CN116082692A - Method for manufacturing foamed polypropylene particles - Google Patents
Method for manufacturing foamed polypropylene particles Download PDFInfo
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- CN116082692A CN116082692A CN202211593655.5A CN202211593655A CN116082692A CN 116082692 A CN116082692 A CN 116082692A CN 202211593655 A CN202211593655 A CN 202211593655A CN 116082692 A CN116082692 A CN 116082692A
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- 239000002245 particle Substances 0.000 title claims abstract description 98
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 57
- -1 polypropylene Polymers 0.000 title claims abstract description 57
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 8
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000011435 rock Substances 0.000 claims abstract description 69
- 238000005187 foaming Methods 0.000 claims abstract description 53
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010298 pulverizing process Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 239000012467 final product Substances 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000002791 soaking Methods 0.000 claims abstract description 12
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 36
- 239000008187 granular material Substances 0.000 claims description 18
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005336 cracking Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000006261 foam material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/042—Nanopores, i.e. the average diameter being smaller than 0,1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
-
- 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
-
- 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
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention provides a manufacturing method of foaming polypropylene particles. The preparation method comprises the following steps: melting and mixing polypropylene resin and modified montmorillonite soft rock particles uniformly; soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material; placing the container into a baking oven for preheating for 5min at 220 ℃, placing the foaming raw material into the container, and placing into the baking oven for foaming for 9s; pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 60-70deg.C under 25-30MPa, and maintaining constant temperature and pressure for 10-20 hr; rapidly releasing pressure to obtain the final product. According to the invention, the montmorillonite soft rock particles are added as the foaming raw material, so that the montmorillonite soft rock expands and contracts in the heating and cooling processes, a microporous structure is formed in the polypropylene material, and on the other hand, the montmorillonite soft rock particles can also increase the mechanical strength of the foamed polypropylene particles.
Description
Technical Field
The invention relates to the technical field of plastic materials, in particular to a manufacturing method of foaming polypropylene particles.
Background
As a general plastic, polypropylene has the characteristics of high temperature resistance, corrosion resistance, no toxicity, no smell, easy processing and the like, and is widely applied to the fields of packaging materials, automobiles and the like. The foam polypropylene particles are novel foam materials which are developed in the mid-80 s abroad and have excellent performance and are used for replacing the traditional foam materials. Compared with the traditional foam polystyrene beads, the following advantages are achieved in performance: 1. excellent thermal stability; 2. excellent mechanical properties; 3. good stress cracking resistance and edible oil resistance, and meets the requirements of greasy food packaging; 4. excellent resistance to chemical attack; 5. good degradation performance and can be recycled. But polypropylene has a low melt strength and is very sensitive to temperature changes. As the processing temperature increases, the melt strength of the polypropylene resin is rapidly reduced, and the gas decomposed by the foaming agent is difficult to keep in the resin, so that the phenomena of bubble wall cracking, gas escape, bubble collapse, bubble merging and the like in the foaming process are easily caused; the melt strength is reduced due to the fact that more heat is released during crystallization, bubbles are easy to damage after foaming, and meanwhile, the mechanical property of the foamed material is also greatly reduced after foaming, so that the problem of how to improve the foaming rate and the foaming stability and simultaneously maintain the mechanical property to the greatest extent is to be solved urgently.
Disclosure of Invention
The technical problems to be solved are as follows: aiming at the technical problems, the invention aims to provide a manufacturing method of foaming polypropylene particles, wherein montmorillonite soft rock particles are added as foaming raw materials, and the montmorillonite soft rock expands and contracts in the heating and cooling processes to form a micropore structure in the polypropylene material, and on the other hand, the mechanical strength of the foaming polypropylene particles can be increased by the montmorillonite soft rock particles.
The technical scheme is as follows: a method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into a baking oven for preheating for 5min at 220 ℃, placing the foaming raw material into the container, and placing into the baking oven for foaming for 9s;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 60-70deg.C under 25-30MPa, and maintaining constant temperature and pressure for 10-20 hr;
(5) Rapidly releasing pressure to obtain the final product.
Preferably, the mass ratio of the polypropylene resin to the modified montmorillonite soft rock particles is 100 (10-20).
