Method for manufacturing textile waste into fiber grade polyester chips applicable to textile processing

Abstract

The present invention provides a method for manufacturing textile waste into fiber grade polyester chips applicable to textile processing. The method comprises textile waste crushing, alcoholysis, filtering and separation, cooling crystallization, pressing, decoloration, distillation purification, preheating, prepolycondensation, polycondensation, cooling strip casting, and cutting into particles. By reducing textile waste to high purity bis(2-hydroxyethyl)terephthalate (hereinafter referred to as BHET), fiber grade polyester chips applicable to textile processing are re-manufactured. Thus, efficient recycling is achieved.

Claims

1. A method for manufacturing textile waste into fiber grade polyester chips applicable to textile processing, comprising the following steps: 1. cutting the textile waste into sheet materials; 2. adding the sheet materials into an alcoholysis device; adding triethylene glycol in the alcoholysis device according to mass percentage ratio 1:2-1:1.25; adding evocating agent n the alcoholysis device; stirring for 1-4 hours under a temperature of 190 C.-260 C. and a pressure of 0.1 MPa-0.4 MPa to obtain a crude Bis(2-Hydroxyethyl) terephthalate (BHET) solution; 3. filtering out solid impurities in the crude BHET solution to obtain a preliminary purified crude BHET solution, 4. cooling and crystalizing the preliminary purified crude BHET solution to obtain crude BHET suspension; 5. pressing the crude BHET suspension to obtain crude BHET cake and to remove triethylene glycol solution that contains impurities; 6. adding glycol of 25%-85% of a volume of the crude BHET cake to the crude BHET cake to obtain a mixture; heating the mixture to 60-150 C., adding in decolorizer that absorbs color into the mixture to achieve decoloring, stirring the mixture, filtering out the decolorizer to obtain a BHET mixed solution; 7. pressing the BHET mixed solution to remove free glycol, thereby obtaining a processed BHET cake; 8. heating the processed BHET cake such that the processed BHET cake becomes a melt; transferring the melt to a distillation device to distill and purify so as to remove the glycol and high-boiling residues, thereby obtaining a refined BHET melt of purity over 99.6%; 9. placing the refined BHET melt into a preheating tank; heating up the refined BHET melt to 200 C.-240 C.; adding catalysts, stabilizers, brighteners and toners into the preheating tank; 10. placing the preheated refined BHET melt into a pre-polycondensation kettle to perform dealcoholization; adding inorganic additives and dispersing agents into the pre-polycondensation kettle; removing glycol from the preheated refined BHET melt by vaporization under low vacuum condition, thereby obtaining a BHET low polymer; 11. filtering the BHET low polymer; placing the filtered BHET low polymer into a final polycondensation reactor to perform polycondensation reaction; wherein a temperature of the polycondensation reaction is controlled within a range from 270-295 C.; intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under high vacuum condition in the final polycondensation reactor, thereby obtaining a PET melt; 12. filtering the PET melt, and then transferring the filtered PET melt to a spinneret which extrudes the filtered PET melt into extruded belts; using an underwater granulator to cool the extruded belts and then crush the extruded belts into granules, thereby obtaining the recycled fiber grade polyester chips.

2. The method as in claim 1, wherein in said step 2, the evocating agent is a compound comprising sodium hydroxide and cobalt acetate.

3. The method as in claim 1 wherein in said step 3, the step of filtering out solid impurities in the crude BHET solution is performed via multi-stage filtration, and filtered solution is output by overflow at high level from the ground.

4. The method as in claim 1, wherein in said step 3, a filter for performing the step of filtering out solid impurities in the crude BHET solution is a backwashable self-cleaning filter.

5. The method as in claim 1, wherein in said step 4, a temperature of performing said step of cooling and crystalizing is controlled within a range from 0 C.-80 C.

6. The method as in claim 1, wherein in said step 6, the decolorizer is a compound that mainly comprises activated aluminium oxide; a filter that performs the step of filtering out the decolorizer has a mesh size of 100-800 m.

7. The method as in claim 1, wherein in said step 8, a temperature of distilling the melt is controlled within a range from 100 C.-260 C., and a degree of vacuum is 20 MPa-12000 Pa.

