CN106626188B - A kind of preparation process of cellulose triacetate thin film - Google Patents
A kind of preparation process of cellulose triacetate thin film Download PDFInfo
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- CN106626188B CN106626188B CN201611229684.8A CN201611229684A CN106626188B CN 106626188 B CN106626188 B CN 106626188B CN 201611229684 A CN201611229684 A CN 201611229684A CN 106626188 B CN106626188 B CN 106626188B
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- cellulose triacetate
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/10—Esters of organic acids, i.e. acylates
- C08L1/12—Cellulose acetate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/10—Esters of organic acids
- C08J2401/12—Cellulose acetate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
A kind of preparation process of cellulose triacetate thin film, the following steps are included: cellulose triacetate dissolves respectively with cellulose triacetate thin film fragment, dissolution filter is remixed, is transported to curtain coating mouth via three screw pump, by curtain coating mouth exclusion to curtain coating supporter, homogeneous transparent casting films are formed on supporter, it after casting films have supportive, is removed, forced air drying, winding, obtains cellulose triacetate thin film.Cellulose triacetate thin film fragment celloidin and triacetate fiber ester celloidin can be made uniformly to mix, gel point present in mixing celloidin can be efficiently reduced, reduce the spot defect in final film-forming products, the mechanical property of film can be improved significantly.
Description
Technical field
The present invention relates to a kind of preparation process of film, in particular to it is a kind of with cellulose triacetate thin film fragment and
Mixed solvent prepares the preparation process of cellulose triacetate thin film.
Background technique
In recent years in constantly universal each display device of liquid crystal display, cellulose triacetate thin film is due to excellent
Different optics, physical characteristic, are widely used in the support and protective film of polaroid.
Cellulose triacetate thin film preparation process generallys use solution film-forming method, and concrete technology is by Triafol T
Ester is dissolved in mixed solvent formation polymer solution (hereinafter referred to as celloidin) and is expelled to celloidin using casting mold through filtering
It is cast on supporter, after the casting films on supporter have supportive, casting films is removed from curtain coating supporter, form profit
Wet film is further dried wetting film, forms a film, winding, to obtain uniform film thickness, three acetic acid of optics isotropic are fine
Tie up cellulose ester film.
In solution film-forming method, cellulose triacetate thin film generates the disadvantages such as relaxation, fold in order to prevent, keeps three vinegar
The optical characteristics of acid cellulose ester film is in claimed range, after removing from the steel band continuously run, it will usually use folder
Both ends in tool clamping cellulose triacetate thin film width direction, (hereinafter referred to as piece side) carry out the stretching in the width direction
Processing.In the piece side for implementing the film of stretch processing, the trace of fixture clamping can be remained, so being not used as finished film.Often
Piece side is cut off from the film of stretched processing, and the part other than piece side is wound as finished product and is packed.
If the discarded piece side cut off from cellulose triacetate thin film, it will lead to that the production cost increases and environmental pollution
The problems such as.Accordingly, it is common practice that often piece side cuts into pieces using pulverizer in industrial production, make it as raw material,
It is dissolved in the mixed solvent, retrieves celloidin, is recycled with this.
Existing cellulose triacetate thin film production technology is as follows:
1 cellulose triacetate celloidin preparation process
The preparation process of existing cellulose triacetate cotton glue mainly includes celloidin mixing liquid preparing process, celloidin mixing
Liquid filtering and constant temperature stand three processes of defoaming.
(1) celloidin mixing liquid preparing process
Mixed solvent is added to reaction kettle, auxiliary agent is added, reaction kettle stirring and jacket water (J.W.) is opened, controls steady revolving speed.
Then be added to after mixing cellulose triacetate and cellulose triacetate thin film fragment according to formula rate 3:2 containing
In the reaction kettle of mixed solvent and auxiliary agent.The dissolution process such as speed of agitator, collet water temperature are adjusted, it is molten to carry out cellulose triacetate
Solution, dissolution time 6h prepare the cellulose triacetate celloidin mixed liquor of homogeneous transparent.
