CN112480540A - Regenerated plastic particle modification process - Google Patents
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- CN112480540A CN112480540A CN202011418000.5A CN202011418000A CN112480540A CN 112480540 A CN112480540 A CN 112480540A CN 202011418000 A CN202011418000 A CN 202011418000A CN 112480540 A CN112480540 A CN 112480540A
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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
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- Compositions Of Macromolecular Compounds (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a regenerated plastic particle modification process, which relates to the technical field of plastic regeneration, and is characterized in that PP (polypropylene) waste and PPO (polyphenylene oxide) waste are used as main materials, nano-filler, plasticizer, compatibilizer, antioxidant and flame retardant are added, and the materials are subjected to melt blending, extrusion and granulation to prepare regenerated plastic particles; the compatibilizer is prepared by reacting N-chlorosuccinamide and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane in a molar ratio of 1: 1. The processing formability of the regenerated plastic particles prepared by the invention is good, and the prepared plastic product simultaneously shows excellent application performance, thereby ensuring the use quality of the regenerated plastic product.
Description
The technical field is as follows:
the invention relates to the technical field of plastic regeneration, in particular to a regenerated plastic particle modification process.
Background art:
the recycled plastic refers to a plastic raw material obtained by processing and processing waste plastics by physical or chemical methods such as pretreatment, melt granulation, modification and the like, and is used for recycling the plastics. The recycled plastic is an effective way for solving the plastic pollution at present, but the recycled plastic has the problems of low strength, poor toughness, low glossiness, poor thermal oxidation stability and the like, and the service quality and the service life of a recycled plastic product are seriously influenced.
At present, the modification treatment of the recycled plastic mainly adopts two modes of physical modification and chemical modification, wherein the physical modification mode has the characteristics of simple and convenient operation and small pollution, but has the defect of limited modification effect; the chemical modification mode is to graft functional groups or structures on polymer molecules, the modification effect is obvious, but a homogeneous system is usually required to be formed by chemical reaction, an organic solvent is inevitably used, and the use of the organic solvent not only increases the processing cost, but also generates waste liquid and influences the processing environment. Therefore, physical modification is better in handling and safety than chemical modification, but the modification effect is yet to be optimized.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a regenerated plastic particle modification process, which takes PP waste and PPO waste as main materials, so that the prepared regenerated plastic has the excellent characteristics of PP and PPO, and the PP and PPO are physically modified by adding a functional additive, thereby simplifying the modification process, reducing the process cost, optimizing the service performance of the prepared regenerated plastic and expanding the application range of the regenerated plastic.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a regenerated plastic particle modification process comprises the steps of taking PP waste and PPO waste as main materials, adding nano filler, plasticizer, compatibilizer, antioxidant and flame retardant, carrying out melt blending, extruding and granulating to obtain regenerated plastic particles; the compatibilizer is prepared by reacting N-chlorosuccinamide and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane in a molar ratio of 1: 1.
The preparation route of the compatibilizer is as follows:
PP is short for polypropylene, PPO is short for polyphenyl ether, and the PP and PPO have advantages and disadvantages when used as processing raw materials of plastic products. In order to reduce the addition amount of the functional additive and further reduce the regeneration cost, the invention uses the PP waste and the PPO waste as main materials, so that the prepared regenerated plastic has the excellent characteristics of PP and PPO, but the problem of poor compatibility exists between PP and PPO, and the filler cannot be uniformly dispersed, thereby directly influencing the processing performance of the regenerated plastic particles and ensuring that the polymer and the filler can not normally exert the action effect.
The compatibilizer is a common functional aid for processing plastic products in the field, and aims to reduce the interfacial tension of substances, enhance the compatibility of polymers, and improve the dispersibility of the filler in the polymers, thereby forming a stable blend. The maleic anhydride grafted polypropylene belongs to a commonly used compatibilizer in the field, and can improve the compatibility of the composite material and the dispersibility of the filler, so that the mechanical strength of the composite material is improved. However, in the research process of the present invention, when the inventor uses the maleic anhydride grafted polypropylene as the compatibilizer, the inventor can not obtain a good compatibility effect all the time, and if the amount of the compatibilizer is increased, the application performance of the processability of the product is affected, so the inventor tries to prepare a novel compatibilizer by using the existing substances in a laboratory to meet the processing requirement of the plastic regeneration of the present invention, and simultaneously expects that the application performance of the product can be optimized.
