CN106280015A - Polypropylene/kaolin composite material and preparation method thereof - Google Patents
Polypropylene/kaolin composite material and preparation method thereof Download PDFInfo
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- CN106280015A CN106280015A CN201610738027.XA CN201610738027A CN106280015A CN 106280015 A CN106280015 A CN 106280015A CN 201610738027 A CN201610738027 A CN 201610738027A CN 106280015 A CN106280015 A CN 106280015A
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- kaolin
- polypropylene
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- octadecylamine
- composite material
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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
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a kind of polypropylene/kaolin composite material and preparation method thereof, it includes 100 parts of polypropylene by weight, 5.5～20.0 parts of hydrophobically modified Kaolin, 0.2～2.0 part of heat stabilizer and 0.2～2.0 part of processing aid, this composite is by first using metal carboxylate modifying agent that Kaolin is carried out intercalation modifying, there is the modified kaolin of hydrophobic property the most again through octadecylamine modification preparation, finally by this hydrophobically modified Kaolin and polypropylene, heat stabilizer, processing aid melt blending prepares, and prepare the rigidity of the PP composite material of gained and heat resistance is all substantially improved.
Description
Technical field
The present invention relates to a kind of PP composite material and preparation method thereof, particularly relate to a kind of kaolinite containing intercalation modifying
Polypropylene/kaolin composite material of soil and preparation method thereof, belongs to polymer composite and forming processing technology field thereof.
Background technology
Polypropylene is a kind of most widely used general-purpose plastics.Compared with other general-purpose plastics, it has low cost, mechanics
The advantage such as function admirable, chemical resistance are good, insulating properties is good, transparency is high and water absorption rate is low, but there is also thermal deformation temperature simultaneously
Spend the shortcomings such as the highest and insufficient strength is preferable.For solving above-mentioned technical problem, mostly at polypropylene composite materials in currently available technology
Material adds the reinforcers such as various granulated filler and glass fibre to improve the heat distortion temperature of PP composite material
And the mechanical property of raising composite, in particular for improving its intensity etc..But above-mentioned Enhancement Method still can not obtain reason
The heat distortion temperature thought and higher intensity, the composite preparing gained can not be applied to some to material stiffness requirement relatively
High and that use ambient temperature is higher situation.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of polypropylene/Kaolin composite wood
Material and preparation method thereof, with the addition of the hydrophobically modified Kaolin through intercalation modifying in this composite, the composite of gained is strong
Spend high, heat-resist, and preparation method is simple to operation.
The present invention is to solve that its technical problem be the technical scheme is that
The invention discloses a kind of polypropylene/kaolin composite material, it includes following each component by weight:
Described hydrophobically modified Kaolin prepares gained by following step:
(1) it is 1.5～4.5:1 to mix homogeneously and obtain mixture in mass ratio with modifying agent by Kaolin, wherein modifying agent
For at least one in carboxylic acid sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is at room temperature joined in dehydrated alcohol stir so that it is be separated into uniform
Suspension slurry, is then centrifuged isolated solid matter by this suspension slurry；Wherein said mixture and dehydrated alcohol
Mass ratio is 1:2～4；
(3) it is that 1:2～4 joins dehydrated alcohol the most at room temperature by gained solid matter in (2) by solid-liquid mass ratio
In stir so that it is be separated into uniform suspension slurry, then gained suspension slurry be centrifuged isolated solids
Matter；After repeating this step 3～5 times, gained solid matter is dried, obtains modified kaolin；
(4) octadecylamine and ethanol are configured to mass percentage concentration be 3～7% the ethanol of octadecylamine molten
Liquid, then joins in the ethanol solution of this octadecylamine and uses the side of ultrasonic disperse by gained modified kaolin in (3)
Formula makes modified kaolin disperse uniformly wherein, and ultrasonic disperse passes through centrifugation and the step being dried after terminating, obtain hydrophobic
Modified kaolin；Wherein said modified kaolin is 1:3～5 with the mass ratio of the ethanol solution of octadecylamine.
Its further technical scheme is:
Described polypropylene be melt flow rate (MFR) be 1～100g/10min COPP and homogeneous polypropylene in extremely
Few one.
