CN100436561C - Formula of aqueous glue without polyvinyl alcohol(PVA) - Google Patents
Formula of aqueous glue without polyvinyl alcohol(PVA) Download PDFInfo
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- CN100436561C CN100436561C CNB200610005067XA CN200610005067A CN100436561C CN 100436561 C CN100436561 C CN 100436561C CN B200610005067X A CNB200610005067X A CN B200610005067XA CN 200610005067 A CN200610005067 A CN 200610005067A CN 100436561 C CN100436561 C CN 100436561C
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Abstract
This invention discloses formula of aqueous glue without poly(vinyl alcohol) (PVA), which can be used to adhere PVA polarizing substrate and lye-saponified TAC supporting film. The formula comprises: water, at least one water-soluble dicarboxylic acid monomer, protonic acid, Lewis acid and shielding agent. The water-soluble dicarboxylic acid monomer can form chemical bonds with hydroxyl groups on PVA polarizing substrate and TAC supporting film via esterification. The protonic acid is used to catalyze the esterification reaction. The shielding agent is used to react with hydroxyl groups on PVA polarizing substrate and TAC supporting film to form semi-acetal structure, which can constitute steric hindrance.
Description
Technical field
The present invention relates to the preparation of a kind of water-base cement (hydrous glue), particularly relate to a kind of composition and method of making the same that is applied in the water-base cement that does not contain polyvinyl alcohol (PVA) in the polaroid processing procedure.
Background technology
As is known to the person skilled in the art, in liquid-crystal display, polaroid is one of indispensable construction components, its purposes is originally not have the light of polarizability, to produce polarization, to be transformed into polarized light, therefore, liquid-crystal display just can utilize this polarized light, adds the torsional property of liquid crystal molecule itself, reaches whether passing through of light of control and presenting of color signal.And in recent years, along with liquid crystal display device is widely used in such as in the various electronicss such as word processor (word processor), computer screen, mobile phone or LCD TV, the demand of polaroid is also increasing.
The cross-section structure of existing polaroid 10 as shown in Figure 1; it consists predominantly of fractal film 12, pressure sensing adhesive layer 14, polyvinyl alcohol (polyvinyl alcohol; be designated hereinafter simply as PVA) polarization matrix layer 18, cellulosetri-acetate (tri-acetyl cellulose; be designated hereinafter simply as TAC) support membrane 16 and 20, and protective layer 22.Sometimes, in order to prevent reflex, the polaroid surface also can give special processing again, for example adds anti-(anti-glare) layer or antireflection (anti-reflection) layer of dazzling of last layer.At present, the polaroid on the market is a main flow with the iodine polarizing sheet still, and this is because the iodine polarizing sheet has high light transmittance, high contrast, and has the polarized light property of wider regional wavelength, and its manufacturing is upward more or less freely, relatively also makes its price comparatively cheap.
The method that prior art is made polaroid 10 is pre-treatment steps such as elder generation is soaked with polyvinyl alcohol (PVA) raw material elder generation process, dyeing, extension; form after the aforementioned PVA polarization matrix layer 18 with polarized light property; re-use through special allotment to contain the TAC support membrane 16 and 20 that PVA hydrogel (hydrogel) handled the upper and lower faces of PVA polarization matrix layer 18 and the saponification through alkali lye (sodium hydroxide or potassium hydroxide) bonding; after super-dry, on TAC support membrane 16 and 20, add pressure-sensing glue, fractal film and protective layer etc. again.
Yet, the special allotment of aforementioned process contain the PVA hydrogel, its preparation process extremely bothers, need elder generation that the high-molecular polyvinyl alcohol powder of optical grade is added in the entry, reheat to 80 ℃ is to 90 ℃ high temperature and need continue stirring until and be colloidal, just cool off at last, whole preparation process needs consuming time more than 3 to 4 hours at least.And except preparing time-consuming shortcoming, the existing PVA of containing hydrogel needs to finish using in 1 to 2 day after preparation is finished usually, and when preserving, especially need significant care, because its colloid property is also unstable, if when cloth glue, lump in the colloid (aggregation) or separated out impurity such as particle, promptly can cause the good rate of product line to descend.
