CN106564129A - Preparation method for infrared reflective liquid crystal polymer particle - Google Patents
Preparation method for infrared reflective liquid crystal polymer particle Download PDFInfo
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- CN106564129A CN106564129A CN201610907119.6A CN201610907119A CN106564129A CN 106564129 A CN106564129 A CN 106564129A CN 201610907119 A CN201610907119 A CN 201610907119A CN 106564129 A CN106564129 A CN 106564129A
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- liquid crystal
- crystal polymer
- external reflection
- polymer particle
- infrared external
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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
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Ophthalmology & Optometry (AREA)
- Toxicology (AREA)
- Food Science & Technology (AREA)
- Liquid Crystal (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a preparation method for an infrared reflective liquid crystal polymer particle. The preparation method comprises the following steps: placing an infrared reflective liquid crystal polymer film in a solution, wherein the density of the solution is close to the density of the infrared reflective liquid crystal polymer film; and carrying out ultrasonic crushing on the infrared reflective liquid crystal polymer film so as to obtain the liquid crystal polymer particle with a side length of less than 150 [mu]m. Through usage of the solution with the density close to the density of the infrared reflective liquid crystal polymer film, the film is effectively prevented from sinking to bottom or floating above during crushing, so influence on crushing effect is avoided.
Description
Technical field
The present invention relates to optical film technology field, and in particular to a kind of preparation side of infrared external reflection liquid crystal polymer particle
Method.
Background technology
The principle of electroresponse infrared external reflection smart window is will to crush the liquid crystal film fragment that infrared external reflection liquid crystal film is obtained
（Namely liquid crystal polymer particle）Be filled in liquid crystal cell, drive carrier liquid crystal to rotate by voltage, the rotation of carrier liquid crystal from
And drive liquid crystal polymer particle to rotate, if the liquid crystal polymer particle length of side is excessive, carrier liquid crystal cannot drive which to rotate, institute
The liquid crystal polymer particle of length of side very little is needed with electroresponse infrared external reflection smart window（The length of side<150 μm), current infrared external reflection liquid
The preparation of crystalline polymer particle has various methods.
Polishing prepares liquid crystal polymer particle：Infrared external reflection liquid crystal polymer film is placed in mortar, is then used
Mortar rod grinding film, controls the time of grinding, so as to obtain the liquid crystal particle of suitable dimension.Liquid crystal particle obtained by polishing
Size is very uneven, it is difficult to meet the demand of electroresponse infrared external reflection smart window.In the same manner, the time that polishing needs is longer, right
The requirement of manpower is higher, and is difficult to obtain a number of liquid crystal polymer particle.
Laser ablation method prepares liquid crystal polymer particle：Using femtosecond or picosecond laser etching liquid crystal polymer film,
Setting q-frequency, laser work power, etch rate, so as to obtain the liquid crystal polymer particle of specific dimensions.Due to infrared anti-
The amount of the 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：The liquid crystal for mixing is filled into after liquid crystal cell, is covered on liquid crystal cell
Upper mask plate, is solidified using ultraviolet light.Photoetching process is too small due to the gap of mask plate, when ultraviolet light polymerization, it may appear that
Light leak, the liquid crystal of surrounding are also cured, and cannot so obtain the sufficiently small liquid crystal particle of size.
Based on above reason, polishing, laser ablation method and photoetching process prepare liquid crystal particle and are difficult to be widely used in system
Make in electroresponse infrared external reflection device.
The content of the invention
The technical problem to be solved is to provide a kind of preparation method 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, comprises the following steps：Will be infrared external reflection liquid crystal polymer thin
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.
Such scheme preferred embodiment in, the solution be saturated aqueous common salt.
In some specific embodiments, also include sifting out not using different size screen cloth after the Ultrasonic Pulverization process
With the process of the liquid crystal polymer particle of size.
In some specific embodiments, ultrasonic power is 100-150W, and 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, Jing ultraviolet light polymerizations, heat cure, the infrared external reflection liquid crystal polymer film for obtaining.
In some specific embodiments, the reflected waveband of the infrared external reflection liquid crystal polymer film is 700-
1100nm。
The invention has the beneficial effects as follows：
All it is difficult to be widely used in make electroresponse infrared for currently used polishing, laser ablation method and photoetching process
Problem in reflection device, the invention provides a kind of preparation method of infrared external reflection liquid crystal polymer particle, including following step
Suddenly：Infrared external reflection liquid crystal polymer film is placed in solution, the density of the solution and the infrared external reflection liquid crystal polymer
Thin film is close, ultrasonication, crushes liquid crystal polymer film using ultrasound wave, can obtain the liquid crystal of 150 μm of length of side ＜
A kind of polymer particle, the solution being close to infrared external reflection liquid crystal polymer film density using density, can effectively prevent thin
Film sinks to bottom when broken or floats on top, affects crushing effect.
