CN108274787A - A kind of active inclined plate coagulation forming biaxially oriented film preparation method - Google Patents
A kind of active inclined plate coagulation forming biaxially oriented film preparation method Download PDFInfo
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- CN108274787A CN108274787A CN201810091349.9A CN201810091349A CN108274787A CN 108274787 A CN108274787 A CN 108274787A CN 201810091349 A CN201810091349 A CN 201810091349A CN 108274787 A CN108274787 A CN 108274787A
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- Prior art keywords
- inclined plate
- active
- biaxially oriented
- coagulation forming
- oriented film
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/24—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
- B29C41/28—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length by depositing flowable material on an endless belt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/34—Component parts, details or accessories; Auxiliary operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/34—Component parts, details or accessories; Auxiliary operations
- B29C41/42—Removing articles from moulds, cores or other substrates
- B29C41/44—Articles of indefinite length
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
- B29C55/143—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively firstly parallel to the direction of feed and then transversely thereto
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of active inclined plate coagulation forming biaxially oriented film preparation methods, include the following steps：Lip of the high viscosity high-molecular resin solution of preparation under a certain pressure through T-type or rack-style casting head, which is ejected into coagulating bath, forms partially solidified gel film, it is directed at the top of inclined plate through active guide roller, it is gradually molded completely with the flow direction of solidification liquid, form gel film of coming into being, then coagulating tank is exported through deflector roll, multi-stage washing device is directed to be washed, enter two-way stretch device after washes clean to stretch, drying unit drying, trimming, metering are entered back into later, are finally wound as finished films.The present invention can high efficiency production surface be smooth, performance is uniform, high performance thin film product in homogeneous thickness, can be also used for the production of ultrathin film of the thickness less than 5 microns.
Description
Technical field
The present invention relates to a kind of method for manufacturing thin film, and in particular to a kind of active inclined plate coagulation forming biaxially oriented film
Preparation method belongs to macromolecule resin thin film forming techniques field.
Background technology
The film that wet tape casting technique is prepared compared with melting extrusion moulding process have better planarization, respectively to
The same sex, lower impurity content, and the film preparation of thermosetting resin is can be used for, receive very extensive research and pass
Note.Wet tape casting technique can be divided into solvent volatilization molding and coagulation forming by molding mode, the former is at high temperature by hygrometric state
Film product is formed after solvent volatilization in film, with a kind of Kapton (Kapton of Chinese invention patent
201410129169.7；A kind of preparation process of Kapton of Chinese invention patent, 201410129600.8) and three acetic acid
Cellulose ester film (a kind of preparation method of cellulose triacetate thin film of Chinese invention patent, 201510369394.2；It is a kind of
The preparation process of cellulose triacetate thin film, 201611229684.8) it is representative, the latter is thin by hygrometric state under coagulation bath condition
Solvent in film cements out after solidification forms primary film and washed drying and obtains film product, using glassine paper as representative
(a kind of acid bath technique for glassine paper production of Chinese invention patent, 201510787511.7).
Wet tape casting technique can be divided into roll-type support, belt support and inclined plate by the method for supporting of hygrometric state film
Formula supports.For ramp type coagulation forming system because simple in structure, equipment control accuracy requirement is relatively low, solidifies bath concentration adjustable extent
Greatly, setting time span is larger, and speed of production is higher, is mainly used in the production technology of wet glass paper.Ramp type solidifies
It is that macromolecule resin material is ejected into coagulation forming in coagulating bath under certain pressure effect by die head to be molded usual technique, is formed
Partially solidified gel film, then be directed on inclined plate the type that is completely solidified into through passive deflector roll and form nascent gel film.Inclined plate pair
Partially solidified gel film is played a supporting role, and partially solidified gel film is solidifying because being flowed by upper and lower surface on inclined plate
Admittedly the collective effect bathed, film internal solvent exchanges fully with solidification liquid, and coagulation efficacy is very high, and is not in film two
Face performance or the inconsistent situation of appearance.But this method requires the setting rate of film very fast in actual application,
Otherwise partially solidified gel film will appear that coagulation grade is too low low without intensity or intensity, and leading for can not stablizing is oblique
On plate, and there is horizontal and vertical striped, seriously receives the problems such as side, even film breakage.Glassine paper relates to during coagulation forming
And acid-base reaction is arrived, therefore setting rate and coagulation efficacy are very high, are suitble to produce using traditional inclined plate method of forming.And for
Other Polymer Systems of the double diffusion coagulation forming of solidification are realized by using concentration difference, such as poly- paraphenylene terephthalamide is to benzene two
Amine, polyparaphenylene's Benzo-dioxazole resin can not realize stabilization because setting rate is slower by existing inclined plate moulding process
Film production.