Described heat stabilizer is phenols, amine, phosphorous acid esters, half Hinered phenols, acryloyl group functional group and monothioester
Compound species and calixarene kind at least one.
Described processing aid is that low molecule esters, metal soap, stearic acid are combined at least one in esters and amide-type.
The mass percentage concentration of the ethanol solution of described octadecylamine is 5～6%.
The invention also discloses the preparation method of a kind of above-mentioned polypropylene/kaolin composite material, the method includes following
Step:
(1) it is 1.5～4.5:1 to mix homogeneously and obtain mixture in mass ratio with modifying agent by Kaolin, wherein modifying agent
For at least one in carboxylic acid sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is at room temperature joined in dehydrated alcohol stir so that it is be separated into uniform
Suspension slurry, is then centrifuged isolated solid matter by this suspension slurry；Wherein said mixture and dehydrated alcohol
Mass ratio is 1:2～4；
(3) it is that 1:2～4 joins dehydrated alcohol the most at room temperature by gained solid matter in (2) by solid-liquid mass ratio
In stir so that it is be separated into uniform suspension slurry, then gained suspension slurry be centrifuged isolated solids
Matter；After repeating this step 3～5 times, gained solid matter is dried, obtains modified kaolin；
(4) octadecylamine and ethanol are configured to mass percentage concentration be 3～7% the ethanol of octadecylamine molten
Liquid, then joins in the ethanol solution of this octadecylamine and uses the side of ultrasonic disperse by gained modified kaolin in (3)
Formula makes modified kaolin disperse uniformly wherein, and ultrasonic disperse passes through centrifugation and the step being dried after terminating, obtain hydrophobic
Modified kaolin；Wherein said modified kaolin is 1:3～5 with the mass ratio of the ethanol solution of octadecylamine；
(5) by the polypropylene of 100 weight portions, 5.5～20.0 gained hydrophobically modified Kaolin in weight portion (4), 0.2～
The processing aid of the heat stabilizer of 2.0 weight portions and 0.2～2.0 weight portions turns in high-speed mixer for dry mixing 3～5min, mixing
Speed is 600～800r/min, and mixing temperature is 23～25 DEG C, obtains pre-composition；It is 40～50 by this pre-composition in draw ratio again:
Melting mixing dispersion in the double screw extruder of 1, and extruding pelletization, obtain polypropylene/kaolin composite material；Wherein twin screw
The extruder temperature of extruder is 175～220 DEG C.
The method have the benefit that: by first using metal carboxylate modifying agent that Kaolin is inserted in the present invention
Layer is modified, has the modified kaolin of hydrophobic property the most again through octadecylamine modification preparation, finally that this hydrophobically modified is high
Ridge soil prepares polypropylene/kaolin composite material, wherein kaolinite with polypropylene, heat stabilizer, processing aid melt blending
Soil lamellar structure is modified the modified interlamellar spacing of agent and expands, then improves through the modified surface hydrophobic of octadecylamine, makes kaolinite
Native and the polyacrylic compatibility improves, and polypropylene molecular chain is easier to enter in Kaolin layer structure, makes Kaolin real
The dispersion of existing nano-scale, so that prepare the rigidity of the PP composite material of gained and heat resistance is substantially improved, can
It is applied to rigidity and heat resistance are required in higher plastic.
Detailed description of the invention
Below in conjunction with specific embodiment 1-4 and comparative example 1-3, the present invention is described in detail.
Raw material used in following specific embodiment and comparative example is as described below, but raw material used in this application
It is not limited to the concrete model of following disclosed raw material.
Polypropylene (PP): EP548R, melt flow rate (MFR) 30g/10min, weight average molecular weight 120,000.
Kaolin: particle diameter 15-25 μm, Yulin Pu Bai Kaolin company limited.
Modifying agent: 1-aminocyclobutane carboxylic acid salt, can be potassium salt, sodium salt or calcium salt.
Octadecylamine: octadecyl primary amine.
Heat stabilizer: dibutyltin oxide.
Processing aid: antioxidant 1010, irgasfos 168.
