CN106751895A - The preparation method of titania modified Polymethyl methacrylate composite - Google Patents
The preparation method of titania modified Polymethyl methacrylate composite Download PDFInfo
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- CN106751895A CN106751895A CN201611107029.5A CN201611107029A CN106751895A CN 106751895 A CN106751895 A CN 106751895A CN 201611107029 A CN201611107029 A CN 201611107029A CN 106751895 A CN106751895 A CN 106751895A
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- polymethyl methacrylate
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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Abstract
The invention discloses a kind of preparation method of titania modified Polymethyl methacrylate composite, belong to modified composite material field.The method is comprised the following steps：(1) titanium dioxide is dried under vacuum；(2) by titanium dioxide, quaternary ammonium salt, kaolin and Polymethyl methacrylate, banburying mixes in banbury, obtains elastomeric compound；(3) elastomeric compound is dried at normal temperatures, by 1:3~5 mass ratio mixes elastomeric compound and benzoyl peroxide banburying；(4) vulcanize in vulcanizing press.There is stronger fracture strength and larger elongation through titania modified Polymethyl methacrylate composite, because titanium dioxide increased the crosslink density of network after vulcanization, macro manifestations are improved for the mechanical property of Polymethyl methacrylate, in addition the quaternary ammonium salt and titanium dioxide in the present invention can cooperate with the fracture strength of enhancing composite, and keep elongation to be substantially unaffected.
Description
Technical field
The invention belongs to modified composite material field, more particularly to a kind of titania modified Polymethyl methacrylate
The preparation method of composite.
Background technology
Composite, is by two or more material of different nature, by method physically or chemically, in macroscopic view
Material of the composition with new capability on (microcosmic).Various materials make up for each other's deficiencies and learn from each other in performance, produce cooperative effect, make to be combined
The combination property of material is better than former composition material and meets a variety of requirements.The matrix material of composite be divided into metal and
Nonmetallic two major class.What metallic matrix was commonly used has aluminium, magnesium, copper, titanium and its alloy.Nonmetal basal body mainly has synthetic resin, rubber
Glue, ceramics, graphite, carbon etc..Reinforcing material mainly has glass fibre, carbon fiber, boron fibre, aramid fiber, silicon carbide fibre, stone
Cotton fiber, whisker, wire and hard particulates etc..
The Chinese patent application of Application No. CN201410058549.6 discloses a kind of preparation of graphene composite material
Method, including：Graphite oxide ultrasonic disperse is obtained the dispersion liquid of graphene oxide in distilled water；By the ball after surface modification
Shape copper powder is configured to the dispersion liquid of spherical copper powder；The dispersion liquid of the dispersion liquid of spherical copper powder and graphene oxide is fully mixed,
The dispersion liquid of graphene oxide composite material is obtained, liquid-phase reduction causes that graphene oxide is reduced into Graphene, obtains graphite
Alkene composite, wherein, the graphene oxide coats the spherical copper powder.Relative to traditional use chemical vapour deposition technique
The method for preparing graphene coated spherical copper powder, the preparation method of this graphene composite material does not need special equipment, thus
Production cost is relatively low.
The content of the invention
The present invention is in order to solve the problems, such as prior art Polymethyl methacrylate easy fracture, there is provided a kind of titanium dioxide
The preparation method of the modified Polymethyl methacrylate composite of titanium, is strengthened by the collaboration of titanium dioxide and quaternary ammonium salt and made
With realizing Polymethyl methacrylate while having the toughness of silicon rubber and stronger fracture.
In order to solve the above-mentioned technical problem, the present invention uses following technical scheme：
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by titanium dioxide under vacuum in 60~70 DEG C of drying, drying time is 60~120min；
(2) by 10~20 parts of titanium dioxide, 60~80 parts of quaternary ammonium salts, 1~10 part of kaolin and 300~450 parts of poly- methyl
Vinylsiloxane banburying mixing in banbury, mixing temperature is 95~100 DEG C, and mixing time is 20~30min, rotating speed 60
~70r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 50~70h at normal temperatures, by 1:3~5 mass ratio is by elastomeric compound and benzoyl peroxide
Banburying mixes, and mixing temperature is 30~40 DEG C, and mixing time is 50~60min, 120~150r/min of rotating speed；
(4) vulcanize in vulcanizing press.
Preferably, the contents of ethylene of Polymethyl methacrylate is 0.16%.
Preferably, the quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride or double dodecyl dimethyl ammonium chlorides
In one or two.
Preferably, the curing temperature of step (4) is 110 DEG C, cure time is 23min, and pressure is 20MPa.
Preferably, step (1) drying temperature is 65 DEG C, drying time is 100min.
Preferably, in step (2) each raw material by weight, 15 parts of titanium dioxide, 70 parts of quaternary ammonium salts, 5.5 parts of kaolinites
Soil and 325 parts of Polymethyl methacrylates.
