CN110791063A - Waste polyester particles containing micropores and preparation method and application thereof - Google Patents
Waste polyester particles containing micropores and preparation method and application thereof Download PDFInfo
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- 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
- C08J9/06—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 chemical blowing agent
- C08J9/10—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 chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- 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
- C08J9/06—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 chemical blowing agent
- C08J9/10—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 chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
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- 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
- C08J9/06—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 chemical blowing agent
- C08J9/10—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 chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/107—Nitroso compounds
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- 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
- C08J2203/18—Binary blends of expanding agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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Abstract
The application relates to the field of polyester recycling, in particular to a waste polyester particle containing micropores and a preparation method and application thereof. A waste polyester particle containing fine pores, which has an average cell diameter of 30 to 200 μm and a relative density of 0.3 to 0.7. The waste polyester particles contain a large amount of microporous structures, have higher stacking density, increase the contact surface of a solvent and solid particles, and improve depolymerization efficiency.
Description
Technical Field
The application relates to the field of recycling of waste polyester, in particular to a waste polyester particle containing micropores and a preparation method and application thereof.
Background
Polyethylene terephthalate (PET) is a polymer of terephthalic acid or dimethyl terephthalate and ethylene glycol. Due to good physical and chemical stability, processability and the like, the composite material is widely applied to the fields of textile clothing, decoration, food packaging and the like. However, because PET has very strong chemical inertness under natural conditions and is difficult to biodegrade, and a large amount of waste polyester exerts a great pressure on the environment, recycling waste polyester products, realizing effective recycling of resources, and reducing environmental pollution become important subjects of the polyester industry.
At present, the recycling of polyester waste materials mainly comprises a physical method and a chemical method. The physical method is mainly to make the waste polyester and the products thereof into regenerated chips through the processes of cutting, crushing, mixing, granulating and the like, and then reuse the regenerated chips, but the quality fluctuation of the regenerated chips is large, so that the preparation and the quality of the fibers are greatly influenced. The chemical method is mainly to depolymerize the waste polyester into raw materials or intermediates for producing the polyester by a chemical treatment method, such as a hydrolysis method, a methanol alcoholysis method, an ethylene glycol alcoholysis method and the like, and obtain high-quality raw material monomers by the procedures of purification, impurity removal and the like. At present, the pretreatment of materials before depolymerization mainly comprises the following steps: the waste silk and waste textile are cut or sheared and put into a depolymerization kettle, for example, the method of the 'pretreatment system of waste fiber and products' disclosed in the publication No. CN 105690600A. However, the bulk density of the waste is low, so that the waste is not easy to be soaked by a solvent, the liquid-solid ratio is increased, and the energy consumption and the material consumption are increased. In addition, waste silk and waste textile are made into foam materials by a friction granulation method, and then are put into a depolymerization kettle for depolymerization, for example, the method of 'recycling process of waste textile containing polyester' disclosed in the publication No. CN 105803585A. However, the rate of depolymerization is significantly reduced due to the larger size of the foam particles.
In addition, Chinese invention patents (such as publication numbers CN106283227A, CN106283226A, CN106279757A and the like) applied by Ningbo Dafa chemical fiber Limited company disclose a method for preparing high-quality melt by taking waste polyester textiles as raw materials, the method comprises the steps of adding alcohol accounting for 1-8% of the mass of the raw materials into the raw materials, feeding the mixture into a screw extruder for blending, melting and extruding, wherein the melt viscosity of the melt discharged from the screw extruder is 0.40-0.50 dl/g, feeding the material into a thermal refining and viscosity adjusting device, and the melt viscosity of the melt discharged from the thermal refining and viscosity adjusting device is 0.620 dl/g-0.685 dl/g. In the applications, the problems of short filter period and large maintenance amount of a vacuum system are effectively solved while the melt viscosity is improved by adding a proper amount of glycol, and the additional value of the product can be improved while the production cost is reduced. These patents still do not solve the technical problem of significant reduction in the rate of depolymerization due to the large size of the foam particles.
Disclosure of Invention
How to overcome the above-mentioned problem that exists among the waste polyester depolymerization process, realize not only improving the bulk density of waste material, can increase the contact surface of solvent and solid particle again, improve depolymerization efficiency and be the key of this application. Accordingly, it is a first object of the present application to provide a waste polyester particle containing micropores, which has a large amount of microporous structures, has a high bulk density, increases a contact surface of a solvent with solid particles, and improves depolymerization efficiency.
