CN113894962A - Preparation method of low-melting-point regenerated PET plastic particles - Google Patents
Preparation method of low-melting-point regenerated PET plastic particles Download PDFInfo
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- CN113894962A CN113894962A CN202110850452.9A CN202110850452A CN113894962A CN 113894962 A CN113894962 A CN 113894962A CN 202110850452 A CN202110850452 A CN 202110850452A CN 113894962 A CN113894962 A CN 113894962A
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- talcum powder
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- 239000002245 particle Substances 0.000 title claims abstract description 39
- 239000004033 plastic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 63
- 239000010452 phosphate Substances 0.000 claims abstract description 63
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 54
- -1 phosphate polyol modified talcum powder Chemical class 0.000 claims abstract description 54
- 229920000570 polyether Polymers 0.000 claims abstract description 54
- 238000002844 melting Methods 0.000 claims abstract description 43
- 230000008018 melting Effects 0.000 claims abstract description 43
- 229920005862 polyol Polymers 0.000 claims abstract description 34
- 238000001125 extrusion Methods 0.000 claims abstract description 28
- 239000004970 Chain extender Substances 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 25
- 239000002667 nucleating agent Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- 239000000155 melt Substances 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 14
- 238000010309 melting process Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 47
- 238000000498 ball milling Methods 0.000 claims description 29
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 25
- 238000004140 cleaning Methods 0.000 claims description 24
- 238000012216 screening Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- 229920001451 polypropylene glycol Polymers 0.000 claims description 14
- 238000005520 cutting process Methods 0.000 claims description 12
- 239000003000 extruded plastic Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000004806 packaging method and process Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 7
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000000454 talc Substances 0.000 claims description 4
- 229910052623 talc Inorganic materials 0.000 claims description 4
- 235000012222 talc Nutrition 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 229920000728 polyester Polymers 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 20
- 239000004593 Epoxy Substances 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 150000008064 anhydrides Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000009512 pharmaceutical packaging Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- 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
-
- 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
-
- 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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
- B29K2067/003—PET, i.e. poylethylene terephthalate
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention relates to the field of polyester materials, and discloses a preparation method of low-melting-point regenerated PET plastic particles. The method comprises four main steps of pretreatment, feeding melting, extrusion cooling and finished product treatment of recovered bottle flakes, wherein ultrasonic treatment is added in the feeding melting process, polyether phosphate polyol modified talcum powder is added as a nucleating agent in the extrusion cooling step, and a crystallization promoter and a chain extender are also added. Compared with the prior art, the invention has the beneficial effects that: the viscosity of the melt is increased, which is beneficial to widening the application range of the product; the process temperature is reduced, the crystal boundary is increased, and the whiteness of the product is improved.
Description
Technical Field
The invention relates to the field of polyester materials, in particular to a preparation method of low-melting-point recycled PET plastic particles.
Background
PET is a thermoplastic linear polyester, a typical high-crystallinity polymer, is a nontoxic and tasteless food package developed after the national banned PVC of the U.S. food and drug administration, the Japanese government and the like is used for food and drug packaging, has the advantages of impact resistance, transparency, no toxicity, high barrier property, low price and the like, can keep excellent physical properties and mechanical properties in a wider temperature range, and therefore, has a wide application range. The comprehensive utilization of the waste PET bottles and PET bottle chips can reduce pollution and increase benefits. The large amount of PET bottles has raised the problem of recycling and secondary utilization, and has received increasing attention from the current society. The recovery device of PET bottles is established by enterprises at home and abroad in a dispute, the recovery rate and the reutilization rate of the PET bottles are improved, the recovery rate of the German PET bottles in 2010 is as high as 93 percent, the annual recovery rate of the Brazil and French PET bottles in 2010 is also over 50 percent, and the recovery amount of the domestic PET bottles is increased year by year. However, when the PET is recycled for secondary use, the PET is degraded, molecular chains are broken, the strength is reduced, and the application of the PET recycled plastic is limited. Meanwhile, the recycled PET contains more impurities than the PET prepared newly, and is easy to yellow in the melt extrusion process, and the like, and the use of the PET recycled plastic is also limited.
