A kind of cellulose triacetate thin film
Technical field
The present invention relates to a kind of cellulose triacetate thin film, in particular to a kind of ultrasonic cavitation and mechanical stirring mixing
The cellulose triacetate thin film reunited when dispersing matting agent, and preventing matting agent from adding by controlling pipe flow speed.
Background technique
In recent years, in constantly universal each display device of liquid crystal display, cellulose triacetate thin film is due to having
Excellent optics, physical characteristic, are widely used in the support and protective film of polaroid.
Cellulose triacetate thin film generallys use solution curtain coating film method.It is that cellulose triacetate is dissolved in solvent
Celloidin is expelled on curtain coating supporter using casting mold by middle formation polymer solution (hereinafter referred to as celloidin) after filtering,
After the casting films on supporter have supportive, casting films are removed from curtain coating supporter, form wetting film, it is further right
Wetting film is dried, and forms a film, winding, so that it is uniform to obtain thickness, optically isotropic film.
Triacetate film obtained by the above method, after being wound into axis, during storage, easily occur adhesion between film and film,
The problems such as moisture absorption, serious quality, use scope and the resting period for influencing product.
In the prior art, it discloses in the production process of cellulose triacetate thin film, a kind of matting agent is added, it can be with
It is effectively improved this problem.And matting agent is nano-scale particle, how to disperse and addition is improvement cellulose triacetate thin film
The moisture absorption, the key point of adhesion.The dispersion of disclosed matting agent and adding method are: matting agent being added and contains dilute celloidin solution
Dispersion slot in carry out mechanical stirring dispersion, mechanical stirring frequency: 100Hz;Handle the time: 1h obtains dispersion liquid;Then in ball
It is ground in grinding machine, handle the time: 4h obtains lapping liquid, wherein 10 μm of particle contents of <: 85%-90%;Finally,
Lapping liquid is mixed with cotton glue after filtering carries out casting film, as shown in Figure 1.It is put into storeroom after being wound into axis, after 2-3 days
There is moisture absorption phenomenon.
But there are the following problems with adding method for above-mentioned matting agent dispersion:
(1) the single mechanical stirring dispersion of matting agent, the time is long, and stirring frequency is big, causes power consumption big, high production cost.
(2) matting agent milling time is long, and 10 μm of particle contents of < are not up to 95% or more, and grinding efficiency is low.
(3) matting agent easily agglomerates in pipeline before filtration, and 10 μm of particle contents increases of > lead to filter core service life
Shorten, increases entreprise cost.
(4) triacetate element film, which is made, in the above method has the defects such as crystal point is more, mist degree is high, transmitance is low, can not
Meet production, and resting period is short, is unfavorable for storing.
Summary of the invention
The technical problem to be solved by the present invention is to be directed to above-mentioned well known cellulose triacetate thin film production method especially
It is related to shortcoming existing for matting agent dispersion adding method, a kind of cellulose triacetate thin film containing matting agent is provided.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of cellulose triacetate thin film is made: cellulose triacetate cotton glue by the method for including following process
Preparation, matting agent dispersion with addition and tape casting, the preparation of the cellulose triacetate cotton glue is: with three acetic acid fibre
Tieing up plain ester particle is raw material, and celloidin solution is made in the mixed solvent in it after completely dissolution;It is characterized in that, three vinegar
In acid cellulose ester film matting agent dispersion with addition process be: by matting agent be added decentralized medium for dilute celloidin dispersion slot in
Dispersion liquid is obtained using the first Vltrasonic device, mechanical stirring composite diffusion 10min-30min, utilizes ball mill grinding dispersion liquid
100min-120min obtains lapping liquid, and after the second Vltrasonic device pipe ultrasonic, a part flows back through reflux line and stores up lapping liquid
Tank, rest part enter filter through ultrasonic pipeline and filter;Wherein reflux line flow velocity < ultrasound pipe flow speed, and reflux line
Flow velocity and ultrasonic pipeline current difference value are between 5-10L/h;Last lapping liquid mixes after static mixer, pressure buffer with cotton glue
It obtains celloidin mixed liquor and enters curtain coating process;The tape casting process is: celloidin mixed solution is cast on stainless steel belt,
It through drying, forms a film, winding obtains the cellulose triacetate thin film containing matting agent.
