CN106280015B - Polypropylene/kaolin composite material and preparation method thereof - Google Patents
Polypropylene/kaolin composite material and preparation method thereof Download PDFInfo
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- CN106280015B CN106280015B CN201610738027.XA CN201610738027A CN106280015B CN 106280015 B CN106280015 B CN 106280015B CN 201610738027 A CN201610738027 A CN 201610738027A CN 106280015 B CN106280015 B CN 106280015B
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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
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Abstract
The invention discloses a kind of polypropylene/kaolin composite materials 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, the composite material is by first metal carboxylate modifying agent being used to carry out intercalation modifying to kaolin, then there is through the modified preparation of octadecylamine the modified kaolin of hydrophobic property again, finally by the hydrophobically modified kaolin and polypropylene, heat stabilizer, processing aid melt blending is prepared, and prepare the rigidity of resulting PP composite material and heat resistance is substantially improved.
Description
Technical field
The present invention relates to a kind of PP composite material and preparation method thereof more particularly to a kind of kaolinites containing intercalation modifying
Polypropylene/kaolin composite material and preparation method thereof of soil, belongs to polymer composite and its forming processing technology field.
Background technique
Polypropylene is a kind of most widely used general-purpose plastics.Compared with other general-purpose plastics, it has at low cost, mechanics
The advantages 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 disadvantages of not high and intensity is not ideal enough.In currently available technology in order to solve the above technical problems, mostly in polypropylene composite materials
The reinforcing fillers such as various granulated fillers and glass fibre are added in material to improve the heat distortion temperature of PP composite material
And the mechanical property of composite material is improved, in particular for improving its intensity etc..But above-mentioned Enhancement Method still cannot be managed
The heat distortion temperature and higher intensity thought, prepare resulting composite material can not be applied to some pairs of material stiffness require compared with
The high and higher situation of use environment temperature.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the present invention provides a kind of polypropylene/kaolin composite woods
Material and preparation method thereof, is added to the hydrophobically modified kaolin through intercalation modifying, resulting composite material is strong in the composite material
Degree is high, heat-resist, and preparation method is simple to operation.
The present invention is to solve technical solution used by its technical problem:
The invention discloses a kind of polypropylene/kaolin composite materials comprising following each components by weight:
The hydrophobically modified kaolin be prepared by following step it is resulting:
It (1) is in mass ratio that 1.5~4.5:1 is uniformly mixed to obtain mixture with modifying agent by kaolin, wherein modifying agent
For at least one of carboxylic acid sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is added at room temperature in dehydrated alcohol and is stirred evenly, be separated into it uniformly
Then suspension slurry is centrifuged the suspension slurry to obtain solid matter；The wherein mixture and dehydrated alcohol
Mass ratio is 1:2~4；
It (3) is that 1:2~4 are added to dehydrated alcohol at room temperature again by solid-liquid mass ratio by obtained solid substance in (2)
In stir evenly, so that it is separated into uniform suspension slurry, then be centrifuged gained suspension slurry to obtain solids
Matter；Obtained solid substance is dried after repeating the step 3~5 time, obtains modified kaolin；
(4) ethyl alcohol for octadecylamine and ethyl alcohol being configured to the octadecylamine that mass percentage concentration is 3~7% is molten
Gained modified kaolin in (3) is then added in the ethanol solution of the octadecylamine and using the side of ultrasonic disperse by liquid
Formula disperses modified kaolin uniformly wherein, by centrifuge separation and dry step after ultrasonic disperse, obtains hydrophobic
Modified kaolin；Wherein the mass ratio of the ethanol solution of the modified kaolin and octadecylamine is 1:3~5.
Its further technical solution is:
The polypropylene be melt flow rate (MFR) be in the copolymer polypropylene and homopolypropylene of 1~100g/10min extremely
Few one kind.