8. The method as in claim 1, wherein in said step 9, the catalysts are antimony catalysts, the stabilizers are phosphorus stabilizers, the brighteners are phthalimide type brighteners and the toners are food grade toners.

9. The method as in claim 1, wherein in said step 11, the intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under 2-4 hours of high vacuum condition of 20-100 Pa.

10. The method as in claim 1, wherein in said step 12, the recycled fiber grade polyester chips eventually obtained have intrinsic viscosity of 0.62-0.72; an amount of terminal carboxyl group 28 mmol/kg; contents of diethylene glycol 1.2%; melting point 258 C.; and contents of additives 0.3-3%.

11. The method as in wherein the textile waste is worn-out clothes or scraps of chemical fiber cloth; and the textile waste contains more than 65% of polyethylene terephthalate (PET).

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0044] FIG. 1 is a flow diagram illustrating the method according to the present invention.

DETAILED DESCRIPTION OF THE INVENTION

Embodiment 1

[0045] A method for manufacturing textile waste into fiber grade polyester chips applicable to textile processing, comprising the following steps:

[0046] 1. cutting the textile waste into sheet materials;

[0047] 2. adding the sheet materials into an alcoholysis device; adding triethylene glycol in the alcoholysis device according to mass percentage ratio 1:2; adding evocating agent in the alcoholysis device; stirring for 1 hour under a temperature of 190 C. and a pressure of 0.1 MPa to obtain a crude Bis(2-Hydroxyethyl) terephthalate (BHET) solution;

[0048] 3. filtering out solid impurities in the crude BHET solution to obtain a preliminary purified crude BHET solution;

[0049] 4. cooling and crystalizing the preliminary purified crude BHET solution to obtain crude BHET suspension;

[0050] 5. pressing the crude BHET suspension to obtain crude BHET cake and to remove triethylene glycol solution that contains impurities;

[0051] 6. adding glycol of 25% of a volume of the crude BHET cake to the crude BHET cake to obtain a mixture; heating the mixture to 60 C., adding in decolorizer that absorbs color into the mixture to achieve decoloring, stirring the mixture, filtering out the decolorizer to obtain a BHET mixed solution;

[0052] 7. pressing the BHET mixed solution to remove free glycol, thereby obtaining a processed BHET cake;

[0053] 8. heating the processed BHET cake such that the processed BHET cake becomes a melt; transferring the melt to a distillation device to distill and purify so as to remove the glycol and high-boiling residues, thereby obtaining a refined BHET melt of purity over 99.6%;

[0054] 9. placing the refined BHET melt into a preheating tank; heating up the refined BHET melt to 200 C.; adding catalysts, stabilizers, brighteners and toners into the preheating tank;

[0055] 10. placing the preheated refined BHET melt into a pre-polycondensation kettle to perform dealcoholization; adding inorganic additives and dispersing agents into the pre-polycondensation kettle; removing glycol from the preheated refined BHET melt by vaporization under low vacuum condition, thereby obtaining a BHET low polymer;

[0056] 11. filtering the BHET low polymer; placing the filtered BHET low polymer into a final polycondensation reactor to perform polycondensation reaction; wherein a temperature of the polycondensation reaction is controlled at 270 C.; intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under high vacuum condition in the final polycondensation reactor, thereby obtaining a PET melt;

[0057] 12. filtering the PET melt, and then transferring the filtered PET melt to a spinneret which extrudes the filtered PET melt into extruded belts; using an underwater granulator to cool the extruded belts and then crush the extruded belts into granules, thereby obtaining recycled fiber grade polyester chips.

[0058] The reason for using triethylene glycol as the solvent is based on the differential characteristics that textile products can turn to liquid by means of alcoholysis while other inorganic impurities and non-polyester plastic materials are insoluble by triethylene glycol. Therefore, by using filters and material output devices, the present invention obtains crude BHET solution by preliminary filtering out impurities such as sand and dust, buttons, zippers and other non-polyester plastic materials.

[0059] Triethylene glycol is selected as a solvent because it has a boiling temperature as high as 285 C. Therefore, triethylene glycol is very suitable to be used for melting and depolymerizing textile waste under a high temperature condition.

[0060] A filter that filters the decolorizer which is inorganic should have appropriate mesh size and should enable quick replacement of a filter net of the filter.