Above-mentioned cellulose triacetate thin film, the decentralized medium of the composite diffusion are dilute celloidins, and dilute celloidin solid content is
2.3 ± 0.1%;The mass ratio of matting agent and decentralized medium are as follows: 100:2.5~100:3.5.
Above-mentioned cellulose triacetate thin film, matting agent dispersion and ultrasonic unit frequency in dispersion slot in adding method:
40KHz-100KHz, mechanical stirring frequency: 0Hz-35Hz.
Above-mentioned cellulose triacetate thin film, < 10um particle content in lapping liquid: 99.5%-100%.
Above-mentioned cellulose triacetate thin film, the second Vltrasonic device ultrasonic frequency range: 10KHz-50KHz;Ultrasonic pipeline
Flow velocity: 10-50L/h, reflux line flow velocity: 5-45L/h.
Above-mentioned cellulose triacetate thin film, the mixed solvent are methylene chloride, butanol, volume ratio 92:8.
The utility model has the advantages that
(1) hair side agent dispersing liquid is by ultrasonic cavitation effect, mechanical stirring compound action, jitter time shorten half with
On, stirring frequency becomes smaller, and reduces power consumption, improves dispersion efficiency.
(2) milling time shortens half, and 10 μm of particle contents of < reach 99.5% or more, improves production efficiency.
(3) it effectively eliminates matting agent through pipe ultrasonic and the ultrasonic pipe flow speed of control by the second Vltrasonic device and filters front tube
Agglomeration in road, 10 μm of particle contents of < maintain 99.5%-100%, so that filter element life extends about 10 times.
(4) in the present invention, reflux line flow velocity < ultrasound pipe flow speed is limited, preferably ultrasonic pipe flow speed and reflux line
Flow velocity difference both guarantees that ultrasonic pipe flow speed is fast between 5-10L/h, prevents matting agent pipeline from reuniting, and stablizes matting agent addition
Amount, cellulose triacetate film performance maintains to stablize after guaranteeing addition matting agent.
(5) cellulose triacetate thin film obtained by the above method, crystal point disadvantage are reduced, and mist degree reduces, transmitance increases,
Moisture absorption point tails off, and product quality, benefit are improved, and product resting period is elongated.
Detailed description of the invention
Fig. 1 is cellulose triacetate thin film preparation section figure in the prior art;
Fig. 2 is the preparation section figure of cellulose triacetate thin film of the present invention.
Corresponding relationship in figure between the title and label of each section is: dispersion slot 1, the first Vltrasonic device 2, ball mill 3,
Two Vltrasonic devices 6, reflux line 10, storage tank 7, ultrasonic pipeline 8, filter 9, through static mixer 11, pressure buffer 12, celloidin pipe
Road 13.
Specific embodiment:
As shown in Fig. 2, it is made after completely dissolution in the mixed solvent using cellulose triacetate particle as raw material
Celloidin solution for standby.The dispersion of matting agent and adding technique: matting agent is added in the dispersion slot 1 containing dilute celloidin, using super
The cavitation effect and mechanical stirring compound action decentralized processing of sound wave, time 10min-30min.Ball milling is added in dispersion liquid
Machine 3 is ground, milling time 100min-120min, controls 10 μm of particle contents of lapping liquid <: 99.5%-
100%.Lapping liquid after 6 pipe ultrasonic of the second Vltrasonic device with certain flow velocity a part through 10 reflux accumulator 7 of reflux line,
A part enters filter 9 through ultrasonic pipeline 8 and filters.Finally, by the matting agent lapping liquid after fine filtering 9 through static mixer 11,
Celloidin mixed liquor is mixed to get with the cotton glue of celloidin pipeline 13 after pressure buffer 12.The celloidin mixed solution prepared is not
It is cast on rust steel steel band, through drying, forms a film, winding obtains the cellulose triacetate thin film containing matting agent.It is wound into axis
Afterwards, it is put into storeroom, occurs moisture absorption phenomenon after 15-20 days.
