CN102001925A - Production method of 2-pentylidene cyclopentanone - Google Patents
Production method of 2-pentylidene cyclopentanone Download PDFInfo
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- CN102001925A CN102001925A CN2010105433792A CN201010543379A CN102001925A CN 102001925 A CN102001925 A CN 102001925A CN 2010105433792 A CN2010105433792 A CN 2010105433792A CN 201010543379 A CN201010543379 A CN 201010543379A CN 102001925 A CN102001925 A CN 102001925A
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- cyclopentanone
- pentylidene
- basic ring
- valeraldehyde
- aluminum oxide
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- YZKUNNFZLUCEET-RMKNXTFCSA-N (2e)-2-pentylidenecyclopentan-1-one Chemical compound CCCC\C=C1/CCCC1=O YZKUNNFZLUCEET-RMKNXTFCSA-N 0.000 title abstract 4
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 claims abstract description 65
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims abstract description 34
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N pentanal Chemical compound CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000009833 condensation Methods 0.000 claims abstract description 18
- 230000005494 condensation Effects 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 71
- 239000007788 liquid Substances 0.000 claims description 31
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 29
- -1 2-pentylidene Chemical group 0.000 claims description 28
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 28
- 230000015572 biosynthetic process Effects 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 20
- 238000004821 distillation Methods 0.000 claims description 17
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 6
- 239000012044 organic layer Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 3
- BGTOWKSIORTVQH-HOSYLAQJSA-N cyclopentanone Chemical group O=[13C]1CCCC1 BGTOWKSIORTVQH-HOSYLAQJSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 9
- 238000006482 condensation reaction Methods 0.000 abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000013067 intermediate product Substances 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 3
- GHBSPIPJMLAMEP-UHFFFAOYSA-N 6-pentyloxan-2-one Chemical compound CCCCCC1CCCC(=O)O1 GHBSPIPJMLAMEP-UHFFFAOYSA-N 0.000 abstract 2
- 239000000706 filtrate Substances 0.000 abstract 2
- 239000011698 potassium fluoride Substances 0.000 abstract 2
- 235000003270 potassium fluoride Nutrition 0.000 abstract 2
- 239000007790 solid phase Substances 0.000 abstract 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 239000012047 saturated solution Substances 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- ZMMRKRFMSDTOLV-UHFFFAOYSA-N cyclopenta-1,3-diene zirconium Chemical compound [Zr].C1C=CC=C1.C1C=CC=C1 ZMMRKRFMSDTOLV-UHFFFAOYSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- AXDZFGRFZOQVBV-UHFFFAOYSA-N 2-chlorocyclopentan-1-one Chemical compound ClC1CCCC1=O AXDZFGRFZOQVBV-UHFFFAOYSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 239000007818 Grignard reagent Substances 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 150000004795 grignard reagents Chemical class 0.000 description 1
- 235000015243 ice cream Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005935 nucleophilic addition reaction Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 235000014214 soft drink Nutrition 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a production method of 2-pentylidene cyclopentanone. In the method, cyclopentanone and valeraldehyde are taken as main raw material components; a used process is a condensation process; a catalyst used in a condensation reaction is potassium fluoride/alumina; after the condensation process, the method also comprises a filtering process and a post-treatment process for filtrate and a solid-phase object; the filtrate is washed with saturated solution of NaCl, dried, distilled under normal pressure and distilled under lowered pressure so as to obtain the 2-pentylidene cyclopentanone; and the solid-phase object is washed with absolute ethyl alcohol, heated and activated so as to obtain the potassium fluoride/alumina. The catalyst used in the method has high activity, is easy for post-treatment and can be used repeatedly; the prepared 2-pentylidene cyclopentanone is fully accordant with the quality index of an intermediate product for synthesizing delta-decalactone; compared with the prior art, the method has short and simple process flow, can particularly reduce pollution caused by sewage drainage and has low cost; and the entire process is more suitable for industrialized continuous production.
Description
Technical field
The present invention relates to the production method of fine chemical product, particularly the production method of the intermediate 2-pentylidene basic ring pentanone of δ-Gui Neizhi series compound.