[0061] The present invention is configured to have a suitable distill temperature and a reasonably adjusted degree of vacuum to facilitate separation of residue impurities out of the BHET, thereby ensuring purity of the material and maximally inhibiting occurrence of by-products.

[0062] The BHET mixed solution obtained in step 6 having improved hue is obtained by adding in the decolorizer that decolorizes by color absorption into the crude BHET cake, stirring sufficiently and subsequently filtering out the decolorizer.

[0063] In step 10, the additives are formed as suspension by mixing and grinding, and by controlling the timing of adding the suspension into the reaction system (i e, adding the suspension to the preheated refined BHET melt when the preheated refined BHET melt has a relative low degree of polymerization, and then stirring the preheated refined BHET melt added with the suspension, and during stirring, also adding in the dispersing agent), the inorganic additives can be sufficiently moist and dispersed.

[0064] Further, in said step 2, the evocating agent is a compound comprising sodium hydroxide and cobalt acetate.

[0065] The use of compound comprising sodium hydroxide and cobalt acetate as the evocating agent can properly meet the needs of the present invention in that it increases the speed and thus the effectiveness of textile waste decomposition.

[0066] Further, in said step 3, the step of filtering out solid impurities in the crude BHET solution is performed via multi-stage filtration, and filtered solution is output by overflow at high level from the ground.

[0067] Based on the differential characteristics that textile products can turn to liquid by means of alcoholysis while other inorganicimpurities and non-polyester plastic materials are insoluble, the present invention uses a filter of multi-stage filtration and outputs filtered solution at high level from the ground, thereby filtering out solid impurities including sand and dust, buttons, zippers and other non-polyester plastic materials,

[0068] Further, in said step 3, a filter for performing the step of filtering out solid impurities in the crude BHET solution is a backwashable self-cleaning filter.

[0069] A backwashable self-cleaning multi-stage filtration filter ensures that the solid impurities including sand and dust, buttons, zippers and other non-polyester plastic materials, in the crude BHET solution can be effectively filtered out.

[0070] Further, in said step 4, a temperature of performing said step of cooling and crystalizing is controlled at 0 C.;

[0071] Further, in said step 6, the decolorizer is a compound that mainly comprises activated aluminium oxide; the filter that performs the step of filtering out the decolorizer has a mesh size of 100-800 m.

[0072] The decolorizer is a compound formula to ensure decoloring effect. The filter that filters the decolorizer which is inorganic should have appropriate mesh size and should enable quick replacement of a filter net of the filter.

[0073] Further, in said step 8, a temperature of distilling the melt is controlled at 100 C., and a degree of vacuum is 20 MPa.

[0074] Further, in said step 9, the catalysts are antimony catalysts, the stabilizers are phosphorus stabilizers, the brighteners are phthalimide type brighteners and the toners are food grade toners.

[0075] The added brighteners and toners can effective improve the hue and appearance of the recycled fiber grade polyester chips, such that a b* value of the eventually obtained recycled fiber grade polyester chips is 6.

[0076] The selected catalysts and stabilizers are suitable for effective polycondensation in the recycling of BHET, and can effective inhibit side reaction.

[0077] Further, in said step 11, the intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under 2-4 hours of high vacuum condition of 20-100 Pa.

[0078] The intrinsic viscosity is effectively increased by properly selecting the degree of vacuum and duration under the selected vacuum condition.

[0079] Further, in said step 12, the recycled fiber grade polyester chips eventually obtained have intrinsic viscosity of 0.62; an amount of terminal carboxyl group 28 mmol/kg; contents of diethylene glycol 1.2%; melting point 258 C.; and contents of additives 0.3-3%.

[0080] Further, the textile waste is worn-out clothes or scraps of chemical fiber cloth; and the textile waste contains more than 65% of polyethylene terephthalate (PET).

[0081] Preferably, the textile waste contains more than 65% mass percentage of PET, while other impurities shall be filtered out.

[0082] In general, percentages of the other impurities in the textile waste are: accessory items such as buttons and zippers 3-6%, non-PET impurities such as cotton yarn 11-25%, and other trivial impurities in the textile waste such as dust, sand and water 1-4%.