Secondly, the matting agent dispersion is with the method for addition, matting agent dispersion utilizes ultrasonic wave, the compound work of mechanical stirring
With dispersion efficiency improves 2 times or more, and wherein 2 supersonic frequency of ultrasonic unit is 40KHz-100KHz, and churned mechanically frequency is
0Hz-35Hz.The second Vltrasonic device 6 is added between storage tank 7 and ultrasonic pipeline 8 and is surpassed by 10 flow-dividing control of reflux line
The flow velocity in sound pipe road 8 had not only solved in ultrasonic pipeline 8 lapping liquid because flow velocity glues the phenomenon that wall causes matting agent to be reunited slowly, but also had protected
It has demonstrate,proved 10 μm of particle contents of < and has reached 99.5%-100%, so that filter core service life extends, product quality is improved.Wherein,
Two Vltrasonic devices, 6 frequency: 10KHz-50KHz, ultrasonic 8 flow velocity of pipeline: 10-50L/h, 10 flow velocity of reflux line: 5-45L/h is returned
10 flow velocity < ultrasound pipeline of flow tube road, 8 flow velocity, and 10 flow velocity of reflux line and ultrasonic 8 flow velocity difference of pipeline are between 5-10L/h.
Triacetate element film of the invention is prepared by following methods:
The preparation of cellulose triacetate cotton glue
The preparation of cellulose triacetate cotton glue mainly includes cotton glue preparation, and cotton glue filtering and constant temperature stand defoaming
Three processes.
(1) prepared by cotton glue
Firstly, mixed solvent, auxiliary agent are added to reaction kettle, stirring apparatus for reaction kettle and collet coolant-temperature gage control dress are opened
It sets, effectively the control range of speeds, is uniformly mixed.Secondly, cellulose triacetate and film crushing object are mixed according to formula rate
It is added in the reaction kettle containing mixed solvent and auxiliary agent after conjunction;The dissolution process parameters such as speed of agitator, collet coolant-temperature gage are adjusted,
Cellulose triacetate dissolution is carried out, dissolution time 6h prepares the cellulose triacetate cotton glue of homogeneous transparent.
(2) cotton glue filters
In cotton glue, it will usually be mixed into mechanical admixture and insoluble matter, need that cotton glue is filtered for multiple times.It first will be molten
The cotton glue that solution is completed is filtered through low efficient filter, is removed in solution by being discharged from reaction kettle under gear pump certain condition
There may be biggish gel piece and other mechanical admixtures, filtrate enters intermediate fluid reservoir.Under gear pump pressurized conditions, filtrate
Repeatedly fining filtering is carried out into plate and frame filter press, it is spare that filtrate enters hold-up vessel.
(3) constant temperature stands defoaming
Cotton glue constant temperature after fine filtering, which is stood, eliminates bubble, carries out in the thermostat for having jacket water (J.W.).Purpose is to remove
The steady temperature removed the bubble in solution, and solution is made to keep curtain coating required.Through constant temperature stand eliminate bubble after cotton glue into
Enter to be cast process.
Matting agent dispersion and addition
Firstly, matting agent utilizes decentralized processing under ultrasonic unit 2 and mechanical stirring compound action, place in dispersion slot 1
Manage the time: 10min-30min obtains dispersion liquid.Wherein, 2 supersonic frequency of ultrasonic unit is 40KHz-100KHz, mechanical stirring
Frequency be 0Hz-35Hz.It is ground secondly, being added in ball mill 3 through pipeline using ball mill, milling time:
10 μm of particle contents of 100min-120min, <: 99.5%-100% obtains lapping liquid, and lapping liquid is slightly imitated after entering storage tank 4
Filtering 5, into storage tank 7, lapping liquid enters 10 circulating reflux storage tank 7 of reflux line in 6 ultrasonication rear portion of device, another
Part enters fine filtering 9 through ultrasonic pipeline 8.Finally, by the matting agent lapping liquid after fine filtering 9 through static mixer 11, pressure
It is mixed to get celloidin mixed liquor with the cotton glue of celloidin pipeline 13 after buffer 12, into curtain coating process.
