature detection ink using same, temperature indicator, method for manufacturing temperature detection material, and product management system |
| CN110770035A (en) * | 2017-06-20 | 2020-02-07 | 索尼公司 | Reversible recording medium |
| CN112339467A (en) * | 2021-01-07 | 2021-02-09 | 虎丘影像（苏州）有限公司 | Fluorine-containing thermosensitive dye microcapsule, preparation method thereof and film |
| CN113429420A (en) * | 2021-06-09 | 2021-09-24 | 江南大学 | Preparation method of high-sensitivity temperature-sensing reversible color-changing microcapsule |
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