Preferably, step (2) mixing temperature is 97.5 DEG C, mixing time is 25min.
Preferably, the rotating speed of step (2) banbury is 65r/min.
Preferably, drying 60h under step (3) elastomeric compound normal temperature.
Preferably, the mass ratio of step (3) elastomeric compound and benzoyl peroxide is 1:4.
The invention has the advantages that：Have through titania modified Polymethyl methacrylate composite
Stronger fracture strength and larger elongation, because titanium dioxide increased the crosslink density of network after vulcanization, cause
Chain entropy declines in Polymethyl methacrylate, and macro manifestations are improved for the mechanical property of Polymethyl methacrylate, in addition
Quaternary ammonium salt and titanium dioxide in the present invention can cooperate with the fracture strength of enhancing composite, and keep elongation not receive substantially
Influence.
Specific embodiment
The present invention is further described in detail with reference to specific embodiment.
Embodiment 1
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by titanium dioxide under vacuum in 65 DEG C of drying, drying time is 90min；
(2) it is 15 parts of titanium dioxide, 70 parts of quaternary ammonium salts, 5.5 parts of kaolin and 325 parts of Polymethyl methacrylates are (poly-
The contents of ethylene of methyl vinyl silicone is 0.16%) the banburying mixing in banbury, and mixing temperature is 97.5 DEG C, banburying
Time is 25min, rotating speed 65r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 60h at normal temperatures, by 1:4 mass ratio mixes elastomeric compound and benzoyl peroxide banburying
Close, mixing temperature is 35 DEG C, and mixing time is 55min, rotating speed 135r/min；
(4) vulcanize in vulcanizing press, curing temperature is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
The quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride and double dodecyl dimethyl ammonium chlorides.
Embodiment 2
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by titanium dioxide under vacuum in 60 DEG C of drying, drying time is 60min；
(2) by 10 parts of titanium dioxide, 60 parts of quaternary ammonium salts, 1 part of kaolin and 300 parts of Polymethyl methacrylates in banburying
Banburying mixing in machine, mixing temperature is 95 DEG C, and mixing time is 20min, rotating speed 60r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 50h at normal temperatures, by 1:3 mass ratio mixes elastomeric compound and benzoyl peroxide banburying
Close, mixing temperature is 30 DEG C, and mixing time is 50min, rotating speed 120r/min；
(4) vulcanize in vulcanizing press, curing temperature is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
The quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride.
Embodiment 3
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by titanium dioxide under vacuum in 70 DEG C of drying, drying time is 120min；
(2) by 20 parts of titanium dioxide, 80 parts of quaternary ammonium salts, 10 parts of kaolin and 450 parts of Polymethyl methacrylates close
Banburying mixing in mill, mixing temperature is 100 DEG C, and mixing time is 30min, rotating speed 70r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 70h at normal temperatures, by 1:5 mass ratio mixes elastomeric compound and benzoyl peroxide banburying
Close, mixing temperature is 40 DEG C, and mixing time is 60min, rotating speed 150r/min；
(4) vulcanize in vulcanizing press, curing temperature is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
The quaternary ammonium salt is double dodecyl dimethyl ammonium chloride kinds.
Embodiment 4
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by titanium dioxide under vacuum in 68 DEG C of drying, drying time is 80min；
(2) by 14 parts of titanium dioxide, 75 parts of quaternary ammonium salts, 6 parts of kaolin and 380 parts of Polymethyl methacrylates in banburying
Banburying mixing in machine, mixing temperature is 94 DEG C, and mixing time is 26min, rotating speed 62r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 65h at normal temperatures, by 1:3 mass ratio mixes elastomeric compound and benzoyl peroxide banburying
Close, mixing temperature is 37 DEG C, and mixing time is 55min, rotating speed 136r/min；
(4) vulcanize in vulcanizing press, curing temperature is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
The quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride.
Reference examples 1
Difference with embodiment 1 is：It is not added with titanium dioxide.
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by 70 parts of quaternary ammonium salts, 5.5 parts of kaolin and 325 parts of Polymethyl methacrylate (poly- methyl ethylene silica
The contents of ethylene of alkane is 0.16%) the banburying mixing in banbury, and mixing temperature is 97.5 DEG C, and mixing time is 25min, is turned
Fast 65r/min, obtains elastomeric compound；
(2) elastomeric compound is dried into 60h at normal temperatures, by 1:4 mass ratio mixes elastomeric compound and benzoyl peroxide banburying
Close, mixing temperature is 35 DEG C, and mixing time is 55min, rotating speed 135r/min；
(3) vulcanize in vulcanizing press, curing temperature is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
The quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride and double dodecyl dimethyl ammonium chlorides.
Reference examples 2
Difference with embodiment 2 is：While quaternary ammonium salt and titanium dioxide in removal step (2).
