CN107841143A - A kind of method for strengthening silicon rubber using liquid crystal polymer fibrillation - Google Patents
A kind of method for strengthening silicon rubber using liquid crystal polymer fibrillation Download PDFInfo
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- CN107841143A CN107841143A CN201711137663.8A CN201711137663A CN107841143A CN 107841143 A CN107841143 A CN 107841143A CN 201711137663 A CN201711137663 A CN 201711137663A CN 107841143 A CN107841143 A CN 107841143A
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- silicon rubber
- liquid crystal
- crystal polymer
- composite material
- fibrillation
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- 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
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention belongs to silicon rubber reinforcement field, relates in particular to the method using liquid crystal polymer fibrillation enhancing silicon rubber.Composite material compositions are made up of heat vulcanized silicone rubber, white carbon, liquid crystal polymer, its preparation method：Composition stock is first according to, is kneaded uniformly on banbury using melting heat mixing method, then vulcanized to obtain silicon rubber based composites.The present invention causes liquid crystal polymer fibrosis to form filamentary structure in process, play grappling effect, the mechanical property of silicon rubber based composites is improved, disclosure satisfy that following silicon rubber based composites take into account flame-retardance and thermal endurance and low-density, the demand for development of high intensity.
Description
Technical field
The invention belongs to reinforcing rubber field, relates in particular to a kind of using liquid crystal polymer fibrillation enhancing silicon rubber
Method.
Background technology
Silastic material is the important materials of Chinese national economy development, and only resident does not provide daily life and medical
Articles for use, and had a very wide range of applications in building, traffic, space flight, electronics and military affairs etc..In recent years, with China
The development of macroeconomic and the raising of scientific and technological level, traditional elastomeric material due to by the level of production and performance deficiency
Limitation, it has been difficult the needs for meeting modern social development.Silicon rubber has low residue, low cigarette and low signature, excellent
The features such as weatherability, flushing resistance.Compared to other silicon rubber use temperature ranges be in general purpose rubber it is most wide, silicon rubber can
To be blended at relatively high temperatures with filler, the demand of different processing technologys is adapted to.But mechanical property after pure silicon rubber
Can not be high, so body silicon rubber can only use proper method to improve its performance using it as matrix.
Liquid crystal high polymer material higher molecular weight and the orderly combination of liquid crystal cause liquid crystal high polymer material to have one
A little excellent characteristics.For example, high intensity and modulus, the thermal coefficient of expansion of very little etc..Further, since liquid crystal high polymer material has
Preferable rheological properties, the superior fiber of high intensity, high-modulus, combination property is obtained by appropriate high temperature process method.
The liquid crystal high polymer material of fibrosis directly serves grappling effect in silicon rubber based composites, to ensureing that silicon rubber is compound
Material mechanical performance has played key effect.
The content of the invention
The problem of existing for prior art, it is an object of the invention to provide a kind of liquid crystal polymer fibrillation to strengthen silicon
The method of rubber, it is therefore an objective to so that liquid crystal high polymer material can form threadiness during melting heat is mixed in composite
Structure, grappling effect is played, so as to reach reinforcing material mechanical property, can meet that following silicon rubber based composites are simultaneous
Care for flame-retardance and thermal endurance and low-density, the demand for development of high intensity.
The technical scheme is that：
A kind of liquid crystal polymer fibrillation strengthens silicon rubber composite material, and composite material compositions are by silicon rubber, white carbon, liquid
Polycrystalline macromolecule forms, and specific mass fraction proportioning is：
Silicon rubber：100 parts；
White carbon：20~40 parts；
Liquid crystal polymer：5~30 parts；
Follow the steps below：
(1) dispensing is carried out according to the composite material compositions；
(2) silicon rubber is plasticated in two-roll mill first, is kneaded uniformly with white carbon after forming homogeneous bag roller,
Obtain mixture；Melting heat is carried out with liquid crystal polymer in banbury to mix, 230~270 DEG C of melting temperature, obtain being kneaded silicon again
Rubber；
(3) melting silicone rubber is stood into 16~48h in 20~30 DEG C of temperature environments, then carries out mill on a mill,
Add vulcanizing agent, 20~50 DEG C of temperature, be kneaded using the general vulcanizing agent of silicon rubber and melting silicone rubber it is uniform, thin logical 20 times with
On reach slice after uniform state；
(4) material is placed in mould, one step cure is carried out using vulcanizing press；Curing temperature is 160~180 DEG C,
Time is 10~40min, and pressure is 10~20MPa, obtains moulding material；
(5) moulding material is subjected to post vulcanization in electric drying oven with forced convection, curing temperature is 190~250 DEG C, the time
For 2~8h, the silicon rubber base heat insulation composite material of resistance to ablation is obtained.