In order to achieve the first object, the following technical solutions are adopted in the present application:
a waste polyester particle containing fine pores, which has an average cell diameter of 30 to 200 μm and a relative density of 0.3 to 0.7.
Preferably, the waste polyester particles have an average cell diameter of 50 to 100 μm and a relative density of 0.35 to 0.68.
Preferably, the recycled polyester of the present application is selected from one or more of recycled polyester bottle chips, polyester pulp, polyester fiber products and polyester waste filaments.
In addition, the present application also provides a method for preparing the above waste polyester granules, comprising the steps of:
1) the recycled waste polyester is classified according to color, quality and form;
2) and (3) carrying out melt granulation in a double-screw extruder, adding a chemical foaming agent in the granulation process, and cooling to form micro holes on the surface and inside of the waste polyester particles.
As a further improvement, the step 2) is firstly carried out densification treatment through a hot friction forming process to prepare a foam material; preferably, the temperature of the hot friction forming process is 150-260 ℃, the pressure is 0.1-10 MPa, and the time is 5-15 min.
As a further improvement, the foaming agent in the step 2) is one or more of foaming agent AC, foaming agent DPT, foaming agent ABIN, foaming agent OBSH and foaming agent NTA.
As a further improvement, the twin-screw extruder in the step 2) is divided into seven areas, the temperature of each area is 220-320 ℃, the feeding percentage of the twin-screw extruder is 15-45%, the rotating speed of the screw is 40-80rpm, and the pressure is 2-10 Mpa.
As a further improvement, the foaming agent in the step 2) can be added and mixed with the recycled polyester material, or can be mixed in a fourth heating zone of the screw; the ratio of the foaming agent to the waste polyester material is 1: 100-500.
As a further improvement, the step 2) twin-screw extruder is added with a filtering device with 100-200 meshes before a die head to remove the refractory large-particle impurities in the regenerated polyester melt.
In addition, the application also provides the application of the waste polyester particles for preparing terephthalic acid, ethylene glycol, ethylene terephthalate and dimethyl terephthalate or oligomer by recycling polyester depolymerization.
Due to the adoption of the technical scheme, the method has the following characteristics:
1) the waste polyester particles contain a large amount of microporous structures, have higher stacking density, and increase the contact surface with ethylene glycol, thereby accelerating the depolymerization reaction rate, improving the yield of depolymerization products, and reducing energy consumption and production cost;
2) the waste polyester granules containing micropores have high specific surface area, and are beneficial to dissolving out residual foaming agent and contained spandex, chinlon and the like;
3) the gradient chain decomposition of different process sections can be realized for the depolymerized liquid, and the impurity content in the depolymerized product can be further reduced.
Drawings
FIG. 1 is a diagram showing the micropore effect of the waste polyester granules containing micropores prepared in example 1.
Detailed Description
Example 1
And cleaning and drying the recycled and classified Polyester (PET) bottle chips and Polyester (PET) pulp blocks, and then carrying out melt granulation in a double-screw extruder. Heating temperatures of all zones of the double-screw extruder are respectively 250 ℃, 260 ℃, 270 ℃, 280 ℃, 275 ℃, 270 ℃, feeding percentage of the screw is 15%, rotating speed is 50rpm, pressure is 3Mpa, foaming agent AC is selectively added to a micropore forming substance, the mass ratio of the foaming agent to the waste polyester is 1:200, the foaming agent is introduced into a fourth heating zone of the screw, and micropores are stably formed after granulation passes through a cooling water tank.
The waste polyester granules containing micropores prepared by the above-mentioned granulating step of microporous waste polyester have an average cell diameter of 85 μm and a relative density of 0.35. Average cell diameter test, the average of 100 average cell diameters was continuously measured as the diameter of the cells using an optical microscope. The method for testing the relative density of the microporous waste polyester refers to the GB1033-86 plastic density and relative density test method.
Putting the waste Polyester (PET) granules containing micropores into a dissolving agent containing N-N dimethylformamide and formic acid in a ratio of 1:1, heating to 120 ℃, fully soaking for 20min, performing solid-liquid separation, rinsing the waste Polyester (PET) granules containing micropores in a purified water cleaning pool, and finally drying at 150 ℃ to prepare the waste polyester granules containing micropores to be subjected to alcoholysis.
