CN110818559A - Method for recycling trimellitic anhydride rectification mother liquor residues - Google Patents
Method for recycling trimellitic anhydride rectification mother liquor residues Download PDFInfo
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- CN110818559A CN110818559A CN201911172010.2A CN201911172010A CN110818559A CN 110818559 A CN110818559 A CN 110818559A CN 201911172010 A CN201911172010 A CN 201911172010A CN 110818559 A CN110818559 A CN 110818559A
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- trimellitic anhydride
- organic phase
- recycling
- mother liquor
- ester
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- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000012452 mother liquor Substances 0.000 title claims abstract description 16
- 238000004064 recycling Methods 0.000 title claims abstract description 13
- 150000002148 esters Chemical class 0.000 claims abstract description 39
- 239000012074 organic phase Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 15
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 13
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000007865 diluting Methods 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 16
- 239000008346 aqueous phase Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 230000032050 esterification Effects 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 229940093499 ethyl acetate Drugs 0.000 claims description 2
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims description 2
- 229940011051 isopropyl acetate Drugs 0.000 claims description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 abstract 1
- 239000012295 chemical reaction liquid Substances 0.000 description 9
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/94—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the iron group metals or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of environment-friendly solvents, and particularly discloses a method for recycling trimellitic anhydride rectification mother liquor residues, which comprises the following steps: the trimellitic anhydride residue and alcohol are esterified to obtain crude ester, and the crude ester is dissolved in a certain amount of organic solventDissolving and diluting the mixed ester, extracting with a diluted acid aqueous solution in a certain proportion, extracting cobalt and manganese metal ions in the trimellitic anhydride residue into a water phase for recovery, sequentially washing the organic phase with pure water to be neutral, and rectifying the washed organic phase to remove the solvent to obtain the mixed ester. The mixed ester prepared by the invention has the ester content of more than 99 percent and the volume resistivity of more than 109Omega cm, the method is simple to operate and convenient to produce, and the resource utilization rate is improved.
Description
Technical Field
The invention relates to the technical field of environment-friendly solvents, in particular to a method for recycling trimellitic anhydride rectification mother liquor residues.
Background
The mixed ester prepared from the trimellitic anhydride rectification mother liquor residue and alcohol can be used as a plasticizer, has low volatility, excellent heat resistance, small migration, good electrical insulation, durability, low toxicity, water resistance and proper compatibility, is suitable for plastics such as polyvinyl chloride, vinyl chloride copolymer, cellulose nitrate, ethyl cellulose and the like, and can also be used as heat-resistant wire and cable materials, plates, sheets, gaskets and the like.
The method can separate the metal ions of cobalt and manganese in the trimellitic anhydride rectification mother liquor residue, and the trimellitic anhydride and the homologues thereof are prepared into mixed ester, so that the useful components in the solid waste can be fully recycled, and the solid waste output is reduced.
After examining a large number of documents, no invention report about the recovery of useful components in the trimellitic anhydride rectification mother liquor residue exists at home and abroad at present.
Disclosure of Invention
The invention aims to provide a method for recycling trimellitic anhydride rectification mother liquor residues, which comprises the steps of carrying out esterification reaction on the trimellitic anhydride rectification mother liquor residues and alcohol, diluting by using an organic solvent, extracting by using a dilute acid aqueous solution, washing by using pure water to be neutral, and removing the solvent to obtain an aqueous solution and mixed ester containing cobalt and manganese metal ions, wherein the aqueous solution can be used for recycling catalyst cobalt and manganese metal ions.
In order to solve the technical problems, the invention provides a method for recycling trimellitic anhydride rectification mother liquor residues, which comprises the following steps:
s1, sequentially adding alcohol, trimellitic anhydride residues and a catalyst into an esterification kettle, heating the esterification kettle and stirring, extracting water generated in the esterification process and excessive alcohol added before the reaction to ensure that the acid is completely esterified, and rectifying to remove excessive solvent to obtain crude ester after the reaction is finished after the temperature is increased to 180 ℃ and 250 ℃ and the reaction is carried out for 3.5-10 h;
s2, reducing the temperature of the esterification kettle to room temperature, and diluting the crude ester and the organic solvent in a mass ratio of 1:1-6 to obtain an organic phase;
s3, diluting the organic phase and the dilute acid water according to the mass ratio of 1:1-6, stirring and extracting for 5-60min, standing and layering, separating out the upper organic phase, and continuing to mix the upper organic phase and the dilute acid water according to the mass ratio of 1:1-6 dilution, repeating the extraction operation for 2-4 times, and collecting the lower aqueous phase;
s4, stirring and washing the organic phase and the pure water solution for 5-30min according to the mass ratio of 1:1-6, standing for layering, continuously stirring and washing the separated organic phase and the pure water solution according to the mass ratio of 1:1-6, and repeating the washing operation for 2-4 times to wash the organic phase to be neutral;
s5, rectifying the washed organic phase to remove the solvent to obtain the mixed ester.
