CN107236193A - A kind of preparation method of polymer microballoon modified polypropylene composite material - Google Patents
A kind of preparation method of polymer microballoon modified polypropylene composite material Download PDFInfo
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- CN107236193A CN107236193A CN201710606210.9A CN201710606210A CN107236193A CN 107236193 A CN107236193 A CN 107236193A CN 201710606210 A CN201710606210 A CN 201710606210A CN 107236193 A CN107236193 A CN 107236193A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/02—Alkylation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/18—Spheres
Abstract
The invention discloses a kind of preparation method of polymer microballoon modified polypropylene composite material, the poly methyl methacrylate polymer colloidal sol microballoon that the present invention passes through addition, weatherability, the heat insulating ability of finished-product material can effectively be improved, handled by colloidal sol, improve the surface strength and stability of microballoon.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation side of polymer microballoon modified polypropylene composite material
Method.
Background technology
The polymer that polypropylene is nontoxic, odorless, tasteless milky is highly crystalline, density only has 0.90-- " 0.91g/
Cm3, is one of kind most light in current all plastics.It is particularly stable to water, and the water absorption rate in water is only 0.01%, point
Son amount about 80,000 one 15 ten thousand.Good moldability, but because big (being 1%~2.5%) the thick articles of shrinkage factor are easily recessed, to some sizes
The higher part of precision, is difficult to reach requirement, product surface good luster.Polyacrylic crystallinity is high, compound with regular structure, thus has
Excellent mechanical property.The absolute value of Mechanical Properties of PP is higher than polyethylene, but still falls within relatively low product in a plastic material
Kind, its tensile strength only can reach 30MPa or slightly higher level.The larger polypropylene of isotactic index has higher stretching strong
Degree, but with the raising of isotactic index, the impact strength of material has declined, but no longer changes after dropping to a certain numerical value.
Temperature and loading speed are very big to polyacrylic Toughness.When temperature is higher than glass transition temperature, impact failure
In ductile rupture, significantly decline in brittle fracture, and impact value less than glass transition temperature.Loading speed is improved, can be made
The temperature that ductile rupture changes to brittle fracture rises.Polypropylene has excellent flexural fatigue resistance, and its product is at normal temperatures
Bent 106 times without damaging.
But under room temperature and low temperature, because the molecular structure regularity of itself is high, so impact strength is poor.Polypropylene
Most prominent performance is exactly counter-bending tired part, is commonly called as polypropylene (PP).Polypropylene has good heat resistance, and product can be at 100 DEG C
Temperatures above carries out disinfection sterilizing, and under conditions of not by external force, 150 DEG C also indeformable.Brittle temperature is one 35 DEG C, low
Embrittlement can occur in -35 DEG C, cold resistance is not so good as polyethylene.There is a 18qC, 0qC, 5 for the reported values of polypropylene glass temperature
DEG C etc., this is also due to people and uses various sample, and the ratio of crystalline phase and amorphous phase contained therein is different, makes nothing in strand
Caused by amorphous proportion chain length is different.Polyacrylic melting temperature about improves 40-50% than polyethylene, about 164-170 DEG C,
100% grade polypropylene fusing point is 176 DEG C.Polyacrylic chemical stability very well, by the concentrated sulfuric acid, concentrated nitric acid corroded by decapacitation
Outside, it is all more stable to other various chemical reagent, but aliphatic hydrocarbon, aromatic hydrocarbon and the chlorinated hydrocabon of low molecule amount etc. can make polypropylene
Soften and be swelled, while its chemical stability also increases with the increase of crystallinity, so polypropylene is adapted to make various
Chemical pipeline and accessory, the good of anticorrosion ability
