CN101130481B - Process for the separation of 2, 6- isopropyl naphthalene and 2, 7- isopropyl naphthalene - Google Patents
Process for the separation of 2, 6- isopropyl naphthalene and 2, 7- isopropyl naphthalene Download PDFInfo
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- CN101130481B CN101130481B CN 200610111722 CN200610111722A CN101130481B CN 101130481 B CN101130481 B CN 101130481B CN 200610111722 CN200610111722 CN 200610111722 CN 200610111722 A CN200610111722 A CN 200610111722A CN 101130481 B CN101130481 B CN 101130481B
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- diisopropylnaphthalene
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- adsorption
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- dipn
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Abstract
The invention discloses a separating method of 2,6-diisopropyl naphthalene and 2,7-diisopropyl naphthalene, which is characterized by the following: adopting the composition of 2,6-diisopropyl naphthalene and 2,7-diisopropyl naphthalene as raw material; selecting adsorbant from Na, Ba or Pd cation Y-zeolite or alpha-zeolite or mordenite or cation from as K or Li Y-zeolite or alpha-zeolite or mordenite; adsorbing with speed at 30mL/h under 20-50 deg. c; selecting toluene or ditoluene as eluent; distilling the eluent or residual adsorbing liquid to obtain the 2, 6-diisopropyl naphthalene with purity at 80. 1-93. 2%. The invention has high product purity and receiving rate, which simplifies the separating course.
Description
Technical field
The present invention relates to a kind of method of from the di-isopropyl naphthalene mixtures, separating 2,6-DIPN, belong to chemical field.
Background technology
2,6-DIPN is called for short 2,6-DIPN, is a kind of important basic organic chemical industry raw material.The NDA that 2,6-DIPN generates after oxidation is called for short 2,6-NDCA, it and ethylene glycol esterification, and the PEN that polycondensation makes, abbreviation PEN is a kind of high performance polyester material.With polyethylene terephthalate commonly used at present, be called for short PET and compare, PEN has better gas barrier property, thermostability, chemical stability and mechanical mechanics property, and its application prospect is more extensive.The application of PEN reaches its maturity, and consumption strengthens gradually, and the demand that drives 2,6-DIPN sharply rises.But because 2, the separation difficulty of 6-DIPN, output is few, expensive, has restricted the application development of PEN.Its separation difficulty subject matter is 2.6-diisopropylnaphthalene and 2, the separation of 7-diisopropylnaphthalene isomers, the general methods such as crystallization, solvent extraction that adopt are separated isomer both at home and abroad, but because the crystallisation process energy consumption is higher, complex process etc. lack a bit, the preparation purifying technique of therefore researching and developing 2,6-DIPN has practical significance to promoting PEN new polyester material application development.
Summary of the invention
Purpose of the present invention just for the shortcoming that overcomes above-mentioned prior art with not enough, and provide a kind of productive rate high, the separation method of colory 2,6-DIPN and 2,6-DIPN, thereby provide good raw material for production of polyester.
The objective of the invention is to realize by following technical proposal:
A kind of 2,6-diisopropylnaphthalene and 2, the separation method of 7-diisopropylnaphthalene, it is characterized in that it is with 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures is raw material, wherein the concentration of 2,6-DIPN is 50%～90%, again with toluene or xylene solvent dissolving raw material, raw material and weight of solvent ratio are 1: 40～50, fixedly adsorbing in the adsorption column, sorbent material is Na, the positively charged ion Y zeolite of Ba or Pd or α zeolite or mordenite, 20～50 ℃ of adsorption temps, rate of adsorption: 30mL/h, sorbent material saturated rear be that eluent carries out wash-out with toluene or dimethylbenzene, its elutriant speed: 200mL/h, eluting temperature: 60～120 ℃, obtain purity and be 89.5～93.2% 2,6-DIPN product.
In the raw material 2, the concentration of 6-diisopropylnaphthalene is 10%～50%, again with toluene or xylene solvent dissolving raw material, raw material and weight of solvent ratio are 1: 40～50, are fixedly adsorbing in the adsorption column, and sorbent material can be that positively charged ion is Y zeolite or α zeolite or the mordenite of K or Li, 20～50 ℃ of adsorption temps, rate of adsorption: 30mL/h, adsorb saturated after the remaining liquid of its absorption to obtain purity through the distillation desolventizing be 80.1～92.5% 2,6-DIPN product.