Background technology
The δ-Gui Neizhi compound is important edible odor additive.Be used in the manufacture craft of food such as candy, soft drink, ice-creams, cooking food, oleomargarine, cake because of it has milk, coconut perfume (or spice), fruital more, extensively used sometimes also as the blending of feed, or as daily essence and flavouring essence for tobacco etc.The alleged 2-pentylidene basic ring pentanone of the present invention is the intermediate product of synthetic δ-Gui Neizhi.At present, the production technique of 2-pentylidene basic ring pentanone mainly includes valeraldehyde and cyclopentanone condensation method, chloro cyclopentanone and Grignard reagent nucleophilic addition(Adn) rearrangement method.Valeraldehyde and cyclopentanone condensation method, employed catalyzer have zirconocene, sodium hydroxide (or potassium hydroxide).Adopt zirconocene to make catalyzer, good catalytic activity, but its price is higher, and preparation process is loaded down with trivial details, thereby use not general in the actual production.Present stage purchases with valeraldehyde and cyclopentanone condensation industrialization in the technology of 2-pentylidene basic ring pentanone, the catalyzer of normal use mostly is sodium hydroxide or potassium hydroxide, though its technical maturity, cost of material is lower, but this technical process is longer, after condensation reaction, also must carry out multiple working procedures such as acid neutralization, sodium-chlor washing, yellow soda ash washing, filtration, drying, distillation, and it is big to exist wastewater discharge again, seriously polluted, that raw material runs off is many, the product yield is lower, and catalyzer such as can not reuse again at defective.
Summary of the invention
The present invention proposes a kind of production method of 2-pentylidene basic ring pentanone, purpose is by preferably being suitable for valeraldehyde and the employed catalyzer of cyclopentanone condensation process, to overcome the existing weak point of other catalyzer, particularly can reduce the pollution that sewage discharge causes, and realize the recycling of catalyzer.
Technical solution of the present invention:
The main raw material component of the inventive method is cyclopentanone, valeraldehyde, and solvent is a toluene.Employed operational path is a condensation process, wherein, cyclopentanone is 1.0 with the ratio of the weight part of valeraldehyde: 0.8-1.0, and the selected catalyzer of described condensation process is Potassium monofluoride/aluminum oxide, and the ratio of cyclopentanone and the weight part of Potassium monofluoride/aluminum oxide is 1: 0.1-0.4; Described operational path also comprises filtration operation after the condensation, and to the aftertreatment technology of filtered liquid and solid formation.The aftertreatment technology of filtered liquid is for distilling with saturated NaCl solution washing, drying, air distillation, step-down; The aftertreatment technology of described solid formation is for to use absolute ethanol washing, and heat-activated is made manipulation of regeneration.
Beneficial effect of the present invention
(1) the prepared 2-pentylidene basic ring pentanone of the present invention meets the quality index of the intermediate product of synthetic δ-Gui Neizhi fully, can satisfy the requirement of perfume industry as deodorant tune;
(2) selected catalyst activity height, the aftertreatment of the present invention is simple, yield is high; The activity of the Potassium monofluoride/aluminum oxide after the regeneration does not obviously reduce, and is reusable.
(3) the present invention compared with prior art, technical process is short and simply, particularly can reduce the pollution that sewage discharge causes, and cost is low, whole technology is more suitable for industrialization continuity production.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
As shown in the figure,
The inventive method comprises cyclopentanone, valeraldehyde condensation process, must be according to quantity than adding solvent toluene, catalyzer Potassium monofluoride/aluminum oxide during condensation reaction; Condensation reaction is carried out filterer's preface after finishing; Filtered liquid after the filtration and solid formation enter the aftertreatment technology flow process more respectively.The aftertreatment technology of filtered liquid is to obtain 2-pentylidene basic ring pentanone with saturated NaCl solution washing, drying, air distillation, step-down distillation back; The aftertreatment technology of solid formation is to adopt absolute ethanol washing, is heated to 110-130 ℃, activates 1.5-2.5 hour, gets regenerated Potassium monofluoride/aluminum oxide.
