CN104403245A - Polyvinyl alcohol polymer thin film with excellent dyeing property and manufacturing method thereof - Google Patents
Polyvinyl alcohol polymer thin film with excellent dyeing property and manufacturing method thereof Download PDFInfo
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- CN104403245A CN104403245A CN201410763324.0A CN201410763324A CN104403245A CN 104403245 A CN104403245 A CN 104403245A CN 201410763324 A CN201410763324 A CN 201410763324A CN 104403245 A CN104403245 A CN 104403245A
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Abstract
The invention discloses a polyvinyl alcohol polymer thin film with an excellent dyeing property and a manufacturing method thereof. When the thin film is infiltrated in distillated water at 30 DEG C for 30-300 seconds, the glycerin mass content in the thin film is decreased to 3% below, and in the width direction of the thin film, the glycerin mass content difference at points of every 5 cm area is less than 1%. The manufacturing method of the thin film comprises the following steps: preparing a film-making stock solution, mixing and stirring the film-making stock solution under a high pressure condition, forming an initial embryophoric membrane by the film-making stock solution, performing infrared heating and drying on the initial embryophoric membrane, and performing thermal treatment with hot-blast air. The manufacturing method of the polyvinyl alcohol polymer thin film disclosed by the invention can effectively solve the problems of uneven dyeing and color spots in preparation of the polarizing film.
Description
Technical field
The invention belongs to technical field of film preparation, be specifically related to a kind of polymer film of polyvinyl alcohol and the manufacture method thereof with excellent dyeing behavior.
Background technology
Polaroid is the important component part of liquid-crystal display (LCD), is mainly used in controlling the opticity through liquid crystal light.Polaroid is generally by polyvinyl alcohol based polymer (PVA) film uniaxial extension, the two sides of the polarization film of dyeing preparation further, pastes as the protective membranes such as cellulose triacetate (TAC) are made.
Along with the extension of LCD area, require the production of larger sized polaroid simultaneously.Relative to small-medium size polaroid, the defect such as color spot easily appears in big size polaroid in making processes, it is uneven to dye, stretching spot, therefore this just has higher requirement to the PVA film that large size optics is homogeneous.
In order to improve the problems such as PVA light polarizing film color spot, stretching spot, patents 200880103776.9,201280015847.6,01115587.6 etc. are proposed by PVA solution being extruded by die head, at roller surface filming, subsequently through some dryer roll drying and forming-films to improve the method for light polarizing film color spot.There will be a known the thickness spot in film TD direction be 12% and following (No. 323077, Japanese Unexamined Patent Publication), hot water in film TD direction cut off temperature spots and be less than 1.5 DEG C (No. 30163, Japanese Unexamined Patent Publications), be No. 30164,0.7-1.3(Japanese Unexamined Patent Publication at the ratio (SM, ST) of the tensile elongation (Sm) in film MD direction and the tensile elongation (ST) in TD direction) etc. make the method for the structure spot of polymer film of polyvinyl alcohol, anisotropy or thickness evenness.Patent 200880102610.5 proposes, by improving glycerol being uniformly distributed in PVA film, to improve the method for dyeing behavior.
But, even if by these methods, in polarizing film, still have defect, fully cannot meet that provide can to the requirement of light polarizing film of large screen being applied to liquid-crystal display.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of polymer film of polyvinyl alcohol and the manufacture method thereof with excellent dyeing behavior, effectively can solve the phenomenon such as dyeing inequality, color spot occurred in light polarizing film preparation.
For achieving the above object, the invention provides following technical scheme:
The invention discloses a kind of polymer film of polyvinyl alcohol with excellent dyeing behavior, this film is the film be made up of the masking stoste containing vinol series polymer and glycerol, after this film infiltrates 30-300s in the distilled water of 30 DEG C, glycerol mass content in film is down to less than 3%, preferably less than 1%, most preferably less than 0.5%, and on the width of film, the glycerol mass content difference of every 5cm region place point is less than 1%, is preferably less than 0.5%, is most preferably less than 0.2%.