In addition, owing to there is increasing liquid-crystal display to be used in such as aspects such as large-scale outdoor display billboard, vehicle, flyer, navigational instruments and satellites, therefore the user is to temperature tolerance and requirement characteristic such as wet fastness on the also increasingly stringent of polaroid in environment, and the iodine polarizing sheet of aforementioned conventional owing to the iodine content in the congenital PVA of the being adsorbed on polarization matrix layer and active easily in time and the influence of environment decay, it is not enough that its temperature tolerance and wet fastness are all disliked, thereby limited the scope of its application.
Summary of the invention
Therefore, main purpose of the present invention promptly is to provide a kind of being applied in not contain PVA water-base cement (hydrous glue) in the polaroid processing procedure, replace prior art and contain the PVA hydrogel, to contain the preparation of PVA hydrogel time-consuming and preserve and shortcoming such as be difficult for to solve prior art.
Another object of the present invention is to provide a kind of be applied in the polaroid processing procedure do not contain the PVA water-base cement form with and preparation method thereof.
Another object of the present invention is to provide a kind of being applied in not contain the PVA water-base cement in the polaroid processing procedure, and can significantly improve the temperature tolerance and the wet fastness of iodine polarizing film.
In order to reach aforementioned purpose, the invention provides a kind of water-base cement composition that does not contain polyvinyl alcohol (PVA), be applied to PVA polarization matrix layer and cellulosetri-acetate (TAC) support membrane handled through the alkali lye saponification between bonding.This water-base cement composition that does not contain PVA includes: water; At least a water-soluble di-carboxylic acid monomer, this monomer can with hydroxyl and the lip-deep hydroxyl generation of this TAC support membrane esterification on this PVA polarization matrix laminar surface, form chemical bonding; Protonic acid is in order to the aforementioned esterification of catalysis; Lewis acid (Lewis acid); And screening agent (masking agent), be used for reacting with this PVA polarization matrix laminar surface or the lip-deep hydroxyl of this TAC support membrane, form half acetal structure, constitute sterically hindered (steric hindrance).
In order to more clearly understand feature of the present invention and technology contents, see also following about detailed description of the present invention and accompanying drawing.Yet described accompanying drawing is only for reference and aid illustration usefulness, is not to be used for the present invention is limited.
Description of drawings
What Fig. 1 illustrated is the cross-section structure of the polaroid of prior art.
What Fig. 2 illustrated is the structural formula of hexanodioic acid.
Fig. 3 illustrates is to use water-base cement that the present invention contains hexanodioic acid under the catalysis of acid, make the TAC support membrane handled through the alkali lye saponification and PVA polarization matrix layer bonding after, as the enlarged diagram of the encircled among Fig. 1.
Description of reference numerals
10 polaroids, 12 fractal films
14 pressure sensing adhesive layer 16TAC support membranes
18PVA polarization matrix layer 18a iodine
20TAC support membrane 22 protective layers
25 encircled, 30 hexanodioic acid molecules
36 two-sided chemical bonding structure 38 single face chemical bonding structures
40 oxalic dialdehydes, 42 half acetal structures
118 hydroxyls, 120 hydroxyls
Embodiment
In order to solve the existing PVA hydrogel too tediously long shortcoming on preparation process that contains, the invention provides a kind of water-base cement (hydrous glue) composition, at first attempt with water-soluble hexanodioic acid (adipicacid; HOOCC
4H
8COOH) monomer replaces the PVA polymeric powder, is prepared into not have the water-base cement of PVA, and its preparation process is simply quick, and owing to be not to be colloidal state, can not be difficult for and agglomeration problems just like the preservation of the hydrogel of prior art.
Hexanodioic acid of the present invention belongs to a kind of di-carboxylic acid (dicarboxylic acid), and for making the required raw material of nylon (Nylon), its structural formula as shown in Figure 2.
According to a preferred embodiment of the invention, water-base cement composition of the present invention does not contain the PVA polymeric powder, and mainly includes water, hexanodioic acid, at least a strong protonic acid, example hydrochloric acid, sulfuric acid or nitric acid, and catalyzer.
According to another preferred embodiment of the invention, water-base cement composition of the present invention mainly includes water, hexanodioic acid, hydrochloric acid, catalyzer and screening agent (masking agent).Wherein, hexanodioic acid also can be replaced by other di-carboxylic acid, for example pentanedioic acid (glutaric acid) or succsinic acid (succinic acid), and be not limited only to hexanodioic acid.