Polypropylene described in specific embodiment 1-4/Kaolin composite wood is carried out according to the preparation process of following preparation method
The preparation of material, this preparation method comprises the steps:
(1) by formula consumption described in table 1 Kaolin mixed homogeneously with modifying agent and obtain mixture；
(2) gained mixture in (1) is at room temperature joined in dehydrated alcohol stir so that it is be separated into uniform
Suspension slurry, is then centrifuged isolated solid matter by this suspension slurry；Wherein said mixture and dehydrated alcohol
Mass ratio is 1:2～4；
(3) it is that 1:2～4 joins dehydrated alcohol the most at room temperature by gained solid matter in (2) by solid-liquid mass ratio
In stir so that it is be separated into uniform suspension slurry, then gained suspension slurry be centrifuged isolated solids
Matter；After repeating this step 3～5 times, gained solid matter is dried, obtains modified kaolin；
(4) octadecylamine of formula consumption and ethanol are configured to mass percentage concentration be 3～7% (preferably 5～
6%) ethanol solution of octadecylamine, then joins the ethanol of this octadecylamine by gained modified kaolin in (3)
In solution and use the mode of ultrasonic disperse to make modified kaolin disperse uniformly wherein, ultrasonic disperse terminate after by centrifugal point
From with dry step, obtain hydrophobically modified Kaolin；
(5) formula consumption is pressed in table 1 by gained hydrophobically modified Kaolin, heat stabilizer and processing aid in polypropylene, (4)
In high-speed mixer for dry mixing 3～5min, mixing rotating speed is 600～800r/min, and mixing temperature is 23～25 DEG C, is premixed
Thing；Again by the melting mixing dispersion in the double screw extruder that draw ratio is 40～50:1 of this pre-composition, and extruding pelletization, obtain
Polypropylene/kaolin composite material；Wherein the extruder temperature of double screw extruder is 175～220 DEG C.
The preparation of polypropylene material described in comparative example 1, this system is carried out according to the preparation process of following preparation method
Preparation Method comprises the steps:
By formula consumption in table 1 by polypropylene, heat stabilizer and processing aid in high-speed mixer for dry mixing 3～5min,
Mixing rotating speed is 600～800r/min, and mixing temperature is 23～25 DEG C, obtains pre-composition；By this pre-composition in draw ratio it is again
Melting mixing dispersion in the double screw extruder of 40～50:1, and extruding pelletization, obtain polypropylene material；Wherein twin-screw extrusion
The extruder temperature of machine is 175～220 DEG C.
Polypropylene/kaolin composite material described in comparative example 2 is carried out according to the preparation process of following preparation method
Preparation, this preparation method comprises the steps:
By formula consumption in table 1 by polypropylene, Kaolin, heat stabilizer and processing aid in high-speed mixer for dry mixing 3
～5min, mixing rotating speed is 600～800r/min, and mixing temperature is 23～25 DEG C, obtains pre-composition；Again this pre-composition is being grown
Footpath than be 40～50:1 double screw extruder in melting mixing dispersion, and extruding pelletization, obtain polypropylene/Kaolin composite wood
Material；Wherein the extruder temperature of double screw extruder is 175～220 DEG C.
Polypropylene/kaolin composite material described in comparative example 3 is carried out according to the preparation process of following preparation method
Preparation, this preparation method comprises the steps:
(1) by formula consumption described in table 1 Kaolin mixed homogeneously with modifying agent and obtain mixture；
(2) gained mixture in (1) is at room temperature joined in dehydrated alcohol stir so that it is be separated into uniform
Suspension slurry, is then centrifuged isolated solid matter by this suspension slurry；Wherein said mixture and dehydrated alcohol
Mass ratio is 1:2～4；
(3) it is that 1:2～4 joins dehydrated alcohol the most at room temperature by gained solid matter in (2) by solid-liquid mass ratio
In stir so that it is be separated into uniform suspension slurry, then gained suspension slurry be centrifuged isolated solids
Matter；After repeating this step 3～5 times, gained solid matter is dried, obtains modified kaolin；
(4) formula consumption is pressed in table 1 by gained modified kaolin, heat stabilizer and processing aid in polypropylene, (3) at height
Being dry mixed 3～5min in speed mixer, mixing rotating speed is 600～800r/min, and mixing temperature is 23～25 DEG C, obtains pre-composition；
Again by the melting mixing dispersion in the double screw extruder that draw ratio is 40～50:1 of this pre-composition, and extruding pelletization, gathered
Propylene/kaolin composite material；Wherein the extruder temperature of double screw extruder is 175～220 DEG C.
