CN105462191B - A kind of liquid-crystal polyester resin compound and preparation method thereof - Google Patents
A kind of liquid-crystal polyester resin compound and preparation method thereof Download PDFInfo
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- CN105462191B CN105462191B CN201511017026.8A CN201511017026A CN105462191B CN 105462191 B CN105462191 B CN 105462191B CN 201511017026 A CN201511017026 A CN 201511017026A CN 105462191 B CN105462191 B CN 105462191B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
The present invention is applied to field of polymer composite material, there is provided a kind of liquid-crystal polyester resin compound and preparation method thereof.The liquid-crystal polyester resin compound, include the following component of following parts by weight：50 70 parts of liquid-crystal polyester resin；0.1 1.2 parts of stabilizer；First 5 40 parts of filler；Second 10 40 parts of filler.
Description
Technical field
The invention belongs to field of polymer composite material, more particularly to a kind of liquid-crystal polyester resin compound and its preparation side
Method.
Background technology
Flowed when liquid-crystal polyester resin (LCP) is due to excellent electrical insulating property, heat resistance, dimensional stability and melting
Property, the fields such as daily living article, electronics, electric, automobile, aerospace are can be widely applied to, can specifically be used as sports goods, printing
Circuit board, packaging for foodstuff, artificial satellite electronic unit, electric and automobile component raw material, even as spacecraft
Outside panel material.
Because LCP materials have the performances such as excellent heat resistance, dimensional stability and high mechanical properties, using LCP materials
The LED reflective mirrors for expecting to be prepared are hardly damaged, and are not susceptible to deform during long-term use, be disclosure satisfy that LED reflective mirrors
The demand of material, therewith, LED reflective mirrors turn into LCP important applied field.However, nevertheless, using LCP preparations
LED reflective mirrors still Shortcomings in use, are mainly reflected in：During long-term use or preservation-particularly
Under illumination and heating condition, aging occurs for LCP, causes LCP brightness to decline, so as to influence the reflectivity of LCP material reflective mirrors,
And then cause the Quality Down of LED reflective mirrors, limit further development of the LCP in LED reflective mirrors field.
The content of the invention
It is an object of the invention to provide a kind of liquid-crystal polyester resin compound, it is intended to solves existing liquid-crystal polyester resin
The LED reflective mirrors of preparation easily produce brightness and reflectivity and reduced, so as to causing LED reflective mirrors matter during use or preservation
The problem of amount declines.
Another object of the present invention is to provide a kind of preparation method of liquid-crystal polyester resin compound.
The present invention is achieved in that a kind of liquid-crystal polyester resin compound, includes the following component of following parts by weight：
Accordingly, a kind of preparation method of liquid-crystal polyester resin compound, comprises the following steps：
Formula according to above-mentioned liquid-crystal polyester resin compound weighs each component；
Processing is dried in the liquid-crystal polyester resin, the first filler, the second filler；
The liquid-crystal polyester resin after the stabilizer and drying process, the first filler, the second filler are mixed
Processing, obtains mixed material；
The mixed material is subjected to melting extrusion, tie rod, cooling, granulation processing.
Liquid-crystal polyester resin compound provided by the invention, the liquid-crystal polyester resin is improved by adding stabilizer and is answered
Compound prevents the aging of the liquid-crystal polyester resin compound, so as to avoid the liquid crystal polyester in the stability of light, heat condition
The brightness of resin complexes and the reduction of reflectivity；Meanwhile two kinds of fillers are added with the liquid-crystal polyester resin compound, can
On the basis of ensureing that the liquid-crystal polyester resin compound has excellent mechanical performance, further to improve liquid crystal polyester tree
The brightness of fat complexes and reflectivity.In addition, the liquid-crystal polyester resin compound has preferable processing characteristics.The present invention carries
The liquid-crystal polyester resin compound of confession, is applicable, but be not limited only to this especially suitable for LED mirror materials.
The preparation method of liquid-crystal polyester resin compound provided by the invention, only need to be by first by liquid-crystal polyester resin, first
After filler, the second filler are dried, then the mixture that liquid-crystal polyester resin, stabilizer, the first filler, the second filler are formed
Material carries out melting extrusion, is granulated i.e. available, the technical maturity, and method is simply controllable, it is easy to accomplish industrialization.
Embodiment
In order that technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining
The present invention, it is not intended to limit the present invention.