(2) celloidin mixed liquor filters
To remove the mechanical admixture and insoluble matter in celloidin mixed liquor, need that celloidin mixed liquor is filtered for multiple times.It is molten
It solves complete celloidin mixed liquor to be discharged from reaction kettle with gear pump, be filtered through coarse filter, it may in mixed solution to remove
There are biggish gel piece and other mechanical admixtures, into intermediate fluid reservoir.It is pressurizeed by gear pump, is carried out into plate and frame filter press
Multiple fine filtering, filtering accuracy are controlled at 5-10 μm, and it is spare that filtrate enters hold-up vessel.
(3) constant temperature stands defoaming
Celloidin mixed liquor after fine filtering carries out constant temperature in the thermostat for having jacket water (J.W.) and stands elimination bubble.Through constant temperature
It stands the celloidin mixed liquor after eliminating bubble and enters curtain coating process.
2 cellulose triacetate thin film casting molding processes
Celloidin mixed liquor prepared by process 1 enters three screw pump, filter, static mixer, bend pipe copper mesh, defeated through pipeline
It is sent to curtain coating mouth.Through in curtain coating mouth exclusion to the casting support continuously run, drying is removed, stretching and drawing, and drying is wound into
Axis.
But in the prior art, there are many defects and deficiencies.Mainly include the following aspects: (1) three acetic acid are fine
It is different in the mixed solvent solubility parameter to tie up cellulose ester film fragment and cellulose triacetate, solution rate is inconsistent, together
When dissolution preparation celloidin viscosity, have differences between solid content, first by cellulose triacetate and three acetic acid in prior art
Cellulose ester film fragment is mixed according to formula rate in advance, is dissolved, be will cause under identical process conditions
Dissolution of raw material is insufficient, will will form a kind of mutually packet between cellulose triacetate thin film fragment and cellulose triacetate
The state covered causes solution rate slow, and dissolution is insufficient, while the more gel point easy to form in celloidin mixed liquor,
Celloidin mixed liquor quality is caused to decline, final gel point can be cast in cellulose triacetate thin film, generate a large amount of not similar shapes
The crystal point and dotted disadvantage of shape and size, and this celloidin solution when removing from supporter, is easy after forming wetting film
It causes removing to remain, influences the optical property and apparent property of cellulose triacetate film.(2) cellulose triacetate thin film is broken
A certain amount of mechanical admixture can be mixed into during processing, transport and storage by mincing, if this some mechanical impurity does not carry out
Coarse filtration, direct fine filtering will affect the filter efficiency and service life of filtering material；(3) cellulose triacetate thin film
Containing a variety of auxiliary agents added in first time film forming procedure in fragment, cellulose triacetate thin film fragment is recycled
When, it needs to determine cellulose triacetate thin film fragment and raw material cellulose triacetate according to the type of manufactured film
Celloidin mixed liquor is prepared after mixed proportion again, mixed dissolution easily causes addition auxiliary agent content inaccuracy and the switching of celloidin type in advance
Inconvenient phenomenon occurs.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of preparation works of cellulose triacetate thin film
Skill, it recycles cellulose triacetate thin film fragment, and can efficiently prepare optical property and apparent property
Excellent cellulose triacetate thin film.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation process of cellulose triacetate thin film, comprising the following steps:
(1) cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360-380 part, normal-temperature dissolution 2-
After 3h, 50-60 DEG C of high temperature, pressurize 1-1.2MPa, dissolves 3-4h, and standing obtains cellulose triacetate cotton glue；
(2) cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380-400 part,
After normal-temperature dissolution 3-4h, 60-80 DEG C of high temperature, pressurize 1.4-1.8MPa, dissolves 4-6h, and standing obtains cellulose triacetate thin film
Fragment cotton glue；
(3) by cellulose triacetate cotton glue and cellulose triacetate thin film fragment cotton glue proportionally 2:3
~4:1 is mixed, and is heated to celloidin mixed liquor, and temperature is controlled at 30-70 DEG C, and heating time is 2-3h, is filtered, filtering
Precision controlling is at 1-10 μm；
(4) filtered celloidin mixed liquor is subjected to high temperature and pressure dissolution, heating and temperature control is at 60-100 DEG C, pressure control
System is in 1.6-3Mpa, time 1-2h, then fine filtering, precision controlling at 1-5 μm, finally to filtered celloidin mixed liquor into
Row is concentrated by evaporation, and control celloidin mixed liquid concentration is 18wt% or more, 22wt% or less.