The compound with the novel structure is prepared from N-chlorosuccinamide and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane through one-step reaction, the preparation raw materials are easy to obtain, the preparation method is simple and convenient, and the application of the compound as a plastic compatibilizer is not reported. The invention not only realizes the new application of the compound as a plastic compatibilizer in the field, but also can obtain the effect which is obviously superior to the commonly used compatibilizer in the field under the condition of low addition amount, thereby improving the processing performance of the regenerated plastic particles, expanding the application range of the regenerated plastic particles and improving the application performance of plastic products processed by the regenerated plastic particles.
The PP waste and the PPO waste are the PP waste and the PPO waste which are washed, dried and crushed into particles, and the impurity content is lower than 0.05 percent.
The nano filler is one of nano white carbon black, nano calcium carbonate and nano talcum powder. The strength of the recycled plastic can be improved by adding the nano-filler, the processing cost is reduced, and the filling performance of the nano-filler is better than that of the conventional filler.
The plasticizer is one of dioctyl phthalate, acetyl tributyl citrate and triisopropyl silicon-based trifluoromethanesulfonate. The plasticizer is added to increase the plasticity of the polymer and enhance the flexibility of the polymer, thereby improving the processability of the recycled plastic. The triisopropyl silyl trifluoromethanesulfonate is not a plasticizer commonly used in the field and is not a known substance capable of serving as a plasticizer, but tests show that the triisopropyl silyl trifluoromethanesulfonate can achieve a plasticizing effect superior to that of dioctyl phthalate and acetyl tributyl citrate, and the application performance, particularly the mechanical performance, of a regenerated plastic product is remarkably improved.
The antioxidant is one or more of antioxidant 168, antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant 1098 and antioxidant 2246. The antioxidant can inhibit and delay the oxidation process of the polymer and improve the aging resistance of the regenerated plastic.
The flame retardant is one or more of antimony trioxide, zinc borate and magnesium hydroxide. The flame retardant is added to improve the flame retardant property of the recycled plastic and enhance the application safety of the recycled plastic.
The mass ratio of the PP waste material to the PPO waste material to the nano filler to the plasticizer to the compatibilizer to the antioxidant to the flame retardant is (50-80): 20-50): 10-20): 5-15): 0.5-5.
The temperature of the melt blending is 200-280 ℃.
The invention leads the polymer to form a melt through melt blending, and utilizes the compatibilizer to promote the compatibility of the polymer and the uniform dispersion of the filler in the polymer to obtain the regenerated plastic particles with uniform composition and structure.
Although the nano filler can be uniformly dispersed in the polymer by adding the compatibilizer, the nano filler is easy to agglomerate due to intermolecular force, electrostatic action, quantum tunneling effect, specific surface area, surface energy and the like, and the uniform dispersion in the polymer cannot be effectively realized.
In order to improve the dispersion uniformity of the nano filler in the polymer under the condition of not increasing the addition amount of the compatibilizer, the surface modification is carried out on the nano filler, and the prepared modified nano filler is used for replacing the nano filler in the technical scheme.
The modified nano filler is prepared by surface modification of nano filler, and the preparation method comprises the following steps: adding triglycidyl isocyanurate into the nano filler, heating to 110-120 ℃, carrying out heat preservation grinding, cooling and nano grinding to obtain the modified nano filler.
The nano filler is one of nano white carbon black, nano calcium carbonate and nano talcum powder.
The mass ratio of the nano filler to the triglycidyl isocyanurate is (10-20) to (5-15).
The invention uses the unique cyclic molecular structure of triglycidyl isocyanurate to include the nano particles, generates steric hindrance effect between the nano particles, reduces the attraction between the nano particles and prevents the formation of nano particle aggregates. And the compatibility between the triglycidyl isocyanurate and the polymer is good, and the uniform dispersion of the nano filler in the polymer can be further promoted.