Preferably, the particle size of the modified montmorillonite soft rock particles is 10-100 μm.
Preferably, the preparation method of the modified montmorillonite soft rock particles comprises the following steps:
s1: pulverizing montmorillonite soft rock into granule to obtain montmorillonite soft rock granule;
s2: taking 250 parts of n-butanol, adding a silane coupling agent KH-550, adding 150 parts of montmorillonite soft rock particle aqueous dispersion, and vigorously stirring and heating to a boiling point;
s3: condensing the steam generated by heating through a condenser, separating n-butanol from water through a knockout, discharging water out of the system, and re-refluxing the n-butanol to participate in the reaction, and keeping the temperature for 4 hours;
s4: cooling to room temperature, vacuum filtering, washing with absolute ethyl alcohol;
s5: drying at 110deg.C for 4 hr, and pulverizing to obtain modified montmorillonite soft rock granule.
Preferably, the mass ratio of the silane coupling agent KH-550 to the montmorillonite soft rock particles is (0.5-2.0): 10.
Preferably, the solids content in the aqueous dispersion of montmorillonite soft rock particles is 12wt.%.
Preferably, the foaming temperature is 220-250 ℃.
The expanded polypropylene particles produced by the above-mentioned method for producing expanded polypropylene particles.
The beneficial effects are that:
1. the montmorillonite soft rock has strong expansibility, so the montmorillonite soft rock particles are added as foaming raw materials, the montmorillonite soft rock expands and contracts in the heating and cooling processes, a microporous structure is formed in the polypropylene material, and on the other hand, the montmorillonite soft rock particles can also increase the mechanical strength of the foamed polypropylene particles.
2. According to the invention, the silane coupling agent KH-550 is adopted to modify the montmorillonite soft rock particles, the surfaces of the montmorillonite soft rock particles are hydrophilic, and the montmorillonite soft rock particles are added into polypropylene, so that the montmorillonite soft rock particles are difficult to disperse and easy to agglomerate, and the dispersibility of the modified montmorillonite soft rock particles is enhanced and are easier to combine with the polypropylene.
3. The invention adopts the supercritical fluid to prepare the nano-pores in the polypropylene material, and the prepared polypropylene material has the foaming material with nano-micro-pores, and has high foaming multiplying power and strong mechanical property.
Detailed Description
The invention provides a manufacturing method of foaming polypropylene particles, which is further described in detail by the following examples in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The preparation method of the modified montmorillonite soft rock particles comprises the following steps:
s1: pulverizing montmorillonite soft rock into granule to obtain montmorillonite soft rock granule;
s2: taking 250 parts of n-butanol, adding a silane coupling agent KH-550, adding 150 parts of montmorillonite soft rock particle aqueous dispersion with a solid content of 12wt.%, and vigorously stirring and heating to a boiling point, wherein the mass ratio of the silane coupling agent KH-550 to the montmorillonite soft rock particles is 0.5:10;
s3: condensing the steam generated by heating through a condenser, separating n-butanol from water through a knockout, discharging water out of the system, and re-refluxing the n-butanol to participate in the reaction, and keeping the temperature for 4 hours;
s4: cooling to room temperature, vacuum filtering, washing with absolute ethyl alcohol;
s5: drying at 110deg.C for 4 hr, and pulverizing to obtain modified montmorillonite soft rock granule with particle diameter of 10-100 μm.