Description of the drawings
Pictorial diagrams of the Fig. 1 for 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 of the infrared external reflection liquid crystal polymer particle for preparing；
Fig. 4 is the average side length of the liquid crystal polymer particle that embodiment 1, embodiment 2 and comparative example 1 are obtained.
Fig. 5 is the length of side variance of the liquid crystal polymer particle that embodiment 1, embodiment 2 and comparative example 1 are obtained.
Specific embodiment
Embodiment 1：
Mixed liquid crystal is filled in liquid crystal cell according to what infrared external reflection liquid crystal polymer film formula was prepared, Jing UV-curings
Change, heat cure, the infrared external reflection liquid crystal polymer film for obtaining, as shown in figure 1, its reflected waveband is 700-1100nm.Will
Infrared external reflection liquid crystal polymer film is scraped from device, with reference to Fig. 2, infrared external reflection liquid crystal polymer film 4 is placed in 40mL
In reagent bottle 2；Saturated aqueous common salt is equipped with, appropriate saturated aqueous common salt is added in reagent bottle 2；Reagent bottle 2 is placed in into 300mL burnings
In cup 3, appropriate mixture of ice and water is added in beaker 3, it is -2-5 DEG C to control the water temperature in sheet glass.Supersonic cell is broken
The probe 1 of broken instrument does not have supersaturation saline solution, it is impossible to touch bottom of bottle, by the power setting of sonicator in 120W, starts
Ultrasonic cell disruption instrument.After smashing 20min, the glass that liquid crystal polymer particle is placed in cleaning is drawn with dropper from reagent bottle 2
On glass piece, and polarized light microscope observing liquid crystal particle is used, its length and width are measured using Linksys32 softwares, record line number of going forward side by side
According to process.Infrared external reflection liquid crystal polymer film is repeated to crush six times according to above-mentioned condition, total grinding time 120min, finally
The infrared external reflection liquid crystal polymer particle for obtaining can cross 100 mesh sieves, i.e. 150 μm of length of side ＜, examine under a microscope and obtain red
External reflectance liquid crystal polymer particle is as shown in figure 3, the length of side distribution uniform of liquid crystal polymer particle as can see from Figure 3.
If necessary to length of side infrared external reflection liquid crystal polymer particle within the specific limits, such as want to screen the length of side in 30-
Infrared external reflection liquid crystal polymer particle in 100 μ ms, first by the saturated aqueous common salt containing liquid crystal particle with 30 μm of screen cloth
Sieve, the liquid crystal particle of 30 μm of length of side ＞ on screen cloth is placed in baking oven after sieve, 50 DEG C or so drying 30min, by screen cloth
Liquid crystal particle scrape, then the fragment of drying is placed in 100 μm of screen cloth and is sieved, you can obtain size in 30-100 μm of model
Infrared external reflection liquid crystal polymer particle in enclosing.
Embodiment 2：
The infrared external reflection liquid crystal polymer film prepared in embodiment 1 is placed in 40mL reagent bottle, is added in vial
Enter appropriate dichloromethane solution（DCM solution）；Vial is placed in 300mL beakers, appropriate frozen water is added in beaker
Mixture, it is -2-5 DEG C to control the water temperature in sheet glass.The probe of ultrasonic cell disruption instrument is not had into supersaturation saline solution, it is impossible to
Bottom of bottle is touched, by the power setting of sonicator in 120W, starts ultrasonic cell disruption instrument.According to embodiment 1
Infrared external reflection liquid crystal polymer film is crushed with identical step.
Embodiment 3：
Ultrasonic Pulverization is carried out according to method same as Example 1, by the power setting of sonicator in 150W, is started super
Sound wave cell crushing instrument.20min being crushed every time, being carried out 4 times, total grinding time 80min, the infrared external reflection liquid crystal for finally obtaining gathers
Polymer particle can cross 100 mesh sieves, i.e. 150 μm of length of side ＜, and the length of side of liquid crystal polymer particle is evenly distributed.