Raw material of the present invention is with in the alkylnaphthalene sepn process 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures, when 2, during the concentration 50%～90% of 6-diisopropylnaphthalene, with toluene or xylene solvent dissolving raw material, raw material and weight of solvent ratio are 1: 40～50, fixedly adsorbing in the adsorption column, selection is cationic Na to the selective adsorbing sorbent material of 2,6-DIPN, the Y zeolite of Ba or Pd or α zeolite or mordenite, 20～50 ℃ of adsorption temps, rate of adsorption: 30mL/h, it is that eluent carries out the agent wash-out with toluene or dimethylbenzene that sorbent material reaches capacity rear, its elutriant speed: 200mL/h, eluting temperature: 60～120 ℃, 2,6～diisopropylnaphthalene product through distillation desolventizing 89.5～93.2%.
In the raw material 2, the concentration of 6-diisopropylnaphthalene is 10%～50%, with toluene or xylene solvent dissolving raw material, raw material and weight of solvent ratio are 1: 40～50, fixedly adsorbing in the adsorption column, selection is to 2, the selective adsorption sorbent material of 7-diisopropylnaphthalene is that positively charged ion is Y zeolite or α zeolite or the mordenite of K or Li, 20～50 ℃ of adsorption temps, rate of adsorption: 30mL/h, adsorb saturated after the remaining liquid of its absorption to obtain purity through the distillation desolventizing be 80.1～92.5% 2,6-DIPN product.
The selection of above-mentioned two kinds of sorbent materials is according in the raw material 2, the concentration of 6-diisopropylnaphthalene and deciding, when 2, the sorbent material of selecting when the concentration of 6-diisopropylnaphthalene is 50%～90% is Y zeolite or α zeolite or the mordenite of cationic Na, Ba or Pd, otherwise selectable sorbent material is Y zeolite or α zeolite or the mordenite of positively charged ion K or Li, thereby improves loading capacity.
Owing to taking technique scheme to make the technology of the present invention compared with the prior art have advantage and the effect that product purity is high, yield is high.
Embodiment
Embodiment 1
Get 2,6-DIPN and 2,7-di-isopropyl naphthalene mixtures is raw material 1kg, wherein the concentration of 2,6-DIPN is 50%, again with 40kg toluene solvant dissolving raw material, fixedly adsorbing in the adsorption column, sorbent material is the Y zeolite of positively charged ion Na, 50 ℃ of adsorption temps, rate of adsorption: 30mL/h, sorbent material saturated rear be that eluent carries out wash-out with toluene, its elutriant speed: 200mL/h, eluting temperature: 60 ℃, obtain purity and be 89.5% 2,6-DIPN product.
Embodiment 2
Get 2,6-DIPN and 2,7-di-isopropyl naphthalene mixtures is raw material 1kg, wherein the concentration of 2,6-DIPN is 70%, again with 45kg xylene solvent dissolving raw material, fixedly adsorbing in the adsorption column, sorbent material is the α zeolite of positively charged ion Ba, 40 ℃ of adsorption temps, rate of adsorption: 30mL/h, sorbent material saturated rear be that eluent carries out wash-out with dimethylbenzene, its elutriant speed: 200mL/h, eluting temperature: 80 ℃, obtain purity and be 91.5% 2,6-DIPN product.
Embodiment 3
Get 2,6-DIPN and 2,7-di-isopropyl naphthalene mixtures is raw material 1kg, wherein the concentration of 2,6-DIPN is 90%, again with 50kg toluene solvant dissolving raw material, fixedly adsorbing in the adsorption column, sorbent material is the mordenite of positively charged ion Pd, 20 ℃ of adsorption temps, rate of adsorption: 30mL/h, sorbent material saturated rear be that eluent carries out wash-out with toluene, its elutriant speed: 200mL/h, eluting temperature: 100 ℃, obtain purity and be 93.2% 2,6-DIPN product.
Embodiment 4
Get 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures are raw material 1kg, wherein 2, the concentration of 6-diisopropylnaphthalene is 10%, with 50kg toluene solvant dissolving raw material, fixedly adsorbing in the adsorption column, sorbent material is the Y zeolite of positively charged ion K again, 20 ℃ of adsorption temps, rate of adsorption: 30mL/h, to obtain purity through the distillation desolventizing be 80.1% 2,6-DIPN product to the remaining liquid of its absorption after sorbent material was saturated.