Currently in order to further improving polyacrylic mechanical property, inorganic additive is often added wherein, but it is inorganic
The poor compatibility of additive and polymer, easily causes the defect of the stability difference of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of polymer microballoon modified polypropene
The preparation method of composite.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of polymer microballoon modified polypropylene composite material, comprises the following steps：
(1) butyl titanate of 10-14 parts by weight is taken, in the deionized water for being added to 20-30 times of its weight, stirring is equal
It is even, the castor oil acid of 1-2 parts by weight is added, stirs 10-20 minutes, obtains sol solution；
(2) methyl methacrylate, the casein mixing of 1-2 parts by weight of 13-20 parts by weight are taken, compound weight is added to
In the absolute ethyl alcohol of 3-5 times of amount, stir, be sent in reactor, be passed through nitrogen, add the peroxide of 0.1-0.2 parts by weight
Change diisopropylbenzene (DIPB), regulation temperature of reaction kettle is 70-80 DEG C, insulated and stirred 1-2 hours, discharging cooling obtains polymer microballoon；
(3) above-mentioned polymer microballoon is taken, adds in above-mentioned sol solution, stirs, the ammonia that concentration is 10-12% is added dropwise
Water, regulation pH is 10-11, and precipitation is washed, dried 1-2 hours at 90-100 DEG C of vacuum by stirring reaction 1-2 hours, filtering, cold
But to normal temperature, polymer sol microballoon is obtained；
(4) above-mentioned polymer sol microballoon is taken, is mixed with the tetramethyl disiloxane of 7-10 parts by weight, is added to compound
It is ultrasonic 3-5 minutes in the absolute ethyl alcohol of 3-5 times of weight, obtain alkylation polymer colloidal sol microballoon；
(5) abovementioned alkyl fluidized polymer colloidal sol microballoon, the stearic acid mixing of 1-2 parts by weight are taken, is sent in reactor, drips
Plus the acrylic acid of 10-12 parts by weight, the platinum dioxide of 0.1-0.3 parts by weight is added after completion of dropping, nitrogen is passed through, in 40-50
Insulation reaction 10-15 hours at DEG C, discharging is cooled to normal temperature, obtains organic siloxane polymer colloidal sol microballoon；
(6) above-mentioned organic siloxane polymer colloidal sol microballoon is taken, mixes, is added to the cross-linked disperse liquid of 2-3 parts by weight
In the deionized water of 2-4 times of compound weight, stir, add the polypropylene of 120-140 parts by weight, protected at 90-95 DEG C
Precipitation is washed in temperature stirring 1-2 hours, discharging, filtering, is dried completely at 60-70 DEG C of vacuum, is produced the polymer microballoon and change
Property PP composite material.
The preparation method of described cross-linked disperse liquid comprises the following steps：
The octamethylcy-clotetrasiloxane of 3-4 parts by weight is taken, in the polyvinylpyrrolidone for being added to 3-4 times of its weight, is stirred
Mix uniform, add calcium propionate, the terpinol of 2-3 parts by weight of 1-2 parts by weight, be sent in ptfe autoclave, raise
Temperature is 105-120 DEG C, sealing thermal insulation 30-40 minutes, discharging, and in the frozen water for being added to 1.7-2 times of compound weight, stirring is equal
It is even, produce.
Advantages of the present invention：
The present invention is blended by the colloidal sol after polymerization with butyl titanate formation, obtained using methyl methacrylate as monomer
To polymer sol microballoon, then handled by the ethanol solution of tetramethyl disiloxane, obtain alkylation polymer colloidal sol micro-
Ball, then mixes it with acrylic acid, passes through the catalytic action of platinum dioxide so that carbon-carbon double bond present in acrylic acid and four
The C=O bond of tetramethyldisiloxane could be formed with the conjugation of effect, while while conjugation reaction that colloidal sol is effectively organic
Change, improve the compatibility of each raw material, improve the stability_intensity of finished-product material；
The present invention can effectively improve finished-product material by the poly methyl methacrylate polymer colloidal sol microballoon of addition
Weatherability, heat insulating ability, handled by colloidal sol, improve the surface strength and stability of microballoon.