The present invention is solved by applying deflector roll transmission to inclined plate coagulation forming front end because of the less efficient appearance of hardening of resin
Horizontal and vertical striped seriously receives the problems such as side, even film breakage, enables to be molded for the resin film of low coagulation efficacy.
By this modified technique, can to can not use melting extrusion, it is conventional be cast molding high-performance special macromolecule resin into
Row film forming expands the functional form and application field of this kind of polymer-function material.
Invention content
It is an object of the invention to overcome traditional inclined plate coagulation forming because of the transverse direction of the less efficient appearance of hardening of resin and indulge
To striped, seriously receive side, even film breakage the problems such as, a kind of preparation method of active formula inclined plate coagulation forming film is provided,
Efficient film forming can be carried out to the speciality polymer resin that can not melt, can not be dissolved in organic solvent, institute is molding
Film surface is smooth, performance is uniform, thickness is uniform.Any it can be dissolved in a kind of organic solvent the present invention may also apply to other
Or the preparation of the macromolecule resin film of inorganic solvent.
The invention is realized in this way：
A kind of active inclined plate coagulation forming biaxially oriented film preparation method, includes the following steps：The high viscosity of preparation
Lip of the high-molecular resin solution under a certain pressure through T-type or rack-style casting head is ejected into forming portion in coagulating bath and segregates
Solid gel film, be directed at the top of inclined plate through active guide roller, the flow direction solidified with liquid gradually be molded to be formed completely and come into being
Then gel film exports coagulating tank through deflector roll, is directed to multi-stage washing device and is washed, enter after washes clean two-way
Stretching device stretches, and enters back into drying unit drying, trimming, metering later, is finally wound as finished films.
The range of viscosities of the high-molecular resin solution is 10000~3000000mpas；
The casting head internal pressure is 0.1~3MPa, and die lip lip width is 0.03~0.5mm, die orifice lip
It extend into 1~30cm under coagulation bath；
Preferably, casting head internal pressure is 0.5~1MPa, and die lip lip width is 0.1~0.2mm, die orifice lip
It extend into 3~8cm under coagulation bath；
The active guide roller quantity is 1~8, and the linear velocity ratio of deflector roll and deflector roll is 0.1~10, deflector roll diameter range
For 3~30cm, deflector roll 1~20cm of spacing contains screw thread nip rolls or curved roll 1~3 in guide roller set；
Preferably, active guide roller quantity is 3~5, and the linear velocity ratio of deflector roll and deflector roll is 1~1.2, deflector roll diameter range
For 5~10cm, deflector roll 2~8cm of spacing contains screw thread nip rolls or curved roll 1~3 in guide roller set；
It is particularly preferred that active guide roller quantity is 4, the linear velocity ratio of deflector roll and deflector roll is 1.1, deflector roll diameter
For 7cm, deflector roll spacing 3cm contains screw thread nip rolls 1 in guide roller set；
The screw thread nip rolls puts sequence：Drive roll 1, drive roll 2, drive roll 3, main thread nip rolls 4, wherein
Three rollers next can be replaced arbitrarily；
Preferably, screw thread nip rolls, which is put, is sequentially：Drive roll 1, drive roll 2, drive roll 3, main thread nip rolls 4；
The active guide roller 1 is 3~30cm with a distance from die lip lip；
The inclined plate surfacing is smooth, and 5~45 ° of angle of inclination can freely adjust, 1~3m of length；
Preferably, inclined plate surfacing, finish reach minute surface grade, 15~25 ° of angle of inclination, 1.5~2.5m of length；
The multi-stage washing device is level Four or more, including washing, alkali cleaning, washing, washing.
Double drawing stretching devices can be step drawing, such as first longitudinal stretching cross directional stretch, or first laterally drawing again
Longitudinal stretching again is stretched, can also be that synchronous bidirectional stretches；
Preferably, double drawing stretching devices are step drawing, further preferably first longitudinal cross directional stretch again；
The solvent of the high viscosity high-molecular resin solution be acid solution, lye and other have the molten of superpower solubility property
Agent.