It is particular in that in storage tank 7 and ultrasonic pipeline 8 and the second Vltrasonic device 6 is added and by reflux reflux line 10
The flow velocity of flow-dividing control ultrasound pipeline 8 had not only solved lapping liquid in ultrasonic pipeline 8 and has re-united phenomenon, but also guaranteed 10 μm of particles of <
Content reaches 99.5%-100%.Wherein 6 frequency of the second Vltrasonic device: 10KHz-50KHz, ultrasonic 8 flow velocity of pipeline: 10-50L/
H, 10 flow velocity of reflux line: 5-50L/h.10 flow velocity < ultrasound pipeline of reflux line, 8 flow velocity, and 10 flow velocity of reflux line and ultrasound
8 flow velocity difference of pipeline is between 5-10L/h.
Finally, by the matting agent lapping liquid after fine filtering 9 after static mixer 11, pressure buffer 12 with celloidin pipeline 13
Cotton glue be mixed to get celloidin mixed liquor, into curtain coating process.
Cellulose triacetate thin film tape casting
Cotton glue containing matting agent prepared by process 1,2 is entered into three screw pump, filter, static mixing through pipeline
Device, is transported to curtain coating mouth at bend pipe copper mesh.Through being dried, removing in curtain coating mouth exclusion to the casting support continuously run,
Stretching and drawing, winding film forming.
The present invention is further illustrated combined with specific embodiments below, but the present invention is not limited thereto.
Embodiment 1
Cellulose triacetate 10Kg, cosolvent 5Kg, plasticizer 0.5Kg are taken, it is abundant to be added into 50Kg in the mixed solvent
Celloidin solution for standby is made after dissolution.1.5Kg matting agent is added 1 in the dispersion slot containing dilute celloidin, ultrasonic unit 2 is utilized
With mechanical stirring compound action decentralized processing, the time: 30min obtains dispersion liquid.Wherein, 2 frequency of ultrasonic unit: 40KHz,
Mechanical stirring frequency: 35Hz.Dispersion liquid addition ball mill 3 is ground, 10 μm of particles of time 100min, < contain
Amount: 99.8%, obtain lapping liquid.Lapping liquid is after 6 pipe ultrasonic of the second Vltrasonic device with certain flow velocity a part through flowing back
10 reflux accumulator 7 of pipeline, a part enter filter 9 through ultrasonic pipeline 8 and filter.Wherein 6 frequency of the second Vltrasonic device: 10KHz,
Ultrasonic 8 flow velocity of pipeline: 10L/h, 10 flow velocity of reflux line: 5L/h.By the matting agent lapping liquid after fine filtering 9 through static mixer
11, celloidin mixed liquor is mixed to get with the cotton glue of celloidin pipeline 13 after pressure buffer 12.The celloidin mixed solution prepared
It is cast on stainless steel belt, through drying, forms a film, winding obtains the cellulose triacetate thin film containing matting agent.It is wound into
Membrane material after axis is put into storeroom, the moisture absorption occurs after 20 days.The above-mentioned film product test data that is made is shown in Table 1.
Embodiment 2
Difference from Example 1 is hair side agent dispersing liquid jitter time: 25min, 2 frequency of ultrasonic unit:
50KHz, mechanical stirring frequency: 20Hz.Lapping liquid handles time 110min, 10 μm of particle contents of <: 99.9%, the second ultrasound dress
6 frequencies: 20KHz are set, ultrasonic 8 flow velocity of pipeline: 15L/h, 10 flow velocity of reflux line: 10L/h.It is put into storeroom after being wound into axis,
There is the moisture absorption after 17 days.The above-mentioned film product test data that is made is shown in Table 1.
Embodiment 3
Difference from Example 1 is hair side agent dispersing liquid jitter time: 30min, 2 frequency of ultrasonic unit:
70KHz, mechanical stirring frequency: 15Hz.Lapping liquid handles time 120min, 10 μm of particle contents of <: 100%, the second ultrasound dress
6 frequencies: 30KHz are set, ultrasonic 8 flow velocity of pipeline: 20L/h, 10 flow velocity of reflux line: 15L/h.Membrane material is put into storage after being wound into axis
There is the moisture absorption after 15 days in room.The above-mentioned apparent test data of film product that is made is shown in Table 1.