The prepared waste polyester (repeating unit) granules containing micropores and ethylene glycol are put into a depolymerization reaction kettle according to the proportion of 1:3 in mole percent, and depolymerization reaction is carried out for 1.5 hours at 196 ℃ under the catalysis of 0.2MPa and 0.2% w of zinc acetate, thus preparing the depolymerization product containing the ethylene glycol terephthalate. The prepared depolymerized liquid passes through a 100-mesh filtering device, and impurities and infusible matters in the depolymerized liquid are filtered out primarily. Obtaining high-purity depolymerization liquid.
In the depolymerization solution after the depolymerization impurity removal step, the content of chinlon is less than 0.03 percent, the content of spandex is less than 0.05 percent, and the alcoholysis rate of PET is 99.2 percent.
And (3) adding the depolymerization liquid after impurity removal and a stabilizer into a pre-polycondensation kettle together, and starting low-vacuum pre-polycondensation reaction twice under the negative pressure condition. The first pre-polycondensation is stably pumped from normal pressure to about 24Kpa absolute pressure, the temperature is controlled at 270 ℃, and the reaction time is 30 min; filtering by using a filter screen with the specification of 150 meshes after the first pre-polycondensation is finished; carrying out second pre-polycondensation reaction on the filtrate, reducing the reaction pressure to 4Kpa absolute, controlling the reaction temperature at 275 ℃ and the reaction time to be 30 min; then, the vacuum pumping is continued, the polycondensation reaction in the high vacuum stage is carried out, the reaction pressure is reduced to 0.2Kpa absolute pressure, the reaction temperature is controlled at 285 ℃, the reaction time is 3 hours, and the high-quality regenerated polyester is prepared.
The prepared regenerated polyester has the intrinsic viscosity value of 0.61dl/g, the melting point of 252 ℃, the ash content of less than or equal to 0.05 percent and the number of agglomerated particles of less than or equal to 1/mg.
Example 2
The recycled and classified Polyester (PET) film and Polyester (PET) fiber products (curtains, carpets, clothes and the like) are densified by a hot friction forming process under the conditions of 220 ℃ of temperature, 3MPa of pressure and 10min of time to prepare the foam material. And then melting and granulating the foam material in a double-screw extruder. Heating temperatures of all zones of the double-screw extruder are 265 ℃, 270 ℃, 275 ℃, 280 ℃, 275 ℃, 270 ℃ and 270 ℃, feeding percentage of the screw is 30%, rotating speed of the screw is 65rpm, pressure is 6Mpa, foaming agent ABIN is selected as a micropore forming substance, the mass ratio of the foaming agent to the waste polyester is 1:250, the foaming agent is mixed in a fourth heating zone of the screw, and micropores are stably formed after the granulation is finished and pass through a cooling water tank.
The waste polyester pellets containing fine pores prepared by the above-mentioned fine pore waste polyester pelletizing step had an average cell diameter of 82 μm and a relative density of 0.55.
Putting the waste Polyester (PET) granules containing micropores into a dissolving agent containing N-N dimethylformamide and formic acid in a ratio of 1:1, heating to 120 ℃, fully soaking for 20min, performing solid-liquid separation, rinsing the waste Polyester (PET) granules containing micropores in a purified water cleaning pool, and finally drying at 150 ℃ to prepare the waste polyester granules containing micropores to be subjected to alcoholysis.
The prepared waste polyester (repeating unit) granules containing micropores and ethylene glycol are put into a depolymerization reaction kettle according to the proportion of 1:3 in mole percent, and depolymerization reaction is carried out for 1.5 hours at 196 ℃ under the catalysis of 0.2MPa and 0.2% w of zinc acetate, thus preparing the depolymerization product containing the ethylene glycol terephthalate. The prepared depolymerized liquid passes through a 100-mesh filtering device, and impurities and infusible matters in the depolymerized liquid are filtered out primarily. Obtaining high-purity depolymerization liquid.
In the depolymerization solution after the depolymerization impurity removal step, the content of the chinlon is less than 0.04 percent, the content of the spandex is less than 0.05 percent, and the alcoholysis rate of the PET is 99.2 percent.
And (3) adding the depolymerization liquid after impurity removal and a stabilizer into a pre-polycondensation kettle together, and starting low-vacuum pre-polycondensation reaction twice under the negative pressure condition. The first pre-polycondensation is stably pumped from normal pressure to about 24Kpa absolute pressure, the temperature is controlled at 270 ℃, and the reaction time is 30 min; filtering by using a filter screen with the specification of 150 meshes after the first pre-polycondensation is finished; carrying out second pre-polycondensation reaction on the filtrate, reducing the reaction pressure to 4Kpa absolute, controlling the reaction temperature at 275 ℃ and the reaction time to be 30 min; then, the vacuum pumping is continued, the polycondensation reaction in the high vacuum stage is carried out, the reaction pressure is reduced to 0.2Kpa absolute pressure, the reaction temperature is controlled at 285 ℃, the reaction time is 3 hours, and the high-quality regenerated polyester is prepared.