Preferably, the film index parameter prepared by the active inclined plate coagulation forming biaxial tension is as follows：Finished product is thin
Film width：200~1500mm, film thickness：0.002~0.1mm, film gauge variation：≤ ± 10%, speed：3~100m/
min；
The positive effect of the present invention is that：The present invention can solve traditional inclined plate coagulation forming because of hardening of resin efficiency
The horizontal and vertical striped of relatively low appearance seriously receives the problems such as side, even film breakage, may be implemented not dissolving in by the technology
The film forming of the thermosetting polymer resin of organic solvent.This method can high efficiency production surface be smooth, performance is equal
One, high performance thin film product in homogeneous thickness can be also used for the production of ultrathin film (thickness is less than 5 microns).The present invention
Linear velocity can be independently adjusted in the active roller of design, is conducive to local directed complete set stretching ratio, realizes final film product
Property regulation；The nip rolls that the present invention designs can effectively prevent the receipts side of the molding gel film in part and out-of-flatness to ask
Topic contributes to the raising of product quality and reduces the loss of follow-up trimming.Two-way stretch device can carry out according to actual needs
Longitudinal or laterally different degree of stretch facilitates the final longitudinally, laterally mechanical performance for adjusting film product.
Description of the drawings
Fig. 1 is the molding structure schematic diagram that the present invention uses, and dotted line is surface of coagulation bath.
Specific implementation mode
It is below in conjunction with the accompanying drawings and common high temperature resistant thermosetting resin poly(p-phenylene terephthalamide) (PPTA) resin, poly-
Present pre-ferred embodiments are provided to the membrane-film preparation process of penylene Benzo-dioxazole resin (PBO), with the present invention will be described in detail
Technical solution.
Embodiment one
Coagulation forming process
Poly(p-phenylene terephthalamide) is dissolved at 90 DEG C in 100% sulfuric acid solution, is made a concentration of 13%
Resin grout liquid, and enter the rack-style casting head 7 that width is 420mm after abundant deaeration, filtering, slurries are ejected into through lip
In dilute sulfuric acid coagulating bath, the active guide roller 1,2,3,4 through 4 a diameter of 70mm is directed at 8 top of inclined plate, is gradually solidified on inclined plate
After obtain complete molding nascent gel film, then export coagulating tank through deflector roll 5 and screw thread nip rolls 6.Wherein die head sprays
Go out pressure and be set as 0.7MPa, die orifice aperture as 0.15mm, lip extend into 5cm under coagulation bath, and active guide roller 1 is from die lip lip
Distance be 5cm, the linear velocity ratios of 4 active guide rollers is 1:1.1:1.1:1.1, top drive roll is screw thread nip rolls 6, inclined plate
Length 1.8m, 20 ° of angle of inclination.
Cleaning process
The nascent gel film being prepared in previous step is imported into rinse bath to clean to obtain clean hygrometric state film,
Rinse bath be set as 5 grades cleaning, i.e. washing, alkali cleaning, washing, washing, washing, cleaning temperature be respectively set to 40 DEG C, 50 DEG C, 40
DEG C, 40 DEG C, 40 DEG C, film residence time in every level-one rinse bath is set as 30s, and afterbody washing uses deionized water.
Biaxial tension and baking operation
Clean hygrometric state film in previous step is imported into longitudinal tensile fixture, stretches 3 times, is then introduced into cross directional stretch dress
2 times of acquisition higher orientation hygrometric state films of intensity of stretching are set, the drying of baking oven case is subsequently introduced, drying warm area is 4, temperature difference
It is set as 90 DEG C, 140 DEG C, 250 DEG C and 300 DEG C, each warm area residence time is 25s, and obtained dry film is received through trimming
High performance film product is obtained after volume.Obtaining film performance parameter is：Finished films width：350mm according to the breadth of front,
Thickness：0.015 ± 0.003mm, tensile strength：275MPa, elongation 13%, speed：10m/min；
Embodiment two
Polyparaphenylene's Benzo-dioxazole resin (PBO) is dissolved at 90 DEG C in 100% sulfuric acid solution, is made a concentration of
8% resin grout liquid, and enter the rack-style casting head that width is 420mm after abundant deaeration, filtering, slurries are sprayed through lip
Going out into dilute sulfuric acid coagulating bath, the active guide roller through 5 a diameter of 70mm is directed at the top of inclined plate, after gradually being solidified on inclined plate
To complete molding nascent gel film, then coagulating tank is exported through deflector roll.Wherein die head ejection pressure is set as 0.5MPa, mould
Mouth aperture is 0.12mm, and lip mouth extend into 5cm under coagulation bath, and active guide roller is 4cm, 4 masters with a distance from die lip lip
The linear velocity ratio of dynamic deflector roll is 1:1.2:1.2:1.1, top drive roll is screw thread nip rolls, inclined plate length 1.8m, angle of inclination
20°.Cleaning process, biaxial tension and baking operation are identical as embodiment two, embodiment three respectively, the film performance finally obtained
Parameter is：Finished films width：350mm, thickness：0.01 ± 0.003mm, tensile strength：290MPa, elongation 11%, speed：
10m/min；
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will be fallen in principle disclosed in the present application
Within scope and spirit.
