CN103831060B - A kind of alcohol ketone device deperoxidation catalysts prepares the method for tower draining - Google Patents

A kind of alcohol ketone device deperoxidation catalysts prepares the method for tower draining Download PDF

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Publication number
CN103831060B
CN103831060B CN201210490513.6A CN201210490513A CN103831060B CN 103831060 B CN103831060 B CN 103831060B CN 201210490513 A CN201210490513 A CN 201210490513A CN 103831060 B CN103831060 B CN 103831060B
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tower
catalyst
reboiler
drainage line
deperoxidation
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CN103831060A (en
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李志刚
张大勇
李英伟
王晖
赵英
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China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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Abstract

The present invention relates to a kind of method that alcohol ketone device deperoxidation catalysts prepares tower draining; Be that intermittent drainage line at the bottom of catalyst preparing tower tower increases a U-shaped pipe continuous drainage line, by the effect of U-shaped pipe, tower prodelta clay water introduced catalyst tower and normally descends stockline, directly enter catalyst tank continuously, in catalyst tank, complete being separated of water and catalyst; Bottom catalyst preparing tower reboiler, intermittent drainage line increases by a restriction orifice, aperture Φ 1 ~ Φ 10mm, makes the ponding in reboiler enter catalyst tank continuously, and discharge capacity, close to ponding generation bottom reboiler, ensures that at the bottom of tower, liquid level is normal; This method ensure that catalyst preparing tower Parameter Stationary is run, and improves catalyst quality, reduces device ring hexane unit consumption 2kg/t, reduces the tert-butyl alcohol, chromic acid consumption each 10%.

Description

A kind of alcohol ketone device deperoxidation catalysts prepares the method for tower draining
Technical field
The present invention relates to a kind of method that alcohol ketone device deperoxidation catalysts prepares tower draining.
Background technology
Alcohol ketone device adopts cyclohexanol, the manufacturing process of cyclohexanone (alcohol ketone) mixture is carried out according to following two successive reactions.
The first step, thiacyclohexane is not having under catalyst action, and be oxidized to cyclohexyl hydroperoxide with oxygen denuded air, reaction equation is as follows:
C6H 12+O 2→C6H 11OOH
Second step, cyclohexyl hydroperoxide is taken off peroxidating directional decomposition in the existence of chromic acid tert-butyl catalyst and is become cyclohexanone, and reaction equation is as follows:
C6H 11OOH→C6H 1OO+H 2O
The catalyst of deperoxidation reaction is chromic acid tert-butyl, and three components is (containing the tert-butyl alcohol 25%; Octyl phosphate 10%; Cyclohexane 65%, plays Solvents Solvent effect) enter catalyst preparing tower, the tert-butyl alcohol and chromic acid generation esterification with chromic acid (concentration 10%) simultaneously, generate chromic acid tert-butyl, this reaction is reversible reaction, and reaction equation is as follows:
This catalyst preparing Deethanizer design is vacuum reaction tower, totally 16 layers of tower tray, and operating condition is 15 ~ 30kPa (absolute pressure), 15 ~ 45 DEG C.Tower bottom reboiler is using 80 DEG C of hot water as heat source.Water and cyclohexane azeotropic in the water that reaction generates and chromic acid solution, most ofly steam from tower top, and a small amount of water lodges at the bottom of tower.When lodging in the hypervolia at the bottom of tower, as the product of reversible reaction, first hypervolia directly affects the generation of positive reaction.Secondly water specific heat is comparatively large, and hypervolia affects tower bottom reboiler heating.In a word, water yield accumulation at the bottom of tower too much causes esterification poor, and catalyst chrome content is low, affects the conversion ratio of deperoxidation reaction, affects the cyclohexane unit consumption of package unit.Therefore 4 ~ 6 hours artificial's drainings are needed once.Drain operation frequently, causes the parameter fluctuation of catalyst tower comparatively large, causes catalyst quality bad, waste catalyst, increase the chemical industry material tert-butyl alcohol, chromic acid consumption.
Summary of the invention
The object of this invention is to provide a kind of method that alcohol ketone device deperoxidation catalysts prepares tower draining, realize continuous drainage at the bottom of catalyst preparing tower tower, reduce artificial drainage number of times.
The method that alcohol ketone device deperoxidation catalysts of the present invention prepares tower draining is that intermittent drainage line at the bottom of catalyst preparing tower tower increases a U-shaped pipe continuous drainage line, by the effect of U-shaped pipe, tower prodelta clay water is introduced catalyst tower and normally descends stockline, directly enter catalyst tank continuously, in catalyst tank, complete being separated of water and catalyst.
Bottom catalyst preparing tower reboiler, intermittent drainage line increases by a restriction orifice, aperture Φ 1 ~ Φ 10mm, makes the ponding in reboiler enter catalyst pans continuously, and discharge capacity, close to ponding generation bottom reboiler, ensures that at the bottom of tower, liquid level is normal.
1, ensure that catalyst preparing tower Parameter Stationary is run, improve catalyst quality, reduce device ring hexane unit consumption 2kg/t, amount to economic benefit about 1,000,000 yuan.
2, reduce the tert-butyl alcohol, chromic acid consumption each 10%, amount to economic benefit about 400,000 yuan.
Accompanying drawing explanation
Continuous drainage process chart at the bottom of Fig. 1 catalyst preparing tower tower.
Wherein: 1 catalyst preparing tower, 2 reboilers, 3V1 valve, 4 catalyst tank, 5V5 valve, 6V2 valve, 7V3 valve, 8V7 valve, 9V6 valve, 10V4 valve, 11U shape pipe, 12 restriction orifices, 13V8 valve.
Detailed description of the invention
Alcohol ketone device deperoxidation catalysts of the present invention prepares the drainage equipment of tower, comprising: restriction orifice, U-shaped pipe and valve; Catalyst preparing tower 1 tower bottom outlet is connected with reboiler 2 tube-side inlet, and the outlet of reboiler tube side is leaded up to connecting line and is connected with entrance at the bottom of catalyst preparing tower tower, separately leads up to V2 valve 6, V5 valve 5 to be connected with catalyst tank 4 import; Reboiler bottom discharge line is connected with the connecting line between V2 valve, V5 valve by V1 valve 3, and restriction orifice 12 is arranged on the pipeline at V1 valve export place; U-shaped pipe 11 low side is connected to before V2 valve inlet on pipeline by V3 valve 7, is high-endly connected on the connecting line between V6 valve 9, V8 valve 13 by V4 valve 10; V8 valve inlet exports with discharge line at the bottom of catalyst preparing tower tower and is connected, and V8 valve export is connected with catalyst tank import by V6 valve, V7 valve 8.
Under normal production status, close V2 valve, open V3 valve, V4 valve, come into operation continuous drainage line at the bottom of catalyst preparing tower tower.
Under normal production status, close V2 valve, open V1, V5 valve, come into operation reboiler continuous drainage orifice plate.Close V1 valve, V5 valve under dead ship condition, prevent material from entering catalyst tank by orifice plate.