The embodiments of the invention provide a kind of liquid-crystal polyester resin compound, include the following component of following parts by weight：
Specifically, in the embodiment of the present invention, it is excellent to assign the compound as matrix composition for the liquid-crystal polyester resin
Heat resistance, dimensional stability and high-mechanical property.In the embodiment of the present invention, the liquid-crystal polyester resin can be all aromatic liquid
Brilliant polyester resin, further, the liquid-crystal polyester resin that number-average molecular weight is 1000-100000 can be selected.
Liquid-crystal polyester resin is polymerized by reaction monomers described in the embodiment of the present invention, specifically, the reaction monomers bag
Include but be not limited to free aromatic diol, at least one of aromatic diamine and aromatic series azanol and aromatic dicarboxylic acid.Enter
One step, on the basis of above-mentioned reaction monomers, the reaction monomers may also include aromatic hydroxy-carboxylic and aromatic series amino
At least one of carboxylic acid.More specifically, the liquid-crystal polyester resin contains at least one of following repeat units：
Repeat unit from aromatic diol：-O-Ar-O-；
Repeat unit from aromatic diamine：-HN-Ar-NH-；
Repeat unit from aromatic series azanol：-HN-Ar-O-；
Repeat unit from aromatic dicarboxylic acid：-OC-Ar-CO-；
Repeat unit from aromatic hydroxy-carboxylic：-O-Ar-CO-；
Repeat unit from aromatic amine yl carboxylic acid：-HN-Ar-CO-；
Wherein, the Ar be penylene and its derivative, biphenylene and its derivative, naphthalene and its derivative, two penylenes by
One kind in aromatic compound and its derivative that carbon or the element of non-carbon are bonded, the signified derivative of the embodiment of the present invention
Thing refers to the aromatic compound that the penylene, biphenylene, one or more hydrogen atoms on naphthalene are substituted by other elements.
As specific embodiment, the content of the liquid-crystal polyester resin is 50-70 parts, concretely 50 parts, 52 parts, 55
Part, 58 parts, 60 parts, 62 parts, 65 parts, 68 parts, the specific deals such as 70 parts.
In the embodiment of the present invention, the stabilizer is to be used to prevent the liquid-crystal polyester resin under light, heat condition occurring
Aging reaction, therefore, the stabilizer is preferably light stabilizer.Further, the light stabilizer preferably includes adjacent hydroxyl
In benzophenone, benzotriazole, salicylic acid esters, triazines, group-substituted acrylonitrile, hindered amine light stabilizer (HALS)
At least one.Further, the stabilizer is preferably Hostavin VSU stabilizers and Nylostab S-EED stable
Agent, wherein, the Nylostab S-EED stabilizers have light stability and thermal stability simultaneously.It is above-mentioned preferable stable
Agent can assign the liquid-crystal polyester resin, particularly all aromatic liquid crystal polyester resin excellent anti-light, heat aging performance, from
And its brightness and the reduction of reflectivity are avoided, the requirement of LED reflective mirrors high brightness and high reflectance can be met.As most
Good embodiment, the stabilizer are Hostavin VSU stabilizers and the production of Clariant companies of Clariant companies production
Nylostab S-EED stabilizers.
As a specific embodiment, the content of the stabilizer is 0.1-1.2 parts, concretely 0.1 part, 0.2 part,
0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1 part, 1.1 parts, the specific deals such as 1.2 parts.
In the embodiment of the present invention, in order to further improve the mechanical strength of the liquid-crystal polyester resin compound, and more preferably
Ground avoids the reduction of the liquid-crystal polyester resin compound reflecting rate and brightness, is added in the liquid-crystal polyester resin compound
Two kinds of filler components.As a preferred embodiment, first filler is glass fibre, whisker, polytetrafluoroethylene (PTFE), titanium dioxide
At least one of silicon, mica, for first filler as enhancing component, the machinery that can improve liquid-crystal polyester resin product is strong
Degree.As another preferred embodiment, second filler is titanium dioxide, zinc oxide, zinc barium, zinc sulphide, barium sulfate, talcum
At least one of powder, calcium carbonate, second filler can improve the liquid-crystal polyester resin compound as blast component
Reflecting rate, improve brightness.
As a specific embodiment, the content of first filler is 5-40 parts, concretely 5 parts, 10 parts, 15 parts,
20 parts, 25 parts, 30 parts, 35 parts, the specific deals such as 40 parts.As another specific embodiment, the content of second filler is
10-40 parts, concretely 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, the specific deals such as 40 parts.
It should be noted that in the embodiment of the present invention, the content of each addO-on therapy need to meet above-mentioned requirements, if content mistake
It is low, it is difficult to play its corresponding effect；If content is too high, can be added on the contrary in the case where the effect of its performance reaches saturation
Originally other performances can even, be influenceed, are unfavorable for the raising of the liquid-crystal polyester resin compound quality on the contrary.