The present invention design philosophy be：
(1) silicon rubber composite material heat resistance and mechanical property are two aspects of a problem, and the two is connected each other
Mutually restrict again, the filler that selection has two kinds of performances of raising concurrently is the study hotspot for strengthening silicon rubber composite material, and annex solution
Polycrystalline macromolecule is one of important channel for strengthening silicon rubber performance.The material not only has prominent heat resistance, but also has
High intensity and modulus, the thermal coefficient of expansion of very little, so mechanical property reinforcement can be carried out to silastic material, there is obvious skill
Art is advanced.
(2) liquid crystal high polymer material in silicone rubber matrix material, its (230~270 DEG C) melt blending at high temperature is made,
Because liquid crystal high polymer material has preferable rheological properties, fibre structure can be obtained in process engineering.The liquid of fibrosis
Polycrystalline macromolecule material directly serves grappling effect in silicon rubber based composites, to ensureing silicon rubber composite material mechanical property
Key effect can have been played.
Compared with prior art, the features of the present invention and beneficial effect are：
The present invention adds liquid crystal high polymer material in silicon rubber so that Mechanical Properties of Silicone Rubber is enhanced.Compared to adding
Add other kinds of reinforcing material, liquid crystal polymer density is low, intensity is high, modulus is big, thermal coefficient of expansion is low, combination property is excellent
More, the synthesis that reinforcement and grappling are played with regard to filamentary structure can be formed directly is mixed with silicon rubber melting heat in whole process
Effect so that processing and forming technology difficulty substantially reduces simultaneously for performance enhancement.It is molded after institute's product tensile strength 1.5~
10MPa, elongation at break are 150~500%, can meet that following silicon rubber based composites take into account flame-retardance and thermal endurance and low close
Degree, the demand for development of high intensity.
Brief description of the drawings
Fig. 1 is SEM figure of the silicon rubber base heat insulation composite material of resistance to ablation obtained in the embodiment of the present invention 1 through ablation experiments
Piece；
Fig. 2 is SEM figure of the silicon rubber base heat insulation composite material of resistance to ablation obtained in the embodiment of the present invention 2 through ablation experiments
Piece；
Embodiment
Technical scheme proposed by the present invention is further described with reference to embodiment, but not as to technical scheme
Limitation.
Stretching experiment is carried out in the embodiment of the present invention to composite and uses GB/T528-2009 standards, sample is that II type is mute
Bell type, rate of extension 500mm/min, take three sample averages.
Embodiment 1
The liquid crystal polymer fibrillation enhancing silicon rubber composite material of the present embodiment, its composition is by methyl vinyl silicone rubber
50 mass parts, the mass parts of methyl phenyl vinyl silicone rubber 50, the mass parts of fume colloidal silica 30, the mass parts of liquid crystal polymer 5,
Formed with the mass parts of cumyl peroxide 2, its moulded products tensile strength is 2.40MPa, and elongation at break is
251.06%, SEM pictures are as shown in figure 1, it will be seen from figure 1 that liquid crystal polymer fibrillation enhancing silicon rubber composite material breaks
Fibre structure be present in breach surface.
The present embodiment liquid crystal polymer fibrillation strengthens the preparation method of silicon rubber composite material, enters according to following steps
OK：
(1) according to silicon rubber methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, fume colloidal silica, liquid crystal
Macromolecule and cumyl peroxide carry out dispensing；
(2) methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber are plasticated first, added after forming bag roller
Enter fume colloidal silica to be kneaded in two-roll mill uniformly, obtain mixture.Again by liquid crystal polymer together with mixture
Carry out melting heat in banbury to mix, melting temperature control is kneaded at 260 DEG C and uniformly keeps 20min, and mixture is cooled into room temperature
Obtain being kneaded uniform elastomeric compound；
(3) elastomeric compound is placed into 24h at room temperature, then carries out mill on a mill, addition vulcanizing agent peroxidating two is different
Propyl benzene, vulcanizing agent is set to be kneaded with elastomeric compound uniformly standby；
(4) material is placed in mould, one step cure is carried out using vulcanizing press.Curing temperature passes through certain temperature
After gradient, 30min is kept at 180 DEG C, pressure 15MPa, obtains moulding material；
(5) moulding material being subjected to post vulcanization in electric drying oven with forced convection, curing temperature is 240 DEG C, time 2h,
Obtain the silicon rubber base heat insulation composite material of resistance to ablation.
Embodiment 2
The liquid crystal polymer fibrillation enhancing silicon rubber composite material of the present embodiment, its composition is by methyl vinyl silicone rubber
50 mass parts, the mass parts of methyl phenyl vinyl silicone rubber 50, the mass parts of fume colloidal silica 25, the mass parts of liquid crystal polymer 10
Formed with the mass parts of cumyl peroxide 2, its moulded products tensile strength is 2.29MPa, elongation at break 218.92%.