Embodiment 4：
Ultrasonic Pulverization is carried out according to method same as Example 1, by the power setting of sonicator in 100W, is started super
Sound wave cell crushing instrument.20min is crushed every time, is carried out 8 times, total grinding time 160min, the infrared external reflection liquid crystal for finally obtaining
Polymer particle can cross 100 mesh sieves, i.e. 150 μm of length of side ＜, and the length of side of liquid crystal polymer particle is evenly distributed.
Comparative example 1：
The infrared external reflection liquid crystal polymer film prepared in embodiment 1 is placed in 40mL reagent bottle；Add in reagent bottle
Enter appropriate deionized water；Reagent bottle is placed in 300mL beakers, appropriate mixture of ice and water is added in beaker, control glass
Water temperature in glass piece is -2-5 DEG C.The probe 1 of ultrasonic cell disruption instrument is not had into supersaturation saline solution, it is impossible to touch bottom of bottle,
By the power setting of sonicator in 120W, start ultrasonic cell disruption instrument.According to embodiment 1 and identical step
Infrared external reflection liquid crystal polymer film is crushed.
Respectively using polarizing microscope to embodiment 1, embodiment 2, the broken infrared external reflection polymerizable mesogenic for obtaining of comparative example 1
Thing particle is observed, and chooses 20 pieces of fragments under field of microscope, measures its length and wide, record with Linksys32 softwares
And data processing is carried out, and obtaining experimental result as shown in Figure 4 and Figure 5, Fig. 4 is what embodiment 1, embodiment 2 and comparative example 1 were 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 are obtained
Embodiment 1 is respectively illustrated in length of side variance, Fig. 4 and Fig. 5（Infrared external reflection liquid crystal polymer film is placed in saturated aqueous common salt
It is damaged）, embodiment 4（Infrared external reflection liquid crystal polymer film is placed in DCM solution and is crushed）With comparative example 1（By infrared external reflection
Liquid crystal polymer film is placed in deionized water and crushes）The liquid crystal polymer particle that each Ultrasonic Pulverization of six Ultrasonic Pulverization is obtained
Average side length and length of side variance, as seen from the figure, carry out ultrasound using liquid crystal polymer film is put in deionized water
Crush, the average side length of the liquid crystal polymer particle for obtaining crushes what is obtained slightly larger than being put in saturated aqueous common salt and DCM solution,
But it is seen from fig 5 that the variance that the ion for obtaining is crushed in deionized water is more than it is put in saturated aqueous common salt and DCM solution
What crushing was obtained, illustrate that the length of side distribution consistency degree for crushing the particle for obtaining is poor, actual demand in practical application, cannot be met.
Claims (9)
1. a kind of preparation method of infrared external reflection liquid crystal polymer particle, it is characterised in that comprise 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 crushed.
2. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that the solution
For saline solution or dichloromethane solution.
3. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that the solution
For saturated aqueous common salt.
4. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that the ultrasound
Also include the process that various sizes of liquid crystal polymer particle is sifted out using different size screen cloth after crushing process.
5. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that ultrasound wave work(
Rate is 100-150W, and the total grinding time of ultrasound is 80-160min.
6. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that crushing process
Solution temperature is -2-5 DEG C.
7. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that the ultrasound
Shattering process can be multiple shattering process.
8. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that described infrared
Reflective liquid crystal thin polymer film is that mixed liquid crystal is filled in liquid crystal cell, Jing ultraviolet light polymerizations, heat cure, and what is obtained is infrared anti-
Penetrate liquid crystal polymer film.
9. the preparation method of infrared external reflection liquid crystal polymer particle according to claim 1, it is characterised in that described infrared
The reflected waveband of reflective liquid crystal thin polymer film is 700-1100nm.
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| CN201610907119.6A CN106564129B (en) | 2016-10-18 | 2016-10-18 | A kind of preparation method of infrared external reflection liquid crystal polymer particle |
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Citations (4)
| 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 |
| US20160215103A1 (en) * | 2013-09-27 | 2016-07-28 | Tufts University | Synthesis of silk fibroin micro- and submicron spheres using a co-flow method |
-
2016
- 2016-10-18 CN CN201610907119.6A patent/CN106564129B/en active Active
Patent Citations (4)
| 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 |
| US20160215103A1 (en) * | 2013-09-27 | 2016-07-28 | Tufts University | Synthesis of silk fibroin micro- and submicron spheres using a co-flow method |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李凤生: "《超细粉体技术》", 31 July 2000, 国防工业出版社 * |
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