The preparation method of titania modified Polymethyl methacrylate composite, comprises the following steps：
(1) by titanium dioxide under vacuum in 60 DEG C of drying, drying time is 60min；
(2) 1 part of kaolin and 300 parts of Polymethyl methacrylate banburyings in banbury are mixed, mixing temperature is
95 DEG C, mixing time is 20min, rotating speed 60r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 50h at normal temperatures, by 1:3 mass ratio mixes elastomeric compound and benzoyl peroxide banburying
Close, mixing temperature is 30 DEG C, and mixing time is 50min, rotating speed 120r/min；
(4) vulcanize in vulcanizing press, curing temperature is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
The quaternary ammonium salt is dodecyl benzyl dimethyl ammonium chloride.
Performance test：
As can be seen from the table, there is stronger breaking through titania modified Polymethyl methacrylate composite
Resistance to spalling and larger elongation, because titanium dioxide increased the crosslink density of network after vulcanization, cause poly- methyl second
Chain entropy declines in alkenyl siloxane, and macro manifestations are improved for the mechanical property of Polymethyl methacrylate, in addition in the present invention
Quaternary ammonium salt and titanium dioxide can cooperate with the fracture strength of enhancing composite, and keep elongation to be substantially unaffected.
The above, preferably specific embodiment only of the invention, protection scope of the present invention not limited to this are any ripe
Those skilled in the art are known in the technical scope of present disclosure, the letter of the technical scheme that can be become apparent to
Altered or equivalence replacement are each fallen within protection scope of the present invention.
Claims (10)
1. the preparation method of titania modified Polymethyl methacrylate composite, it is characterised in that including following step
Suddenly：
(1) by titanium dioxide under vacuum in 60~70 DEG C of drying, drying time is 60~120min；
(2) by 10~20 parts of titanium dioxide, 60~80 parts of quaternary ammonium salts, 1~10 part of kaolin and 300~450 parts of poly- ethylene methacrylics
Radical siloxane in banbury banburying mixing, mixing temperature be 95~100 DEG C, mixing time be 20~30min, rotating speed 60~
70r/min, obtains elastomeric compound；
(3) elastomeric compound is dried into 50~70h at normal temperatures, by 1:3~5 mass ratio is by elastomeric compound and benzoyl peroxide banburying
Mixing, mixing temperature is 30~40 DEG C, and mixing time is 50~60min, 120~150r/min of rotating speed；
(4) vulcanize in vulcanizing press.
2. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, the contents of ethylene of Polymethyl methacrylate is 0.16%.
3. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, the quaternary ammonium salt is the one kind in dodecyl benzyl dimethyl ammonium chloride or double dodecyl dimethyl ammonium chlorides
Or two kinds.
4. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, step (1) drying temperature is 65 DEG C, and drying time is 100min.
5. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
Be characterised by, in step (2) each raw material by weight, 15 parts of titanium dioxide, 70 parts of quaternary ammonium salts, 5.5 parts of kaolin and 325 parts
Polymethyl methacrylate.
6. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, step (2) mixing temperature is 97.5 DEG C, and mixing time is 25min.
7. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, the rotating speed of step (2) banbury is 65r/min.
8. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, 60h is dried under step (3) elastomeric compound normal temperature.
9. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, the mass ratio of step (3) elastomeric compound and benzoyl peroxide is 1:4.
10. the preparation method of titania modified Polymethyl methacrylate composite according to claim 1, its
It is characterised by, the curing temperature of step (4) is 110 DEG C, and cure time is 23min, and pressure is 20MPa.
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| CN201611107029.5A CN106751895A (en) | 2016-12-06 | 2016-12-06 | The preparation method of titania modified Polymethyl methacrylate composite |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101460560A (en) * | 2006-04-12 | 2009-06-17 | 蓝星有机硅法国公司 | Hot-vulcanizable polyorganosiloxane compositions useful particularly for manufacturing electrical cables or wires |
| CN104845378A (en) * | 2015-03-20 | 2015-08-19 | 国家电网公司 | Silicon rubber composition with high-voltage electric corrosion resistance for composite insulator and preparation method of silicon rubber composition |
| CN105694471A (en) * | 2016-04-17 | 2016-06-22 | 北京化工大学 | Preparation method of ceramizing fire-resistant silicon rubber |
-
2016
- 2016-12-06 CN CN201611107029.5A patent/CN106751895A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101460560A (en) * | 2006-04-12 | 2009-06-17 | 蓝星有机硅法国公司 | Hot-vulcanizable polyorganosiloxane compositions useful particularly for manufacturing electrical cables or wires |
| CN104845378A (en) * | 2015-03-20 | 2015-08-19 | 国家电网公司 | Silicon rubber composition with high-voltage electric corrosion resistance for composite insulator and preparation method of silicon rubber composition |
| CN105694471A (en) * | 2016-04-17 | 2016-06-22 | 北京化工大学 | Preparation method of ceramizing fire-resistant silicon rubber |
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