Embodiment
Embodiment 1
A kind of preparation method of polymer microballoon modified polypropylene composite material, comprises the following steps：
(1) butyl titanate of 10 parts by weight is taken, in the deionized water for being added to 20 times of its weight, is stirred, 1 is added
The castor oil acid of parts by weight, stirs 10 minutes, obtains sol solution；
(2) methyl methacrylate, the casein mixing of 1 parts by weight of 13 parts by weight are taken, 3 times of compound weight is added to
Absolute ethyl alcohol in, stir, be sent in reactor, be passed through nitrogen, add the cumyl peroxide of 0.1 parts by weight,
It is 70 DEG C to adjust temperature of reaction kettle, insulated and stirred 1 hour, discharging cooling, obtains polymer microballoon；
(3) above-mentioned polymer microballoon is taken, adds in above-mentioned sol solution, stirs, the ammoniacal liquor that concentration is 10% is added dropwise,
It is 10 to adjust pH, stirring reaction 1 hour, and precipitation is washed in filtering, is dried 1 hour at 90 DEG C of vacuum, is cooled to normal temperature, obtains poly-
Compound colloidal sol microballoon；
(4) above-mentioned polymer sol microballoon is taken, is mixed with the tetramethyl disiloxane of 7 parts by weight, compound weight is added to
In the absolute ethyl alcohol of 3 times of amount, ultrasound 3 minutes obtains alkylation polymer colloidal sol microballoon；
(5) abovementioned alkyl fluidized polymer colloidal sol microballoon, the stearic acid mixing of 1 parts by weight are taken, is sent in reactor, is added dropwise
The platinum dioxide of 0.1 parts by weight is added after the acrylic acid of 10 parts by weight, completion of dropping, nitrogen is passed through, the insulation reaction at 40 DEG C
10 hours, discharging was cooled to normal temperature, obtains organic siloxane polymer colloidal sol microballoon；
(6) above-mentioned organic siloxane polymer colloidal sol microballoon is taken, mixes, is added to mixed with the cross-linked disperse liquid of 2 parts by weight
In the deionized water for closing 2 times of weight of material, stir, add the polypropylene of 120 parts by weight, insulated and stirred 1 is small at 90-95 DEG C
When, discharge, precipitation is washed in filtering, it is dry complete at 60 DEG C of vacuum, produce the polymer microballoon modified polypropene composite wood
Material.
The preparation method of described cross-linked disperse liquid comprises the following steps：
The octamethylcy-clotetrasiloxane of 3 parts by weight is taken, in the polyvinylpyrrolidone for being added to 3 times of its weight, stirring is equal
It is even, calcium propionate, the terpinol of 2 parts by weight of 1 parts by weight are added, is sent in ptfe autoclave, rise temperature is 105
DEG C, sealing thermal insulation 30 minutes discharges, and in the frozen water for being added to 1.7 times of compound weight, stirs, produces.
Embodiment 2
(1) butyl titanate of 14 parts by weight is taken, in the deionized water for being added to 30 times of its weight, is stirred, 2 are added
The castor oil acid of parts by weight, stirs 20 minutes, obtains sol solution；
(2) methyl methacrylate, the casein mixing of 2 parts by weight of 20 parts by weight are taken, 5 times of compound weight is added to
Absolute ethyl alcohol in, stir, be sent in reactor, be passed through nitrogen, add the cumyl peroxide of 0.2 parts by weight,
It is 80 DEG C to adjust temperature of reaction kettle, insulated and stirred 2 hours, discharging cooling, obtains polymer microballoon；
(3) above-mentioned polymer microballoon is taken, adds in above-mentioned sol solution, stirs, the ammoniacal liquor that concentration is 12% is added dropwise,
It is 11 to adjust pH, stirring reaction 2 hours, and precipitation is washed in filtering, is dried 1-2 hours at 100 DEG C of vacuum, is cooled to normal temperature, obtains
Polymer sol microballoon；
(4) above-mentioned polymer sol microballoon is taken, is mixed with the tetramethyl disiloxane of 10 parts by weight, compound weight is added to
In the absolute ethyl alcohol of 5 times of amount, ultrasound 5 minutes obtains alkylation polymer colloidal sol microballoon；
(5) abovementioned alkyl fluidized polymer colloidal sol microballoon, the stearic acid mixing of 2 parts by weight are taken, is sent in reactor, is added dropwise
The platinum dioxide of 0.3 parts by weight is added after the acrylic acid of 12 parts by weight, completion of dropping, nitrogen is passed through, the insulation reaction at 50 DEG C
15 hours, discharging was cooled to normal temperature, obtains organic siloxane polymer colloidal sol microballoon；
(6) above-mentioned organic siloxane polymer colloidal sol microballoon is taken, mixes, is added to the cross-linked disperse liquid of 2-3 parts by weight
In the deionized water that 4 times of compound weight, stir, add the polypropylene of 140 parts by weight, insulated and stirred 2 is small at 95 DEG C
When, discharge, precipitation is washed in filtering, it is dry complete at 70 DEG C of vacuum, produce the polymer microballoon modified polypropene composite wood
Material.