Table 1 specific embodiment 1-4 and comparative example's 1-3 formula consumption (unit: kg)
The above-mentioned polypropylene material preparing gained and polypropylene/kaolin composite material are molded into the test of standard batten draw
Stretching intensity and heat distortion temperature, wherein the testing standard of hot strength is ISO 527-2, and draw speed is 50mm/min；Heat becomes
The testing standard of shape temperature is ISO 75-2, load 0.45MPa, and test result sees table 2.
Table 2 specific embodiment 1-4 and comparative example's 1-3 gained batten test result
By the comparison of above-mentioned comparative example and specific embodiment it can be seen that any kaolinic compared to being not added with
Polypropylene material, no matter whether add is modified kaolin or hydrophobically modified Kaolin, as long as with the addition of Kaolin, poly-
Heat distortion temperature and the hot strength of propylene material are improved, but effect inconspicuous；And only with the addition of unmodified Kaolin
PP composite material, its heat distortion temperature and hot strength are higher than virgin pp material but less than herein described composite wood
Material；Further, with the addition of and be only modified the Kaolin that agent is modified in polypropylene material, its heat distortion temperature and hot strength exist
A more excellent step on the basis of only with the addition of kaolinic PP composite material, but still with the addition of first warp not as good as described herein
Modifier modification is again through kaolinic thermostability and the hot strength of octadecylamine modification.
This is because Kaolin is a kind of inorganic laminated silicic acid containing aluminum being made up of silicon-oxy tetrahedron and alumina octahedral
Salt mineral, its interlayer has certain unsymmetric structure, and this stratiform provides containing the entrance that aluminosilicate structure is intercalator can
Can, intercalator can be replaced by follow-up monomer or polymer as presoma, and can be polymerized at phyllosilicate sheet interlayer, make
Sheet interlayer spacing expands so that peeling-off, and is dispersed in polymeric matrix, thus realizes poly-in the range of nanoscale
Compound and the intercalation synthesis of inorganic lamellar material.Polypropylene/kaolin composite material described herein and common polypropylene
Kaolin composite material is compared, the kaolinic addition of hydrophobically modified make PP composite material have higher hot strength and
Heat distortion temperature, its good mechanical properties, thermostability are high, it is possible to be applied to auto industry.
The foregoing is only the preferred embodiments of the present invention.It should be pointed out that, in the feelings without departing from the principle of the invention
Under condition, also can make some improvement and modification, be accordingly to be regarded as protection scope of the present invention.
Claims (6)
1. polypropylene/kaolin composite material, it is characterised in that: include following each component by weight:
Described hydrophobically modified Kaolin prepares gained by following step:
(1) being 1.5～4.5:1 to mix homogeneously and obtain mixture in mass ratio with modifying agent by Kaolin, wherein modifying agent is carboxylic
At least one in acid sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is at room temperature joined in dehydrated alcohol stir so that it is be separated into uniform suspension
Serosity, is then centrifuged isolated solid matter by this suspension slurry；Wherein said mixture and the quality of dehydrated alcohol
Ratio is 1:2～4；
(3) it is that 1:2～4 joins in dehydrated alcohol the most at room temperature and stirs by gained solid matter in (2) by solid-liquid mass ratio
Mix uniformly so that it is be separated into uniform suspension slurry, then gained suspension slurry be centrifuged isolated solid matter；Again
After repeating this step 3～5 times, gained solid matter is dried, obtains modified kaolin；
(4) octadecylamine and ethanol are configured to the ethanol solution of octadecylamine that mass percentage concentration is 3～7%, so
After gained modified kaolin in (3) joined in the ethanol solution of this octadecylamine and uses the mode of ultrasonic disperse to make to change
Property Kaolin disperse uniformly wherein, ultrasonic disperse terminate after by centrifugation and the step that is dried, obtain hydrophobically modified high
Ridge soil；Wherein said modified kaolin is 1:3～5 with the mass ratio of the ethanol solution of octadecylamine.