Liquid-crystal polyester resin compound provided in an embodiment of the present invention, the liquid crystal is improved by adding two kinds of stabilizers
Polyester resin compound prevents the aging of the liquid-crystal polyester resin compound, so as to avoid in the stability of light, heat condition
State the brightness of liquid-crystal polyester resin compound and the reduction of reflectivity；Meanwhile it is added with the liquid-crystal polyester resin compound
Two kinds of fillers, the excellent mechanical performance of the liquid-crystal polyester resin compound can be both ensured, it is bright that and can further improves it
Degree and reflectivity.In addition, the liquid-crystal polyester resin compound has preferable processing characteristics.Liquid provided in an embodiment of the present invention
Brilliant polyester resin compound, is applicable especially suitable for LED mirror materials.
Liquid-crystal polyester resin compound described in the embodiment of the present invention can be prepared by following methods.
Accordingly, the embodiment of the present invention additionally provides a kind of preparation method of liquid-crystal polyester resin compound, including following
Step：
S01. each component is weighed according to the formula of above-mentioned liquid-crystal polyester resin compound；
S02. processing is dried in the liquid-crystal polyester resin, the first filler, the second filler；
S03. the liquid-crystal polyester resin after the stabilizer and drying process, the first filler, the second filler are carried out
Mixed processing, obtain mixed material；
S04. melting extrusion, tie rod, cooling, granulation after mixed material progress feeding are handled.
Specifically, in above-mentioned steps S01, the formula of the liquid-crystal polyester resin compound and its each preferable case, as above
Described in text, in order to save length, here is omitted.
As specific embodiment, the liquid-crystal polyester resin is prepared by following methods, specifically includes following steps：
S011., at least two reaction monomers are provided, polycondensation reaction is carried out and prepares liquid crystal polyester prepolyer；
S012. liquid-crystal polyester resin is prepared in liquid crystal polyester prepolymer progress solid phase polycondensation.
In above-mentioned steps S011, the reaction monomers are as described above.As being preferable to carry out, the polycondensation reaction is being carried out
Before, in addition to the reaction monomers are pre-processed using acylation agent.The reaction monomers can be improved by pretreatment
Reactivity, specifically, the acylation agent includes but is not limited to acetyl group agent, the acetyl group agent can will be described anti-
Answer monomer to carry out acetylation process, improve its reactivity.
The polycondensation reaction can use the conventional method in this area to realize, including but not limited to solution polycondensation, body
Condensation methods.
In above-mentioned steps S012, the solid state condensation reaction to above-mentioned liquid-crystal polyester resin prepolymer, it is necessary to be heated
Processing.But specific heating-up temperature, it is variant because of the selected reaction monomers, it can not limit in the lump herein.It is described
The methods of heating can be by heating plate, hot blast, high temperature fluid.In addition, in order to remove the accessory substance of solid state condensation reaction, can
Using inert gas purge or utilize vacuum removing.
In above-mentioned steps S02, in order to avoid water content is too high in the liquid-crystal polyester resin, the first filler, the second filler
The liquid-crystal polyester resin composite properties of preparation are adversely affected, it is necessary to by the liquid-crystal polyester resin, the first filler,
Processing is dried in two fillers.As the presently preferred embodiments, the temperature of the drying process is 130-160 DEG C, reaction time 3-5
Hour, more preferably 4 hours or so.
In above-mentioned steps S03, by the liquid-crystal polyester resin after the stabilizer and drying process, the first filler,
Two fillers carry out mixed processing, and the mixed processing can be realized by automatic blender, certainly, can also use other to realize
Mixed uniformly mode is realized.
The embodiment of the present invention carries out melting mixing using double screw extruder, is manufactured by extrusion, tie rod, cooling, granulation
Go out liquid-crystal polyester resin compound, the process conditions of melting extrusion processing are：Fused under 300-600RPM screw speed, spiral shell
Cylinder temperature is 320 DEG C -370 DEG C, and control vacuum is in 0.5MPa-0.8MPa.
The preparation method of liquid-crystal polyester resin compound provided in an embodiment of the present invention, only need to be by first by liquid crystal polyester tree
After fat, the first filler, the second filler are dried, then liquid-crystal polyester resin, stabilizer, the first filler, the second filler formed
Mixed material carry out melting extrusion, be granulated i.e. available, the technical maturity, and method is simply controllable, it is easy to accomplish industrialization.
