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Method for synthesizing 1,4-naphthoquinone through catalyzing ionic liquid
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A technology of ionic liquid and naphthoquinone, which is applied in the field of preparation of carbocyclic compounds, can solve the problems of high price and environmental pollution, achieve high selectivity, good separation, and solve the effects of poor reaction selectivity
Active Publication Date: 2015-02-25
四川东材绝缘技术有限公司
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In this type of synthesis method, ceric sulfate (CN 85100335A), cerium carbonate (Tetrahedron Letters, 1987, 28 (10): 1067-1068), ceric ammonium sulfate (Liebigs Annalen der Chemic, 1873, 167: 357-359 ), chromium trioxide and periodic acid (Tetrahedron Letters, 2001, 42: 3355-3357) are oxidants, and the yield of 1,4-naphthoquinone is about 80% to 90%, but these oxidants are all heavy metals Salt, high price, serious environmental pollution
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Embodiment 1-1
[0021] 13kg naphthalene, 0.13kg ionic liquid [Bu 3 NH][HSO 4 ], 70kg of acetic acid and 13kg of co-solvent petroleum ether were added to the reactor, and the temperature was raised to 90°C under stirring, and 134kg of aqueous hydrogen peroxide solution with a concentration of 30% by mass was added dropwise within 1.5 to 2.5 hours. , filtered out the insoluble precipitate, and the filtrate was extracted with cyclohexane, washed with water, dried, and then distilled under reduced pressure to obtain 7.49kg of 1,4-naphthoquinone with a yield of 46.7%.
Embodiment 1-2
[0023] 13.0kg naphthalene, 0.52kg ionic liquid [Et 3 NH][HSO 4 ], 110kg of acetic acid and 13kg of co-solvent cyclohexane were added to the reactor, and the temperature was raised to 90°C under stirring, and 113.5kg of aqueous hydrogen peroxide solution with a mass percentage concentration of 30% was added dropwise within 1.5 to 2.5 hours. After 2 hours, the insoluble precipitate was filtered out, and the filtrate was extracted with cyclohexane, washed with water, dried, and then distilled under reduced pressure to obtain 9.42kg of 1,4-naphthoquinone with a yield of 58.7%.
Embodiment 1-3
[0025] 13kg naphthalene, 1.3kg ionic liquid [Et 3 N(CH 2 ) 4 SO 3 H][HSO 4 ], 65kg of acetic acid, 13kg of co-solvent (chlorobenzene:xylene = 1:3 mass ratio) were added to the reactor, the temperature was raised to 60°C under stirring, and 170kg of mass percentage was added dropwise within 1.5 to 2.5 hours. The concentration was 30% Aqueous hydrogen peroxide solution, dropwise, keep warm for 2.5 hours, filter out the insoluble precipitate, extract the filtrate with cyclohexane, wash with water, dry, then carry out vacuum distillation to obtain 6.32kg of 1,4-naphthoquinone with a yield of 39.4% .
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Abstract
The invention discloses a method for synthesizing 1,4-naphthoquinone by catalyzing an ionic liquid. The method is characterized in that 130 mass parts of naphthalene, 1.3-13 mass parts of an ionic liquid, 650 to 1,300 mass parts of acetic acid, 130 mass parts of a booster solvent are added into a reactor, the temperature is increased to 50 to 100 DEG C during stirring, 1,135 to 3,400 mass parts of a hydrogen peroxide water solution with the mass concentration of 30 percent is completely dripped within 1.5 to 2.5 hours, after dripping, heat-insulating reaction lasts for 2 to 5 hours, then filtering is performed, insoluble precipitates are eliminated, a filter liquor is extracted by a resolvent cyclohexane, organic phases are taken, after water washing and drying, reduced pressure distillation is performed, and remnants are the prepared 1,4-naphthoquinone. According to the invention, the method provided by the invention has the characteristics of environment friendless, simplicity and convenience in operation, fast reaction speed and the like, the product cost is low, the commercial effect is excellent, and the practicability is strong.
Description
technical field [0001] The present invention belongs to the preparation of carbocyclic compounds. The invention relates to a method for catalyzing and synthesizing 1,4-naphthoquinone by an ionic liquid, and the prepared 1,4-naphthoquinone is used as a chemical raw material. Background technique [0002] 1,4-Naphthoquinone is an important fine chemical raw material, mainly used as an intermediate in medicine, pesticide, organic dyes, spices, etc., as well as a polymerization regulator for synthetic rubber and resin. It is also used in new papermaking and textiles. Organization plays an important role. Therefore, with the increasing demand for 1,4-naphthoquinone, it is of great significance to develop a preparation method suitable for industrial production of naphthoquinone. [0003] In the prior art, the gas-phase oxidation method and the liquid-phase oxidation method of naphthalene are mainly used in industry to prepare 1,4-naphthoquinone. The gas phase oxidation method m...
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