CN114014754A - Application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate - Google Patents
Application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate Download PDFInfo
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- CN114014754A CN114014754A CN202111264266.3A CN202111264266A CN114014754A CN 114014754 A CN114014754 A CN 114014754A CN 202111264266 A CN202111264266 A CN 202111264266A CN 114014754 A CN114014754 A CN 114014754A
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- 229920000139 polyethylene terephthalate Polymers 0.000 title claims abstract description 75
- 239000005020 polyethylene terephthalate Substances 0.000 title claims abstract description 75
- -1 polyethylene terephthalate Polymers 0.000 title claims abstract description 28
- 238000006136 alcoholysis reaction Methods 0.000 title claims abstract description 20
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical compound CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 239000002699 waste material Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000706 filtrate Substances 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 11
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 239000007810 chemical reaction solvent Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 239000000178 monomer Substances 0.000 abstract description 22
- 239000003054 catalyst Substances 0.000 abstract description 10
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- QPKOBORKPHRBPS-UHFFFAOYSA-N bis(2-hydroxyethyl) terephthalate Chemical compound OCCOC(=O)C1=CC=C(C(=O)OCCO)C=C1 QPKOBORKPHRBPS-UHFFFAOYSA-N 0.000 abstract 1
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 239000005337 ground glass Substances 0.000 description 16
- 239000002585 base Substances 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 238000003760 magnetic stirring Methods 0.000 description 8
- 239000011541 reaction mixture Substances 0.000 description 8
- 238000004128 high performance liquid chromatography Methods 0.000 description 7
- 238000004445 quantitative analysis Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000004064 recycling Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000034659 glycolysis Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000004437 phosphorous atom Chemical group 0.000 description 2
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
- 229920000426 Microplastic Polymers 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000014171 carbonated beverage Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000006140 methanolysis reaction Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate. The catalyst provided by the invention has high catalytic activity, does not contain metal, has strong thermal stability, is not easy to decompose at high temperature, and is easy to recycle; the technical scheme provided by the invention can degrade PET 100% under a certain condition, has high BHET monomer selectivity and easy separation of reaction products, and solves the problems of metal residue, low yield, low reaction rate and the like in the ethylene glycol alcoholysis process of waste PET in the prior art.
Description
Technical Field
The invention belongs to the field of polymer plastic degradation, and particularly relates to application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate.
Background
Polyethylene terephthalate (PET) is obtained by direct esterification of high-Purity Terephthalic Acid (PTA) and Ethylene Glycol (EG) and then further polycondensation, has the advantages of good air tightness, high transparency, light weight, excellent mechanical property, chemical stability, no smell, no odor, no toxicity and the like, and is widely applied to the fields of fiber films, food packaging, mineral water bottles, carbonated beverage bottles and the like. PET production and consumption are increasing year by year, resulting in the production of large quantities of PET waste; meanwhile, the waste PET is difficult to degrade in natural environment, and causes the problems of white pollution, micro plastic pollution and the like to the environment; therefore, recycling of waste PET is attracting much attention.
At present, the recovery of waste PET comprises a physical recovery method and a chemical recovery method, wherein the physical recovery method accounts for more than 90% in China, the physical recovery method is a method for obtaining a new PET material through simple high-temperature melt molding, but the physical recovery method has the problems of degraded use, reduced product quality, reduced molecular weight and intrinsic viscosity, secondary pollution, limited recovery times and the like. The chemical recovery method converts the waste PET into monomers through chemical reaction, is not limited by PET raw material sources, does not reduce the quality of regenerated products, and can realize efficient closed-loop recycling of the waste PET. In addition, the chemical recovery method can also be used for producing products such as polyurethane, unsaturated polyester and the like. Therefore, compared with a physical recovery method, the chemical recovery method is a more effective method for recovering the waste PET, and can improve the utilization level of resources. The chemical recovery processes mainly include pyrolysis, hydrolysis, glycolysis, methanolysis, other alcoholysis processes and amine/ammonolysis processes. Among them, the glycolysis method has the advantages of less volatilization of solvent, less reaction substance, mild reaction condition, continuous production, direct repolymerization of main product ethylene terephthalate (BHET) into new PET, and the like, and is considered to be one of the most promising methods. However, the glycol alcoholysis method is still mostly used for chemically recycling PET and adopts a catalyst containing heavy metals, and heavy metal residues exist in the product; the problems of low yield, low reaction rate and the like exist in the prior art of adopting a nonmetal catalyst to degrade PET.