The present invention studies discovery, and the polymer film of polyvinyl alcohol possessing These characteristics stretches in follow-up dyeing and there will not be the phenomenons such as inequality, color spot that dye fixing preparation in the process of light polarizing film.
In the present invention, the thickness of described film is preferably 50-80 μm.
The invention also discloses a kind of manufacture method with the polymer film of polyvinyl alcohol of excellent dyeing behavior, comprise the following steps:
1) the masking stoste of polymer film of polyvinyl alcohol is prepared;
2) by masking stoste mixing and stirring under 100-150 DEG C of condition of high voltage;
3) the masking stoste of mixing and stirring is spued on dryer roll with membranaceous, form initial embryophoric membrane;
4) from roller sur-face peeling when initial embryophoric membrane water ratio on dryer roll arrives 10%-25%, dried by the Infrared Heating of 50-120 DEG C, obtained film;
5) film after drying, by the hot blast thermal treatment of 90-150 DEG C, obtains the polymer film of polyvinyl alcohol with excellent dyeing behavior by damping.
By the control of above-mentioned preparation method, particularly the Infrared Heating of masking stoste mix and blend, 50-120 DEG C under 100-150 DEG C of condition of high voltage is dried and the hot blast thermal treatment of 90-150 DEG C, can obtain the polymer film of polyvinyl alcohol possessing These characteristics.
Above-mentioned steps 1) in, masking stoste can be selected by vinol series polymer, softening agent, tensio-active agent and solvent composition, vinol series polymer accounts for the 10%-60% of masking stoste total mass, the content of softening agent is the 7%-15% of vinol series polymer quality, the content of tensio-active agent is the 0.01%-3% of vinol series polymer quality, and surplus is solvent.The polymerization degree of vinol series polymer is preferably 1000-5000, alcoholysis degree is preferably more than 99%, solvent preferably water, softening agent is the mixture of glycerol or glycerol and other polyvalent alcohol, and tensio-active agent preferably uses anionic or nonionic surface active agent.
Above-mentioned steps 2) in, the masking stoste method that mix and blend can be selected under 100-150 DEG C of condition of high voltage has: material initially passes into the purification high-pressure steam of 100-150 DEG C, the stirring completing material with mix, last regulator solution concentration; Be warming up to mixing of materials and dissolving within the scope of 100-150 DEG C gradually by autoclave, last regulator solution concentration.Solution dissolved state and glycerol content change are evaluated in sampling per hour, until in continuous two batch sample the error of glycerol actual content and glycerol theoretical content within 2% and solution dissolve completely, just can think mixing and stirring.
Above-mentioned steps 3) in, the film that preferred film forming thickness is even, planeness is good, such as by air pressure extrude masking stoste by the method for die slit film forming, by Screw Extrusion masking stoste by the method for slit film forming, melt extrude the method etc. of masking stoste by slit film forming by screw rod, die head preferably has the die types of rack-style runner.
Above-mentioned steps 5) in, adopt air-floatation type oven to film thermal process, heat treatment time is 1-180s.
The invention also discloses a kind of polarizing film, this polarizing film is made by described polymer film of polyvinyl alcohol and obtains.
Beneficial effect of the present invention is:
The present invention studies discovery, after polymer film of polyvinyl alcohol infiltrates 30-300s in the distilled water of 30 DEG C, if the remnants of glycerol and distribution meet certain requirements, so this film stretches in follow-up dyeing and there will not be the phenomenons such as inequality, color spot that dye fixing preparation in the process of light polarizing film.And the present invention is by the control of preparation method, particularly the Infrared Heating of masking stoste mix and blend, 50-120 DEG C under 100-150 DEG C of condition of high voltage is dried and the hot blast thermal treatment of 90-150 DEG C, can obtain the polymer film of polyvinyl alcohol possessing These characteristics.
Embodiment
In order to make object of the present invention, technical scheme and beneficial effect clearly, will be described in detail the preferred embodiments of the present invention below.