Example 2
The preparation method of the modified montmorillonite soft rock particles comprises the following steps:
s1: pulverizing montmorillonite soft rock into granule to obtain montmorillonite soft rock granule;
s2: taking 250 parts of n-butanol, adding a silane coupling agent KH-550, adding 150 parts of montmorillonite soft rock particle aqueous dispersion with a solid content of 12wt.%, and vigorously stirring and heating to a boiling point, wherein the mass ratio of the silane coupling agent KH-550 to the montmorillonite soft rock particles is 1.0:10;
s3: condensing the steam generated by heating through a condenser, separating n-butanol from water through a knockout, discharging water out of the system, and re-refluxing the n-butanol to participate in the reaction, and keeping the temperature for 4 hours;
s4: cooling to room temperature, vacuum filtering, washing with absolute ethyl alcohol;
s5: drying at 110deg.C for 4 hr, pulverizing to obtain modified montmorillonite soft rock granule with particle diameter of 10-100 μm
Example 3
The preparation method of the modified montmorillonite soft rock particles comprises the following steps:
s1: pulverizing montmorillonite soft rock into granule to obtain montmorillonite soft rock granule;
s2: taking 250 parts of n-butanol, adding a silane coupling agent KH-550, adding 150 parts of montmorillonite soft rock particle aqueous dispersion with a solid content of 12wt.%, and vigorously stirring and heating to a boiling point, wherein the mass ratio of the silane coupling agent KH-550 to the montmorillonite soft rock particles is 1.5:10;
s3: condensing the steam generated by heating through a condenser, separating n-butanol from water through a knockout, discharging water out of the system, and re-refluxing the n-butanol to participate in the reaction, and keeping the temperature for 4 hours;
s4: cooling to room temperature, vacuum filtering, washing with absolute ethyl alcohol;
s5: drying at 110deg.C for 4 hr, pulverizing to obtain modified montmorillonite soft rock granule with particle diameter of 10-100 μm
Example 4
The preparation method of the modified montmorillonite soft rock particles comprises the following steps:
s1: pulverizing montmorillonite soft rock into granule to obtain montmorillonite soft rock granule;
s2: taking 250 parts of n-butanol, adding a silane coupling agent KH-550, adding 150 parts of montmorillonite soft rock particle aqueous dispersion with a solid content of 12wt.%, and vigorously stirring and heating to a boiling point, wherein the mass ratio of the silane coupling agent KH-550 to the montmorillonite soft rock particles is 2.0:10;
s3: condensing the steam generated by heating through a condenser, separating n-butanol from water through a knockout, discharging water out of the system, and re-refluxing the n-butanol to participate in the reaction, and keeping the temperature for 4 hours;
s4: cooling to room temperature, vacuum filtering, washing with absolute ethyl alcohol;
s5: drying at 110deg.C for 4 hr, pulverizing to obtain modified montmorillonite soft rock granule with particle diameter of 10-100 μm
Example 5
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:10 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into an oven, preheating for 5min at 220 ℃, placing the foaming raw material into the container, placing into the oven, and foaming for 9s at 240 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65deg.C under 28MPa, and maintaining constant temperature and pressure for 15 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 6
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into an oven, preheating for 5min at 220 ℃, placing the foaming raw material into the container, placing into the oven, and foaming for 9s at 240 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65deg.C under 28MPa, and maintaining constant temperature and pressure for 15 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 7
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:20 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into an oven, preheating for 5min at 220 ℃, placing the foaming raw material into the container, placing into the oven, and foaming for 9s at 240 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65deg.C under 28MPa, and maintaining constant temperature and pressure for 15 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 8
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Preheating the container in an oven at 220 ℃ for 5min, placing the foaming raw material in the container, placing the container in the oven, and foaming for 9s at 220 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65deg.C under 28MPa, and maintaining constant temperature and pressure for 15 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 9
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into an oven, preheating for 5min at 220 ℃, placing the foaming raw material into the container, placing into the oven, and foaming for 9s at 230 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65deg.C under 28MPa, and maintaining constant temperature and pressure for 15 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 10
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container in an oven for preheating for 5min at 220 ℃, placing the foaming raw material in the container, placing the container in the oven, and foaming for 9s at 250 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65deg.C under 28MPa, and maintaining constant temperature and pressure for 15 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 11
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into an oven, preheating for 5min at 220 ℃, placing the foaming raw material into the container, placing into the oven, and foaming for 9s at 240 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 60deg.C, maintaining the temperature and pressure at 25MPa for 20 hr;
(5) Rapidly releasing pressure to obtain the final product.
Example 12
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into an oven, preheating for 5min at 220 ℃, placing the foaming raw material into the container, placing into the oven, and foaming for 9s at 240 ℃;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 70deg.C under 30MPa, and maintaining constant temperature and pressure for 10 hr;
(5) Rapidly releasing pressure to obtain the final product.
Comparative example 1
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Crushing polypropylene resin into particles, placing the particles into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 65 ℃, keeping the temperature and the pressure at 28MPa, and keeping the temperature and the pressure at constant temperature for 15 hours;
(2) Rapidly releasing pressure to obtain the final product.