Embodiment 4
Difference from Example 1 is hair side agent dispersing liquid jitter time: 25min, 2 frequency of ultrasonic unit:
85KHz, mechanical stirring frequency: 10Hz.Lapping liquid handles time 110min, 10 μm of particle contents of <: 99.5%, the second ultrasound dress
6 frequencies: 40KHz are set, ultrasonic 8 flow velocity of pipeline: 25L/h, 10 flow velocity of reflux line: 20L/h.Membrane material is put into storage after being wound into axis
There is the moisture absorption after 18 days in room.The above-mentioned apparent test data of film product that is made is shown in Table 1.
Embodiment 5
Difference from Example 1 is hair side agent dispersing liquid jitter time: 20min, 2 frequency of ultrasonic unit:
100KHz, mechanical stirring frequency: 0Hz.Lapping liquid handles time 120min, 10 μm of particle contents of <: 99.8%, the second ultrasound dress
6 frequencies: 50KHz are set, ultrasonic 8 flow velocity of pipeline: 30L/h, 10 flow velocity of reflux line: 25L/h.Membrane material is put into storage after being wound into axis
There is the moisture absorption after 20 days in room.The above-mentioned apparent test data of film product that is made is shown in Table 1.
Comparative example 1
Cellulose triacetate 10Kg, cosolvent 5Kg, plasticizer 0.5Kg are taken, it is abundant to be added into 50Kg in the mixed solvent
Celloidin solution for standby is made after dissolution.1.5Kg matting agent is added 1 in the dispersion slot containing dilute celloidin, decentralized processing 1h is obtained
Dispersion liquid.Wherein, mechanical stirring frequency: dispersion liquid addition ball mill 3 is ground, 10 μ of time 4h, < by 100Hz
M particle content: 85%, obtain lapping liquid.Lapping liquid is mixed to get celloidin with the cotton glue of celloidin pipeline 13 after filtering 9 and mixes
Liquid.The celloidin mixed solution prepared is cast on stainless steel belt, through drying, is formed a film, and winding obtains cellulose triacetate
Film.The above-mentioned film product test data that is made is shown in Table 1.
Comparative example 2
Cellulose triacetate 10Kg, cosolvent 5Kg, plasticizer 0.5Kg are taken, it is abundant to be added into 50Kg in the mixed solvent
Celloidin solution for standby is made after dissolution.1.5Kg matting agent is added 1 in the dispersion slot containing dilute celloidin, decentralized processing 2h is obtained
Dispersion liquid.Wherein, mechanical stirring frequency: dispersion liquid addition ball mill 3 is ground, 10 μ of time 4h, < by 100Hz
M particle content: 88%, obtain lapping liquid.Lapping liquid is mixed to get celloidin with the cotton glue of celloidin pipeline 13 after filtering 9 and mixes
Liquid.The celloidin mixed solution prepared is cast on stainless steel belt, through drying, is formed a film, and winding obtains cellulose triacetate
Film.The above-mentioned film product test data that is made is shown in Table 1.
The above-mentioned apparent test data of film product that is made is shown in Table 1.
Evaluation method
The performances such as moisture absorption point, mist degree, crystal point, transmitance and the filtration core service life of film product are made by test.Its
Described in the moisture absorption point test for daily monitoring, place 20 days after statistical test result;Other described tests are on-line checking knot
Fruit.
Table 1
Title |
Moisture absorption point/m2 |
Crystal point number/m2 |
Mist degree/% |
Transmitance/% |
The filtration core service life/t |
Embodiment 1 |
2 |
23 |
0.02 |
92.2 |
10 |
Embodiment 2 |
1 |
21 |
0.02 |
92.3 |
9 |
Embodiment 3 |
1 |
18 |
0.02 |
92.8 |
10 |
Embodiment 4 |
3 |
20 |
0.02 |
92.6 |
8 |
Embodiment 5 |
2 |
22 |
0.02 |
92.5 |
8 |
Comparative example 1 |
35 |
58 |
0.05 |
91.0 |
1 |
Comparative example 2 |
40 |
60 |
0.05 |
91.0 |
1 |