Above-mentioned catalyzer can include inorganic metal salt again, for example zinc chloride (ZnCl
2) or aluminum chloride (AlCl
3), serve as preferred with the effect of zinc chloride gained again wherein.Zinc chloride belongs to a kind of Lewis acid, is taken as reserving agent or catalyzer and uses in other field.
In addition, in other embodiments of the invention, catalyzer also may use metal oxide, for example zinc oxide or aluminum oxide.
Screening agent can be twain-aldehyde compound (dialdehyde), for example oxalic dialdehyde (glyoxal) or methyl-glyoxal (methylglyoxal), wherein again with add oxalic dialdehyde effect serve as preferred.
See also Fig. 3, the water-base cement that is to use the present invention to contain hexanodioic acid that it illustrates makes the TAC support membrane of handling through the alkali lye saponification 20 bonding with PVA polarization matrix layer 18 under acid catalysis, as the enlarged diagram of encircled among Fig. 1 25.According to a preferred embodiment of the invention, the processing of PVA polarization matrix layer 18 is same as the prior art, through pre-treatments such as soaked, iodine staining and extensions, makes absorption iodine 18a in the PVA polarization matrix layer 18.
As shown in Figure 3, have many hydroxyls (hydroxyl group) 118 and 120 on the surface of PVA polarization matrix layer 18 and on the surface of TAC support membrane 20, esterification takes place and forms effective two-sided chemical bonding structure 36 in the hexanodioic acid molecule 30 in these hydroxyls and the water-base cement composition of the present invention, makes that TAC support membrane 20 and PVA polarization matrix layer 18 can close adhesion.
On the other hand, owing to be positioned at the hydroxyl on same surface, the single face reaction also may take place with the hexanodioic acid molecule 30 in the water-base cement composition of the present invention in the hydroxyl 118 that for example is located on PVA polarization matrix layer 18 surface, forms invalid chemical bonding 38.This invalid single face chemical bonding structure 38 that is caused by competitive effect can cause the decline of bonding effect between film and the film.Therefore, as shown in Figure 3, the present invention painstakingly adds screening agent oxalic dialdehyde (glyoxal) 40 again in water-base cement, it can be reacted with the hydroxyl on same surface, form half acetal structure 42, constitute sterically hinderedly, use and impel most hexanodioic acid molecule 30 can carry out two-sided reaction, form effective bonding.
Below, the spy enumerates several embodiment, describes water-base cement preparation of compositions method of the present invention in detail.Each moiety in the water-base cement composition of the present invention all reaches the high purity of optical-grade, can be buied by the chemical supplier.
Embodiment one
The hexanodioic acid monomer of the capacity of weighing earlier, and it is dissolved in the hot water that is heated to about 50 ℃ to 60 ℃, can stir in the heat-processed, the concentration of hexanodioic acid in the aqueous solution is reached about 1 to 10 weight percent (wt.%).In addition, in the aqueous solution, add hydrochloric acid, zinc chloride and oxalic dialdehyde, make the concentration of hydrochloric acid in the aqueous solution reach 0.1M to 1.0M respectively, oxalic dialdehyde concentration reach about 3 to 10 weight percents, and the chlorination zinc concentration reaches about 1 to 10 weight percent.About heated and stirred can obtain clear colourless aqueous solution water-base cement finished product after ten minutes.
Embodiment two
The pentanedioic acid of the capacity of weighing (glutaric acid) monomer, and it is dissolved in the hot water that is heated to about 50 ℃ to 60 ℃, can stir in the heat-processed, the concentration of pentanedioic acid in the aqueous solution is reached about 1 to 10 weight percent.In addition, in the aqueous solution, add hydrochloric acid, zinc chloride and oxalic dialdehyde, make the concentration of hydrochloric acid in the aqueous solution reach 0.1M to 1.0M respectively, oxalic dialdehyde concentration reach about 3 to 10 weight percents, and the chlorination zinc concentration reaches about 1 to 10 weight percent.About heated and stirred can obtain clear colourless aqueous solution water-base cement finished product after ten minutes.
Embodiment three
The succsinic acid of the capacity of weighing (succinic acid) monomer, and it is dissolved in the hot water that is heated to about 50 ℃ to 60 ℃, can stir in the heat-processed, the concentration of succsinic acid in the aqueous solution is reached about 1 to 10 weight percent.In addition, in the aqueous solution, add hydrochloric acid, zinc chloride and oxalic dialdehyde, make the concentration of hydrochloric acid in the aqueous solution reach 0.1M to 1.0M respectively, oxalic dialdehyde concentration reach about 3 to 10 weight percents, and the chlorination zinc concentration reaches about 1 to 10 weight percent.About heated and stirred can obtain clear colourless aqueous solution water-base cement finished product after ten minutes.