Embodiment 2

[0083] A method for manufacturing textile waste into fiber grade polyester chips applicable to textile processing, comprising the following steps:

[0084] 1. cutting the textile waste into sheet materials;

[0085] 2. adding the sheet materials into an alcoholysis device; adding triethylene glycol in the alcoholysis device according to mass percentage ratio 1:1.25; adding evocating agent in the alcoholysis device; stirring for 4 hours under a temperature of 260 C. and a pressure of 0.4 MPa to obtain a crude Bis(2-Hydroxyethyl) terephthalate (BHET) solution;

[0086] 3. filtering out solid impurities in the crude BHET solution to obtain a preliminary purified crude BHET solution;

[0087] 4. cooling and crystalizing the preliminary purified crude BHET solution to obtain crude BHET suspension;

[0088] 5. pressing the crude BHET suspension to obtain crude BHET cake and to remove triethylene glycol solution that contains impurities;

[0089] 6. adding glycol of 85% of a volume of the crude BHET cake to the crude BHET cake to obtain a mixture; heating the mixture to 150 C., adding in decolorizer that absorbs color into the mixture to achieve decoloring, stirring the mixture, filtering out the decolorizer to obtain a BHET mixed solution;

[0090] 7. pressing the BHET mixed solution to remove free glycol, thereby obtaining a processed BHET cake;

[0091] 8. heating the processed BHET cake such that the processed BHET cake becomes a melt; transferring the melt to a distillation device to distill and purify so as to remove the glycol and high-boiling residues, thereby obtaining a refined BHET melt of purity over 99.6%;

[0092] 9. placing the refined BHET melt into a preheating tank; heating up the refined BHET melt to 240 C.; adding catalysts, stabilizers, brighteners and toners into the preheating tank;

[0093] 10. placing the preheated refined BHET melt into a pre-polycondensation kettle to perform dealcoholization; adding inorganic additives and dispersing agents into the pre-polycondensation kettle; removing glycol from the preheated refined BHET melt by vaporization under low vacuum condition, thereby obtaining a BHET low polymer;

[0094] 11. filtering the BHET low polymer; placing the filtered BHET low polymer into a final polycondensation reactor to perform polycondensation reaction; wherein a temperature of the polycondensation reaction is controlled at 295 C.; intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under high vacuum condition in the final polycondensation reactor, thereby obtaining a PET melt;

[0095] 12. filtering the PET melt, and then transferring the filtered PET melt to a spinneret which extrudes the filtered PET melt into extruded belts; using an underwater granulator to cool the extruded belts and then crush the extruded belts into granules, thereby obtaining recycled fiber grade polyester chips.

[0096] Further, in said step 2, the evocating agent is a compound comprising sodium hydroxide and cobalt acetate.

[0097] Further, in said step 3, the step of filtering out solid impurities in the crude BHET solution is performed via multi-stage filtration, and filtered solution is output by overflow at high level from the ground.

[0098] Further, in said step 3, a filter for performing the step of filtering out solid impurities in the crude BHET solution is a backwashable self-cleaning filter.

[0099] Further, in said step 4, a temperature of performing said step of cooling and crystalizing is controlled at 80 C.

[0100] Further, in said step 6, the decolorizer is a compound that mainly comprises activated aluminium oxide; a filter that performs the step of filtering out the decolorizer has a mesh size of 800 m.

[0101] Further, in said step 8, a temperature of distilling the melt is controlled at 260 C., and a degree of vacuum is 12000 Pa.

[0102] Further, in said step 9, the catalysts are antimony catalysts, the stabilizers are phosphorus stabilizers, the brighteners are phthalimide type brighteners and the toners are food grade toners.

[0103] Further, in said step 11, the intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under 4hours of high vacuum condition of 100 Pa.

[0104] Further, in said step 12, the recycled fiber grade polyester chips eventually obtained have intrinsic viscosity of 0.72; an amount of terminal carboxyl group 28 mmol/kg; contents of diethylene glycol 1.2%; melting point 258 C.; and contents of additives 3%.

[0105] Further, the textile waste is worn-out clothes or scraps of chemical fiber cloth; and the textile waste contains more than 65% of polyethylene terephthalate (PET).