The preparation method of described cross-linked disperse liquid comprises the following steps：
The octamethylcy-clotetrasiloxane of 4 parts by weight is taken, in the polyvinylpyrrolidone for being added to 4 times of its weight, stirring is equal
It is even, calcium propionate, the terpinol of 3 parts by weight of 2 parts by weight are added, is sent in ptfe autoclave, rise temperature is 120
DEG C, sealing thermal insulation 40 minutes discharges, and in the frozen water for being added to 2 times of compound weight, stirs, produces.
Performance test：
The tensile strength of conventional polypropylene material is that 91-98.4MPa, notch impact strength are 10-11.4KJ/m2；
The tensile strength of the composite of the present invention is that 100-106MPa, notch impact strength are 12.79-15.8KJ/m2。
As can be seen that the composite of the present invention has higher mechanical property.
Claims (2)
1. a kind of preparation method of polymer microballoon modified polypropylene composite material, it is characterised in that comprise the following steps：
(1) butyl titanate of 10-14 parts by weight is taken, in the deionized water for being added to 20-30 times of its weight, is stirred, plus
Enter the castor oil acid of 1-2 parts by weight, stir 10-20 minutes, obtain sol solution；
(2) methyl methacrylate, the casein mixing of 1-2 parts by weight of 13-20 parts by weight are taken, compound weight 3- is added to
In 5 times of absolute ethyl alcohol, stir, be sent in reactor, be passed through nitrogen, add the peroxidating two of 0.1-0.2 parts by weight
Isopropylbenzene, regulation temperature of reaction kettle is 70-80 DEG C, insulated and stirred 1-2 hours, discharging cooling, obtains polymer microballoon；
(3) above-mentioned polymer microballoon is taken, adds in above-mentioned sol solution, stirs, the ammoniacal liquor that concentration is 10-12% is added dropwise,
Regulation pH is 10-11, and precipitation is washed, dried 1-2 hours at 90-100 DEG C of vacuum by stirring reaction 1-2 hours, filtering, cooling
To normal temperature, polymer sol microballoon is obtained；
(4) above-mentioned polymer sol microballoon is taken, is mixed with the tetramethyl disiloxane of 7-10 parts by weight, compound weight is added to
It is ultrasonic 3-5 minutes in 3-5 times of absolute ethyl alcohol, obtain alkylation polymer colloidal sol microballoon；
(5) abovementioned alkyl fluidized polymer colloidal sol microballoon, the stearic acid mixing of 1-2 parts by weight are taken, is sent in reactor, is added dropwise
The platinum dioxide of 0.1-0.3 parts by weight is added after the acrylic acid of 10-12 parts by weight, completion of dropping, nitrogen is passed through, at 40-50 DEG C
Lower insulation reaction 10-15 hours, discharging, is cooled to normal temperature, obtains organic siloxane polymer colloidal sol microballoon；
(6) above-mentioned organic siloxane polymer colloidal sol microballoon is taken, is mixed with the cross-linked disperse liquid of 2-3 parts by weight, is added to mixing
In the deionized water for expecting 2-4 times of weight, stir, add the polypropylene of 120-140 parts by weight, be incubated and stir at 90-95 DEG C
Mix 1-2 hours, discharge, filtering is washed precipitating, it is dry complete at 60-70 DEG C of vacuum, produce the polymer microballoon and be modified and gather
Acrylic composite.
2. a kind of preparation method of polymer microballoon modified polypropylene composite material according to claim 1, its feature exists
In the preparation method of described cross-linked disperse liquid comprises the following steps：
The octamethylcy-clotetrasiloxane of 3-4 parts by weight is taken, in the polyvinylpyrrolidone for being added to 3-4 times of its weight, stirring is equal
It is even, calcium propionate, the terpinol of 2-3 parts by weight of 1-2 parts by weight are added, is sent in ptfe autoclave, temperature is raised
For 105-120 DEG C, sealing thermal insulation 30-40 minutes discharges, and in the frozen water for being added to 1.7-2 times of compound weight, stirs,
Produce.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987393A (en) * | 2017-12-25 | 2018-05-04 | 桐城市祥泰塑业有限公司 | A kind of Nano sol composite polypropylene plastic material and preparation method thereof |
-
2017
- 2017-07-24 CN CN201710606210.9A patent/CN107236193A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987393A (en) * | 2017-12-25 | 2018-05-04 | 桐城市祥泰塑业有限公司 | A kind of Nano sol composite polypropylene plastic material and preparation method thereof |
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