Polypropylene/kaolin composite material the most according to claim 1, it is characterised in that: described polypropylene is melt flow
Dynamic speed be 1～100g/10min COPP and homogeneous polypropylene at least one.
Polypropylene/kaolin composite material the most according to claim 1, it is characterised in that: described heat stabilizer be phenols,
In the compound species of amine, phosphorous acid esters, half Hinered phenols, acryloyl group functional group and monothioester and calixarene kind at least
A kind of.
Polypropylene/kaolin composite material the most according to claim 1, it is characterised in that: described processing aid is low point
Sub-esters, metal soap, stearic acid are combined at least one in esters and amide-type.
Polypropylene/kaolin composite material the most according to claim 1, it is characterised in that: the second of described octadecylamine
The mass percentage concentration of alcoholic solution is 5～6%.
6. a preparation method for polypropylene/kaolin composite material described in any claim in claim 1 to 5, its
It is characterised by: comprise the steps:
(1) being 1.5～4.5:1 to mix homogeneously and obtain mixture in mass ratio with modifying agent by Kaolin, wherein modifying agent is carboxylic
At least one in acid sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is at room temperature joined in dehydrated alcohol stir so that it is be separated into uniform suspension
Serosity, is then centrifuged isolated solid matter by this suspension slurry；Wherein said mixture and the quality of dehydrated alcohol
Ratio is 1:2～4；
(3) it is that 1:2～4 joins in dehydrated alcohol the most at room temperature and stirs by gained solid matter in (2) by solid-liquid mass ratio
Mix uniformly so that it is be separated into uniform suspension slurry, then gained suspension slurry be centrifuged isolated solid matter；Again
After repeating this step 3～5 times, gained solid matter is dried, obtains modified kaolin；
(4) octadecylamine and ethanol are configured to the ethanol solution of octadecylamine that mass percentage concentration is 3～7%, so
After gained modified kaolin in (3) joined in the ethanol solution of this octadecylamine and uses the mode of ultrasonic disperse to make to change
Property Kaolin disperse uniformly wherein, ultrasonic disperse terminate after by centrifugation and the step that is dried, obtain hydrophobically modified high
Ridge soil；Wherein said modified kaolin is 1:3～5 with the mass ratio of the ethanol solution of octadecylamine；
(5) by the polypropylene of 100 weight portions, 5.5～20.0 gained hydrophobically modified Kaolin in weight portion (4), 0.2～2.0 weights
The heat stabilizer of amount part and the processing aid of 0.2～2.0 weight portions at high-speed mixer for dry mixing 3～5min, mixing rotating speed are
600～800r/min, mixing temperature is 23～25 DEG C, obtains pre-composition；It is 40～50:1 by this pre-composition in draw ratio again
Melting mixing dispersion in double screw extruder, and extruding pelletization, obtain polypropylene/kaolin composite material；Wherein twin screw squeezes
The extruder temperature going out machine is 175～220 DEG C.
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| CN201610738027.XA CN106280015B (en) | 2016-08-26 | 2016-08-26 | Polypropylene/kaolin composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521685A (en) * | 2020-11-23 | 2021-03-19 | 江苏金发科技新材料有限公司 | Hydrophobic polyolefin composition and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885212A (en) * | 2014-12-09 | 2016-08-24 | 林建君 | Preparation method of modified kaolin reinforced polypropylene material |
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- 2016-08-26 CN CN201610738027.XA patent/CN106280015B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885212A (en) * | 2014-12-09 | 2016-08-24 | 林建君 | Preparation method of modified kaolin reinforced polypropylene material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521685A (en) * | 2020-11-23 | 2021-03-19 | 江苏金发科技新材料有限公司 | Hydrophobic polyolefin composition and preparation method thereof |
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