Method for continuously extracting beta-methylnaphthalene crude product from methylnaphthalene enrichment liquor

A technology for methylnaphthalene enriched liquid and crude methylnaphthalene, applied in separation methods, chemical instruments and methods, solution crystallization, etc., can solve problems such as increasing separation difficulty and affecting the purity and yield of β-methylnaphthalene, Achieve the effects of good removability, increased thickness and hardness, and high hardness

Active Publication Date: 2018-08-24
PENG CHEN NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Known from above-mentioned prior art, by adding methods such as solvent recrystallization or melt crystallization, not only can improve the degree of separation of α-methylnaphthalene and β-methylnaphthalene, improve the purity of β-methylnaphthalene, and can improve to a certain extent The yield of β-methylnaphthalene, but all use high-purity methylnaphthalene enriched liquid as raw material, if the methylnaphthalene contains impurities such as biphenyl and indole, it will increase the difficulty of separation and affect the concentration of β-methylnaphthalene. The purity and yield of naphthalene

Method used

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  • Method for continuously extracting beta-methylnaphthalene crude product from methylnaphthalene enrichment liquor

Examples

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Effect test

Embodiment 1

[0026] (1) After cleaning the aluminum sheet with acetone and deionized water ultrasonically for 15 minutes at a power of 250W, place it in an electrolyte solution of ethanol and perchloric acid with a volume ratio of 4:1, at a voltage of 15v, at 4 °C, electrochemically polished for 2 min to obtain a pretreated aluminum sheet.

[0027] (2) The pretreated aluminum sheet is used as the anode, the graphite plate is the cathode, and the 0.5moL / L sulfuric acid solution containing 0.3g / L cerium salt or molybdate is used as the electrolyte, at 100V, at 0.1°C, Carry out an anodic oxidation for 3-6 hours, take out the aluminum oxide film that has been oxidized once, and soak it in the mixed solution of phosphoric acid and chromic acid. The soaking process is as follows: the first stage, soak in the mixed solution at a temperature of 30°C for 20 minutes; In the second stage, heat the mixed solution to 60°C at a speed of 4°C / min, and keep soaking for 120 minutes; in the third stage, stop...

Embodiment 2

[0032] (1) After cleaning the aluminum sheet with acetone and deionized water ultrasonically for 30 minutes at a power of 300W, place it in the electrolyte solution of ethanol and perchloric acid with a volume ratio of 4:1, and at a voltage of 20v, at 4 °C, electrochemically polished for 4 minutes to obtain a pretreated aluminum sheet.

[0033] (2) The pretreated aluminum sheet is used as the anode, the graphite plate is the cathode, and the 0.8moL / L sulfuric acid solution containing 0.5g / L cerium salt or molybdate is used as the electrolyte, at 150V, at 1°C, Carry out an anodic oxidation for 6 hours, take out the aluminum oxide film that has been oxidized once, and soak it in the mixed solution of phosphoric acid and chromic acid. stage, heat the mixed solution to 80°C at a speed of 6°C / min, and keep soaking for 160 minutes; in the third stage, stop heating, cool the mixed solution to 20°C at a speed of 10°C / hour, and continue soaking for 80 minutes, Remove the acidic soluti...

Embodiment 3

[0038] (1) After cleaning the aluminum sheet with acetone and deionized water ultrasonically for 20 minutes at a power of 280W, it is placed in an electrolyte solution of ethanol and perchloric acid with a volume ratio of 4:1, at a voltage of 18v, at 4 °C, electrochemically polished for 3 minutes to obtain a pretreated aluminum sheet.

[0039] (2) The pretreated aluminum sheet is used as the anode, the graphite plate is the cathode, and the 0.6moL / L sulfuric acid solution containing 0.4g / L cerium salt or molybdate is used as the electrolyte, at 120V, at 0.5°C, Carry out an anodic oxidation for 4 hours, take out the aluminum oxide film that has been oxidized once, and soak it in the mixed solution of phosphoric acid and chromic acid. stage, heat the mixed solution to 70°C at a rate of 5°C / min, and keep soaking for 150 minutes; in the third stage, stop heating, cool the mixed solution to 18°C ​​at a rate of 9°C / hour, and continue soaking for 70 minutes. Remove the acidic soluti...

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Abstract

The invention provides a method for continuously extracting a beta-methylnaphthalene crude product from a methylnaphthalene enrichment liquor. The method comprises steps as follows: methylnaphthalenefractions are treated with an ammonium bisulfate water liquor and a heptane and ethanol amine mixed liquor sequentially, separation is performed, an upper-layer oil phase is taken, and alkyl methylnaphthalene subjected to secondary purification is obtained; an entrainer is added to alkyl methylnaphthalene subjected to secondary purification, indirect reduced pressure distillation operation is performed, the reduced pressure distillation is performed under the vacuum degree of minus 0.09 MPa and at the tower top temperature of 80 DEG C and the tower bottom temperature of 150 DEG C, a gas phasepasses through a porous alumina membrane/carbon fiber filler cold trap at the tower top, and the beta-methylnaphthalene crude product is obtained; the beta-methylnaphthalene crude product is put in afreezing microtome and frozen and crystalized at the temperature of subzero 25 DEG C to subzero 15 DEG C, separation is performed, then, redisliquor is performed at the temperature of 36-40 DEG C, andbeta-methylnaphthalene is obtained, wherein the porous alumina membrane/carbon fiber filler cold trap comprises alternate porous alumina layers and carbon fiber layers.

Description

technical field [0001] The invention belongs to the technical field of beta-methylnaphthalene separation, in particular to a method for continuously extracting crude beta-methylnaphthalene from methylnaphthalene enriched liquid. Background technique [0002] Both β-methylnaphthalene and α-methylnaphthalene are important organic chemical raw materials. β-methylnaphthalene is more widely used than α-methylnaphthalene. It can be used to produce textile auxiliaries, lubricants and plant growth regulators. The pure β-methylnaphthalene can be used as a raw material for the synthesis of vitamin K drugs and feed additives. At present, the separation of β-methylnaphthalene and α-methylnaphthalene is mainly based on the difference in melting point, and the purity of the prepared β-methylnaphthalene is 95%, but the yield is only 40%, and the prepared Nitrogen-containing compounds such as indole and quinoline contained in β-methylnaphthalene affect its application in medicine and feed....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/00C07C7/06C07C7/14C07C7/152C07C15/24B01D9/04B01D5/00
CPCB01D5/003B01D9/00B01D2009/0086C07C7/005C07C7/06C07C7/14C07C7/152C07C15/24
Inventor 谈勇谈俊江晓龙陈亮胡涛
Owner PENG CHEN NEW MATERIALS TECH CO LTD
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