Embodiment four
The hexanodioic acid monomer of the capacity of weighing, and it is dissolved in the hot water that is heated to about 50 ℃ to 60 ℃, can stir in the heat-processed, the concentration of hexanodioic acid in the aqueous solution is reached about 1 to 10 weight percent.In addition, in the aqueous solution, add hydrochloric acid, aluminum chloride (AlCl
3) and screening agent oxalic dialdehyde, make the concentration of hydrochloric acid in the aqueous solution reach 0.1M to 1.0M respectively, oxalic dialdehyde concentration reach about 3 to 10 weight percents, and the concentration of aluminum chloride reaches about 1 to 10 weight percent.About heated and stirred can obtain clear colourless aqueous solution water-base cement finished product after ten minutes.
Embodiment five
The pentanedioic acid monomer of the capacity of weighing, and it is dissolved in the hot water that is heated to about 50 ℃ to 60 ℃, can stir in the heat-processed, the concentration of pentanedioic acid in the aqueous solution is reached about 1 to 10 weight percent.In addition, in the aqueous solution, add hydrochloric acid, aluminum chloride and oxalic dialdehyde, make the concentration of hydrochloric acid in the aqueous solution reach 0.1M to 1.0M respectively, oxalic dialdehyde concentration reach about 3 to 10 weight percents, and the concentration of aluminum chloride reaches about 1 to 10 weight percent.About heated and stirred can obtain clear colourless aqueous solution water-base cement finished product after ten minutes.
Embodiment six
The succsinic acid monomer of the capacity of weighing, and it is dissolved in the hot water that is heated to about 50 ℃ to 60 ℃, can stir in the heat-processed, the concentration of succsinic acid in the aqueous solution is reached about 1 to 10 weight percent.In addition, in the aqueous solution, add hydrochloric acid, aluminum chloride and oxalic dialdehyde, make the concentration of hydrochloric acid in the aqueous solution reach 0.1M to 1.0M respectively, oxalic dialdehyde concentration reach about 3 to 10 weight percents, and the concentration of aluminum chloride reaches about 1 to 10 weight percent.About heated and stirred can obtain clear colourless aqueous solution water-base cement finished product after ten minutes.
Comparative example one
Will be in hot water through the PVA powder dissolution of weighing, heating, and in addition violent stirring are to avoid caking or to separate out particle.Afterwards, when stirring, above-mentioned solution is cooled to room temperature.Then, add pure water, the moisture so that compensation loses because of heating filters above-mentioned solution again, with the composition that lumps in the filtering solution, produces weight percent concentration and is about 5% PVA hydrogel.The time for preparing above-mentioned PVA hydrogel was about about a few hours.
Comparative example two:
Will be in hot water through the PVA powder dissolution of weighing, heating, and in addition violent stirring are to avoid caking.Afterwards, when stirring, above-mentioned solution is cooled to room temperature, and in stirring and the process of cooling, adds boric acid and zinc chloride again.Then, add pure water, the moisture so that compensation loses because of heating filters above-mentioned solution again, with the composition that lumps in the filtering solution, produces weight percent concentration and is about 5% PVA hydrogel.
Comparative example three:
Will be in hot water through the PVA powder dissolution of weighing, heating, and in addition violent stirring are to avoid caking.Afterwards, when stirring, above-mentioned solution is cooled to room temperature, and in stirring and the process of cooling, adds hydrochloric acid, oxalic dialdehyde and zinc chloride again.Then, add pure water, the moisture so that compensation loses because of heating filters above-mentioned solution again, with the composition that lumps in the filtering solution, produces weight percent concentration and is about 5% PVA hydrogel.The time for preparing above-mentioned PVA hydrogel was about about a few hours.