(5) celloidin mixed liquor is transported to curtain coating mouth via three screw pump, is squeezed by curtain coating mouth onto curtain coating supporter,
It forms homogeneous transparent casting films on supporter to be removed after casting films have supportive, forced air drying, winding obtains
Cellulose triacetate thin film.
The preparation process of above-mentioned cellulose triacetate thin film exists to the heating and temperature control of cellulose esters celloidin mixed liquor
40-60 DEG C, to filtered cellulose esters celloidin mixed liquor heating and temperature control at 70-90 DEG C, pressure is controlled in 2-2.6MPa.
The preparation process of above-mentioned cellulose triacetate thin film, mixed solvent are made of main solvent and cosolvent, main solvent
For at least one of methylene chloride and methyl acetate, ratio is 80wt% or more, 90wt% or less；Cosolvent be n-butanol and
At least one of methanol, n-butanol additional proportion are 0.3wt%~3wt%, and methanol additional proportion is 10wt%~20wt%.
The preparation process of above-mentioned cellulose triacetate thin film is thin to Triafol T and cellulose triacetate respectively
Film fragment is filtered, and filtering accuracy is 5-10 μm.
The preparation process of above-mentioned cellulose triacetate thin film needs before the heating of cellulose esters celloidin mixed liquor to fibre
The mixed solvent for supplementing 3%-5%wt (weight) in plain ester celloidin mixed liquor is tieed up, and 30-60 DEG C of control is required to heating temperature,
Preferable temperature is controlled at 40-50 DEG C.
The preparation process of above-mentioned cellulose triacetate thin film needs to carry out to cellulose esters celloidin mixed liquor after fine filtering
Dissolved under pressure is heated, heating temperature requires to be preferably controlled in 70-90 DEG C, and pressure is preferably controlled in 2-2.6MPa.
Compared with prior art, technical solution provided by the present invention can finally make cellulose triacetate thin film broken
Object cotton glue and cellulose triacetate cotton glue uniformly mix, and can efficiently reduce present in cellulose esters celloidin mixed liquor
Gel point reduces the spot defect in final film-forming products, can improve the mechanical property of film significantly.It can accomplish difference simultaneously
The random switching of diaphragm kind recycles and the switching requirement of celloidin piece kind meeting cellulose triacetate thin film fragment
Meanwhile it can efficiently prepare the excellent film of optical characteristics.
Detailed description of the invention
Fig. 1 is existing celloidin preparation process；
Each label respectively indicates in figure are as follows: E-11, mixed solvent preparation unit, E-22, mixing cotton glue preparation unit, E-
3, storage tank 1 in cotton glue, storage tank 2 in E-44, mixing cotton glue, V-11, mixing cotton glue coarse filter, V-22, first are mixed
Grade sheet frame filter plant, V-33, second level plate-frame filtering equipment.
Fig. 2 is present invention mixing celloidin preparation process；
Each label respectively indicates in figure are as follows: E-1, cellulose triacetate cotton glue preparation unit E-2, Triafol T
Ester film fragment cotton glue preparation unit, E-3, mixed solvent preparation unit, E-4, celloidin blending tank, E-5, static mixing
Device, E-7, high-temperature pressurizing reaction kettle, E-8, condensing tower, E-9, mixed solvent recycling can, V-1, cellulose triacetate cotton glue
Coarse filter, V-2, cellulose triacetate thin film fragment cotton glue coarse filter, V-3, plate-frame filtering equipment, V-4, fine mistake
Filter.