The prepared regenerated polyester has the intrinsic viscosity value of 0.60dl/g, the melting point of 248 ℃, the ash content of less than or equal to 0.05 percent and the number of agglomerated particles of less than or equal to 1/mg.
Example 3
And cleaning and drying the recycled and classified Polyester (PET) bottle chips and Polyester (PET) pulp blocks, and then carrying out melt granulation in a double-screw extruder. Heating temperatures of all zones of the double-screw extruder are respectively 260 ℃, 270 ℃, 280 ℃, 285 ℃, 275 ℃, 270 ℃ and 270 ℃, screw feeding percentage is 45%, rotation speed is 45rpm, pressure is 75Mpa, screw feeding percentage is 45%, screw rotation speed is 65rpm, pressure is 8.5Mpa, foaming agent DPT and foaming agent ADC are selected as micropore forming substances, the ratio is 1:1, the mass ratio of the foaming agent to the waste polyester is 1:500, the foaming agent is mixed in a fourth heating zone of the screw in a feeding mode, and after granulation is finished, micropores are stably formed after passing through a cooling water tank.
The waste polyester pellets containing fine pores prepared by the above-mentioned fine pore waste polyester pelletizing step had an average cell diameter of 75 μm and a relative density of 0.68.
Putting the waste Polyester (PET) granules containing micropores into a dissolving agent containing N-N dimethylformamide and formic acid in a ratio of 1:1, heating to 120 ℃, fully soaking for 20min, performing solid-liquid separation, rinsing the waste Polyester (PET) granules containing micropores in a purified water cleaning pool, and finally drying at 150 ℃ to prepare the waste polyester granules containing micropores to be subjected to alcoholysis.
The prepared waste polyester (repeating unit) granules containing micropores and ethylene glycol are put into a depolymerization reaction kettle according to the proportion of 1:3 in mole percent, and depolymerization reaction is carried out for 1.5 hours at 196 ℃ under the catalysis of 0.2MPa and 0.2% w of zinc acetate, thus preparing the depolymerization product containing the ethylene glycol terephthalate. The prepared depolymerized liquid passes through a 100-mesh filtering device, and impurities and infusible matters in the depolymerized liquid are filtered out primarily. Obtaining high-purity depolymerization liquid.
In the depolymerization solution after the depolymerization impurity removal step, the content of chinlon is less than 0.03 percent, the content of spandex is less than 0.05 percent, and the alcoholysis rate of PET is 99.5 percent.
And (3) adding the depolymerization liquid after impurity removal and a stabilizer into a pre-polycondensation kettle together, and starting low-vacuum pre-polycondensation reaction twice under the negative pressure condition. The first pre-polycondensation is stably pumped from normal pressure to about 24Kpa absolute pressure, the temperature is controlled at 270 ℃, and the reaction time is 30 min; filtering by using a filter screen with the specification of 150 meshes after the first pre-polycondensation is finished; carrying out second pre-polycondensation reaction on the filtrate, reducing the reaction pressure to 4Kpa absolute, controlling the reaction temperature at 275 ℃ and the reaction time to be 30 min; then, the vacuum pumping is continued, the polycondensation reaction in the high vacuum stage is carried out, the reaction pressure is reduced to 0.2Kpa absolute pressure, the reaction temperature is controlled at 285 ℃, the reaction time is 3 hours, and the high-quality regenerated polyester is prepared.
The prepared regenerated polyester has the intrinsic viscosity value of 0.62dl/g, the melting point of 251 ℃, the ash content of less than or equal to 0.05 percent and the number of agglomerated particles of less than or equal to 1/mg.
Comparative example 1
The recycled and classified Polyester (PET) bottle chips and Polyester (PET) pulp blocks are washed and dried, and then are subjected to melt granulation in a screw extruder. The heating temperature of each zone of the double-screw extruder is respectively 250 ℃, 260 ℃, 270 ℃, 280 ℃, 275 ℃, 270 ℃, the screw feeding percentage is 20 percent, the rotating speed is 50rpm, the pressure is 5.5Mpa, and the specification of the filtering device is 200 meshes. The extruded material belt passes through a cooling water tank and is cut into granules.