In the present invention, the measuring method of glycerol content is as follows:
Testing sample is dropped into DMSO-d
6make concentration become about 5 quality %, dissolve with 2h after being warming up to 90 DEG C, use 500MHz,
1h-NMR and with PD(pulse delay time) 20s, measure temperature 30 DEG C, the condition of cumulative number 256 times measures, and measured the content of softening agent in each sample by obtained NMR spectrum.Such as, the occasion of glycerol is used in softening agent, according to the NMR spectrum that above-mentioned test obtains, can detect at the crest (integrated intensity of crest is Sp) near 1.5ppm of crest methylene radical 2 hydrogen partials of (integrated intensity of crest is Sg), PVA near 3.3ppm of methylene radical 2 hydrogen partials of glycerol respectively, use its integrated intensity and the glycerol amount R(quality % in PVA system film can be calculated with following formula): R=(92/44) × (Sg/Sp) × 100.
embodiment 1
The manufacture of polymer film of polyvinyl alcohol is carried out in accordance with the following steps:
1) in mass ratio, polyvinyl alcohol: glycerol: sodium lauryl sulphate: water=10:0.7:0.001:90, preparation masking stoste, wherein the polymerization degree of polyvinyl alcohol is 5000, and saponification deg is 99.7%.
2) masking stoste is added autoclave, mixing speed 300r/min, under 100 DEG C of conditions, material is mixed.Solution dissolved state and glycerol content change are evaluated in sampling per hour, and stir after reaching 4h, in continuous two batch sample, the error of the theoretical content of glycerol actual content and glycerol is 1.8%, and solution dissolves completely.
3) the masking stoste of mixing and stirring is extruded by twin screw extruder, be extruded on dryer roll by hanger-style die, form initial embryophoric membrane.
4) initial embryophoric membrane is from roller sur-face peeling when on dryer roll, water ratio is 20%, is dried, obtained film by the Infrared Heating of 70 DEG C.
5) film after drying adopts the hot blast thermal treatment of air-floatation type oven 130 DEG C, and heat treatment time is 60s, obtains polymer film of polyvinyl alcohol by damping.The thickness of film is 50 μm.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 160s, its glycerol mass content is down to 0.4%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all less than 0.2%.Film through dyeing stretch fixing after, without any color spot, the bad phenomenon such as painted.
embodiment 2
The manufacture of polymer film of polyvinyl alcohol is carried out in accordance with the following steps:
1) in mass ratio, polyvinyl alcohol: glycerol: sodium lauryl sulphate: water=60:9:1.8:29, preparation masking stoste, wherein the polymerization degree of polyvinyl alcohol is 5000, and saponification deg is 99.7%.
2) masking stoste is added autoclave, mixing speed 300r/min, under 150 DEG C of conditions, material is mixed.Solution dissolved state and glycerol content change are evaluated in sampling per hour, and stir after reaching 6h, in continuous two batch sample, the error of the theoretical content of glycerol actual content and glycerol is 1.1%, and solution dissolves completely.
3) the masking stoste of mixing and stirring is extruded by twin screw extruder, be extruded on dryer roll by hanger-style die, form initial embryophoric membrane.
4) initial embryophoric membrane is from roller sur-face peeling when on dryer roll, water ratio is 20%, is dried, obtained film by the Infrared Heating of 70 DEG C.
5) film after drying adopts the hot blast thermal treatment of air-floatation type oven 130 DEG C, and heat treatment time is 60s, obtains polymer film of polyvinyl alcohol by damping.The thickness of film is 80 μm.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 30s, its glycerol mass content is down to 2.8%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all less than 1%.Film through dyeing stretch fixing after, without any color spot, the bad phenomenon such as painted.
embodiment 3
The manufacture of polymer film of polyvinyl alcohol is carried out in accordance with the following steps:
1) in mass ratio, polyvinyl alcohol: glycerol: sodium lauryl sulphate: water=30:3:0.045:67, preparation masking stoste, wherein the polymerization degree of polyvinyl alcohol is 5000, and saponification deg is 99.7%.
2) masking stoste is added autoclave, mixing speed 300r/min, under 130 DEG C of conditions, material is mixed.Solution dissolved state and glycerol content change are evaluated in sampling per hour, and stir after reaching 6h, in continuous two batch sample, the error of the theoretical content of glycerol actual content and glycerol is 0.9%, and solution dissolves completely.
