CN106564129B - A kind of preparation method of infrared external reflection liquid crystal polymer particle - Google Patents
A kind of preparation method of infrared external reflection liquid crystal polymer particle Download PDFInfo
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- CN106564129B CN106564129B CN201610907119.6A CN201610907119A CN106564129B CN 106564129 B CN106564129 B CN 106564129B CN 201610907119 A CN201610907119 A CN 201610907119A CN 106564129 B CN106564129 B CN 106564129B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/04—Making granules by dividing preformed material in the form of plates or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
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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
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/0074—Production of other optical elements not provided for in B29D11/00009- B29D11/0073
- B29D11/00788—Producing optical films
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- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Ophthalmology & Optometry (AREA)
- Toxicology (AREA)
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- Liquid Crystal (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention discloses a kind of preparation methods of infrared external reflection liquid crystal polymer particle, the following steps are included: infrared external reflection liquid crystal polymer film is placed in solution, the density of the solution is close with the infrared external reflection liquid crystal polymer film, ultrasonication, liquid crystal polymer film is crushed using ultrasonic wave, the liquid crystal polymer particle of 150 μm of available side length <, using a kind of density and the close solution of infrared external reflection liquid crystal polymer film density, film can be effectively prevented to sink to bottom when broken or float on top, influence crushing effect.
Description
Technical field
The present invention relates to optical film technology fields, and in particular to a kind of preparation side of infrared external reflection liquid crystal polymer particle
Method.
Background technique
The principle of electroresponse infrared external reflection smart window is the liquid crystal film fragment that will be crushed infrared external reflection liquid crystal film and obtain
(namely liquid crystal polymer particle) is filled into liquid crystal cell, drives the rotation of carrier liquid crystal by voltage, the rotation of carrier liquid crystal from
And liquid crystal polymer particle is driven to rotate, if liquid crystal polymer particle side length is excessive, carrier liquid crystal is unable to drive its rotation, institute
The liquid crystal polymer particle (side length < 150 μm) of side length very little is needed with electroresponse infrared external reflection smart window, at present infrared external reflection liquid
There are many methods for the preparation of crystalline polymer particle.
Polishing prepares liquid crystal polymer particle: infrared external reflection liquid crystal polymer film being placed in mortar, is then used
Mortar stick grinding film, controls the time of grinding, to obtain the liquid crystal particle of suitable dimension.Liquid crystal particle obtained by polishing
Size is very uneven, is difficult meet the needs of electroresponse infrared external reflection smart window.Similarly, the time that polishing needs is longer, right
Manpower it is more demanding, and be difficult to obtain a certain number of liquid crystal polymer particles.
Laser ablation method prepares liquid crystal polymer particle: liquid crystal polymer film is etched using femtosecond or picosecond laser,
Set q-frequency, laser work power, etch rate, to obtain the liquid crystal polymer particle of specific dimensions.Due to infrared anti-
The amount of liquid crystal polymer particle needed for emitter part is less, so not economical enough using laser ablation method.
Photoetching process prepares liquid crystal polymer particle: after the liquid crystal mixed is filled into liquid crystal cell, covering on liquid crystal cell
Upper mask plate, is solidified using ultraviolet light.Photoetching process is since the gap of mask plate is too small, when ultraviolet light solidification, it may appear that
The liquid crystal of light leakage, surrounding is also cured, and is unable to get the sufficiently small liquid crystal particle of size in this way.
Based on the above reasons, polishing, laser ablation method and photoetching process preparation liquid crystal particle are difficult to be widely used in making
Make in electroresponse infrared external reflection device.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of preparation methods of infrared external reflection liquid crystal polymer particle.
The technical solution used in the present invention is:
A kind of preparation method of infrared external reflection liquid crystal polymer particle, comprising the following steps: by infrared external reflection polymerizable mesogenic
Object film is placed in solution, and the density of the solution is close with the infrared external reflection liquid crystal polymer film, ultrasonication.
In some specific embodiments, the solution is saline solution or dichloromethane solution.
In the preferred embodiment of above scheme, the solution is saturated salt solution.
It further include being sifted out not using different size sieve after the Ultrasonic Pulverization process in some specific embodiments
With the process of the liquid crystal polymer particle of size.
In some specific embodiments, ultrasonic power 100-150W, the total grinding time of ultrasound is 80-
160min。
In some specific embodiments, crushing process solution temperature is -2-5 DEG C.
In some specific embodiments, the ultrasonication process can be multiple shattering process.
In some specific embodiments, the infrared external reflection liquid crystal polymer film is that mixed liquid crystal is filled into liquid
In brilliant box, solidify through ultraviolet light, heat cure, obtained infrared external reflection liquid crystal polymer film.