Fig. 3 is cellulose triacetate thin film casting technique；
Each label respectively indicates in figure are as follows: 1, curtain coating nozzle, 2, curtain coating supporter before drum, 3, curtain coating supporter, 4, curtain coating branch
Drum after support body, 5, stretching-machine, 6, drying box, 7, winding room.
Specific embodiment
1 cellulose triacetate celloidin mixing liquid preparing process
Cellulose esters cotton glue preparation unit E-1 is used in the embodiment of the present invention, cellulose triacetate thin film is broken
Object cotton glue preparation unit E-2 and mixed solvent preparation unit E-3 passes through pipeline P-1 by adjusting needle valve and metering pump respectively
It is attached with P-2 (see Fig. 2).In addition, pipeline P-3 connection comes from cellulose esters cotton glue in celloidin preparation unit E-1, in pipe
It is provided with cellulose esters cotton glue coarse filter V-1 in the P-3 of road, filters out insoluble mechanical admixture；Pipeline P-4 connection comes from cotton
Cellulose triacetate thin film fragment cotton glue, is provided with cellulose triacetate in pipeline P-4 in glue preparation unit E-2
Film crushing object cotton glue coarse filter V-2, filters out the insoluble impurities in cellulose triacetate thin film fragment.It will be primary
Filtered cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue carry out primary in celloidin blending tank E-4
Mixing, obtains cellulose esters celloidin mixed liquor, and mixed cellulose esters celloidin mixed liquor primary in process 1 is passed through aciculiform tune
Valve is saved, three screw pump is delivered in static mixer E-5 by pipeline P-5 carries out second of uniformly mixing, conveys via pipeline P-6
Into plate-frame filtering equipment V-3, first time fine filtering is carried out, the cellulose esters celloidin mixed liquor after first time fine filtering is logical
It crosses three screw pump to be transported in high-temperature pressurizing reaction kettle E-7 by pipeline P-7, and the solvent of high temperature evaporation is returned by pipeline P-10
It receives into mixed solvent recycling can E-9.Cellulose esters celloidin mixed liquor after high-temperature pressurizing heating for dissolving, it is defeated through piping P-8
Send into fine filter V-4, after fine filtering again, by pipeline P-9 be transported to concentration condensing tower E-8 in carry out it is dense
Contracting obtains the cellulose esters celloidin mixed liquor for meeting concentration requirement.Auxiliary agent filtering, polymeric membrane can be used in above-mentioned filter type
Material filtering, the filtering of metal sintering core and plate-frame filtering.
2 cellulose triacetate thin film casting molding processes
Cellulose esters celloidin mixed liquor obtained in process 1 is passed through into three screw pump, bend pipe copper mesh, into curtain coating mouth, stream
Prolong the cellulose esters celloidin mixed liquor in mouth to squeeze out under the pressure of screw pump from curtain coating mouth seam, uniformly exclusion is to continuously running ground
It is cast on supporter.Casting apparatus is a closed-cycle system, passes through air-supply and heat conducting pipe two ways heating curtain coating supporter
Upper wetting film makes wetting film be dried to the film with certain water capacity and mechanical strength, reaches drum removing before curtain coating supporter
It is removed at axis, while hot wind takes away the solvent of part volatilization, into solution storage tanks, in case recycling.Removing
Wetting film afterwards enters stretching-machine, is advanced by fixture clamping traction in stretching-machine, continues drying into drying box, sufficiently dry
Afterwards, after being balanced via tandem-driving bogie, reach winding area, it is sliced while, embossing while after wound, obtain the three of homogeneous transparent
Cellulose acetate ester film.