The phosphazene base is a kind of aprotic strong base, the structure of which at least comprises one P atom and four N atoms, the P atom and the N atoms are combined through covalent bonds, Schwesinger and the like name the phosphazene base as P according to the difference of the number of P ═ N in the molecule1To P5. The alkali is characterized by strong alkalinity which is stronger than that of other amine or amidine alkali, and most phosphazene alkali can catalyze the ring-opening polymerization of cyclic monomers. The invention takes phosphazene base as a catalyst to carry out high-efficiency alcoholysis on the waste PET, and provides a new method for recycling the waste PET.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing the application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate aiming at the defects of the prior art.
In order to solve the technical problem, the invention discloses application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate (PET), wherein the reaction equation is as follows:
wherein the phosphazene base comprises t-BuP1、t-BuP2、t-BuP3、t-BuP4、t-BuP5。
Wherein the polyethylene terephthalate includes, but is not limited to, waste polyethylene terephthalate; the waste polyethylene terephthalate includes, but is not limited to, waste beverage bottles.
Wherein the usage amount of the phosphazene base is 5-100 mu L/g of polyethylene terephthalate, preferably 20-70 mu L/g of polyethylene terephthalate, and more preferably 20-40 mu L/g of polyethylene terephthalate.
The alcohol compound is used as a reaction solvent, and the polyethylene terephthalate is subjected to alcoholysis reaction under the catalysis of phosphazene base to obtain a polyethylene terephthalate (BHET) monomer.
Wherein the alcohol compound is ethylene glycol.
Wherein the mass ratio of the polyethylene terephthalate to the alcohol compound is 1: 2-6, preferably 1: 4-5.
Wherein the reaction temperature is 160-200 ℃, preferably 170-200 ℃, and further preferably 180-190 ℃.
Wherein the pressure of the reaction is 1.0 atm.
Wherein the reaction time is 0.5-3 h, preferably 1-3 h.
After the alcoholysis reaction is finished, carrying out first filtration to obtain a first filtrate; adding water into the obtained first filtrate, and carrying out second filtration to obtain a second filtrate; evaporating the obtained second filtrate, cooling and crystallizing to obtain the ethylene glycol terephthalate crystal.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) the catalyst used in the method provided by the invention does not contain metal, the problem of heavy metal residue of a product in the alcoholysis process of the waste PET glycol in the prior art is solved, and meanwhile, the catalyst has strong thermal stability, is not easy to decompose at high temperature, is convenient for recycling, and has wide application prospect.
(2) The catalyst provided by the invention has high catalytic activity, can degrade PET by 100% under a certain condition, has high BHET monomer selectivity and yield, and solves the problems of low reaction rate, low yield and the like in the ethylene glycol alcoholysis process of waste PET in the prior art.
Drawings
The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
FIG. 1 is a PET alcoholysis experiment device, in which 1 is a magnetic stirrer, 2 is a precise electronic temperature controller, 3 is an oil bath pan, 4 is a 25mL ground glass reaction tube, and 5 is a magnetic rotor.
Detailed Description
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Experiments were carried out in the examples described below using the apparatus shown in FIG. 1.
The degradation rate of PET and the selectivity and yield of the product BHET described in the following examples were calculated according to the equations (1) (2) (3), respectively:
yield of the product BHET ═ degradation rate of PET x selectivity of the product BHET x 100% (3)
Example 1
1g of waste PET, 4g of ethylene glycol solvent, 30. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor2And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 185 ℃ and the pressure to be 1atm, and reacting for 1.5 h. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 89.2%.
Example 2
1g of a glass reaction tube with a 25mL ground mouth equipped with a thermometer and a magnetic stirring rotor was added in sequenceWaste PET, 4g of ethylene glycol solvent, 30. mu. L t-BuP2And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 190 ℃ and the pressure to be 1atm, and reacting for 1.5 h. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 93.8%.
Example 3
1g of waste PET, 4g of ethylene glycol solvent, 20. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor2And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 185 ℃, and the pressure to be 1atm, and reacting for 2 hours. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 87.7%.
Example 4
1g of waste PET, 4g of ethylene glycol solvent, 40. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor2And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 180 ℃ and the pressure to be 1atm, and reacting for 1.5 h. After the reaction was completed, the reaction mixture was filtered while it was hot,unreacted PET was separated and dried to constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 91.8%.
Example 5
1g of waste PET, 5g of ethylene glycol solvent, 40. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor2And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 185 ℃, and the pressure to be 1atm, and reacting for 1 h. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 92.4%.
Example 6
1g of waste PET, 5g of ethylene glycol solvent, 30. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor2And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 190 ℃ and the pressure to be 1atm, and reacting for 1 h. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution is subjected to volume fixing in a 1000mL volumetric flask by deionized water, and the BHET yield is passed through high-efficiency liquidQuantitative analytical determination of phase chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 89.1%.