Below provide embodiment again
Embodiment one
(1) preparation of catalyzer Potassium monofluoride/aluminum oxide:
The Potassium monofluoride of 580g is dissolved in the 1000mL water, add 1000g and be 100 purpose particulate alumina, and temperature of reaction is set is 65 ℃, stir to reaction end in 1 hour, evaporate to dryness institute water content then heats up, solid formation promptly was prepared into Potassium monofluoride/aluminium oxide catalyst after under the envrionment temperature about 120 ℃ dry 4 hours.
(2) condensation reaction of cyclopentanone, valeraldehyde: add 420g cyclopentanone, above-mentioned prepared 150g Potassium monofluoride/aluminum oxide and 1000mL toluene in three neck containers, container is fixing appropriate.The stirring rod of mechanical stirrer is stretched in the liquid of three neck containers, again thermometer, constant pressure funnel and reflux exchanger are connected with three neck containers.In constant pressure funnel, add the valeraldehyde of 336g and the mixed solution of 1000mL toluene, stir on the limit, the limit drips described valeraldehyde and toluene mixture liquid, keeping temperature of reaction is about 30 ℃, be controlled in two hours and dropwise, and continue to stir one hour, to cooled and filtered, get filtered liquid and solid formation.
(3) 2-pentylidene basic ring pentanone is extracted in the filtered liquid aftertreatment: with above-mentioned filtered liquid with saturated NaCl solution washing, wherein organic layer anhydrous Na
2SO
4After the drying, the air distillation cut reclaims toluene and cyclopentanone; Underpressure distillation, pressure are 3mmHg, and temperature is 98-100 ℃, and cut extracts 2-pentylidene basic ring pentanone product.Its yield is 88.6%, and stratographic analysis purity reaches 99.7%.
(4) catalyzer Potassium monofluoride/aluminum oxide is reclaimed in the solid formation aftertreatment: the solid formation absolute ethanol washing after will filtering, put it into again and be heated to 120 ℃ in the baking oven, and kept 2 hours, promptly reclaim Potassium monofluoride/aluminum oxide.Repeat to do the condensation catalyst use of cyclopentanone, valeraldehyde again, the yield of the 2-pentylidene basic ring pentanone that obtains is 87.5%, slightly reduces than initial result of use.
Embodiment two:
(1) preparation of catalyzer Potassium monofluoride/aluminum oxide:
The preparation method is described with embodiment one.
(2) condensation reaction of cyclopentanone, valeraldehyde: add 500g cyclopentanone, prepared 150g Potassium monofluoride/aluminum oxide and 1000mL toluene in three neck containers, container is fixing appropriate.The stirring rod of mechanical stirrer is stretched in the liquid of three neck containers, again thermometer, constant pressure funnel and reflux exchanger are connected with three neck containers.In constant pressure funnel, add the valeraldehyde of 460g and the mixed solution of 1000mL toluene, stir on the limit, the limit drips described valeraldehyde and toluene mixture liquid, keeping temperature of reaction is about 30 ℃, be controlled in two hours and dropwise, and continue to stir one hour, to cooled and filtered, get filtered liquid and solid formation.
(3) 2-pentylidene basic ring pentanone is extracted in the filtered liquid aftertreatment: with above-mentioned filtered liquid with saturated NaCl solution washing, wherein organic layer anhydrous Na
2SO
4After the drying, the air distillation cut reclaims toluene and cyclopentanone; Underpressure distillation, pressure are 3mmHg, and temperature is 98-100 ℃, and cut extracts 2-pentylidene basic ring pentanone product.Its yield is 82.3%, and stratographic analysis purity reaches 99.1%.
(4) catalyzer Potassium monofluoride/aluminum oxide is reclaimed in the solid formation aftertreatment: the solid formation absolute ethanol washing after will filtering, put it into again and be heated to 120 ℃ in the baking oven, and kept 2 hours, promptly reclaim Potassium monofluoride/aluminum oxide, repeat to do the condensation catalyst use of cyclopentanone, valeraldehyde again, the yield of the 2-pentylidene basic ring pentanone that obtains is 83.5%, does not have considerable change than initial result of use.
Embodiment three:
(1) preparation of catalyzer Potassium monofluoride/aluminum oxide:
The preparation method is described with embodiment one.
