CN108586944B - Wollastonite/polypropylene composite material and preparation method thereof - Google Patents

Wollastonite/polypropylene composite material and preparation method thereof Download PDF

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CN108586944B
CN108586944B CN201810466049.4A CN201810466049A CN108586944B CN 108586944 B CN108586944 B CN 108586944B CN 201810466049 A CN201810466049 A CN 201810466049A CN 108586944 B CN108586944 B CN 108586944B
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wollastonite
composite material
polypropylene
polypropylene composite
calcium carbonate
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CN108586944A (en
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鲁平才
赵银主
董银春
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Jiangsu Bi Gold New Material Stock Co ltd
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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
    • C08L23/14—Copolymers of propene
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • 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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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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Abstract

The invention discloses a wollastonite/polypropylene composite material and a preparation method thereof. The wollastonite/polypropylene composite material comprises the following components in parts by weight: 65-85 parts of polypropylene; 5-10 parts of a toughening agent; surface treatment of wollastonite, 10-25 parts; 0.1-1 part of lubricant; the surface-treated wollastonite is prepared by the following preparation method: wollastonite and a surface treating agent are mixed according to the mass ratio of 100: 0.5-3, adding the mixture into powder surface modification equipment, and performing surface coating treatment on wollastonite; the surface treating agent is selected from one or more of suberic acid, terephthalic acid and phthalic acid. The invention also discloses a preparation method of the composition. The wollastonite/polypropylene composite material has excellent flowability and mechanical property.