Publication No. CN110643154A discloses a PET tackifying method, which comprises the following steps: setting the processing temperature of an internal mixer or a double-screw extruder to be 200-300 ℃, firstly adding PET until the PET forms a viscous state, and then simultaneously adding inorganic non-metal nanoparticles rich in hydroxyl and a silane coupling agent, wherein the silane coupling agent comprises a silane coupling agent containing an epoxy group, and uniformly stirring the silane coupling agent and the silane coupling agent together to realize the tackifying of the PET. The tackifying method provided by the invention has the characteristics of simplicity, low cost and capability of simultaneously tackifying different PET. This solution, although increasing the viscosity, does not reduce the melting point of the product and the extrusion temperature is still too high.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of low-melting-point recycled PET plastic particles, which can improve the viscosity of a PET melt and improve the whiteness of PET particles, and is simple and easy to implement.
The preparation method comprises the following steps:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate polyol modified talcum powder and a crystallization promoter into the melt liquid after ultrasonic treatment, adding a chain extender after uniformly stirring, extruding plastic bracing pieces after uniformly stirring, wherein the extrusion temperature is 180-200 ℃, and drying the extruded plastic bracing pieces after water cooling;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
In order to ensure the purity of the recovered bottle flakes as much as possible, the recovered bottle flakes are screened and cleaned, dried and then put into a melting device, the melting device creates a vacuum condition or an inert gas protective atmosphere, ultrasonic conditions are applied in the melting process to reduce the melting point of the bottle flakes, and documents show that the PET is yellowed due to the fact that the melting temperature is too high. Meanwhile, ultrasonic can decompose partial high molecular chains, the number of hydroxyl and carboxyl in the molten liquid is increased, more crystal nuclei can be formed when the nucleating agent is added, so that more crystal boundaries are generated, the existence of the crystal boundaries is favorable for increasing the whiteness of the regenerated PET, the refinement of the crystal grains is also favorable for improving the toughness of the product, and the addition of the crystallization promoter is favorable for improving the crystallization degree and increasing the crystal boundaries. In addition, since the nucleating agent and the crystallization promoter are white particles themselves, it is also advantageous to increase the whiteness of the product. The subsequently added chain extender can grow the melt single chains and increase the viscosity of the melt. And finally, cooling the extruded plastic brace with water, drying the brace with air, cutting the brace into granular particles, preparing the granular particles into products, and screening and packaging the products. The nucleating agent used by the invention is polyether phosphate ester polyol modified talcum powder, and because the modifier is provided with polyether and a plurality of hydroxyl groups, the nucleating agent used by the invention has the effects of reducing the melting point and chain extension, and can offset the viscosity reduction caused by the increase of crystallization.
Preferably, the preparation method of the polyether phosphate polyol modified talcum powder comprises the following steps:
A. soaking talcum powder in acetic acid solution with pH of 3-5 for 5-10min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder;
C. mixing phosphate modified talcum powder with polypropylene glycol, adding a catalyst, reacting for 20-24h at the temperature of 160-180 ℃, cleaning and drying to obtain the polyether phosphate polyol modified talcum powder.
The nucleating agent used by the invention is polyether phosphate ester polyol modified talcum powder, and because the modifier is provided with polyether and a plurality of hydroxyl groups, the nucleating agent used by the invention has the effects of reducing the melting point and chain extension, and can offset the viscosity reduction caused by the increase of crystallization. Step A is to enable the talcum powder to have an activated surface and be easily compounded with polyether phosphate ester polyol, and the ball milling in step C is to increase the compounding capacity of the activated talcum powder and the polyether phosphate ester polyol.
Preferably, in the step B, the ball milling speed is 200-300r/min, and the ball milling time is 0.5-1 h.
Preferably, in the step C, the material ratio of the phosphate modified talcum powder to the polypropylene glycol is 1-1.2: 7-8; the catalyst is dibutyltin dilaurate.
Preferably, the chain extender is one or more of a bisoxazoline chain extender, a diepoxide chain extender, a diisocyanate chain extender and an anhydride chain extender; the addition amount of the chain extender is 5-8 wt%.
Preferably, the crystallization promoter in the step (3) is polyether with the molar mass of 1000-3000; the addition amount of the crystallization promoter is 3-5 wt%.
The polyether is used as the crystallization promoter, so that the melting point of the melt can be reduced, and the yellowing of the product caused by overhigh extrusion temperature of the melt can be prevented.
Preferably, the screening of step (1) is sorted by a color sorter; ultrasonic cleaning with water or ethanol at room temperature for 20-30min, and alternately washing with water and ethanol; the drying method is spin-drying.