In some specific embodiments, the reflected waveband of the infrared external reflection liquid crystal polymer film is 700-
1100nm。
The beneficial effects of the present invention are:
It is all difficult to be widely used in making electroresponse for currently used polishing, laser ablation method and photoetching process
The problems in infrared external reflection device, the present invention provides a kind of preparation methods of infrared external reflection liquid crystal polymer particle, including with
Lower step: infrared external reflection liquid crystal polymer film is placed in solution, and the density of the solution and the infrared external reflection liquid crystal are poly-
It closes object film to be close, ultrasonication is crushed liquid crystal polymer film using ultrasonic wave, 150 μm of available side length <'s
Liquid crystal polymer particle can effectively be prevented using a kind of density and the close solution of infrared external reflection liquid crystal polymer film density
Only film sinks to bottom when broken or floats on top, influences crushing effect.
Detailed description of the invention
Fig. 1 is the pictorial diagram of infrared external reflection liquid crystal polymer film；
Fig. 2 is infrared external reflection liquid crystal polymer particle preparation process schematic diagram；
Fig. 3 is the microscope figure for the infrared external reflection liquid crystal polymer particle being prepared；
Fig. 4 is the average side length for the liquid crystal polymer particle that embodiment 1, embodiment 2 and comparative example 1 obtain.
Fig. 5 is the side length variance for the liquid crystal polymer particle that embodiment 1, embodiment 2 and comparative example 1 obtain.
Specific embodiment
Embodiment 1:
Mixed liquid crystal is filled into liquid crystal cell according to what infrared external reflection liquid crystal polymer film formula was prepared, through ultraviolet light
Solidification, heat cure, obtained infrared external reflection liquid crystal polymer film, as shown in Figure 1, its reflected waveband is 700-1100nm.
Infrared external reflection liquid crystal polymer film is scraped from device, referring to Fig. 2, infrared external reflection liquid crystal polymer film 4 is placed in
In 40mL reagent bottle 2；It is equipped with saturated salt solution, suitable saturated salt solution is added in reagent bottle 2；Reagent bottle 2 is placed in
In 300mL beaker 3, suitable mixture of ice and water is added in beaker 3, controlling the water temperature in sheet glass is -2-5 DEG C.It will be ultrasonic
The probe 1 of wave cell crushing instrument does not have supersaturated saline solution, cannot touch bottom of bottle, and the power setting of sonicator is existed
120W starts ultrasonic cell disruption instrument.After smashing 20min, liquid crystal polymer particle is drawn with dropper from reagent bottle 2 and is placed in
On clean sheet glass, and polarized light microscope observing liquid crystal particle is used, measures its length and wide using Linksys32 software, record
And carry out data processing.Infrared external reflection liquid crystal polymer film is repeated to crush six times according to above-mentioned condition, total grinding time
120min, the infrared external reflection liquid crystal polymer particle finally obtained can sieve with 100 mesh sieve, i.e. 150 μm of side length <, under the microscope
Observation obtains infrared external reflection liquid crystal polymer particle as shown in figure 3, the side length of liquid crystal polymer particle is divided as can see from Figure 3
Cloth is more uniform.
If necessary to the infrared external reflection liquid crystal polymer particle of side length in a certain range, screening side length is such as wanted in 30-
Infrared external reflection liquid crystal polymer particle in 100 μ ms, first by 30 μm of sieve of the saturated salt solution containing liquid crystal particle
It is sieved, 30 μm of side length > of liquid crystal particle on sieve is placed in baking oven after sieve, 50 DEG C or so drying 30min will be on sieve
Liquid crystal particle scrape, then the fragment of drying is placed in 100 μm of sieve and is sieved, size can be obtained in 30-100 μm of model
Enclose interior infrared external reflection liquid crystal polymer particle.
Embodiment 2:
The infrared external reflection liquid crystal polymer film being prepared in embodiment 1 is placed in 40mL reagent bottle, in vial
It is middle that suitable dichloromethane solution (DCM solution) is added；Vial is placed in 300mL beaker, is added in beaker suitable
Mixture of ice and water, controlling the water temperature in sheet glass is -2-5 DEG C.The probe of ultrasonic cell disruption instrument is not had into supersaturated saline solution,
Bottom of bottle cannot be touched, by the power setting of sonicator in 120W, starts ultrasonic cell disruption instrument.According to implementation
Example 1 is crushed infrared external reflection liquid crystal polymer film with identical step.
Embodiment 3:
Ultrasonic Pulverization is carried out in the same manner as shown in Example 1, by the power setting of sonicator in 150W, is opened
Dynamic ultrasonic cell disruption instrument.20min is crushed every time, is carried out 4 times, total grinding time 80min, the infrared external reflection liquid finally obtained
Crystalline polymer particle can sieve with 100 mesh sieve, i.e. 150 μm of side length <, and the side length of liquid crystal polymer particle is evenly distributed.