Specifically, the alcohol in the S1 is n-butanol and isooctanol.
Specifically, the organic solvent in S2 is one or more of benzene, xylene, cyclohexane, butyl acetate, n-propyl acetate, isopropyl acetate, and ethyl acetate.
Specifically, the dilute acid water solution in S3 is one or more of sulfuric acid, hydrochloric acid, acetic acid, and phosphoric acid, and the concentration of the dilute acid water (in mass percent of the water solution) is 0.1-5%.
Specifically, in S3, the metal ions manganese and cobalt in the aqueous phase are collected.
Specifically, the temperature of the pure water solution in the S4 is 25-50 ℃.
The invention has the beneficial effects that: the mixed ester prepared by the invention has the ester content of more than 99 percent and the volume resistivity of more than 109Omega cm, simple method operation, convenient production and improved resource utilization rate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1:
adding 2000g of isooctanol, 1000g of trimellitic anhydride residue and 2.5g of catalyst tetraisopropyl titanate into an ester exchange kettle in sequence, stirring and heating to 220 ℃, and reacting for 5 hours; opening vacuum, gradually reducing the temperature of the reaction liquid from 7500Pa to 500Pa, reducing the temperature of the reaction liquid from 220 ℃ to 160 ℃, finishing dealcoholization, continuously reducing the temperature of the reaction liquid to room temperature to obtain mixed ester crude ester, adding 6000g of toluene, stirring and diluting for 0.5h, then adding 6000g of 5% dilute sulfuric acid aqueous solution, stirring and extracting for 30min, standing and layering, separating out a lower-layer aqueous phase, continuously and organically repeating the extraction operation for 3 times, collecting the aqueous phase for recovering cobalt and manganese metal ions, and extracting 93% of cobalt and manganese metal ions into the dilute acid aqueous phase by detection. The organic phase was further added with 6000g of pure water, and washing was repeated 3 times to neutrality. And removing the solvent from the organic phase to obtain the mixed ester. The content of the ester in the mixed ester is 99.16 percent through detection, and the volume resistivity of the mixed ester is more than 109Ω·cm。
Example 2:
adding 2000g of isooctanol, 1000g of trimellitic anhydride residue and 2.5g of catalyst tetraisopropyl titanate into an ester exchange kettle in sequence, and stirringHeating to 220 ℃ and reacting for 5 h; opening vacuum, gradually reducing the temperature of the reaction liquid from 7500Pa to 500Pa, reducing the temperature of the reaction liquid from 220 ℃ to 160 ℃, finishing dealcoholization, continuously reducing the temperature of the reaction liquid to room temperature to obtain mixed ester crude ester, adding 6000g of butyl acetate, stirring and diluting for 0.5h, adding 6000g of 1% dilute sulfuric acid aqueous solution, stirring and extracting for 30min, standing and layering, separating out a lower-layer aqueous phase, continuously and organically repeating the extraction operation for 3 times, collecting the aqueous phase for recovering cobalt and manganese metal ions, and extracting more than 99% of the cobalt and manganese metal ions into the dilute acid aqueous phase by detection. The organic phase was further added with 6000g of pure water, and washing was repeated 3 times to neutrality. And removing the solvent from the organic phase to obtain the mixed ester. The detection shows that the ester content in the mixed ester is 99.32 percent, and the volume resistivity of the mixed ester is more than 109Ω·cm。
Example 3:
adding 2000g of isooctanol, 1000g of trimellitic anhydride residue and 2.5g of catalyst tetraisopropyl titanate into an ester exchange kettle in sequence, stirring and heating to 220 ℃, and reacting for 5 hours; opening vacuum, gradually reducing the temperature of the reaction liquid from 7500Pa to 500Pa, reducing the temperature of the reaction liquid from 220 ℃ to 160 ℃, finishing dealcoholization, continuously reducing the temperature of the reaction liquid to room temperature to obtain crude ester, adding 8000g of cyclohexane, stirring and diluting for 0.5h, then adding 6000g of 3% dilute sulfuric acid aqueous solution, stirring and extracting for 30min, standing and layering, separating a lower-layer aqueous phase, organically and continuously repeating the extraction operation for 3 times, collecting the aqueous phase for recovering cobalt and manganese metal ions, and extracting 95% of cobalt and manganese metal ions into the dilute acid aqueous phase by detection. The organic phase was further added with 6000g of pure water, and washing was repeated 3 times to neutrality. Removing the solvent from the organic phase to obtain mixed ester, wherein the content of the ester in the mixed ester is detected to be 99.22%, and the volume resistivity of the mixed ester is larger than 109Ω·cm。
In the above examples, the content of metal ions extracted into the aqueous phase and the content of ester in the mixed ester were different due to the different solubility of the organic solvent and the different concentration of the dilute acid.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (6)
1. A method for recycling trimellitic anhydride rectification mother liquor residues is characterized by comprising the following steps:
s1, sequentially adding alcohol, trimellitic anhydride residues and a catalyst into an esterification kettle, heating the esterification kettle and stirring, extracting water and excessive alcohol generated in the esterification process, finishing the reaction after the temperature is increased to 180 ℃ and 250 ℃ and the reaction lasts for 3.5-10h, and removing excessive solvent through rectification to obtain crude ester;
s2, reducing the temperature of the esterification kettle to room temperature, and diluting the crude ester and the organic solvent in a mass ratio of 1:1-6 to obtain an organic phase;
s3, diluting the organic phase and the dilute acid water according to the mass ratio of 1:1-6, stirring and extracting for 5-60min, standing and layering, separating out the upper organic phase, and continuing to mix the upper organic phase and the dilute acid water according to the mass ratio of 1:1-6 dilution, repeating the extraction operation for 2-4 times, and collecting the lower aqueous phase;
s4, stirring and washing the extracted organic phase and the pure water solution for 5-30min according to the mass ratio of 1:1-6, standing for layering, continuously stirring and washing the separated organic phase and the pure water solution according to the mass ratio of 1:1-6, and repeating the washing operation for 2-4 times to wash the organic phase to be neutral;
s5, rectifying the washed organic phase to remove the solvent to obtain the mixed ester.