The heat stabilizer is phenols, amine, phosphorous acid esters, half Hinered phenols, acryloyl group functional group and monothioester
Compound species and at least one of calixarene kind.
The processing aid is at least one of low molecule esters, metal soap, the compound esters of stearic acid and amides.
The mass percentage concentration of the ethanol solution of the octadecylamine is 5~6%.
The invention also discloses a kind of preparation methods of above-mentioned polypropylene/kaolin composite material, and this method includes following
Step:
It (1) is in mass ratio that 1.5~4.5:1 is uniformly mixed to obtain mixture with modifying agent by kaolin, wherein modifying agent
For at least one of carboxylic acid sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is added at room temperature in dehydrated alcohol and is stirred evenly, be separated into it uniformly
Then suspension slurry is centrifuged the suspension slurry to obtain solid matter；The wherein mixture and dehydrated alcohol
Mass ratio is 1:2~4；
It (3) is that 1:2~4 are added to dehydrated alcohol at room temperature again by solid-liquid mass ratio by obtained solid substance in (2)
In stir evenly, so that it is separated into uniform suspension slurry, then be centrifuged gained suspension slurry to obtain solids
Matter；Obtained solid substance is dried after repeating the step 3~5 time, obtains modified kaolin；
(4) ethyl alcohol for octadecylamine and ethyl alcohol being configured to the octadecylamine that mass percentage concentration is 3~7% is molten
Gained modified kaolin in (3) is then added in the ethanol solution of the octadecylamine and using the side of ultrasonic disperse by liquid
Formula disperses modified kaolin uniformly wherein, by centrifuge separation and dry step after ultrasonic disperse, obtains hydrophobic
Modified kaolin；Wherein the mass ratio of the ethanol solution of the modified kaolin and octadecylamine is 1:3~5；
(5) by the polypropylene of 100 parts by weight, gained hydrophobically modified kaolin in 5.5~20.0 parts by weight (4), 0.2~
Dry-mixed 3~5min, mixing turn in a high speed mixer for the heat stabilizer of 2.0 parts by weight and the processing aid of 0.2~2.0 parts by weight
Speed is 600~800r/min, and mixing temperature is 23~25 DEG C, obtains pre-composition；It is again 40~50 in draw ratio by the pre-composition:
Melting mixing is dispersed in 1 double screw extruder, and extruding pelletization, obtains polypropylene/kaolin composite material；Wherein twin-screw
The extruder temperature of extruder is 175~220 DEG C.
The method have the benefit that: it is slotting by first using metal carboxylate modifying agent to carry out kaolin in the present invention
Layer is modified, then has the modified kaolin of hydrophobic property through the modified preparation of octadecylamine again, finally by hydrophobically modified height
Polypropylene/kaolin composite material is prepared in ridge soil and polypropylene, heat stabilizer, processing aid melt blending, wherein kaolinite
The modified interlamellar spacing of modified dose of native lamellar structure expands, then improves through the modified surface hydrophobic of octadecylamine, makes kaolinite
It is native to be improved with polyacrylic compatibility, and polypropylene molecular chain is easier to enter in kaolin layer structure, keeps kaolin real
The dispersion of existing nano-scale, so that prepare the rigidity of resulting PP composite material and heat resistance is substantially improved, it can
Applied in the plastic products more demanding to rigidity and heat resistance.
Specific embodiment
The present invention is described in detail by 1-4 and comparative example 1-3 combined with specific embodiments below.
Raw material used in following specific embodiments 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 materials.
Polypropylene (PP): EP548R, melt flow rate (MFR) 30g/10min, weight average molecular weight 120,000.
Kaolin: 15-25 μm of partial size, Yulin Pu white kaolinic Co., Ltd.
Modifying agent: 1-aminocyclobutane carboxylic acid salt can be sylvite, sodium salt or calcium salt.
Octadecylamine: octadecyl primary amine.
Heat stabilizer: dibutyltin oxide.
Processing aid: antioxidant 1010, irgasfos 168.