3) the masking stoste of mixing and stirring is extruded by twin screw extruder, be extruded on dryer roll by hanger-style die, form initial embryophoric membrane.
4) initial embryophoric membrane is from roller sur-face peeling when on dryer roll, water ratio is 25%, is dried, obtained film by the Infrared Heating of 120 DEG C.
5) film after drying adopts the hot blast thermal treatment of air-floatation type oven 150 DEG C, and heat treatment time is 60s, obtains polymer film of polyvinyl alcohol by damping.The thickness of film is 75 μm.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 300s, its glycerol mass content is down to 0.3%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all less than 0.2%.Film through dyeing stretch fixing after, without any color spot, the bad phenomenon such as painted.
embodiment 4
The manufacture of polymer film of polyvinyl alcohol is carried out in accordance with the following steps:
1) in mass ratio, polyvinyl alcohol: glycerol: sodium lauryl sulphate: water=30:3:0.045:67, preparation masking stoste, wherein the polymerization degree of polyvinyl alcohol is 5000, and saponification deg is 99.7%.
2) masking stoste is added autoclave, mixing speed 300r/min, under 130 DEG C of conditions, material is mixed.Solution dissolved state and glycerol content change are evaluated in sampling per hour, and stir after reaching 6h, in continuous two batch sample, the error of the theoretical content of glycerol actual content and glycerol is 1.0%, and solution dissolves completely.
3) the masking stoste of mixing and stirring is extruded by twin screw extruder, be extruded on dryer roll by hanger-style die, form initial embryophoric membrane.
4) initial embryophoric membrane is from roller sur-face peeling when on dryer roll, water ratio is 10%, is dried, obtained film by the Infrared Heating of 50 DEG C.
5) film after drying adopts the hot blast thermal treatment of air-floatation type oven 90 DEG C, and heat treatment time is 180s, obtains polymer film of polyvinyl alcohol by damping.The thickness of film is 75 μm.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 160s, its glycerol mass content is down to 0.3%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all less than 0.2%.Film through dyeing stretch fixing after, without any color spot, the bad phenomenon such as painted.
embodiment 5
The manufacture of polymer film of polyvinyl alcohol is carried out in accordance with the following steps:
1) in mass ratio, polyvinyl alcohol: glycerol: sodium lauryl sulphate: water=30:3:0.045:67, preparation masking stoste, wherein the polymerization degree of polyvinyl alcohol is 5000, and saponification deg is 99.7%.
2) masking stoste is added autoclave, mixing speed 300r/min, under 130 DEG C of conditions, material is mixed.Solution dissolved state and glycerol content change are evaluated in sampling per hour, and stir after reaching 6h, in continuous two batch sample, the error of the theoretical content of glycerol actual content and glycerol is 0.8%, and solution dissolves completely.
3) the masking stoste of mixing and stirring is extruded by twin screw extruder, be extruded on dryer roll by hanger-style die, form initial embryophoric membrane.
4) initial embryophoric membrane is from roller sur-face peeling when on dryer roll, water ratio is 20%, is dried, obtained film by the Infrared Heating of 70 DEG C.
5) film after drying adopts the hot blast thermal treatment of air-floatation type oven 150 DEG C, and heat treatment time is 60s, obtains polymer film of polyvinyl alcohol by damping.The thickness of film is 75 μm.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 160s, its glycerol mass content is down to 0.4%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all less than 0.2%.Film through dyeing stretch fixing after, without any color spot, the bad phenomenon such as painted.
comparative example 1
Relative to embodiment 5, difference is that masking stoste is not through step 2) mix and blend of autoclave, but directly enter step 3) masking stoste is extruded by twin screw extruder, other are consistent.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 160s, its glycerol mass content is down to 3.6%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all greater than 1.6%.Film through dyeing stretch fixing after, there is color spot, the bad phenomenon such as painted.
comparative example 2
Relative to embodiment 5, difference is in step 4), and initial embryophoric membrane is from roller sur-face peeling when on dryer roll, water ratio is 20%, and dry obtained film by the Hot-blast Heatings of 70 DEG C, other are consistent.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 160s, its glycerol mass content is down to 1.8%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all greater than 1.1%.Film through dyeing stretch fixing after, there is a small amount of color spot, the bad phenomenon such as painted.
comparative example 3
Relative to embodiment 5, difference is in step 5), and the film after oven dry adopts the hot-rolling thermal treatment of 150 DEG C, and heat treatment time is 1s, and other are consistent.