Embodiment 4:
Ultrasonic Pulverization is carried out in the same manner as shown in Example 1, by the power setting of sonicator in 100W, is opened
Dynamic ultrasonic cell disruption instrument.20min is crushed every time, is carried out 8 times, total grinding time 160min, the infrared external reflection finally obtained
Liquid crystal polymer particle can sieve with 100 mesh sieve, i.e. 150 μm of side length <, and the side length of liquid crystal polymer particle is evenly distributed.
Comparative example 1:
The infrared external reflection liquid crystal polymer film being prepared in embodiment 1 is placed in 40mL reagent bottle；In reagent bottle
It is middle that suitable deionized water is added；Reagent bottle is placed in 300mL beaker, suitable mixture of ice and water is added in beaker, is controlled
Water temperature in sheet glass processed is -2-5 DEG C.The probe 1 of ultrasonic cell disruption instrument is not had into supersaturated saline solution, bottle cannot be touched
Bottom starts ultrasonic cell disruption instrument by the power setting of sonicator in 120W.According to embodiment 1 with it is identical
Step is crushed infrared external reflection liquid crystal polymer film.
Respectively using petrographic microscope to embodiment 1, embodiment 2, the broken obtained infrared external reflection polymerizable mesogenic of comparative example 1
Object particle is observed, and 20 pieces of fragments under field of microscope are chosen, and measures its length and wide, record with Linksys32 software
And data processing is carried out, obtain that experimental result is as shown in Figure 4 and Figure 5, Fig. 4 is what embodiment 1, embodiment 2 and comparative example 1 obtained
The average side length of liquid crystal polymer particle, Fig. 5 are the liquid crystal polymer particle that embodiment 1, embodiment 2 and comparative example 1 obtain
It respectively illustrates embodiment 1(in side length variance, Fig. 4 and Fig. 5 infrared external reflection liquid crystal polymer film is placed in saturated salt solution
It is damaged), infrared external reflection liquid crystal polymer film is placed in DCM solution and is crushed by embodiment 4() and comparative example 1(by infrared external reflection
Liquid crystal polymer film is placed in deionized water and is crushed) the obtained liquid crystal polymer particle of six each Ultrasonic Pulverizations of Ultrasonic Pulverization
Average side length and side length variance, as seen from the figure, using by liquid crystal polymer film be put in deionized water carry out ultrasound
It crushing, the average side length of obtained liquid crystal polymer particle, which is slightly larger than, is put into what crushing in saturated salt solution and DCM solution obtained,
But it is seen from fig 5 that the variance of the ion crushed in deionized water be greater than be put into saturated salt solution and DCM solution
What crushing obtained, illustrate that the side length distribution consistency degree for crushing obtained particle is poor, actual demand is unable to satisfy in practical application.
Claims (5)
1. a kind of preparation method of infrared external reflection liquid crystal polymer particle, which comprises the following steps: by infrared external reflection
Liquid crystal polymer film is placed in solution, and the density of the solution is close with the infrared external reflection liquid crystal polymer film, is surpassed
Sound is broken, and the solution is saturated salt solution, and crushing process solution temperature is -2-5 DEG C, and the ultrasonication process is repeatedly broken
Broken process.
2. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, which is characterized in that the ultrasound
It further include the process that various sizes of liquid crystal polymer particle is sifted out using different size sieve after crushing process.
3. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, which is characterized in that ultrasonic wave function
Rate is 100-150W, and the total grinding time of ultrasound is 80-160min.
4. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, which is characterized in that described infrared
Reflective liquid crystal thin polymer film is that mixed liquid crystal is filled into liquid crystal cell, is solidified through ultraviolet light, heat cure, and what is obtained is infrared anti-
Penetrate liquid crystal polymer film.
5. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, which is characterized in that described infrared
The reflected waveband of reflective liquid crystal thin polymer film is 700-1100nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584663A (en) * | 2008-05-22 | 2009-11-25 | 广州瑞济生物技术有限公司 | Novel delivery system of Duoxitasai lipidosome for injection and preparation method thereof |
| CN104829785A (en) * | 2015-03-16 | 2015-08-12 | 华南师范大学 | Infrared reflective liquid crystal high-molecular thin film and preparation method thereof |
| CN105652549A (en) * | 2016-03-04 | 2016-06-08 | 深圳市国华光电科技有限公司 | Electric response intelligent glass, preparation method thereof and light regulation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3049068A1 (en) * | 2013-09-27 | 2016-08-03 | Tufts University | Synthesis of silk fibroin micro- and submicron spheres using a co-flow method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584663A (en) * | 2008-05-22 | 2009-11-25 | 广州瑞济生物技术有限公司 | Novel delivery system of Duoxitasai lipidosome for injection and preparation method thereof |
| CN104829785A (en) * | 2015-03-16 | 2015-08-12 | 华南师范大学 | Infrared reflective liquid crystal high-molecular thin film and preparation method thereof |
| CN105652549A (en) * | 2016-03-04 | 2016-06-08 | 深圳市国华光电科技有限公司 | Electric response intelligent glass, preparation method thereof and light regulation method thereof |
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