Because the raw material of the PET regenerated particles is PET bottle flakes, the bottle flakes are pretreated before melting in order to ensure the purity of the raw material. The ultrasonic cleaning process is helpful for the decomposition of PET besides removing surface impurities, and is used for laying a cushion for the subsequent crystallization process.
Preferably, the melting process in the step (2) is performed in an inert gas atmosphere or in a vacuum state; the inert gas is argon or nitrogen.
Preferably, the nucleating agent is added in the amount of 1 to 3 wt% in step (3).
Preferably, the nucleating agent is talcum powder, and the particle size of the polyether phosphate polyol modified talcum powder is d:1 μm < d <10 μm.
In order to nucleate the crystal grains as much as possible and refine the crystal grains as much as possible, the particle size of the polyether phosphate polyol modified talc should be as small as possible.
Compared with the prior art, the invention has the beneficial effects that:
1. the viscosity of the melt is increased, which is beneficial to widening the application range of the product;
2. the process temperature is reduced, the crystal boundary is increased, and the whiteness of the product is improved.
Detailed Description
The present invention will be further described with reference to the following examples. The devices, reagents and methods referred to in the present invention are those known in the art unless otherwise specified.
Example 1
Preparation of nucleating agent:
A. soaking talcum powder in acetic acid solution with pH of 4 for 8min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder; the ball milling speed is 250r/min, and the ball milling time is 1 h;
C. mixing phosphate modified talcum powder and polypropylene glycol, adding dibutyltin dilaurate, reacting for 24h at 170 ℃, cleaning and drying to obtain polyether phosphate polyol modified talcum powder; the material ratio of the phosphate modified talcum powder to the polypropylene glycol is 1: 7; the particle size of the obtained polyether phosphate polyol modified talcum powder is that d is 1 mu m and is less than 10 mu m;
preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate ester polyol modified talcum powder and polyether into the melt liquid after ultrasonic treatment, adding a bis-epoxy chain extender after uniformly stirring, extruding plastic bracing pieces after uniformly stirring, wherein the extrusion temperature is 190 ℃, and drying the extruded plastic bracing pieces after water cooling; the addition amount of the polyether phosphate polyol modified talcum powder is 2 wt%, the addition amount of the diepoxy chain extender is 7 wt%, and the addition amount of the polyether is 4 wt%;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Example 2
Preparation of nucleating agent:
A. soaking talcum powder in acetic acid solution with pH of 4 for 8min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder; the ball milling speed is 250r/min, and the ball milling time is 1 h;
C. mixing phosphate modified talcum powder and polypropylene glycol, adding dibutyltin dilaurate, reacting for 24h at 170 ℃, cleaning and drying to obtain polyether phosphate polyol modified talcum powder; the material ratio of the phosphate modified talcum powder to the polypropylene glycol is 1: 8; the particle size of the obtained polyether phosphate polyol modified talcum powder is that d is 1 mu m and is less than 10 mu m;
preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate ester polyol modified talcum powder and polyether into the melt liquid after ultrasonic treatment, adding a bis-epoxy chain extender after uniformly stirring, extruding plastic bracing pieces after uniformly stirring, wherein the extrusion temperature is 190 ℃, and drying the extruded plastic bracing pieces after water cooling; the addition amount of the polyether phosphate polyol modified talcum powder is 2 wt%, the addition amount of the diepoxy chain extender is 7 wt%, and the addition amount of the polyether is 4 wt%;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Example 3
Preparation of nucleating agent:
A. soaking talcum powder in acetic acid solution with pH of 4 for 8min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder; the ball milling speed is 250r/min, and the ball milling time is 1 h;
C. mixing phosphate modified talcum powder and polypropylene glycol, adding dibutyltin dilaurate, reacting for 24h at 170 ℃, cleaning and drying to obtain polyether phosphate polyol modified talcum powder; the material ratio of the phosphate modified talcum powder to the polypropylene glycol is 1.2: 7; the particle size of the obtained polyether phosphate polyol modified talcum powder is that d is 1 mu m and is less than 10 mu m;
preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate ester polyol modified talcum powder and polyether into the melt liquid after ultrasonic treatment, adding a bis-epoxy chain extender after uniformly stirring, extruding plastic bracing pieces after uniformly stirring, wherein the extrusion temperature is 190 ℃, and drying the extruded plastic bracing pieces after water cooling; the addition amount of the polyether phosphate polyol modified talcum powder is 2 wt%, the addition amount of the diepoxy chain extender is 7 wt%, and the addition amount of the polyether is 4 wt%;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Example 4