The invention has the beneficial effects that: according to the invention, the PP waste and the PPO waste are used as main materials, and the nano filler, the plasticizer, the compatibilizer, the antioxidant and the flame retardant are added to prepare the regenerated plastic particles, so that the investment cost of the raw materials is reduced, the regeneration processing technology is greatly simplified, the regeneration utilization of the PP waste and the PPO waste is scientifically realized, and the waste of resources and the pollution to the environment after the waste are avoided; the prepared recycled plastic particles have good processing formability, and the prepared plastic products simultaneously show excellent application performance, thereby ensuring the use quality of the recycled plastic products.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The compatibilizers in the following examples were prepared using the following steps:
adding 0.05mol of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane and 0.05mol of N-chlorosuccinamide into 250mL of tetrahydrofuran, heating to 60 ℃ for heat preservation reaction, starting to dropwise add a 5% sodium bicarbonate solution (0.05mol of sodium bicarbonate in terms of solid) after 15min, continuing to perform heat preservation reaction at 60 ℃ for 30min after dropwise addition, decompressing and concentrating to recover tetrahydrofuran, adding 100mL of water into a concentrate after the tetrahydrofuran is recovered, stirring for 15min, standing for 30min, filtering, washing with water, drying, and grinding into powder to obtain the compatibilizer.1H NMR(DMSO-d6,400MHz),δ:8.87(s,1H),7.03(s,2H),4.21(s,1H),3.83(q,6H),2.76-2.68(m,4H),2.49-2.38(m,6H),1.49(s,1H),1.37(m,2H),1.21(t,9H),0.56(m,2H)；ESI-MS:m/z＝379.23[M+1]+.
Example 1
Adding 75 parts of PP waste and 45 parts of PPO waste into a high-speed mixer, adding 10 parts of nano calcium carbonate (with the average particle size of 50nm), 15 parts of dioctyl phthalate, 10 parts of the prepared compatibilizer, 1 part of antioxidant 1010 and 1 part of zinc borate, uniformly mixing, and then feeding into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6And (3) extruding and granulating at 280 ℃ and the screw rotating speed of 200r/min to obtain the regenerated plastic granules.
Example 2
Example 2 was obtained by replacing the plasticizer in example 1 with an equal amount of acetyl tributyl citrate from dioctyl phthalate.
Adding 75 parts of PP waste and 45 parts of PPO waste into a high-speed mixer, adding 10 parts of nano calcium carbonate (with the average particle size of 50nm), 15 parts of acetyl tributyl citrate, 10 parts of the prepared compatibilizer, 1 part of antioxidant 1010 and 1 part of zinc borate, uniformly mixing, and then feeding into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6And (3) extruding and granulating at 280 ℃ and the screw rotating speed of 200r/min to obtain the regenerated plastic granules.
Example 3
Example 3 was obtained by replacing the plasticizer in example 1 with dioctyl phthalate by the equivalent amount of triisopropylsilyl triflate.
Adding 75 parts of PP waste and 45 parts of PPO waste into a high-speed mixer, adding 10 parts of nano calcium carbonate (with the average particle size of 50nm), 15 parts of triisopropyl silicon-based trifluoromethanesulfonate, 10 parts of the prepared compatibilizer, 1 part of antioxidant 1010 and 1 part of zinc borate, uniformly mixing, and then feeding into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6And (3) extruding and granulating at 280 ℃ and the screw rotating speed of 200r/min to obtain the regenerated plastic granules.
Example 4
Example 4 was obtained by replacing the nano-filler of example 1 with nano-talc (average particle size 50nm) in equal amount from nano-calcium carbonate.
75 parts of PP waste and 45 parts of PPO waste are added into a high-speed mixer, and then 10 parts of nano talcum powder (with the average particle size of 50nm), 15 parts of dioctyl phthalate and 10 parts of the additive prepared by the method are addedThe solvent, 1 part of antioxidant 1010 and 1 part of zinc borate are uniformly mixed and then sent into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6And (3) extruding and granulating at 280 ℃ and the screw rotating speed of 200r/min to obtain the regenerated plastic granules.
Example 5
Example 5 was obtained by replacing the nanofiller from example 1 with an equivalent amount of modified nanocalcium carbonate.
Preparing modified nano calcium carbonate: adding 8g of triglycidyl isocyanurate into 15g of nano calcium carbonate (the average particle size is 50nm), heating to 115 ℃, preserving heat, grinding for 30min, cooling, and nano grinding to obtain the modified nano calcium carbonate.
Adding 75 parts of PP waste and 45 parts of PPO waste into a high-speed mixer, adding 10 parts of modified nano calcium carbonate (with the average particle size of 50nm), 15 parts of dioctyl phthalate, 10 parts of the prepared compatibilizer, 1 part of antioxidant 1010 and 1 part of zinc borate, uniformly mixing, and then sending into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6And (3) extruding and granulating at 280 ℃ and the screw rotating speed of 200r/min to obtain the regenerated plastic granules.
Comparative example 1
Comparative example 1 was obtained by replacing the compatibilizer in example 1 with maleic anhydride grafted polypropylene.