Example 7
1g of waste PET, 4g of ethylene glycol solvent, 30. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor4And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 185 ℃ and the pressure to be 1atm, and reacting for 1.5 h. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Under these conditions, the degradation rate of PET was 100% and the yield of BHET monomer was 78.2%.
Example 8
1g of waste PET, 4g of ethylene glycol solvent, 40. mu. L t-BuP were added sequentially to a 25mL ground glass reaction tube equipped with a thermometer and a magnetic stirring rotor4And (3) putting the ground glass reaction tube into an oil bath for heating, controlling the reaction temperature to be 185 ℃ and the pressure to be 1atm, and reacting for 1.5 h. After the reaction was completed, the reaction mixture was filtered while it was hot, and unreacted PET was separated and dried to a constant weight. Adding a certain amount of deionized water into the filtrate for dissolving, and filtering to separate incompletely degraded flocculent oligomer. The filtered solution was made to volume with deionized water in a 1000mL volumetric flask and the BHET yield was determined by quantitative analysis by high performance liquid chromatography. Then, the solution in the volumetric flask was rotary evaporated at 70 ℃ to 60mL, cooled at 0 ℃ for 12 hours to precipitate white acicular BHET crystals, which were then dried and recrystallized to obtain pure BHET monomer. Degradation of PET under these conditionsThe rate was 100%, and the yield of BHET monomer was 82.2%.
Example 9
Under the same reaction conditions as in example 2, after the catalyst was used for the first time, the precipitated white acicular BHET crystals were filtered to obtain a catalyst containing t-BuP2And the unreacted glycol solution filtrate is placed in a vacuum drying oven at 60 ℃ to remove trace moisture, fresh glycol solution is supplemented before the next use, and 1g of waste PET is added to carry out a PET alcoholysis experiment. When the catalyst is used for the second time, the degradation rate of PET is 100 percent, and the yield of BHET monomer is 88.4 percent.
The present invention provides a method and a concept for the application of phosphazene base in the catalytic alcoholysis of polyethylene terephthalate, and a method and a way for implementing the technical scheme are many, and the above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (10)
1. The application of phosphazene base in catalytic alcoholysis of polyethylene terephthalate.
2. Use according to claim 1, wherein the polyethylene terephthalate is waste polyethylene terephthalate.
3. The use according to claim 1, wherein the phosphazene base is used in an amount of 5 to 100 μ L/g of polyethylene terephthalate.
4. The use of claim 1, wherein the alcoholysis reaction of polyethylene terephthalate is carried out under the catalysis of phosphazene base by using alcohol compound as reaction solvent.
5. Use according to claim 4, wherein the alcoholic compound is ethylene glycol.
6. The use according to claim 4, wherein the mass ratio of the polyethylene terephthalate to the alcohol compound is 1 (2-6).
7. The use according to claim 4, wherein the reaction temperature is 160-200 ℃.
8. Use according to claim 4, wherein the pressure of the reaction is 1.0 atm.
9. The use according to claim 4, wherein the reaction time is 0.5 to 3 hours.
10. The use of claim 4, wherein after the alcoholysis reaction is completed, a first filtration is performed to obtain a first filtrate; adding water into the obtained first filtrate, and carrying out second filtration to obtain a second filtrate; evaporating the obtained second filtrate, cooling and crystallizing to obtain the ethylene glycol terephthalate crystal.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591168A (en) * | 2022-03-31 | 2022-06-07 | 南京大学 | Heteroatom-doped zinc oxide catalyzed waste PET glycolysis method |
| CN115055175A (en) * | 2022-06-16 | 2022-09-16 | 南京大学 | Preparation method of defect-state zinc oxide nanosheet catalyst for alcoholysis of PET |
-
2021
- 2021-10-28 CN CN202111264266.3A patent/CN114014754A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| KAZUKI FUKUSHIMA 等: "Unexpected Efficiency of Cyclic Amidine Catalysts in Depolymerizing Poly(ethylene terephthalate)", 《JOURNAL OF POLYMER SCIENCE, PART A: POLYMER CHEMISTRY 》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591168A (en) * | 2022-03-31 | 2022-06-07 | 南京大学 | Heteroatom-doped zinc oxide catalyzed waste PET glycolysis method |
| CN114591168B (en) * | 2022-03-31 | 2023-06-09 | 南京大学 | Method for catalyzing waste PET glycol alcoholysis by using heteroatom doped zinc oxide |
| CN115055175A (en) * | 2022-06-16 | 2022-09-16 | 南京大学 | Preparation method of defect-state zinc oxide nanosheet catalyst for alcoholysis of PET |
| CN115055175B (en) * | 2022-06-16 | 2023-05-16 | 南京大学 | Preparation method of defect-state zinc oxide nano-sheet catalyst for alcoholysis of PET |
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Application publication date: 20220208 |