Claims (1)

1. an alcohol ketone device deperoxidation catalysts prepares the method for tower draining; It is characterized in that: intermittent drainage line at the bottom of catalyst preparing tower tower increases a U-shaped pipe continuous drainage line, by the effect of U-shaped pipe, tower prodelta clay water is introduced catalyst tower and normally descends stockline, directly enter catalyst tank continuously, in catalyst tank, complete being separated of water and catalyst;
Bottom catalyst preparing tower reboiler, intermittent drainage line increases by a restriction orifice, aperture Φ 1 ~ Φ 10mm, makes the ponding in reboiler enter catalyst tank continuously, and discharge capacity, close to ponding generation bottom reboiler, ensures that at the bottom of tower, liquid level is normal.
CN201210490513.6A 2012-11-27 2012-11-27 A kind of alcohol ketone device deperoxidation catalysts prepares the method for tower draining Active CN103831060B (en)

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CN201210490513.6A CN103831060B (en) 2012-11-27 2012-11-27 A kind of alcohol ketone device deperoxidation catalysts prepares the method for tower draining

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Application Number Priority Date Filing Date Title
CN201210490513.6A CN103831060B (en) 2012-11-27 2012-11-27 A kind of alcohol ketone device deperoxidation catalysts prepares the method for tower draining

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CN103831060A CN103831060A (en) 2014-06-04
CN103831060B true CN103831060B (en) 2016-04-06

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Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4004965A (en) * 1972-01-10 1977-01-25 Maloney-Crawford Tank Corporation Vertical flameless reboiler for reconcentrating liquid desiccant
JP3667546B2 (en) * 1999-01-22 2005-07-06 ホシザキ電機株式会社 Drainage equipment
CN101172931B (en) * 2006-11-01 2011-11-16 肖藻生 Improved process for producing cyclohexanol and pimelinketone
CN202452096U (en) * 2012-03-02 2012-09-26 乳山市日晟机械制造有限公司 Pressure maintaining tube type drainer

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