Claims (8)
1. a kind of active inclined plate coagulation forming biaxially oriented film preparation method, it is characterised in that include the following steps：Height is viscous
Lip of the degree high-molecular resin solution under a certain pressure through T-type or rack-style casting head, which is ejected into coagulating bath, forms part
The gel film of solidification is directed at the top of inclined plate through active guide roller, is gradually molded completely with the flow direction of solidification liquid, is formed just
Raw gel film, then exports coagulating tank through deflector roll, is directed to multi-stage washing device and is washed, and enters after washes clean double
It is stretched to stretching device, enters back into drying unit drying, trimming, metering later, be finally wound as the preparation method of finished films.
2. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 1, it is characterised in that：Die head
Internal pressure is 0.1~3MPa, and die lip lip width is 0.03~0.5mm, die lip lip extend into 1 under coagulation bath~
30cm。
3. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 1 or claim 2, it is characterised in that：
Active guide roller quantity is 1~8, and the linear velocity ratio of deflector roll and deflector roll is 0.1~10, and deflector roll diameter range is 3~30cm, deflector roll
1~20cm of spacing contains screw thread nip rolls or curved roll 1~3 in guide roller set, and active guide roller is with a distance from die lip lip
For 3~30cm.
4. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 3, it is characterised in that：It is each
The rotating speed of root active guide roller can be adjusted independently；Spacing between each active guide roller can be adjusted independently.
5. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 1, it is characterised in that：Inclined plate
Surfacing, finish reach minute surface grade, 5~45 ° of angle of inclination, 1~3m of length.
6. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 1, it is characterised in that：It is multistage
Wash mill is level Four or more, including washing, alkali cleaning, washing, washing.
7. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 1, it is characterised in that：Double drawings
Stretching is step drawing or synchronous bidirectional stretching, and the step drawing includes first longitudinal stretching cross directional stretch or first laterally drawing again
Stretch longitudinal stretching again.
8. active inclined plate coagulation forming biaxially oriented film preparation method according to claim 1, it is characterised in that：
The solvent of the high viscosity high-molecular resin solution be acid solution, lye and other have the solvent of superpower solubility property.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810091349.9A CN108274787B (en) | 2018-01-30 | 2018-01-30 | Preparation method of active inclined plate solidification forming biaxial tension film |
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| CN201810091349.9A CN108274787B (en) | 2018-01-30 | 2018-01-30 | Preparation method of active inclined plate solidification forming biaxial tension film |
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| CN108274787A true CN108274787A (en) | 2018-07-13 |
| CN108274787B CN108274787B (en) | 2020-09-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110587885A (en) * | 2019-08-29 | 2019-12-20 | 陈晓东 | Multistage swash plate forming device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1316026A (en) * | 1998-07-28 | 2001-10-03 | 连津格股份公司 | Method and device for producing cellulosic moulded parts |
| CN103978707A (en) * | 2014-04-17 | 2014-08-13 | 常州纺织服装职业技术学院 | Washing technology of 1,3,4-oxadiazole acid-containing wet casting film |
| CN104610557A (en) * | 2013-11-01 | 2015-05-13 | 中国科学院化学研究所 | Regenerated cellulose membrane, functional membrane, and preparation method of regenerated cellulose membrane and functional membrane |
-
2018
- 2018-01-30 CN CN201810091349.9A patent/CN108274787B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1316026A (en) * | 1998-07-28 | 2001-10-03 | 连津格股份公司 | Method and device for producing cellulosic moulded parts |
| CN104610557A (en) * | 2013-11-01 | 2015-05-13 | 中国科学院化学研究所 | Regenerated cellulose membrane, functional membrane, and preparation method of regenerated cellulose membrane and functional membrane |
| CN103978707A (en) * | 2014-04-17 | 2014-08-13 | 常州纺织服装职业技术学院 | Washing technology of 1,3,4-oxadiazole acid-containing wet casting film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110587885A (en) * | 2019-08-29 | 2019-12-20 | 陈晓东 | Multistage swash plate forming device |
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