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Fixed bed-based continuous catalytic esterification production method

A production method and fixed bed technology, applied in the field of oleochemical industry, can solve the problems of large amount of methanol used, reduced resin activity, increased production steps, etc. Effect

Active Publication Date: 2012-11-28
ZHONGGU TIANKE TIANJIN BIOENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic literature and related patents have many reports on the catalytic esterification technology of these two catalysts, and have their own advantages and disadvantages: the catalytic esterification technology of liquid acid—concentrated sulfuric acid as a catalyst has high catalytic activity, and can reduce the acid value to 3mgKOH / g or less, but it has strong corrosion to equipment, produces a large amount of waste water, and has side reactions, intermittent production, and high labor intensity; fixed-bed catalytic esterification technology with strong acid resin as filler realizes continuous production. Less side reactions, no waste water discharge, no corrosion to equipment, but low catalytic activity, secondary esterification is required to reduce the acid value to below 3mgKOH / g, the amount of methanol used is large, and at the same time, the resin will absorb pigments after a period of operation Impurities block the pores of the resin, resulting in a decrease in resin activity, requiring activation and regeneration of the resin, thus increasing the number of production steps

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A fixed-bed continuous catalytic esterification production method, comprising the steps of:

[0019] (1) Mix the raw material with methanol with a mass percentage of more than 99.5% according to the mass ratio of 1:0.8. The raw material is used to remove impurities, and the acid value of the water with a mass percentage of less than 0.05% is 78.2mgKOH / g of deodorized distillate;

[0020] (2) Mix the mixture solution obtained in step (1) with sulfuric acid at a mass ratio of 1:0.001 and heat it to 80°C, then carry out esterification reaction through a fixed bed equipped with D061 strong acid resin, and the flow rate is controlled At 0.5 times the resin volume per hour, the pressure is controlled at 0.1MPa;

[0021] (3) On-line neutralization of the solution treated in step (2) with lye so that the pH value is controlled at 7, and the lye is an aqueous sodium hydroxide solution with a mass concentration of 20%;

[0022] (4) Dealing alcohol and water under reduced press...

Embodiment 2

[0025] A fixed-bed continuous catalytic esterification production method, comprising the steps of:

[0026] (1) Mix the raw material with methanol with a mass percentage of more than 99.5% according to the mass ratio of 1:0.5. The raw material is used to remove impurities, and the acid value of the water with a mass percentage of less than 0.1% is 85.4mgKOH / g of deodorized distillate;

[0027] (2) Mix the mixture liquid obtained in step (1) with hydrochloric acid at a mass ratio of 1:0.002 and heat it to 90°C, then carry out esterification reaction through a fixed bed equipped with NKC-9 strong acid resin, The flow rate is controlled at 0.4 times the resin volume per hour, and the pressure is controlled at 0.1MPa;

[0028] (3) Online neutralization of the solution treated in step (2) with lye so that the pH value is controlled at 8, and the lye is an aqueous sodium hydroxide solution with a mass concentration of 30%;

[0029] (4) Dealing alcohol and water under reduced pres...

Embodiment 3

[0032] A fixed-bed continuous catalytic esterification production method, comprising the steps of:

[0033] (1) Mix the raw material with methanol with a mass percentage of more than 99.5% according to the mass ratio of 1:0.1. The raw material is used to remove impurities, and the acid value of the water with a mass percentage of 0.3% or less is 15.3mgKOH / g of swill oil;

[0034] (2) Mix the mixture solution obtained in step (1) with nitric acid at a mass ratio of 1:0.0025 and heat it to 70°C, then carry out esterification reaction through a fixed bed equipped with HD-8 strong acid resin, The flow rate is controlled at 0.6 times the resin volume per hour, and the pressure is controlled at 0.15MPa;

[0035] (3) On-line neutralization of the solution treated in step (2) with lye so that the pH value is controlled at 7, and the lye is an aqueous sodium hydroxide solution with a mass concentration of 10%;

[0036] (4) Dealing alcohol and water under reduced pressure on the feed...

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Abstract

The invention discloses a fixed bed-based continuous catalytic esterification production method. The fixed bed-based continuous catalytic esterification production method comprises the following steps of 1, mixing a raw material and a lower alcohol having a concentration above 99.5%, wherein the raw material is high-acid value waste vegetable and animal oil or a deodorizer distillate which does not contain impurities and has moisture content of 0.05 to 0.5%, 2, merging a mixed material liquid obtained by the step 1 and an acid, heating to a temperature of 50 to 100 DEG C, and carrying out an esterification reaction process by a fixed bed with a highly acidic resin, 3, carrying out on-line neutralization by an alkali solution, 4, carrying out reduced pressure removal of an alcohol and water, and 5, carrying out reduced pressure distillation to obtain a purified low fatty acid ester. The fixed bed-based continuous catalytic esterification production method can reduce a raw material acid value to below 3mgKOH / g only by one step, avoid secondary esterification, reduce a use amount of a solvent by 50%, reduce energy consumption and solvent consumption by 50%, avoid resin regeneration treatment and realize a service life above 2 years.

Description

technical field [0001] The invention relates to an improved fixed-bed continuous catalytic esterification production method, in particular to the industry of biodiesel and natural VE, and belongs to the field of oleochemical industry. Background technique [0002] In the process of producing fatty acid methyl ester—biodiesel with high acid value waste animal and vegetable oil as raw material and natural VE with DD oil (deodorized distillate) as raw material, it is necessary to combine the free fatty acid in the raw material with the action of acidic catalyst Methanol or ethanol is converted into fatty acid methyl ester or ethyl ester. At present, the acid catalyst of the manufacturer mainly involves liquid acid-concentrated sulfuric acid and strong acid resin. Domestic literature and relevant patents have many reports on the catalytic esterification technology of these two catalysts, and have their own advantages and disadvantages: the catalytic esterification technology of ...

Claims

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Application Information

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IPC IPC(8): C11C3/04
Inventor 陈学兵曹玉平蒋一鸣倪少利周学晋安然王静
Owner ZHONGGU TIANKE TIANJIN BIOENG