Embodiment 5
Get 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures are raw material 1kg, wherein 2, the concentration of 6-diisopropylnaphthalene is 30%, with 45kg xylene solvent dissolving raw material, fixedly adsorbing in the adsorption column, sorbent material is the Y zeolite of cationic Li again, 50 ℃ of adsorption temps, rate of adsorption: 30mL/h, to obtain purity through the distillation desolventizing be 88.3% 2,6-DIPN product to the remaining liquid of its absorption after sorbent material was saturated.
Embodiment 6
Get 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures are raw material 1kg, wherein 2, the concentration of 6-diisopropylnaphthalene is 50%, with 40kg toluene solvant dissolving raw material, fixedly adsorbing in the adsorption column, sorbent material is the mordenite of positively charged ion Li again, 50 ℃ of adsorption temps, rate of adsorption: 30mL/h, to obtain purity through the distillation desolventizing be 92.5% 2,6-DIPN product to the remaining liquid of its absorption after sorbent material was saturated.
Claims (2)
1. one kind 2,6-diisopropylnaphthalene and 2, the separation method of 7-diisopropylnaphthalene, it is characterized in that: it is with 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures is raw material, wherein the concentration of 2,6-DIPN is 50%～90%, again with toluene or xylene solvent dissolving raw material, raw material and weight of solvent ratio are 1: 40～50, fixedly adsorbing in the adsorption column, sorbent material is Na, the positively charged ion Y zeolite of Ba or Pd or α zeolite or mordenite, 20～50 ℃ of adsorption temps, rate of adsorption: 30mL/h, sorbent material saturated rear be that eluent carries out wash-out with toluene or dimethylbenzene, its elutriant speed: 200mL/h, eluting temperature: 60～120 ℃, it is 2,6～diisopropylnaphthalene product of 89.5～93.2% that elutriant obtains purity through the distillation desolventizing.
2. a 6-diisopropylnaphthalene and 2, the separation method of 7-diisopropylnaphthalene, it is characterized in that: it is with 2,6-diisopropylnaphthalene and 2,7-di-isopropyl naphthalene mixtures is raw material, wherein 2, the concentration of 6-diisopropylnaphthalene is 10%～50%, and with toluene or xylene solvent dissolving raw material, raw material and weight of solvent ratio are 1: 40～50 again, fixedly adsorbing in the adsorption column, sorbent material can be that positively charged ion is the mordenite of K or Li, 20～50 ℃ of adsorption temps, rate of adsorption: 30mL/h, adsorb saturated after the remaining liquid of its absorption to obtain purity through the distillation desolventizing be 2,6～diisopropylnaphthalene product of 80.1～92.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610111722 CN101130481B (en) | 2006-08-25 | 2006-08-25 | Process for the separation of 2, 6- isopropyl naphthalene and 2, 7- isopropyl naphthalene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610111722 CN101130481B (en) | 2006-08-25 | 2006-08-25 | Process for the separation of 2, 6- isopropyl naphthalene and 2, 7- isopropyl naphthalene |
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| Publication Number | Publication Date |
|---|---|
| CN101130481A CN101130481A (en) | 2008-02-27 |
| CN101130481B true CN101130481B (en) | 2013-01-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200610111722 Expired - Fee Related CN101130481B (en) | 2006-08-25 | 2006-08-25 | Process for the separation of 2, 6- isopropyl naphthalene and 2, 7- isopropyl naphthalene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107389811B (en) * | 2017-07-05 | 2020-05-05 | 江苏中烟工业有限责任公司 | Method for measuring diisopropyl naphthalene in cigarette tipping paper |
| CN110172017A (en) * | 2019-05-28 | 2019-08-27 | 北京石油化工学院 | A method of high-purity naphthalic acid is prepared by raw material of naphthalene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4992622A (en) * | 1988-12-26 | 1991-02-12 | Chiyoda Corporation | Method of separating 2,6-diisopropylnaphthalene from a mixture containing diisopropylnaphthalene isomers |
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- 2006-08-25 CN CN 200610111722 patent/CN101130481B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4992622A (en) * | 1988-12-26 | 1991-02-12 | Chiyoda Corporation | Method of separating 2,6-diisopropylnaphthalene from a mixture containing diisopropylnaphthalene isomers |
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| CN101130481A (en) | 2008-02-27 |
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