Preparation of nucleating agent:
A. soaking talcum powder in acetic acid solution with pH of 4 for 8min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder; the ball milling speed is 250r/min, and the ball milling time is 1 h;
C. mixing phosphate modified talcum powder and polypropylene glycol, adding dibutyltin dilaurate, reacting for 24h at 170 ℃, cleaning and drying to obtain polyether phosphate polyol modified talcum powder; the material ratio of the phosphate modified talcum powder to the polypropylene glycol is 1: 7; the particle size of the obtained polyether phosphate polyol modified talcum powder is that d is 1 mu m and is less than 10 mu m;
preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate ester polyol modified talcum powder and polyether into the melt liquid after ultrasonic treatment, adding a bis-epoxy chain extender after uniformly stirring, extruding plastic bracing pieces after uniformly stirring, wherein the extrusion temperature is 190 ℃, and drying the extruded plastic bracing pieces after water cooling; the addition amount of the polyether phosphate polyol modified talcum powder is 1 wt%, the addition amount of the diepoxy chain extender is 7 wt%, and the addition amount of the polyether is 4 wt%;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Example 5
Preparation of nucleating agent:
A. soaking talcum powder in acetic acid solution with pH of 4 for 8min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder; the ball milling speed is 250r/min, and the ball milling time is 1 h;
C. mixing phosphate modified talcum powder and polypropylene glycol, adding dibutyltin dilaurate, reacting for 24h at 170 ℃, cleaning and drying to obtain polyether phosphate polyol modified talcum powder; the material ratio of the phosphate modified talcum powder to the polypropylene glycol is 1: 7; the particle size of the obtained polyether phosphate polyol modified talcum powder is that d is 1 mu m and is less than 10 mu m;
preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate ester polyol modified talcum powder and polyether into the melt liquid after ultrasonic treatment, adding a bis-epoxy chain extender after uniformly stirring, extruding plastic bracing pieces after uniformly stirring, wherein the extrusion temperature is 190 ℃, and drying the extruded plastic bracing pieces after water cooling; the addition amount of the polyether phosphate polyol modified talcum powder is 3 wt%, the addition amount of the diepoxy chain extender is 7 wt%, and the addition amount of the polyether is 4 wt%;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Comparative example 1
Preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding unmodified talcum powder and polyether into the melt liquid after ultrasonic treatment, adding the diepoxy chain extender after uniformly stirring, extruding plastic braces after uniformly stirring, wherein the extrusion temperature is 200 ℃, and drying the extruded plastic braces after water cooling; the addition amount of the polyether phosphate polyol modified talcum powder is 5wt%, the addition amount of the diepoxy chain extender is 7 wt%, and the addition amount of the polyether is 4 wt%;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Comparative example 2
Preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recovered bottle flakes pretreated in the step (1) into melting equipment, and heating until the recovered bottle flakes are melted;
(3) and (3) extrusion cooling: uniformly stirring the molten liquid, extruding plastic braces after uniformly stirring, wherein the extrusion temperature is 240 ℃, and drying the extruded plastic braces after water cooling;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Comparative example 3
Preparing regenerated PET plastic particles:
(1) feeding and melting: putting the recovered bottle flakes into melting equipment, heating until the recovered bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(2) and (3) extrusion cooling: uniformly stirring the molten liquid, extruding plastic braces after uniformly stirring, wherein the extrusion temperature is 240 ℃, and drying the extruded plastic braces after water cooling;
(3) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Comparative example 4
Preparing regenerated PET plastic particles:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: uniformly stirring the molten liquid, extruding plastic braces after uniformly stirring, wherein the extrusion temperature is 240 ℃, and drying the extruded plastic braces after water cooling;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
Melting point measurement: the melting point of the polymer was determined by scanning the sample with a differential scanning calorimeter for 3 temperature ramping cycles between 30 ℃ and 280 ℃ and the results are shown in Table 1.
The whiteness of the product was measured and the results are shown in Table 1.