(2) condensation reaction of cyclopentanone, valeraldehyde: add 500g cyclopentanone, prepared 200g Potassium monofluoride/aluminum oxide and 1000mL toluene in three neck containers, container is fixing appropriate.The stirring rod of mechanical stirrer is stretched in the liquid of three neck containers, again thermometer, constant pressure funnel and reflux exchanger are connected with three neck containers.In constant pressure funnel, add the valeraldehyde of 500g and the mixed solution of 1000mL toluene, stir on the limit, the limit drips described valeraldehyde and toluene mixture liquid, keeping temperature of reaction is about 30 ℃, be controlled in two hours and dropwise, and continue to stir one hour, to cooled and filtered, get filtered liquid and solid formation.
(3) 2-pentylidene basic ring pentanone is extracted in the filtered liquid aftertreatment: with above-mentioned filtration with saturated NaCl solution washing, wherein organic layer anhydrous Na
2SO
4After the drying, the air distillation cut reclaims toluene and cyclopentanone; Underpressure distillation, pressure are 3mmHg, and temperature is 98-100 ℃, and cut extracts 2-pentylidene basic ring pentanone product.Its yield is 85.3%, and stratographic analysis purity reaches 99.4%.
(4) catalyzer Potassium monofluoride/aluminum oxide is reclaimed in the solid formation aftertreatment: the solid formation absolute ethanol washing after will filtering, put it into again and be heated to 120 ℃ in the baking oven, and kept 2 hours, promptly reclaim Potassium monofluoride/aluminum oxide, repeat to do the condensation catalyst use of cyclopentanone, valeraldehyde again, the yield of the 2-pentylidene basic ring pentanone that obtains is 82.7%, slightly reduces than initial result of use.
Embodiment four:
(1) preparation of catalyzer Potassium monofluoride/aluminum oxide:
The preparation method is described with embodiment one.
(2) condensation reaction of cyclopentanone, valeraldehyde: add 500g cyclopentanone, prepared 50g Potassium monofluoride/aluminum oxide and 1000mL toluene in three neck containers, container is fixing appropriate.The stirring rod of mechanical stirrer is stretched in the liquid of three neck containers, again thermometer, constant pressure funnel and reflux exchanger are connected with three neck containers.In constant pressure funnel, add the valeraldehyde of 500g and the mixed solution of 1000mL toluene, stir on the limit, the limit drips described valeraldehyde and toluene mixture liquid, keeping temperature of reaction is about 30 ℃, be controlled in two hours and dropwise, and continue to stir one hour, to cooled and filtered, get filtered liquid and solid formation.
(3) 2-pentylidene basic ring pentanone is extracted in the filtered liquid aftertreatment: with above-mentioned filtered liquid with saturated NaCl solution washing, wherein organic layer anhydrous Na
2SO
4After the drying, the air distillation cut reclaims toluene and cyclopentanone; Underpressure distillation, pressure are 3mmHg, and temperature is 98-100 ℃, and cut extracts 2-pentylidene basic ring pentanone product.Its yield is 62.7%, and stratographic analysis purity reaches 99.5%.
(4) catalyzer Potassium monofluoride/aluminum oxide is reclaimed in the solid formation aftertreatment: the solid formation absolute ethanol washing after will filtering, put it into afterwards and be heated to 120 ℃ in the baking oven, and kept 2 hours, promptly reclaim Potassium monofluoride/aluminum oxide, repeat to do the condensation catalyst use of cyclopentanone, valeraldehyde again, the yield of the 2-pentylidene basic ring pentanone that obtains is 60.4%, slightly reduces than initial result of use.
Embodiment five:
(1) preparation of catalyzer Potassium monofluoride/aluminum oxide:
The preparation method is described with embodiment one.
(2) condensation reaction of cyclopentanone, valeraldehyde: add 500g cyclopentanone, prepared 150g Potassium monofluoride/aluminum oxide and 1000mL toluene in three neck containers, container is fixing appropriate.The stirring rod of mechanical stirrer is stretched in the liquid of three neck containers, again thermometer, constant pressure funnel and reflux exchanger are connected with three neck containers.In constant pressure funnel, add the valeraldehyde of 400g and the mixed solution of 1000mL toluene, stir on the limit, the limit drips described valeraldehyde and toluene mixture liquid, keeping temperature of reaction is about 30 ℃, be controlled in two hours and dropwise, and continue to stir one hour, to cooled and filtered, get filtered liquid and solid formation.