2. The method for recycling trimellitic anhydride rectification mother liquor residues according to claim 1, characterized in that the alcohol in S1 is n-butanol or isooctanol.
3. The method for recycling trimellitic anhydride rectification mother liquor residues according to claim 1, wherein the organic solvent in S2 is one or more of benzene, xylene, cyclohexane, butyl acetate, n-propyl acetate, isopropyl acetate and ethyl acetate.
4. The method for recycling trimellitic anhydride rectification mother liquor residues according to claim 1, characterized in that the dilute acid aqueous solution in S3 is one or more of sulfuric acid, hydrochloric acid, acetic acid and phosphoric acid, and the concentration of the dilute acid aqueous solution is 0.1-5%.
5. The method for recycling trimellitic anhydride rectification mother liquor residues according to claim 1, wherein metal ions manganese and cobalt in an aqueous phase are collected in S3.
6. The method for recycling trimellitic anhydride rectification mother liquor residues according to claim 1, characterized in that the temperature of the pure water solution in S4 is 25-50 ℃.
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| CN201911172010.2A CN110818559A (en) | 2019-11-26 | 2019-11-26 | Method for recycling trimellitic anhydride rectification mother liquor residues |
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| CN201911172010.2A CN110818559A (en) | 2019-11-26 | 2019-11-26 | Method for recycling trimellitic anhydride rectification mother liquor residues |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111004374A (en) * | 2019-11-26 | 2020-04-14 | 南通百川新材料有限公司 | Method for preparing alkyd resin based on trimellitic anhydride rectification heavy residual liquid |
| CN112521827A (en) * | 2020-11-13 | 2021-03-19 | 南通百川新材料有限公司 | Method for recycling waste residues generated in production process of trimellitic anhydride |
| CN113151686A (en) * | 2020-12-08 | 2021-07-23 | 南通百川新材料有限公司 | Equipment and method for recovering cobalt-manganese mixture in trimellitic anhydride production residues |
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|---|---|---|---|---|
| US4298759A (en) * | 1980-12-19 | 1981-11-03 | Standard Oil Company (Indiana) | Separation of cobalt and manganese from trimellitic acid process residue by extraction, ion exchanger and magnet |
| US4372875A (en) * | 1979-06-12 | 1983-02-08 | Dynamit Nobel Aktiengesellschaft | Method for obtaining and reusing of oxidation catalyst in the Witten DMT process |
| US4410449A (en) * | 1979-12-14 | 1983-10-18 | Dynamit Nobel Aktiengesellschaft | Recovery and reuse of heavy-metal oxidation catalyst from the Witten DMT process |
| CN1931850A (en) * | 2006-08-31 | 2007-03-21 | 江阴市百川化学工业有限公司 | Continuous production process of high purity trimellitic anhydride with trimellitic acid |
| CN105017022A (en) * | 2015-07-20 | 2015-11-04 | 浙江大学 | Method for methyl esterification recovery and recycle of PTA oxidation residue |
| CN106008204A (en) * | 2016-05-31 | 2016-10-12 | 百川化工(如皋)有限公司 | Method for synthesizing trimellitic triesters |
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| CN111004374A (en) * | 2019-11-26 | 2020-04-14 | 南通百川新材料有限公司 | Method for preparing alkyd resin based on trimellitic anhydride rectification heavy residual liquid |
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| CN113151686A (en) * | 2020-12-08 | 2021-07-23 | 南通百川新材料有限公司 | Equipment and method for recovering cobalt-manganese mixture in trimellitic anhydride production residues |
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