Comparative example 2
A method for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin with the mass ratio of 100:15 and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) The container is placed in an oven for preheating for 5min at 220 ℃, the foaming raw material is placed in the container, and the container is placed in the oven for foaming for 9s at 240 ℃.
Density measurements were made with reference to GB/T1033.1-2008 and the expansion ratio was calculated.
Tensile testing was performed at a speed of 50mm/min on an XLL-100 tensile tester according to GBl040-79 standard.
Flexural performance test tensile testing was performed at a speed of 25mm/min on an XLL-100-type tensile tester according to GBl040-79 standard.
The impact performance test of the simply supported beam is carried out according to GBl040-79 standard, and a notch pattern is adopted on an XCJ-500 impact experiment machine.
TABLE 1
| Expansion ratio | Tensile Strength (MPa) | Flexural Strength (MPa) | Notched impact Strength (kJ/m) 2 ) | |
| Example 5 | 0.41 | 28.2 | 42.6 | 25.1 |
| Example 6 | 0.50 | 29.1 | 43.3 | 25.9 |
| Example 7 | 0.47 | 29.5 | 43.5 | 26.1 |
| Example 8 | 0.43 | 29.4 | 43.4 | 25.4 |
| Example 9 | 0.46 | 29.3 | 43.4 | 25.8 |
| Example 10 | 0.48 | 29.2 | 43.3 | 25.9 |
| Example 11 | 0.43 | 29.0 | 43.2 | 25.2 |
| Example 12 | 0.51 | 28.6 | 42.9 | 26.1 |
| Comparative example 1 | 0.35 | 29.8 | 43.7 | 18.4 |
| Comparative example 2 | 0.37 | 29.4 | 43.3 | 20.7 |
Claims (8)
1. A process for producing expanded polypropylene particles, comprising the steps of:
(1) Melting and mixing polypropylene resin and modified montmorillonite soft rock particles uniformly;
(2) Soaking in water for 24h, and drying the surface moisture to obtain a foaming raw material;
(3) Placing the container into a baking oven for preheating for 5min at 220 ℃, placing the foaming raw material into the container, and placing into the baking oven for foaming for 9s;
(4) Pulverizing into particles, placing into a high-pressure extraction kettle of a supercritical fluid extraction device, heating to 60-70deg.C under 25-30MPa, and maintaining constant temperature and pressure for 10-20 hr;
(5) Rapidly releasing pressure to obtain the final product.
2. The method for producing expanded polypropylene particles according to claim 1, wherein the ratio of the polypropylene resin to the modified montmorillonite soft rock particles is 100 (10-20).
3. The method for producing expanded polypropylene particles according to claim 1, wherein the modified montmorillonite soft rock particles have a particle diameter of 10 to 100 μm.
4. The method for producing expanded polypropylene particles according to claim 1, wherein the modified montmorillonite soft rock particles are produced by:
s1: pulverizing montmorillonite soft rock into granule to obtain montmorillonite soft rock granule;
s2: taking 250 parts of n-butanol, adding a silane coupling agent KH-550, adding 150 parts of montmorillonite soft rock particle aqueous dispersion, and vigorously stirring and heating to a boiling point;
s3: condensing the steam generated by heating through a condenser, separating n-butanol from water through a knockout, discharging water out of the system, and re-refluxing the n-butanol to participate in the reaction, and keeping the temperature for 4 hours;
s4: cooling to room temperature, vacuum filtering, washing with absolute ethyl alcohol;
s5: drying at 110deg.C for 4 hr, and pulverizing to obtain modified montmorillonite soft rock granule.
5. The method for producing expanded polypropylene particles according to claim 4, wherein the mass ratio of said silane coupling agent KH-550 to montmorillonite soft rock particles is (0.5-2.0): 10.
6. The method for producing expanded polypropylene particles according to claim 4, wherein said aqueous dispersion of montmorillonite soft rock particles has a solids content of 12% by weight.
7. The method for producing expanded polypropylene particles according to claim 1, wherein the foaming temperature is 220 to 250 ℃.
8. Foamed polypropylene particles produced by the process for producing foamed polypropylene particles according to any one of claims 1 to 7.
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