Embodiment 1
1 cellulose triacetate celloidin mixing liquid preparing process
(1) cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360 parts, after normal-temperature dissolution 3h,
60 DEG C of high temperature, pressurize 1.2MPa, dissolves 3h, and standing obtains cellulose esters cotton glue, filters, and filtering accuracy is controlled at 10 μm；(2)
Cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380 parts, high after normal-temperature dissolution 4h
80 DEG C of temperature, pressurize 1.8MPa, dissolves 6h, and standing obtains cellulose triacetate thin film fragment cotton glue, filters, filtering accuracy
Control is at 10 μm；
(3) by cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue, proportionally 3:2 is mixed
It closes, and supplements the mixed solvent of 3%wt (weight) into celloidin mixed liquor, cellulose esters celloidin mixed liquor is heated, temperature
40 DEG C of degree, heating time is 2h, and filtering, filtering accuracy is controlled at 10 μm；
(4) filtered cellulose esters celloidin mixed liquor is subjected to high temperature and pressure dissolution, heating and temperature control is at 60 DEG C, pressure
Power control is in 1.6MPa, time 60min, then fine filtering, and precision controlling is at 5 μm, finally to filtered cellulose esters cotton
Glue mixed liquor is evaporated concentration, and control celloidin concentration is 18wt%.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.
Embodiment 2
1 cellulose triacetate celloidin mixing liquid preparing process
(1) cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360 parts, after normal-temperature dissolution 3h,
60 DEG C of high temperature, pressurize 1.2MPa, dissolves 3h, and standing obtains cellulose esters cotton glue, filters, and filtering accuracy is controlled at 10 μm；(2)
Cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380 parts, high after normal-temperature dissolution 4h
80 DEG C of temperature, pressurize 1.8MPa, dissolves 6h, and standing obtains cellulose triacetate thin film fragment cotton glue, filters, filtering accuracy
Control is at 10 μm；
(3) by cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue, proportionally 3:2 is mixed
It closes, and supplements the mixed solvent of 3%wt (weight) into celloidin mixed liquor, cellulose esters celloidin mixed liquor is heated, temperature
40 DEG C of degree, heating time is 2h, and filtering, filtering accuracy is controlled at 8 μm；
(4) filtered cellulose esters celloidin mixed liquor is subjected to high temperature and pressure dissolution, heating and temperature control is at 70 DEG C, pressure
Power control is in 2MPa, time 60min, then fine filtering, and precision controlling is at 5 μm, finally to filtered cellulose esters celloidin
Mixed liquor is evaporated concentration, and control celloidin concentration is 18wt%.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.
Embodiment 3
1 cellulose triacetate celloidin mixing liquid preparing process
(1) cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360 parts, after normal-temperature dissolution 3h,
60 DEG C of high temperature, pressurize 1.2MPa, dissolves 3h, and standing obtains cellulose esters cotton glue, filters, and filtering accuracy is controlled at 10 μm；
(2) cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380 parts, room temperature
After dissolving 4h, 80 DEG C of high temperature, pressurize 1.8MPa, dissolves 6h, and standing obtains cellulose triacetate thin film fragment cotton glue, mistake
Filter, filtering accuracy are controlled at 10 μm；
(3) by cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue, proportionally 3:2 is mixed
It closes, and supplements the mixed solvent of 4%wt (weight) into celloidin mixed liquor, cellulose esters celloidin mixed liquor is heated, temperature
40 DEG C of degree, heating time is 2h, and filtering, filtering accuracy is controlled at 5 μm；
(4) filtered cellulose esters celloidin mixed liquor is subjected to high temperature and pressure dissolution, heating and temperature control is at 80 DEG C, pressure
Power control is in 2.2MPa, time 60min, then fine filtering, and precision controlling is at 1 μm, finally to filtered cellulose esters cotton
Glue mixed liquor is evaporated concentration, and control celloidin concentration is 18wt%.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.
Embodiment 4
1 cellulose triacetate celloidin mixing liquid preparing process
(1) cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360 parts, after normal-temperature dissolution 3h,
60 DEG C of high temperature, pressurize 1.2MPa, dissolves 3h, and standing obtains cellulose esters cotton glue, filters, and filtering accuracy is controlled at 10 μm；
(2) cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380 parts, room temperature
After dissolving 4h, 80 DEG C of high temperature, pressurize 1.8MPa, dissolves 6h, and standing obtains cellulose triacetate thin film fragment cotton glue, mistake
Filter, filtering accuracy are controlled at 10 μm；
(3) by cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue, proportionally 3:2 is mixed
It closes, and supplements the mixed solvent of 5%wt (weight) into celloidin mixed liquor, cellulose esters celloidin mixed liquor is heated, temperature
40 DEG C of degree, heating time is 2h, and filtering, filtering accuracy is controlled at 5 μm；
(4) filtered cellulose esters celloidin mixed liquor is subjected to high temperature and pressure dissolution, heating and temperature control is at 90 DEG C, pressure
Power control is in 2.6MPa, time 60min, then fine filtering, and precision controlling is at 1 μm, finally to filtered cellulose esters cotton
Glue mixed liquor is evaporated concentration, and control celloidin concentration is 18wt%.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.