This polymer film of polyvinyl alcohol infiltrates in the distilled water of 30 DEG C, and after infiltrating time 160s, its glycerol mass content is down to 2.2%, and the film width after infiltrating, the glycerol mass content difference of every 5cm region place point is all greater than 1.5%.Film through dyeing stretch fixing after, there is a small amount of color spot, the bad phenomenon such as painted.
The test result of above-described embodiment and comparative example is gathered as follows:
What finally illustrate is, above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by above preferred embodiment to invention has been detailed description, but those skilled in the art are to be understood that, various change can be made to it in the form and details, and not depart from claims of the present invention limited range.
Claims (9)
1. one kind has the polymer film of polyvinyl alcohol of excellent dyeing behavior, this film is the film be made up of the masking stoste containing vinol series polymer and glycerol, it is characterized in that: after this film infiltrates 30-300s in the distilled water of 30 DEG C, glycerol mass content in film is down to less than 3%, and on the width of film, the glycerol mass content difference of every 5cm region place point is less than 1%.
2. polymer film of polyvinyl alcohol according to claim 1, it is characterized in that: after this film infiltrates 30-300s in the distilled water of 30 DEG C, glycerol mass content in film is down to less than 1%, and on the width of film, the glycerol mass content difference of every 5cm region place point is less than 0.5%.
3. polymer film of polyvinyl alcohol according to claim 2, it is characterized in that: after this film infiltrates 30-300s in the distilled water of 30 DEG C, glycerol mass content in film is down to less than 0.5%, and on the width of film, the glycerol mass content difference of every 5cm region place point is less than 0.2%.
4. the polymer film of polyvinyl alcohol according to claim 1,2 or 3, is characterized in that: the thickness of described film is 50-80 μm.
5. there is a manufacture method for the polymer film of polyvinyl alcohol of excellent dyeing behavior, it is characterized in that: comprise the following steps:
1) the masking stoste of polymer film of polyvinyl alcohol is prepared;
2) by masking stoste mixing and stirring under 100-150 DEG C of condition of high voltage;
3) the masking stoste of mixing and stirring is spued on dryer roll with membranaceous, form initial embryophoric membrane;
4) from roller sur-face peeling when initial embryophoric membrane water ratio on dryer roll arrives 10%-25%, dried by the Infrared Heating of 50-120 DEG C, obtained film;
5) film after drying, by the hot blast thermal treatment of 90-150 DEG C, obtains the polymer film of polyvinyl alcohol with excellent dyeing behavior by damping.
6. the manufacture method of polymer film of polyvinyl alcohol according to claim 5, it is characterized in that: in described step 1), masking stoste is by vinol series polymer, softening agent, tensio-active agent and solvent composition, vinol series polymer accounts for the 10%-60% of masking stoste total mass, the content of softening agent is the 7%-15% of vinol series polymer quality, the content of tensio-active agent is the 0.01%-3% of vinol series polymer quality, and surplus is solvent; Described softening agent at least comprises glycerol.
7. the manufacture method of polymer film of polyvinyl alcohol according to claim 5, it is characterized in that: described step 2) in, solution dissolved state and glycerol content change are evaluated in sampling per hour, until in continuous two batch sample the error of glycerol actual content and glycerol theoretical content within 2% and solution dissolve completely.
8. the manufacture method of polymer film of polyvinyl alcohol according to claim 5, is characterized in that: in described step 5), and adopt air-floatation type oven to film thermal process, heat treatment time is 1-180s.
9. a polarizing film, is characterized in that: made by the polymer film of polyvinyl alcohol described in Claims 1-4 any one and obtain.
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| CN107286543A (en) * | 2017-05-27 | 2017-10-24 | 中国石油化工集团公司 | A kind of polyvinyl alcohol optical film and preparation method thereof |
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