Illustrated with reference to specific embodiment, it should be appreciated that following embodiments are that optimization formula component is formed
Technical scheme, be not intended to limit the present invention the range of choice for recipe ingredient.
Embodiment 1
A kind of liquid-crystal polyester resin compound, including each component as described in the embodiment 1 of table 1, wherein, liquid-crystal polyester resin
All aromatic liquid crystal polyester resin, stabilizer selected from the production of Jiangsu water special material Manufacturing Co., Ltd select Clariant
The composition of the Hostavin VSU stabilizers of company's production and the Nylostab S-EED stabilizers of Clariant companies production,
First filler is glass fibre, and the second filler is titanium dioxide.
The preparation method of the liquid-crystal polyester resin compound, comprises the steps：
S11. each component is weighed according to the formula of above-mentioned liquid-crystal polyester resin compound；
S12., the liquid-crystal polyester resin, the first filler, the second filler are dried to processing 4 hours at 130 DEG C；
S13. by the liquid-crystal polyester resin after the stabilizer and drying process, the first filler, the second filler certainly
Mixed processing is carried out in dynamic mixer, obtains mixed material；
S14. the mixed material is put into double screw extruder and carries out melting extrusion, tie rod, cooling, granulation processing.
Embodiment 2
A kind of liquid-crystal polyester resin compound, including each component as described in the embodiment 2 of table 1, wherein, liquid-crystal polyester resin
All aromatic liquid crystal polyester resin, stabilizer selected from the production of Jiangsu water special material Manufacturing Co., Ltd select Clariant
The composition of the Hostavin VSU stabilizers of company's production and the Nylostab S-EED stabilizers of Clariant companies production,
First filler is glass fibre, and the second filler is titanium dioxide.
The preparation method of the liquid-crystal polyester resin compound, described in embodiment 1.
Embodiment 3
A kind of liquid-crystal polyester resin compound, including each component as described in the embodiment 3 of table 1, wherein, liquid-crystal polyester resin
All aromatic liquid crystal polyester resin, stabilizer selected from the production of Jiangsu water special material Manufacturing Co., Ltd select Clariant
The composition of the Hostavin VSU stabilizers of company's production and the Nylostab S-EED stabilizers of Clariant companies production,
First filler is glass fibre, and the second filler is titanium dioxide.
The preparation method of the liquid-crystal polyester resin compound, described in embodiment 1.
Comparative example 1
A kind of liquid-crystal polyester resin compound, including each component as described in the comparative example 1 of table 1, wherein, liquid-crystal polyester resin
All aromatic liquid crystal polyester resin selected from the production of Jiangsu water special material Manufacturing Co., Ltd, the first filler is glass fibers
Dimension, the second filler is titanium dioxide.
The preparation method of the liquid-crystal polyester resin compound, described in embodiment 1.
Liquid-crystal polyester resin compound prepared by 1-3 of the embodiment of the present invention and comparative example 1 is as injection raw material, using note
Molding machine injection molding, then carries out performance test, and the method for performance test is as follows：
(1) tensile strength：Tested by ASTM D-638.
(2) melt viscosity：Using capillary rheometer (RH2000) under conditions of 330 DEG C and 1000/s obtained by measure
The melt viscosity of resin complexes.
(3) colour brightness is poor：The resin complexes of testing example 1 and the gained of comparative example 1 are distinguished using spectrophotometric color measurement instrument
Colour intensity value in ultraviolet accelerated aging test case before and after 80 DEG C of UV exposures 7 days, after calculating exposure brightness become
Change value is Δ L.
(4) reflectivity：Reflectivity of the gained compound under 460nm visible rays is tested using Albedometer, then
Compound is placed in 80 DEG C of baking ovens after 3 days same condition test its reflectivity again, is recorded in table 2 respectively.
Test result is as shown in table 2 below.
Table 1
Table 2
As shown in Table 2, all aromatic liquid crystal polyester resin compound manufactured in embodiment 1-3 and comparative example 1 all has
Excellent mechanical strength, melt viscosity is low and processing characteristics is good.But the color of the resin complexes manufactured in embodiment 1-3 is bright
Degree and reflectivity stability are obviously improved compared with the resin compounded manufactured in comparative example 1.As can be seen here, institute of the embodiment of the present invention
State stabilizer and can effectively solve the problem that the problem of liquid-crystal polyester resin compound brightness decline, reflecting rate reduce.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (7)
1. a kind of liquid-crystal polyester resin compound as LCP mirror materials, it is characterised in that including following parts by weight
Following component：
The stabilizer is light stabilizer, and the light stabilizer includes Hostavin VSU stabilizers and Nylostab S-EED are steady
Determine agent, first filler is at least one of glass fibre, whisker, polytetrafluoroethylene (PTFE), silica, mica；Described
Two fillers are titanium dioxide, zinc oxide, zinc barium, zinc sulphide, barium sulfate, talcum powder, calcium carbonate, at least one of barium sulfate.