Embodiment 5
1 cellulose triacetate celloidin mixing liquid preparing process
(1) cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360 parts, after normal-temperature dissolution 3h,
60 DEG C of high temperature, pressurize 1.2MPa, dissolves 3h, and standing obtains cellulose esters cotton glue, filters, and filtering accuracy is controlled at 10 μm；
(2) cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380 parts, room temperature
After dissolving 4h, 80 DEG C of high temperature, pressurize 1.8MPa, dissolves 6h, and standing obtains cellulose triacetate thin film fragment cotton glue, mistake
Filter, filtering accuracy are controlled at 10 μm；
(3) by cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue, proportionally 3:2 is mixed
It closes, and supplements the mixed solvent of 5%wt (weight) into celloidin mixed liquor, cellulose esters celloidin mixed liquor is heated, temperature
40 DEG C of degree, heating time is 2h, and filtering, filtering accuracy is controlled at 5 μm；
(4) by filtered cellulose esters celloidin mixed liquor carry out high temperature and pressure dissolution, heating and temperature control at 100 DEG C,
Pressure control is in 3MPa, time 60min, then fine filtering, and precision controlling is at 1 μm, finally to filtered cellulose esters cotton
Glue mixed liquor is evaporated concentration, and control celloidin concentration is 18wt%.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.
Comparative example 1
1 cellulose triacetate celloidin mixing liquid preparing process
Cellulose triacetate raw material and cellulose triacetate thin film fragment are mixed according to mass ratio 3:2 in advance
It closing, is sufficiently dissolved in reaction kettle with mixed solvent, and be heated to 40 DEG C, carry out coarse filtration, filtering accuracy is 10 μm, into
The static uniformly mixing of row, by it is quiet be mixed it is even after cellulose esters celloidin mixed liquor carry out fine filtering, filtering accuracy is 10 μm, so
It is afterwards 18% by cellulose esters celloidin mixed liquor cooling concentration to mass concentration, is used for curtain coating.Sampling and testing cellulose esters cotton
Glue mixed liquor performance.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.Sampling carries out film performance test.
Comparative example 2
1 cellulose triacetate celloidin mixing liquid preparing process
Cellulose triacetate raw material and cellulose triacetate thin film fragment are mixed according to mass ratio 3:2 in advance
It closes, is sufficiently dissolved, and be heated to 40 DEG C, be filtered with mixed solvent in reaction kettle, filtering accuracy is 10 μm, is carried out
Static uniformly mixing, by it is quiet be mixed it is even after cellulose esters celloidin mixed liquor carry out high-temperature heating dissolved under pressure, heating temperature is
80 DEG C, pressure 2.2Mpa, the cellulose esters celloidin mixed liquor after high-temperature heating dissolved under pressure is subjected to second of fine filtering,
5 μm of filtering accuracy, it is 18% that the celloidin after second of fine filtering, which is delivered to cooling concentration to mass concentration in cooling tower, is supplied
Curtain coating uses.Gel point number in cellulose esters celloidin mixed liquor after sampling and testing cooling concentration.
2 cellulose triacetate thin film casting molding processes
Cellulose triacetate celloidin mixed liquor is transported to curtain coating mouth via three screw pump, passes through curtain coating mouth exclusion to stream
Prolong on supporter, forms homogeneous transparent casting films on supporter and removed after casting films have supportive, air blast is dry
Dry, winding obtains cellulose triacetate thin film.Sampling carries out film performance test, and test result is as shown in table 1.