Test comparison with the water-base cement in aforementioned different embodiment and the comparative example, the Measurement and analysis that comprises thermotolerance, wet fastness, the effect of finding adding Lewis acid zinc chloride (embodiment one to embodiment three) is more preferable than the effect that adds Lewis acid aluminum chloride (embodiment four to embodiment six), and the water-base cement (embodiment one to embodiment six) that does not contain polyvinyl alcohol (PVA) of the present invention is better than conventional P VA water-base cement (comparative example one is to comparative example three).Wherein, the test of aforesaid thermotolerance, wet fastness is that the TAC support membrane that utilizes the water-base cement in different embodiment and the comparative example that PVA polarization matrix layer and the saponification through alkali lye were handled is bonding, cuts sample then respectively, is immersed in 50 ℃ the hot water to test.The result shows, aspect heat-moisture resistance, the sample that adds the Lewis acid zinc chloride all can be kept more than three days, film just can occur and peel off (peeling) phenomenon, and in identical test environment, the sample that imposes traditional PVA (5%) hydrogel (comparative example one is to comparative example three) film then promptly occurred and peels off phenomenon in 50 minutes.
The above only is the preferred embodiments of the present invention, and all equivalent variations and modifications of being done according to claim scope of the present invention all should belong to covering scope of the present invention.
Claims (9)
1. water-base cement composition that does not contain polyvinyl alcohol is applied to bonding between polyvinyl alcohol polarization matrix layer and saponification was handled through alkali lye the cellulosetri-acetate support membrane, and this water-base cement composition that does not contain polyvinyl alcohol includes:
Water;
At least a water-soluble di-carboxylic acid monomer, can with hydroxyl and the lip-deep hydroxyl generation of this cellulosetri-acetate support membrane esterification on this polyvinyl alcohol polarization matrix laminar surface, form chemical bonding;
Protonic acid is in order to the aforesaid esterification of catalysis;
Lewis acid; And
Screening agent is used for reacting with this polyvinyl alcohol polarization matrix laminar surface or the lip-deep hydroxyl of this cellulosetri-acetate support membrane, constitutes sterically hindered.
2. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 1, wherein said di-carboxylic acid select oneself diacid, pentanedioic acid and succsinic acid.
3. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 2, the concentration of wherein said di-carboxylic acid reaches 1 to 10 weight percent.
4. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 1, wherein said protonic acid is selected from hydrochloric acid, sulfuric acid or nitric acid.
5. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 4, the concentration of wherein said protonic acid reaches 0.1M to 1.0M.
6. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 1, wherein said Lewis acid is selected from zinc chloride or aluminum chloride.
7. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 6, wherein said lewis acidic concentration reaches 1 to 10 weight percent.
8. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 1, wherein said screening agent comprises oxalic dialdehyde and methyl-glyoxal.
9. the water-base cement composition that does not contain polyvinyl alcohol as claimed in claim 8, the concentration of wherein said screening agent reaches 3 to 10 weight percents.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610005067XA CN100436561C (en) | 2006-01-17 | 2006-01-17 | Formula of aqueous glue without polyvinyl alcohol(PVA) |
| HK07111762A HK1106544A1 (en) | 2006-01-17 | 2007-10-31 | Polyvinyl alcohol (pva)-free hydrous glue composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610005067XA CN100436561C (en) | 2006-01-17 | 2006-01-17 | Formula of aqueous glue without polyvinyl alcohol(PVA) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101003710A CN101003710A (en) | 2007-07-25 |
| CN100436561C true CN100436561C (en) | 2008-11-26 |
Family
ID=38703096
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200610005067XA Active CN100436561C (en) | 2006-01-17 | 2006-01-17 | Formula of aqueous glue without polyvinyl alcohol(PVA) |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN100436561C (en) |
| HK (1) | HK1106544A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033259A (en) * | 2010-11-15 | 2011-04-27 | 深圳市三利谱光电科技股份有限公司 | Ultra-thin transmission type polarizer for liquid crystal display |
| CN102928910A (en) * | 2012-11-22 | 2013-02-13 | 上海康耐特光学股份有限公司 | Polarized light 3D (three dimensional) lens and production method therefor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54102331A (en) * | 1978-01-30 | 1979-08-11 | Res Inst For Prod Dev | Water-soluble adhesive |
-
2006
- 2006-01-17 CN CNB200610005067XA patent/CN100436561C/en active Active
-
2007
- 2007-10-31 HK HK07111762A patent/HK1106544A1/en unknown
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54102331A (en) * | 1978-01-30 | 1979-08-11 | Res Inst For Prod Dev | Water-soluble adhesive |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101003710A (en) | 2007-07-25 |
| HK1106544A1 (en) | 2008-03-14 |
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