Polypropylene/kaolin composite wood described in specific embodiment 1-4 is carried out according to the preparation step of following preparation methods
The preparation of material, the preparation method include the following steps:
(1) kaolin is uniformly mixed to obtain mixture with modifying agent by formulation dosage described in table 1；
(2) gained mixture in (1) is added at room temperature in dehydrated alcohol and is stirred evenly, be separated into it uniformly
Then suspension slurry is centrifuged the suspension slurry to obtain solid matter；The wherein mixture and dehydrated alcohol
Mass ratio is 1:2~4；
It (3) is that 1:2~4 are added to dehydrated alcohol at room temperature again by solid-liquid mass ratio by obtained solid substance in (2)
In stir evenly, so that it is separated into uniform suspension slurry, then be centrifuged gained suspension slurry to obtain solids
Matter；Obtained solid substance is dried after repeating the step 3~5 time, obtains modified kaolin；
(4) by the octadecylamine of formulation dosage and ethyl alcohol be configured to mass percentage concentration be 3~7% (preferably 5~
6%) gained modified kaolin in (3) is then added to the ethyl alcohol of the octadecylamine by the ethanol solution of octadecylamine
Disperse modified kaolin uniformly wherein, passes through centrifugation point after ultrasonic disperse
From with dry step, obtain hydrophobically modified kaolin；
(5) by formulation dosage in table 1 by gained hydrophobically modified kaolin, heat stabilizer and processing aid in polypropylene, (4)
Dry-mixed 3~5min in a high speed mixer, mixing revolving speed are 600~800r/min, and mixing temperature is 23~25 DEG C, are premixed
Object；By the pre-composition, melting mixing is dispersed in the double screw extruder that draw ratio is 40~50:1 again, and extruding pelletization, is obtained
Polypropylene/kaolin composite material；Wherein the extruder temperature of double screw extruder is 175~220 DEG C.
The preparation of polypropylene material described in embodiment 1 is compared according to the preparation step of following preparation methods, the system
Preparation Method includes the following steps:
By formulation dosage in table 1 by polypropylene, heat stabilizer and processing aid dry-mixed 3~5min in a high speed mixer,
Mixing revolving speed is 600~800r/min, and mixing temperature is 23~25 DEG C, obtains pre-composition；It is in draw ratio by the pre-composition again
Melting mixing is dispersed in the double screw extruder of 40~50:1, and extruding pelletization, obtains polypropylene material；Wherein twin-screw extrusion
The extruder temperature of machine is 175~220 DEG C.
Polypropylene/kaolin composite material described in embodiment 2 is compared according to the preparation step of following preparation methods
Preparation, which includes the following steps:
By formulation dosage in table 1 by polypropylene, kaolin, heat stabilizer and processing aid in a high speed mixer dry-mixed 3
~5min, mixing revolving speed are 600~800r/min, and mixing temperature is 23~25 DEG C, obtain pre-composition；Again by the pre-composition in length
Diameter disperses than melting mixing in the double screw extruder for 40~50:1, and extruding pelletization, obtains polypropylene/kaolin composite wood
Material；Wherein the extruder temperature of double screw extruder is 175~220 DEG C.