Evaluation method:
Celloidin mixed liquor performance test: taking cotton glue 100ml with clean transparent beaker, seal, after defoaming,
Under dark room conditions, a piece of parallel polaroid is placed respectively in beaker front and rear sides, with An Intense Beam of Light from polaroid front irradiation, is penetrated
Celloidin solution observes the number of contained insoluble particles in this 100ml celloidin.It records test data (gel point quantity/100ml).
The test of cellulose triacetate thin film crystal point quantity: 1 × 1m of full width wide sheet base is taken at random2, marked with 10cm × 10cm
Ruler randomly selects 10 sections, amplifies 10 × 5 times under an optical microscope, counts cellulose triacetate thin film this 10 respectively
Crystal point quantity in section calculates average value, is converted into 1 × 1m2Interior crystal point quantity (a/m2)。
Using the light transmittance and haze value of mist degree tester test single thin film, test data is recorded.
Cellulose triacetate thin film Mechanics Performance Testing: cellulose triacetate thin film mechanical property is according to GB/
10403-2006 " stretched plastic film method for testing performance " is tested.
1 celloidin quality of table and film performance comparison
Claims (5)
1. a kind of preparation process of cellulose triacetate thin film, which comprises the following steps:
(1), cellulose triacetate and mixed solvent ratio are added according to 100 parts: 360-380 part, normal-temperature dissolution 2-3h
Afterwards, 50-60 DEG C of high temperature, pressurize 1-1.2MPa, dissolves 3-4h, and standing obtains cellulose esters cotton glue；
(2), cellulose triacetate thin film fragment and mixed solvent ratio are added according to 100 parts: 380-400 part, often
After temperature dissolution 3-4h, 60-80 DEG C of high temperature, pressurize 1.4-1.8MPa, dissolves 4-6h, it is broken that standing obtains cellulose triacetate thin film
Mince cotton glue；
(3), by cellulose esters cotton glue and cellulose triacetate thin film fragment cotton glue, proportionally 2:3~4:1 is carried out
Mixing, heats celloidin mixed liquor, and temperature is controlled at 30-70 DEG C, and heating time is 2-3h, filtering, filtering accuracy control
At 1-10 μm；
(4), filtered celloidin mixed liquor is subjected to high temperature and pressure dissolution, at 60-100 DEG C, pressure controls heating and temperature control
In 1.6-3Mpa, time 1-2h, then fine filtering, precision controlling are finally evaporated filtered celloidin dense at 1-5 μm
Contracting, obtains cellulose esters celloidin mixed liquor, and control celloidin concentration is 18wt% or more, 22wt% or less；
(5), cellulose esters celloidin mixed liquor is transported to curtain coating mouth via three screw pump, is supported by curtain coating mouth exclusion to curtain coating
On body, homogeneous transparent casting films being formed on supporter and are removed after casting films have supportive, forced air drying is received
Volume, obtains cellulose triacetate thin film.
2. the preparation process of cellulose triacetate thin film according to claim 1, which is characterized in that celloidin mixed liquor
Heating and temperature control at 40-60 DEG C, to filtered celloidin mixed liquor heating and temperature control at 70-90 DEG C, pressure control exists
2-2.6MPa。
3. the preparation process of cellulose triacetate thin film according to claim 2, which is characterized in that mixed solvent is by leading
Solvent and cosolvent composition, main solvent are at least one of methylene chloride and methyl acetate, and ratio is 80wt% or more,
90wt% or less；Cosolvent is at least one of n-butanol and methanol.
4. the preparation process of cellulose triacetate thin film according to claim 3, which is characterized in that respectively to cellulose
Ester cotton glue and cellulose triacetate thin film fragment cotton glue are filtered, and filtering accuracy is 5-10 μm.
5. the preparation process of cellulose triacetate thin film according to claim 4, which is characterized in that step is given in (3)
Before the heating of celloidin mixed liquor, need to supplement the mixed solvent of wt 3%-5% into celloidin mixed liquor, and to heating temperature requirement
Control is at 30-60 DEG C.
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