The present embodiment liquid crystal polymer fibrillation strengthens the preparation method of silicon rubber composite material, enters according to following steps
OK：
(1) according to silicon rubber methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, fume colloidal silica, benzo
Oxazine resin, zirconium boride, carbon fiber and cumyl peroxide carry out dispensing；
(2) methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber are plasticated first, added after forming bag roller
Enter fume colloidal silica to be kneaded in two-roll mill uniformly, obtain mixture.Again by liquid crystal polymer together with mixture
Carry out melting heat in banbury to mix, melting temperature control is kneaded at 230 DEG C and uniformly keeps 20min, and mixture is cooled into room temperature
Obtain being kneaded uniform elastomeric compound；
(3) elastomeric compound is placed into 24h at room temperature, then carries out mill on a mill, addition vulcanizing agent peroxidating two is different
Propyl benzene, vulcanizing agent is set to be kneaded with elastomeric compound uniformly standby；
(4) material is placed in mould, one step cure is carried out using vulcanizing press.Curing temperature passes through certain temperature
After gradient, 30min is kept at 180 DEG C, pressure 15MPa, obtains moulding material；
(5) moulding material being subjected to post vulcanization in electric drying oven with forced convection, curing temperature is 240 DEG C, time 2h,
Obtain the silicon rubber base heat insulation composite material of resistance to ablation.
Embodiment 3
The liquid crystal polymer fibrillation enhancing silicon rubber composite material of the present embodiment, its composition is by methyl vinyl silicone rubber
50 mass parts, the mass parts of methyl phenyl vinyl silicone rubber 50, the mass parts of fume colloidal silica 25, the mass parts of liquid crystal polymer 15
Formed with the mass parts of cumyl peroxide 2, its moulded products tensile strength is 2.07MPa, elongation at break 205.89%.
The present embodiment liquid crystal polymer fibrillation strengthens the preparation method of silicon rubber composite material, enters according to following steps
OK：
(1) according to silicon rubber methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, fume colloidal silica, benzo
Oxazine resin, zirconium boride, carbon fiber and cumyl peroxide carry out dispensing；
(2) methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber are plasticated first, added after forming bag roller
Enter fume colloidal silica to be kneaded in two-roll mill uniformly, obtain mixture.Again by liquid crystal polymer together with mixture
Carry out melting heat in banbury to mix, melting temperature control is kneaded at 250 DEG C and uniformly keeps 20min, and mixture is cooled into room temperature
Obtain being kneaded uniform elastomeric compound；
(3) elastomeric compound is placed into 24h at room temperature, then carries out mill on a mill, addition vulcanizing agent peroxidating two is different
Propyl benzene, vulcanizing agent is set to be kneaded with elastomeric compound uniformly standby；
(4) material is placed in mould, one step cure is carried out using vulcanizing press.Curing temperature passes through certain temperature
After gradient, 30min is kept at 180 DEG C, pressure 15MPa, obtains moulding material；
(5) moulding material being subjected to post vulcanization in electric drying oven with forced convection, curing temperature is 240 DEG C, time 2h,
Obtain the silicon rubber base heat insulation composite material of resistance to ablation.
Embodiment result shows that the present invention improves the mechanical property of silicon rubber based composites, and liquid crystal polymer is molten
Melt the collective effect that reinforcement and grappling are served in blending process engineering, simplify process.Meet that following silicon rubber base is answered
Condensation material takes into account flame-retardance and thermal endurance and low-density, the demand for development of high intensity.
Claims (6)
1. a kind of liquid crystal polymer fibrillation strengthens silicon rubber composite material, it is characterised in that composite material compositions by silicon rubber,
White carbon, liquid crystal polymer composition, specific mass fraction proportioning are：
Silicon rubber：100 parts；
White carbon：20~40 parts；
Liquid crystal polymer：5~30 parts；
Its moulded products tensile strength is 1.5~10MPa, and elongation at break is 150~500%.
2. liquid crystal polymer fibrillation according to claim 1 strengthens silicon rubber composite material, it is characterised in that the silicon
Rubber is one or both of methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber.
3. liquid crystal polymer fibrillation according to claim 1 strengthens silicon rubber composite material, it is characterised in that described white
Carbon black is one or both of fume colloidal silica and precipitated silica.
4. liquid crystal polymer fibrillation according to claim 1 strengthens silicon rubber composite material, it is characterised in that the liquid
Polycrystalline macromolecule is polyterephthalamide class.