2. it is used as the liquid-crystal polyester resin compound of LCP mirror materials as claimed in claim 1, it is characterised in that described
Liquid-crystal polyester resin is all aromatic liquid crystal polyester resin.
3. it is used as the liquid-crystal polyester resin compound of LCP mirror materials as claimed in claim 1 or 2, it is characterised in that institute
State liquid-crystal polyester resin to be polymerized by reaction monomers, the reaction monomers are free aromatic diol, aromatic diamine and virtue
At least one of fragrant race's azanol and aromatic dicarboxylic acid.
4. it is used as the liquid-crystal polyester resin compound of LCP mirror materials as claimed in claim 3, it is characterised in that described
Reaction monomers also include at least one of aromatic hydroxy-carboxylic and aromatic amine yl carboxylic acid.
5. it is used as the liquid-crystal polyester resin compound of LCP mirror materials as claimed in claim 1 or 2, it is characterised in that institute
State liquid-crystal polyester resin and contain at least one of following repeat units：
Repeat unit from aromatic diol：-O-Ar-O-；
Repeat unit from aromatic diamine：-HN-Ar-NH-；
Repeat unit from aromatic series azanol：-HN-Ar-O-；
Repeat unit from aromatic dicarboxylic acid：-OC-Ar-CO-；
Repeat unit from aromatic hydroxy-carboxylic：-O-Ar-CO-；
Repeat unit from aromatic amine yl carboxylic acid：-HN-Ar-CO-；
Wherein, the Ar be penylene and its derivative, biphenylene and its derivative, naphthalene and its derivative, two penylenes by carbon or
One kind in aromatic compound and its derivative that the element of non-carbon is bonded.
6. a kind of preparation method of the liquid-crystal polyester resin compound as LCP mirror materials, comprises the following steps：
Formula according to the liquid-crystal polyester resin compound for being used as LCP mirror materials as described in claim 1-5 is any weighs
Each component；
Processing is dried in the liquid-crystal polyester resin, the first filler, the second filler；
The liquid-crystal polyester resin after the stabilizer and drying process, the first filler, the second filler are subjected to mixed processing,
Obtain mixed material；
By the mixed material melting extrusion, tie rod, cooling, granulation processing.
7. the preparation method of the liquid-crystal polyester resin compound as LCP mirror materials as claimed in claim 6, its feature
It is, the liquid-crystal polyester resin is prepared by following methods, specifically includes following steps：
At least two reaction monomers are provided, polycondensation reaction is carried out and prepares liquid crystal polyester prepolyer；
Liquid-crystal polyester resin is prepared in liquid crystal polyester prepolymer progress solid phase polycondensation.
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| CN105733219A (en) * | 2016-04-13 | 2016-07-06 | 珠海万通特种工程塑料有限公司 | Liquid crystal polyester composition |
| CN106633859A (en) * | 2016-12-29 | 2017-05-10 | 江苏沃特特种材料制造有限公司 | Wholly aromatic liquid crystal polyester resin as well as preparation method and application thereof |
| WO2021117607A1 (en) * | 2019-12-11 | 2021-06-17 | 大塚化学株式会社 | Liquid crystal polymer composition, liquid crystal polymer molded body, and camera module |
| CN116426093A (en) * | 2020-06-09 | 2023-07-14 | 华为技术有限公司 | Plastic for antenna element |
| CN114773792A (en) * | 2022-04-21 | 2022-07-22 | 江苏沃特特种材料制造有限公司 | Voice coil motor inner wall track material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102649869A (en) * | 2011-02-28 | 2012-08-29 | 住友化学株式会社 | Liquid crystal polyester composition and process for producing the same |
| CN104725619A (en) * | 2013-12-19 | 2015-06-24 | 金发科技股份有限公司 | Liquid crystal polyester, liquid crystal polyester composition composed of liquid crystal polyester, and applications of liquid crystal polyester composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649869A (en) * | 2011-02-28 | 2012-08-29 | 住友化学株式会社 | Liquid crystal polyester composition and process for producing the same |
| CN104725619A (en) * | 2013-12-19 | 2015-06-24 | 金发科技股份有限公司 | Liquid crystal polyester, liquid crystal polyester composition composed of liquid crystal polyester, and applications of liquid crystal polyester composition |
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