Embodiment 3

[0106] A method for manufacturing textile waste into fiber grade polyester chips applicable to textile processing, comprising the following steps;

[0107] 1. cutting the textile waste into sheet materials;

[0108] 2. adding the sheet materials into an alcoholysis device: adding triethylene glycol in the alcoholysis device according to mass percentage ratio 1:1.5; adding evocating agent in the alcoholysis device; stirring for 3 hours under a temperature of 200 C. and a pressure of 0.25 MPa to obtain a crude Bis(2-Hydroxyethyl) terephthalate (BHET) solution;

[0109] 3. filtering out solid impurities in the crude BHET solution to obtain a preliminary purified crude BHET solution;

[0110] 4. cooling and crystalizing the preliminary purified crude BHET solution to obtain crude BHET suspension;

[0111] 5. pressing the crude BHET suspension to obtain crude BHET cake and to remove triethylene glycol solution that contains impurities,

[0112] 6. adding glycol of 60% of a volume of the crude BHET cake to the crude BHET cake to obtain a mixture; heating the mixture to 100 C., adding in decolorizer that absorbs color into the mixture to achieve decoloring, stirring the mixture, filtering out the decolorizer to obtain a BHET mixed solution;

[0113] 7. pressing the BHET mixed solution to remove free glycol, thereby obtaining a processed BHET cake;

[0114] 8. heating the processed BHET cake such that the processed BHET cake becomes a melt; transferring the melt to a distillation device to distill and purify so as to remove the glycol and high-boiling residues, thereby obtaining a refined BHET melt of purity over 99.6%;

[0115] 9. placing the refined BHET melt into a preheating tank; heating up the refined BHET melt to 220 C.; adding catalysts, stabilizers, brighteners and toners into the preheating tank;

[0116] 10. placing the preheated refined BHET melt into a pre-polycondensation kettle to perform dealcoholization; adding inorganic additives and dispersing agents into the pre-polycondensation kettle; removing glycol from the preheated refined BHET melt by vaporization under low vacuum condition, thereby obtaining a BHET low polymer;

[0117] 11. filtering the BHET love polymer; placing the filtered BHET low polymer into a final polycondensation reactor to perform polycondensation reaction; wherein a temperature of the polycondensation reaction is controlled at 280 C.; intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under high vacuum condition in the final polycondensation reactor, thereby obtaining a PET melt;

[0118] 12. filtering the PET melt, and then transferring the filtered PET melt to a spinneret which extrudes the filtered PET melt into extruded belts; using an underwater granulator to cool the extruded belts and then crush the extruded belts into granules, thereby obtaining recycled fiber grade polyester chips.

[0119] Further, in said step 2, the evocating agent is a compound comprising sodium hydroxide and cobalt acetate.

[0120] Further, in said step 3, the step of filtering out solid impurities in the crude BHET solution is performed via multi-stage filtration, and filtered solution is output by overflow at high level from the ground.

[0121] Further, in said step 3, a filter for performing the step of filtering out solid impurities in the crude BHET solution is a backwashable self-cleaning filter.

[0122] Further, in said step 4, a temperature of performing said step of cooling and crystalizing is controlled at 40 C.

[0123] Further, in said step 6, the decolorizer is a compound that mainly comprises activated aluminium oxide; a filter that performs the step of filtering out the decolorizer has a mesh size of 100-800 m.

[0124] Further, in said step 8, a temperature of distilling the melt is controlled at 200 C., and a degree of vacuum is 10000 Pa.

[0125] Further, in said step 9, the catalysts are antimony catalysts, the stabilizers are phosphorus stabilizers, the brighteners are phthalimide type brighteners and the toners are food grade toners.

[0126] Further, in said step 11, the intrinsic viscosity of the filtered BHET low polymer under polycondensation reaction is increased under 3hours of high vacuum condition of 80 Pa.

[0127] Further, in said step 12, the recycled fiber grade polyester chips eventually obtained have intrinsic viscosity of 0.7; an amount of terminal carboxyl group 28 mmol/kg, contents of diethylene glycol 1.2%; melting point 258 C.; and contents of additives 0.3-3%.

[0128] Further, the textile waste is worn-out clothes or scraps of chemical fiber cloth; and the textile waste contains more than 65% of polyethylene terephthalate (PET).