5. a kind of preparation method of liquid crystal polymer fibrillation enhancing silicon rubber composite material, it is characterised in that according to following step
It is rapid to carry out：
(1) dispensing is carried out according to composite material compositions；
(2) silicon rubber is plasticated in two-roll mill first, is kneaded uniformly, obtains with white carbon after forming homogeneous bag roller
Mixture；Then mixture is carried out into melting heat in banbury with liquid crystal polymer to mix, 230~270 DEG C of melting temperature, obtained
Melting silicone rubber；
(3) melting silicone rubber is stood into 16~48h in 20~30 DEG C of temperature environments, then carries out mill on a mill, add
Enter vulcanizing agent, 20~50 DEG C of temperature, be kneaded uniformly using the general vulcanizing agent of silicon rubber and melting silicone rubber, it is thin logical more than 20 times
Reach slice after uniform state；
(4) material is placed in mould, one step cure is carried out using vulcanizing press；Curing temperature is 160~180 DEG C, the time
For 10~40min, pressure is 10~20MPa, obtains moulding material；
(5) moulding material is subjected to post vulcanization in electric drying oven with forced convection, curing temperature is 190~250 DEG C, the time 2
~8h, obtain the silicon rubber base heat insulation composite material of resistance to ablation.
6. strengthen the preparation method of silicon rubber composite material, its feature according to the liquid crystal polymer fibrillation described in claim 5
It is：The general vulcanizing agent of described silicon rubber is one kind or two in cumyl peroxide, benzoyl peroxide and double 25
More than kind, vulcanizing agent is 0.5~5 mass parts.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711137663.8A CN107841143A (en) | 2017-11-16 | 2017-11-16 | A kind of method for strengthening silicon rubber using liquid crystal polymer fibrillation |
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| CN201711137663.8A CN107841143A (en) | 2017-11-16 | 2017-11-16 | A kind of method for strengthening silicon rubber using liquid crystal polymer fibrillation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054399A (en) * | 2018-09-21 | 2018-12-21 | 莆田市涵江华源电子有限公司 | A kind of heat-resisting melting silicone rubber and preparation method thereof |
| CN113214647A (en) * | 2021-06-04 | 2021-08-06 | 四川大学 | Liquid crystal modified flexible ablation-resistant material and preparation method thereof |
| CN113547656A (en) * | 2021-07-22 | 2021-10-26 | 安徽昊华环保科技有限公司 | Production method of corrosion-resistant rubber molded sieve plate |
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| JP2006249327A (en) * | 2005-03-11 | 2006-09-21 | Shin Etsu Chem Co Ltd | Curable silicone rubber composition and method for producing composite molded product of liquid crystal polymer with silicone rubber |
| CN102070905A (en) * | 2010-12-09 | 2011-05-25 | 平高集团有限公司 | Composite silicon rubber and preparation method thereof |
| CN103030889A (en) * | 2012-12-29 | 2013-04-10 | 重庆理工大学 | Liquid crystal polymer reinforced and toughened GFRPP composite and preparation method thereof |
| CN103756272A (en) * | 2014-01-02 | 2014-04-30 | 广东聚石化学股份有限公司 | High-performance TLCP (Thermotropic Liquid Crystal Polymer) fiber reinforced PBT (Polybutylece Terephthalate) composite material and preparation method thereof |
-
2017
- 2017-11-16 CN CN201711137663.8A patent/CN107841143A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006249327A (en) * | 2005-03-11 | 2006-09-21 | Shin Etsu Chem Co Ltd | Curable silicone rubber composition and method for producing composite molded product of liquid crystal polymer with silicone rubber |
| CN102070905A (en) * | 2010-12-09 | 2011-05-25 | 平高集团有限公司 | Composite silicon rubber and preparation method thereof |
| CN103030889A (en) * | 2012-12-29 | 2013-04-10 | 重庆理工大学 | Liquid crystal polymer reinforced and toughened GFRPP composite and preparation method thereof |
| CN103756272A (en) * | 2014-01-02 | 2014-04-30 | 广东聚石化学股份有限公司 | High-performance TLCP (Thermotropic Liquid Crystal Polymer) fiber reinforced PBT (Polybutylece Terephthalate) composite material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054399A (en) * | 2018-09-21 | 2018-12-21 | 莆田市涵江华源电子有限公司 | A kind of heat-resisting melting silicone rubber and preparation method thereof |
| CN113214647A (en) * | 2021-06-04 | 2021-08-06 | 四川大学 | Liquid crystal modified flexible ablation-resistant material and preparation method thereof |
| CN113547656A (en) * | 2021-07-22 | 2021-10-26 | 安徽昊华环保科技有限公司 | Production method of corrosion-resistant rubber molded sieve plate |
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Application publication date: 20180327 |