Adding 75 parts of PP waste and 45 parts of PPO waste into a high-speed mixer, adding 10 parts of nano calcium carbonate (with the average particle size of 50nm), 15 parts of dioctyl phthalate, 10 parts of maleic anhydride grafted polypropylene, 1 part of antioxidant 1010 and 1 part of zinc borate, uniformly mixing, and then sending into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6280 deg.C screwThe rotating speed is 200r/min, and the regenerated plastic particles are obtained by extrusion granulation.
Comparative example 2
Comparative example 2 was obtained by replacing the compatibilizer in example 1 with N- (β -aminoethyl) - γ -aminopropyltriethoxysilane.
Adding 75 parts of PP waste material and 45 parts of PPO waste material into a high-speed mixer, adding 10 parts of nano calcium carbonate (with the average particle size of 50nm), 15 parts of dioctyl phthalate, 10 parts of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, 1 part of antioxidant 1010 and 1 part of zinc borate, uniformly mixing, and then sending into a double-screw extruder for melt blending, wherein the temperature of the double-screw extruder is as follows: t is1＝200℃、T2＝230℃、T3＝250℃、T4＝260℃、T5＝270℃、T6And (3) extruding and granulating at 280 ℃ and the screw rotating speed of 200r/min to obtain the regenerated plastic granules.
The recycled plastic granules prepared in the above examples and comparative examples were processed into plastic products by injection molding process, respectively, the mold temperature of the injection molding machine was 120 ℃, the head temperature was 270 ℃, the pressure holding pressure was 5MPa, and the pressure holding time was 60s, and the performance of the prepared plastic products was tested, and the results are shown in table 1.
TABLE 1
Testing the tensile strength according to standard ASTM D638;
testing the Izod impact strength according to standard ASTM D256;
flexural strength was tested according to standard ASTM D790.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A regenerated plastic particle modification process is characterized in that: taking PP waste and PPO waste as main materials, adding nano filler, plasticizer, compatibilizer, antioxidant and flame retardant, and performing melt blending, extrusion and granulation to prepare regenerated plastic particles; the compatibilizer is prepared by reacting N-chlorosuccinamide and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane in a molar ratio of 1: 1.
2. The recycled plastic particle modification process of claim 1, wherein: the PP waste and the PPO waste are the PP waste and the PPO waste which are washed, dried and crushed into particles, and the impurity content is lower than 0.05 percent.
3. The recycled plastic particle modification process of claim 1, wherein: the nano filler is one of nano white carbon black, nano calcium carbonate and nano talcum powder.
4. The recycled plastic particle modification process of claim 1, wherein: the plasticizer is one of dioctyl phthalate, acetyl tributyl citrate and triisopropyl silicon-based trifluoromethanesulfonate.
5. The recycled plastic particle modification process of claim 1, wherein: the antioxidant is one or more of antioxidant 168, antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant 1098 and antioxidant 2246.
6. The recycled plastic particle modification process of claim 1, wherein: the flame retardant is one or more of antimony trioxide, zinc borate and magnesium hydroxide.
7. The recycled plastic particle modification process of claim 1, wherein: the mass ratio of the PP waste material to the PPO waste material to the nano filler to the plasticizer to the compatibilizer to the antioxidant to the flame retardant is (50-80): 20-50): 10-20): 5-15): 0.5-5.
8. The recycled plastic particle modification process of claim 1, wherein: the temperature of the melt blending is 200-280 ℃.
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| CN202011418000.5A CN112480540A (en) | 2020-12-07 | 2020-12-07 | Regenerated plastic particle modification process |
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| CN202011418000.5A CN112480540A (en) | 2020-12-07 | 2020-12-07 | Regenerated plastic particle modification process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521634A (en) * | 2022-10-15 | 2022-12-27 | 温州市和沐环保科技有限公司 | Regenerated flame-retardant plastic particle and processing technology thereof |
| CN116656145A (en) * | 2023-06-09 | 2023-08-29 | 界首市奥胜达塑业有限公司 | Regenerated plastic particles and production process thereof |
-
2020
- 2020-12-07 CN CN202011418000.5A patent/CN112480540A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521634A (en) * | 2022-10-15 | 2022-12-27 | 温州市和沐环保科技有限公司 | Regenerated flame-retardant plastic particle and processing technology thereof |
| CN116656145A (en) * | 2023-06-09 | 2023-08-29 | 界首市奥胜达塑业有限公司 | Regenerated plastic particles and production process thereof |
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Application publication date: 20210312 |