(3) 2-pentylidene basic ring pentanone is extracted in the filtered liquid aftertreatment: with above-mentioned filtered liquid with saturated NaCl solution washing, wherein organic layer anhydrous Na
2SO
4After the drying, the air distillation cut reclaims toluene and cyclopentanone; Underpressure distillation, pressure are 3mmHg, and temperature is 98-100 ℃, and cut extracts 2-pentylidene basic ring pentanone product.Its yield is 73.3%, and stratographic analysis purity reaches 99.1%.
(4) catalyzer Potassium monofluoride/aluminum oxide is reclaimed in the solid formation aftertreatment: the solid formation absolute ethanol washing after will filtering, put it into again and be heated to 120 ℃ in the baking oven, and kept 2 hours, promptly reclaim Potassium monofluoride/aluminum oxide, repeat to do the condensation catalyst use of cyclopentanone, valeraldehyde again, the yield of the 2-pentylidene basic ring pentanone that obtains is 55.8%, does not have considerable change than initial result of use.
To sum up, the present invention has reached the goal of the invention of expection.
Claims (4)
1. the production method of a 2-pentylidene basic ring pentanone, the main raw material component is cyclopentanone, valeraldehyde, solvent toluene, employed operational path is a condensation process, wherein, cyclopentanone is 1.0 with the ratio of the weight part of valeraldehyde: 0.8-1.0 is characterized in that: the selected catalyzer of described condensation process is Potassium monofluoride/aluminum oxide, and the ratio of cyclopentanone and the weight part of Potassium monofluoride/aluminum oxide prepared product is 1: 0.1-0.4.
2. the production method of a kind of 2-pentylidene basic ring pentanone according to claim 1, it is characterized in that: described operational path also comprises filtration operation after the condensation, and to the aftertreatment technology of filtered liquid and solid formation, described filtered liquid aftertreatment technology is for distilling with saturated NaCl solution washing, drying, air distillation, step-down; The aftertreatment technology of described solid formation is heated to 110-130 ℃ for to use absolute ethanol washing, activates 1.5-2.5 hour.
3. the production method of a kind of 2-pentylidene basic ring pentanone according to claim 2 is characterized in that: described filtered liquid is with saturated NaCl solution washing, wherein organic layer anhydrous Na
2SO
4After the drying, the air distillation cut reclaims toluene and cyclopentanone; Underpressure distillation, pressure are 3mmHg, and temperature is 98-100 ℃, and cut extracts 2-pentylidene basic ring pentanone.
4. the production method of a kind of 2-pentylidene basic ring pentanone according to claim 2 is characterized in that: the solid formation absolute ethanol washing after the described filtration, put it into again and be heated to 120 ℃ in the baking oven, and kept 2 hours, promptly reclaim Potassium monofluoride/aluminum oxide.
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| CN104910000A (en) * | 2015-05-25 | 2015-09-16 | 张家港市振方化工有限公司 | Preparation method of 2-heptylidene-cyclopentanon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006072775A2 (en) * | 2005-01-04 | 2006-07-13 | The Queen's University Of Belfast | Ionic liquids with a cation comprising a basic moiety |
| WO2006077277A1 (en) * | 2005-01-18 | 2006-07-27 | Metso Paper, Inc. | Method for removing an edge bank formed at the edge of a coated web in curtain coating effected as a dry edge coating process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006072775A2 (en) * | 2005-01-04 | 2006-07-13 | The Queen's University Of Belfast | Ionic liquids with a cation comprising a basic moiety |
| WO2006077277A1 (en) * | 2005-01-18 | 2006-07-27 | Metso Paper, Inc. | Method for removing an edge bank formed at the edge of a coated web in curtain coating effected as a dry edge coating process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910000A (en) * | 2015-05-25 | 2015-09-16 | 张家港市振方化工有限公司 | Preparation method of 2-heptylidene-cyclopentanon |
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