The relative density of the waste polyester pellets prepared through the above waste polyester granulation step was 1.27.
The dissolving agent is selected from N-N dimethylformamide and formic acid according to the ratio of 1:1, the dipping time is controlled to be 30min, the dipping temperature is 110 ℃, the waste polyester (repeating unit) and ethylene glycol are in a molar percentage of 1:3, the depolymerization reaction temperature is 200 ℃, the pressure is 0.2MPa, and the depolymerization time is 2.5 hours, so that the final depolymerized liquid contains 0.10% of chinlon, 0.12% of spandex and 98.2% of PET alcoholysis rate.
And (3) adding the depolymerization liquid after impurity removal and a stabilizer into a pre-polycondensation kettle together, and starting low-vacuum pre-polycondensation reaction twice under the negative pressure condition. The first pre-polycondensation is stably pumped from normal pressure to about 24Kpa absolute pressure, the temperature is controlled at 270 ℃, and the reaction time is 30 min; filtering by using a filter screen with the specification of 150 meshes after the first pre-polycondensation is finished; carrying out second pre-polycondensation reaction on the filtrate, reducing the reaction pressure to 4Kpa absolute, controlling the reaction temperature at 275 ℃ and the reaction time to be 30 min; then, the vacuum pumping is continued, the polycondensation reaction in the high vacuum stage is carried out, the reaction pressure is reduced to 0.2Kpa absolute pressure, the reaction temperature is controlled at 285 ℃, the reaction time is 3 hours, and the high-quality regenerated polyester is prepared.
The prepared regenerated polyester has the intrinsic viscosity value of 0.60dl/g, the melting point of 245 ℃, the ash content of less than or equal to 0.15 percent and the number of agglomerated particles of less than or equal to 5/mg.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present disclosure, including any person skilled in the art, having the benefit of the present disclosure. Various modifications to these embodiments will be readily apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A waste polyester particle containing fine pores, characterized in that the waste polyester particle has an average cell diameter of 30 to 200 μm and a relative density of 0.3 to 0.7.
2. The waste polyester particle containing fine pores according to claim 1, wherein the waste polyester particle has an average cell diameter of 50 to 100 μm and a relative density of 0.35 to 0.68.
3. The waste polyester particle containing fine pores according to claim 1, wherein the recycled polyester is one or more selected from the group consisting of recycled polyester bottle chips, polyester pulp, polyester fiber products and polyester waste filaments.
4. The method for preparing waste polyester granules according to claim 1, comprising the steps of:
1) the recycled waste polyester is classified according to color, quality and form;
2) and (3) carrying out melt granulation in a double-screw extruder, adding a chemical foaming agent in the granulation process, and cooling to form micro holes on the surface and inside of the waste polyester particles.
5. The method of claim 4, wherein step 2) is carried out by densification by a hot friction forming process to form a foam; preferably, the temperature of the hot friction forming process is 150-260 ℃, the pressure is 0.1-10 MPa, and the time is 5-15 min.
6. The method of claim 4, wherein the blowing agent of step 2) is one or more of blowing agent AC, blowing agent DPT, blowing agent ABIN, blowing agent OBSH, and blowing agent NTA.
7. The method as claimed in claim 4, wherein the twin-screw extruder in the step 2) is divided into seven zones, the temperature of each zone is 220 ℃ and 320 ℃, the feeding percentage of the twin-screw extruder is 15-45%, the screw rotation speed is 40-80rpm, and the pressure is 2-10 MPa.
8. The method of claim 4, wherein the blowing agent of step 2) is added and mixed with the recycled polyester material, or mixed in the fourth heating zone of the screw; the ratio of the foaming agent to the waste polyester material is 1: 100-500.
9. The method as claimed in claim 4, wherein the twin-screw extruder in step 2) is provided with a 100-200 mesh filtering device before the die head to remove the refractory large particle impurities in the regenerated polyester melt.
10. The use of the waste polyester granules according to any of claims 1 to 3 for the depolymerization of recycled polyester to produce terephthalic acid, ethylene glycol, ethylene terephthalate and/or oligomers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911107887.3A CN110791063B (en) | 2019-11-13 | 2019-11-13 | Waste polyester particles containing micropores and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911107887.3A CN110791063B (en) | 2019-11-13 | 2019-11-13 | Waste polyester particles containing micropores and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
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| CN110791063A true CN110791063A (en) | 2020-02-14 |
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