Description

Wollastonite/polypropylene composite material and preparation method thereof
Technical Field
The invention belongs to the field of processing of high polymer materials, and particularly relates to a high-strength high-fluidity impact-resistant wollastonite/polypropylene composite material and a preparation method thereof.
Background
Wollastonite is used as a functional reinforcing filler with the largest amount in the world at present, and the wollastonite is added into polypropylene (PP) to obviously improve the performance indexes of the PP, such as strength, rigidity, heat resistance, scratch resistance and the like, so that the wollastonite/PP composite material is gradually concerned by people. Chinese patent CN102532692A discloses a method for improving flying stone impact resistance by filling needle-shaped wollastonite with polypropylene, which has the disadvantage that for wollastonite which is a strong hydrophilic material, the wollastonite is not subjected to surface modification to improve the hydrophobicity, so that the mechanical properties of the wollastonite/polypropylene composite material still leave room for improvement, especially the impact resistance of the composite material. Chinese patent CN102875899A discloses a preparation method of wollastonite toughened and reinforced polypropylene composite material, but the flowability of the finally obtained composite material in the invention is poor, and the requirement of injection molding manufacturers on the high flowability of large-scale part materials at present cannot be met.
Disclosure of Invention
The invention provides a wollastonite/polypropylene composite material, which improves the flowability and the mechanical property.
The wollastonite/polypropylene composite material comprises the following components in parts by weight:
Figure BDA0001662108030000011
the surface-treated wollastonite is prepared by the following preparation method: wollastonite and a surface treating agent are mixed according to the mass ratio of 100: 0.5-3, adding the mixture into powder surface modification equipment, and performing surface coating treatment on wollastonite; the surface treating agent is selected from one or more of suberic acid, terephthalic acid and phthalic acid.
Further preferably, the composition of the wollastonite/polypropylene composite material comprises the following components in parts by weight:
Figure BDA0001662108030000012
the wollastonite is the wollastonite coated with nano calcium carbonate, and the length-diameter ratio of the wollastonite is 10: 1-20: 1, preferably 12: 1-16: 1. The length-diameter ratio is the ratio of the length to the diameter of the wollastonite.
The mass ratio of the wollastonite to the surface treating agent is preferably 100: 1 to 2.
The powder surface modification equipment is a CLG series powder surface modification machine. The temperature of the surface coating treatment is 140-150 ℃, and the treatment time is 10-15 min.
The polypropylene is copolymerized polypropylene, the melt index is more than or equal to 60g/10min (230 ℃, 2.16Kg), the crystallinity is more than or equal to 70 percent, and the isotacticity is more than or equal to 98 percent. Specifically, the polypropylene is selected from a product of Korean PolyMirae corporation, brand EA5076, or China petrochemical Yangzi petrochemical company, Inc., brand M30V.
The toughening agent is selected from ethylene-octene copolymer (POE) and ethylene propylene terpolymer (EPDM).
The lubricant is selected from one or more of polyethylene wax, solid paraffin and liquid paraffin.
The preparation method of the wollastonite/polypropylene composite material comprises the following steps:
(1) adding wollastonite and a surface treating agent into powder surface modification equipment, and carrying out surface coating treatment on the wollastonite to obtain surface treated wollastonite;
(2) mixing the surface treated wollastonite, the polypropylene, the toughening agent and the lubricant, and extruding and granulating.
Has the advantages that:
the wollastonite coated with the nano calcium carbonate is selected, so that the specific surface area of the wollastonite is increased, and more active points on the surface of the wollastonite can react with the modifier.
The invention selects suberic acid, terephthalic acid and phthalic acid as surface modifiers, calcium salt generated by the reaction of the surface modifiers and wollastonite or nano calcium carbonate is an effective polypropylene β nucleating agent, and the wollastonite can be used for strengthening PP and toughening PP at the same time, so that the impact resistance of PP is improved.
The suberic acid, the terephthalic acid and the phthalic acid have low toxicity and small harm to workers.
Compared with the general modification equipment such as a high-speed mixer, the special atomizing and spraying device of the CLG series powder surface modifier can mix and modify wollastonite powder and a modifier in an atomized state, so that the modification efficiency is improved, the modification time is shortened, and the problems of uneven mixing of the powder and the modifier, long mixing time, serious wollastonite structure damage and the like in the high-speed mixer are solved.
The invention adopts PP with specific parameters, which can improve the fluidity of the final product.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples used raw materials and equipment:
polypropylene (PP): trade name EA5076, PolyMirae corporation, Korea
Polypropylene (PP): M30V, China petrochemical Yangzi petrochemical company Limited
Ethylene-octene copolymer (POE): trade designation 8130, Dow chemical USA
Ethylene Propylene Diene Monomer (EPDM): Nordel-4760P, Dow chemical USA
Coating wollastonite with nano calcium carbonate: aspect ratios were 12:1 and 16:1, respectively, Nippon Donghui mining Co., Ltd. The following preparation methods (or other literature-reported methods) may also be employed: firstly, the quicklime is digested by water at normal temperature (CaO + H)2O＝Ca(OH)21kg of quicklime is digested with 500ml of water, i.e. 500g of water) for 1h to prepare lime milk. Then filtering the lime milk to remove quicklime residues, then injecting the lime milk into a reaction kettle, simultaneously adding wollastonite, and introducing CO2And (3) reacting the gas, controlling the reaction temperature to be about 50 ℃, after 20min of reaction, adjusting the pH of the solution to be 7, and finishing the reaction to obtain the wollastonite coated with the nano calcium carbonate.
Wollastonite (without surface coating treatment of nano calcium carbonate): aspect ratio of 12:1, Toxico mineral Limited, Xinyu
Suberic acid: changzhou Kanglong chemical Co Ltd
Terephthalic acid: jiangxi Min an environmental protection science and technology Limited
Phthalic acid: shanghai Jiachen chemical Co Ltd
Polyethylene wax: h105, Qingdao Haohao chemical industry
Solid paraffin: 64# Cia Huahui Plastic Material trade company of Cyprinus Carpio City of Fujian quan
Liquid paraffin: 15# Cinji oil and oil Co Ltd
CLG-200D powder surface modification machine: shanghai Koelix machines, Inc
High-speed mixer: zhang Jia gang City Star big mechanical Co Ltd
Example 1
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of suberic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then coating wollastonite, PP (EA5076), POE and polyethylene wax with the treated nano calcium carbonate according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 2
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 16:1) and 1Kg of suberic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then coating wollastonite, PP (EA5076), POE and polyethylene wax with the treated nano calcium carbonate according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 3
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of phthalic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then coating wollastonite, PPEA (5076), POE and polyethylene wax with the treated nano calcium carbonate according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 4
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of terephthalic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, mixing the treated wollastonite, PPEA5076, POE and polyethylene wax according to the proportion that PP/POE/wollastonite/polyethylene wax is 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 5
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1), 0.5Kg of suberic acid and 0.5Kg of terephthalic acid are subjected to surface treatment on the wollastonite coated with the nano calcium carbonate in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, mixing the treated wollastonite, PPEA5076, POE and polyethylene wax according to the proportion that PP/POE/wollastonite/polyethylene wax is 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 6
100Kg of wollastonite (the length-diameter ratio is 12:1) which is not coated with nano calcium carbonate and 1Kg of suberic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, mixing the treated wollastonite, PP (EA5076), POE and polyethylene wax according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 7
100Kg of wollastonite coated with nano calcium carbonate (aspect ratio 12:1) and 1Kg of suberic acid were subjected to surface treatment in a high-speed mixer (treatment temperature: 150 ℃ C., treatment time 10 min). Then coating wollastonite, PP (EA5076), POE and polyethylene wax with the treated nano calcium carbonate according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 8
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of suberic acid are subjected to surface treatment on the wollastonite coated with the nano calcium carbonate in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, mixing the treated wollastonite, PP (M30V), POE and polyethylene wax according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 9
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of suberic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, the treated wollastonite, PP (EA5076), EPDM and polyethylene wax are mixed according to the ratio of PP/EPDM/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 10
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of suberic acid are subjected to surface treatment on the wollastonite coated with the nano calcium carbonate in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, the treated wollastonite, PP (EA5076), EPDM, and paraffin wax were mixed in a ratio of PP/EPDM/wollastonite/paraffin wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 11
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of suberic acid are subjected to surface treatment on the wollastonite coated with the nano calcium carbonate in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, the treated wollastonite, PP (EA5076), EPDM, and liquid paraffin were mixed in such a manner that PP/EPDM/wollastonite/liquid paraffin was 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 12
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 2Kg of suberic acid are subjected to surface treatment on the wollastonite coated with the nano calcium carbonate in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, mixing the treated wollastonite, PP (EA5076), POE and polyethylene wax according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Example 13
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 2Kg of suberic acid are subjected to surface treatment on the wollastonite coated with the nano calcium carbonate in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then, mixing the treated wollastonite, the PPEA5076, the POE and the polyethylene wax according to the proportion that the PP/POE/wollastonite/polyethylene wax is 65: 10: 25: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Comparative example 1
Coating wollastonite, PPEA (5076), POE and polyethylene wax with the non-surface-treated nano calcium carbonate, wherein the ratio of PP/POE/wollastonite/polyethylene wax is 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Comparative example 2
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of pimelic acid are subjected to surface treatment on the wollastonite in a CLG-200D powder surface modifying machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then coating wollastonite, PP (EA5076), POE and polyethylene wax with the treated nano calcium carbonate according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
Comparative example 3
100Kg of wollastonite coated with nano calcium carbonate (the length-diameter ratio is 12:1) and 1Kg of adipic acid are used for carrying out surface treatment on the wollastonite in a CLG-200D powder surface modification machine (the treatment temperature is 150 ℃, and the treatment time is 10 min). Then coating wollastonite, PP (EA5076), POE and polyethylene wax with the treated nano calcium carbonate according to the ratio of PP/POE/wollastonite/polyethylene wax of 70: 10: 20: 0.4 part by weight of the mixture is extruded and granulated on an extruder, and then is injection molded into a standard sample strip for a series of performance tests.
The results of the performance tests are shown in table 1.
TABLE 1
Figure BDA0001662108030000061
The data show that the wollastonite/polypropylene composite material prepared by using the nanometer calcium carbonate coated wollastonite treated by suberic acid, terephthalic acid or phthalic acid as a raw material and then mixing the raw material with polypropylene, a toughening agent and a lubricant according to a certain proportion has high strength and high fluidity and excellent impact resistance, and is suitable for the requirements of the injection molding industry on the processing and forming performance and the use performance of large parts.
The high-strength high-flow impact-resistant polypropylene composite material and the preparation method thereof provided by the invention are described in detail above. While the principles and embodiments of this invention have been described herein using specific examples, the foregoing examples have been provided merely to facilitate an understanding of the principles and core concepts of the invention, and it will be appreciated by those skilled in the art that changes and modifications may be made thereto without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims.