Polypropylene/kaolin composite material described in embodiment 3 is compared according to the preparation step of following preparation methods
Preparation, which includes the following steps:
(1) kaolin is uniformly mixed to obtain mixture with modifying agent by formulation dosage described in table 1；
(2) gained mixture in (1) is added at room temperature in dehydrated alcohol and is stirred evenly, be separated into it uniformly
Then suspension slurry is centrifuged the suspension slurry to obtain solid matter；The wherein mixture and dehydrated alcohol
Mass ratio is 1:2~4；
It (3) is that 1:2~4 are added to dehydrated alcohol at room temperature again by solid-liquid mass ratio by obtained solid substance in (2)
In stir evenly, so that it is separated into uniform suspension slurry, then be centrifuged gained suspension slurry to obtain solids
Matter；Obtained solid substance is dried after repeating the step 3~5 time, obtains modified kaolin；
(4) by formulation dosage in table 1 by gained modified kaolin, heat stabilizer and processing aid in polypropylene, (3) in height
Dry-mixed 3~5min in fast mixing machine, mixing revolving speed are 600~800r/min, and mixing temperature is 23~25 DEG C, obtain pre-composition；
By the pre-composition, melting mixing is dispersed in the double screw extruder that draw ratio is 40~50:1 again, and extruding pelletization, is gathered
Propylene/kaolin composite material；Wherein the extruder temperature of double screw extruder is 175~220 DEG C.
1 specific embodiment 1-4 of table and comparative example 1-3 formulation dosage (unit: kg)
Resulting polypropylene material is prepared and polypropylene/kaolin composite material is molded into the test of standard batten and draws for above-mentioned
Intensity and heat distortion temperature are stretched, wherein the testing standard of tensile strength is ISO 527-2, tensile speed 50mm/min；Thermal change
The testing standard of shape temperature is ISO 75-2, and load 0.45MPa, test result is referring to table 2.
Batten test result obtained by 2 specific embodiment 1-4 of table and comparative example 1-3
It can be seen that by the comparison of above-mentioned comparative example and specific embodiment any kaolinic compared to being not added with
Polypropylene material, though addition whether be modified kaolin or hydrophobically modified kaolin, as long as being added to kaolin, gather
The heat distortion temperature and tensile strength of propylene material are improved, but effect is not obvious；And only it is added to unmodified kaolin
PP composite material, heat distortion temperature and tensile strength are higher than virgin pp material but are lower than herein described composite wood
Material；Further, only modified dose of modified kaolin is added in polypropylene material, heat distortion temperature and tensile strength exist
It is only added to a more excellent step on the basis of kaolinic PP composite material, but still is first passed through not as good as described herein be added to
The kaolinic heat resistance and tensile strength that modifier modification is modified through octadecylamine again.
This is because kaolin is a kind of inorganic laminated silicic acid containing aluminium being made of oxygen-octahedron and alumina octahedral
Salt mineral, interlayer have certain unsymmetric structure, which provides for the entrance of intercalator can
Can, intercalator can be replaced as presoma by subsequent monomer or polymer, and can be polymerize in phyllosilicate piece interlayer, be made
Piece interlamellar spacing expands so that peeling-off, and it is evenly dispersed in a polymer matrix, to be realized within the scope of nanoscale poly-
Close the intercalation synthesis of object and inorganic lamellar material.Polypropylene/kaolin composite material described herein and common polypropylene
Kaolin composite material is compared, hydrophobically modified it is kaolinic be added so that PP composite material tensile strength with higher and
Heat distortion temperature, good mechanical properties, heat resistance are high, can be applied to auto industry.
The above description is only a preferred embodiment of the present invention.It should be pointed out that in the feelings for not departing from the principle of the invention
It under condition, can also make several improvements and modification, be accordingly to be regarded as protection scope of the present invention.
Claims (5)
1. a kind of polypropylene/kaolin composite material, it is characterised in that: including following each components by weight:
The hydrophobically modified kaolin be prepared by following step it is resulting:
It (1) is in mass ratio that 1.5~4.5:1 is uniformly mixed to obtain mixture with modifying agent by kaolin, wherein modifying agent is carboxylic
At least one of sour sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is added at room temperature in dehydrated alcohol and is stirred evenly, it is made to be separated into uniform suspension
Then slurries are centrifuged the suspension slurry to obtain solid matter；The wherein quality of the mixture and dehydrated alcohol
Than for 1:2~4；
(3) obtained solid substance in (2) is added in dehydrated alcohol by solid-liquid mass ratio for 1:2~4 at room temperature again and is stirred
It mixes uniformly, so that it is separated into uniform suspension slurry, then be centrifuged gained suspension slurry to obtain solid matter；Again
Obtained solid substance is dried after repeating the step 3~5 time, obtains modified kaolin；
(4) octadecylamine and ethyl alcohol are configured to the ethanol solution for the octadecylamine that mass percentage concentration is 5~6%, so
Gained modified kaolin in (3) is added in the ethanol solution of the octadecylamine afterwards and makes to change by the way of ultrasonic disperse
Property kaolin uniformly disperse wherein, by centrifuge separation and dry step after ultrasonic disperse, obtain hydrophobically modified height
Ridge soil；Wherein the mass ratio of the ethanol solution of the modified kaolin and octadecylamine is 1:3~5.