TABLE 1
| Serial number | Melting Point (. degree.C.) | Whiteness degree |
| Example 1 | 233 | 98％ |
| Example 2 | 226 | 97％ |
| Example 3 | 234 | 97％ |
| Example 4 | 228 | 98％ |
| Example 5 | 232 | 96％ |
| Comparative example 1 | 258 | 93％ |
| Comparative example 2 | 251 | 80％ |
| Comparative example 3 | 246 | 76％ |
| Comparative example 4 | 250 | 65％ |
The melting point results of comparative examples 1-5 and comparative example 1 show that the melting point of the recycled PET can be reduced by surface modification of the nucleating agent, and the reason for this is probably because the melting point is reduced by the polyether after modification of the nucleating agent; secondly, as can be seen from the melting point results comparing comparative example 1 with comparative examples 2 to 4, comparative example 1 has a higher melting point temperature, which is probably because the addition of the chain extender in comparative example 1 increases the length of the PET chain, which decreases the mobility between molecules; the melting point of comparative example 3 is lower than that of comparative examples 2 and 4 probably because the ultrasonic action decomposes a part of the polymer chains, so that the molecular chains of comparative example 3 become short. It can be seen from the whiteness of comparative examples 1 to 5 and comparative examples 2 to 4 that the examples with the nucleating agent added have better whiteness, probably because examples 1 to 5 have more grain boundaries, and the light is reflected more and thus becomes whitish, and the nucleating agent and the chain extender are also white themselves, and have a certain whiteness promoting effect. And the effect of examples 1-5 is better than that of comparative example 1, probably because the polyether group in the nucleating agent of examples 1-5 lowers the melting point, enabling the product to be extruded at a lower extrusion temperature.
Claims (10)
1. A preparation method of low-melting-point recycled PET plastic particles is characterized by comprising the following steps:
(1) pretreatment of recovered bottle flakes: screening the recovered bottle flakes, and then cleaning and drying the selected recovered bottle flakes;
(2) feeding and melting: putting the recycled bottle flakes pretreated in the step (1) into melting equipment, heating until the recycled bottle flakes are melted, and carrying out ultrasonic treatment in the melting process;
(3) and (3) extrusion cooling: adding polyether phosphate polyol modified talcum powder and a crystallization promoter into the melt liquid after ultrasonic treatment, adding a chain extender after uniformly stirring, extruding plastic braces after uniformly stirring, wherein the extrusion temperature is 180-210 ℃, and drying the extruded plastic braces after water cooling;
(4) and (3) finished product treatment: cutting the plastic strips into granular particles, preparing products, and packaging after screening.
2. The method of claim 1, wherein the polyether phosphate polyol modified talc is prepared by a method comprising:
A. soaking talcum powder in acetic acid solution with pH of 3-5 for 5-10min, vacuum filtering, and drying to obtain pretreated talcum powder;
B. mixing the pretreated talcum powder with phosphate, then carrying out ball milling, carrying out suction filtration after ball milling, cleaning and drying to obtain phosphate modified talcum powder;
C. mixing phosphate modified talcum powder with polypropylene glycol, adding a catalyst, reacting for 20-24h at the temperature of 160-180 ℃, cleaning and drying to obtain the polyether phosphate polyol modified talcum powder.
3. The method as claimed in claim 2, wherein in step B, the ball milling speed is 300-600r/min, and the ball milling time is 0.5-1 h.
4. The method according to claim 2, wherein in step C, the material ratio of the phosphate ester-modified talc to the polypropylene glycol is 1-1.2: 7-8; the catalyst is dibutyltin dilaurate.
5. The method of claim 1, wherein the chain extender is a diepoxy chain extender; the addition amount of the chain extender is 5-8 wt%.
6. The method of claim 1, wherein the screening of step (1) is performed by color sorting; ultrasonic cleaning with water or ethanol at room temperature for 20-30min, and alternately washing with water and ethanol; the drying method is spin-drying.
7. The method according to claim 1, wherein the melting in the step (2) is performed in an inert gas atmosphere or in a vacuum state; the inert gas is argon or nitrogen.
8. The method according to claim 1, wherein the nucleating agent is added in an amount of 2 to 5wt% in step (3).
9. The method according to claim 4, wherein the particle size of the polyether phosphate polyol-modified talc is d:1 μm < d <10 μm.
10. The method according to claim 1, wherein the crystallization promoter in the step (3) is a polyether having a molar mass of 1000-3000; the addition amount of the crystallization promoter is 3-5 wt%.
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| CN106009545A (en) * | 2016-06-28 | 2016-10-12 | 周开雄 | Method for producing film sheet by direct melting of recovered waste PET (polyethylene terephthalate) andfilm sheet |
| CN109486135A (en) * | 2018-11-30 | 2019-03-19 | 广东威林工程塑料股份有限公司 | One kind can be used in, the molding high performance PE T composite material and preparation method of low mould temperature rapid crystallization |
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