Claims (5)

1. The wollastonite/polypropylene composite material is characterized by comprising the following components in parts by weight:
Figure FDA0002383997370000011
the surface-treated wollastonite is prepared by the following preparation method: wollastonite and a surface treating agent are mixed according to the mass ratio of 100: 0.5-3, adding the mixture into powder surface modification equipment, and performing surface coating treatment on wollastonite; the surface treating agent is selected from one or more of suberic acid, terephthalic acid and phthalic acid; the wollastonite is the wollastonite coated with nano calcium carbonate, and the length-diameter ratio of the wollastonite is 10: 1-20: 1; the powder surface modification equipment is a CLG series powder surface modification machine.
2. The wollastonite/polypropylene composite material as defined in claim 1, wherein the polypropylene is a polypropylene copolymer, and the melt index is not less than 60g/10min, the crystallinity is not less than 70%, and the isotacticity is not less than 98%.
3. Wollastonite/polypropylene composite material as claimed in claim 1 wherein the toughening agent is selected from ethylene-octene copolymer (POE), Ethylene Propylene Diene Monomer (EPDM).
4. The wollastonite/polypropylene composite material as set forth in claim 1, wherein the lubricant is selected from one or more of polyethylene wax, paraffin wax and liquid paraffin wax.
5. The preparation method of the wollastonite/polypropylene composite material as set forth in any one of claims 1 to 4 comprises the following steps:
(1) adding wollastonite and a surface treating agent into powder surface modification equipment, and carrying out surface coating treatment on the wollastonite to obtain surface treated wollastonite;
(2) mixing the surface treated wollastonite, the polypropylene, the toughening agent and the lubricant, and extruding and granulating.
CN201810466049.4A 2018-05-16 2018-05-16 Wollastonite/polypropylene composite material and preparation method thereof Active CN108586944B (en)

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CN114196120A (en) * 2021-12-29 2022-03-18 江苏兆鋆新材料股份有限公司 Polypropylene composite material and preparation method thereof
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CN103059415A (en) * 2013-01-16 2013-04-24 合肥杰事杰新材料股份有限公司 Needle-like wollastonite modified polypropylene composite material and preparation method thereof

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