2. polypropylene/kaolin composite material according to claim 1, it is characterised in that: the polypropylene is melt flow
Dynamic rate is at least one of copolymer polypropylene and homopolypropylene of 1~100g/10min.
3. polypropylene/kaolin composite material according to claim 1, it is characterised in that: the heat stabilizer be phenols,
At least one of amine, phosphorous acid esters, the compound species of acryloyl group functional group and monothioester and calixarene kind.
4. polypropylene/kaolin composite material according to claim 1, it is characterised in that: the processing aid is low point
At least one of the compound esters of sub- esters, metal soap, stearic acid and amides.
5. polypropylene/kaolin composite material preparation method described in any claim in a kind of Claims 1-4,
It is characterized in that: including the following steps:
It (1) is in mass ratio that 1.5~4.5:1 is uniformly mixed to obtain mixture with modifying agent by kaolin, wherein modifying agent is carboxylic
At least one of sour sodium, carboxylic acid potassium and calcium carboxylates；
(2) gained mixture in (1) is added at room temperature in dehydrated alcohol and is stirred evenly, it is made to be separated into uniform suspension
Then slurries are centrifuged the suspension slurry to obtain solid matter；The wherein quality of the mixture and dehydrated alcohol
Than for 1:2~4；
(3) obtained solid substance in (2) is added in dehydrated alcohol by solid-liquid mass ratio for 1:2~4 at room temperature again and is stirred
It mixes uniformly, so that it is separated into uniform suspension slurry, then be centrifuged gained suspension slurry to obtain solid matter；Again
Obtained solid substance is dried after repeating the step 3~5 time, obtains modified kaolin；
(4) octadecylamine and ethyl alcohol are configured to the ethanol solution for the octadecylamine that mass percentage concentration is 5~6%, so
Gained modified kaolin in (3) is added in the ethanol solution of the octadecylamine afterwards and makes to change by the way of ultrasonic disperse
Property kaolin uniformly disperse wherein, by centrifuge separation and dry step after ultrasonic disperse, obtain hydrophobically modified height
Ridge soil；Wherein the mass ratio of the ethanol solution of the modified kaolin and octadecylamine is 1:3~5；
(5) by gained hydrophobically modified kaolin, 0.2~2.0 weight in the polypropylene of 100 parts by weight, 5.5~20.0 parts by weight (4)
Dry-mixed 3~5min, mixing revolving speed are the processing aid of the heat stabilizer and 0.2~2.0 parts by weight of measuring part in a high speed mixer
600~800r/min, mixing temperature are 23~25 DEG C, obtain pre-composition；It is again 40~50:1's in draw ratio by the pre-composition
Melting mixing is dispersed in double screw extruder, and extruding pelletization, obtains polypropylene/kaolin composite material；Wherein twin-screw squeezes
The extruder temperature of machine is 175~220 DEG C out.
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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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| CN105885212A (en) * | 2014-12-09 | 2016-08-24 | 林建君 | Preparation method of modified kaolin reinforced polypropylene material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105885212A (en) * | 2014-12-09 | 2016-08-24 | 林建君 | Preparation method of modified kaolin reinforced polypropylene material |
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