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Method for preparing biological diesel oil from waste animals and plants grease

A technology of animal and vegetable oils and biodiesel, which is applied in the preparation of liquid hydrocarbon mixtures, biological raw materials, biofuels, etc., can solve the problems of high reaction temperature, difficulty in complete reaction, and poor effect of water removal, and achieve full esterification reaction , less equipment investment, faster speed

Inactive Publication Date: 2012-08-15
JIANGSU ZHONGSHENG GAOKE ENVIRONMENTAL CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

The disadvantage of this one-time addition of reflux reaction is that the generated moisture (reaction water, self-contained water) is always in the reactor, and the reaction between low-carbon alcohol and fatty acid in the raw material is a reversible process, and the presence of moisture in the reaction system will make the fatty acid The esterification reaction with low-carbon alcohols is difficult to completely react, which in turn affects the rate of the esterification reaction and the equilibrium conversion rate. Esterification produces a high acid value, which affects the subsequent second step of the base-catalyzed reaction. For example, soap is easily produced during the base-catalyzed transesterification reaction. class by-products
Although this method can take out the moisture produced by the reaction through methanol vapor and be separated, the disadvantage is that the esterification reaction is operated under pressure, and the methanol vapor phase in the reactor is easy to leak, which increases unsafe factors; secondly, methanol is released from the reactor. The upper part is added, because the temperature in the reactor is higher than the vaporization temperature of methanol, most of the methanol has actually been vaporized after entering the reactor, so that only part of the methanol vapor is sucked into the reaction system in the form of bubbles by stirring to form a gas-liquid reaction with the oil (liquid phase). Two-phase reaction, due to the mass transfer resistance between the gas and liquid phases, the reaction mainly occurs at the gas-liquid phase interface, resulting in a decrease in the effect of the esterification reaction; moreover, the vaporization of methanol entering the reactor also suppresses the water contained in the reactor. Methanol vapor is discharged quickly, resulting in poor water take-out effect, which also reduces the rate of esterification reaction to a certain extent, and affects the subsequent second step of base-catalyzed reaction
But shortcoming is the same as above-mentioned CN1995288, and methyl alcohol also enters in the reaction system with gaseous form, and the methanol of vapor phase and liquid phase grease form gas-liquid two-phase, because catalyst is solid acid catalyst, actual reaction system is gas-liquid-solid three-phase reaction, Due to the mass transfer resistance between the gas-liquid-solid three-phase, it will also reduce the rate of the esterification reaction, resulting in a decrease in the effect of the esterification reaction; secondly, the reaction temperature is relatively high, the energy consumption is relatively large, and a methanol vaporizer and corresponding controls need to be added The system and equipment are inconvenient to operate, resulting in difficulty in process control

Method used

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  • Method for preparing biological diesel oil from waste animals and plants grease

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: In 3M 3 In the reactor, add 2000KG of acidified oil (the main component is fatty acid, acid value 189.3mgKOH / g oil, the oil content is very low and no transesterification reaction is necessary), stir and heat at about 65°C, add catalyst sulfuric acid 20KG, liquid phase methanol Continuously pumping from the bottom of the reactor, the temperature of the reactor rises to about 75°C to carry out the esterification reaction, the vapor phase (methanol, water) coming out from the top of the reactor directly enters the methanol rectification tower, and the liquid phase methanol after the water is separated, Return and add from the bottom of the reactor. When the acid value drops to 0.75mgKOH / g, the esterification reaction ends (about 2 hours), and the reaction solution settles for 4 hours (or directly centrifuged), and the sulfuric acid catalyst and a small amount of impurities in the lower layer are separated. , to obtain the upper layer crude biodiesel (acid value...

Embodiment 2

[0016] Example 2: In 3M 3 In the reactor, add clay oil (the main component is vegetable oil, a small amount of fatty acid, acid value 14.21mgKOH / g oil) 2000KG, stir and heat at about 65°C, add catalyst sulfuric acid 18KG, and continuously add liquid phase methanol from the bottom of the reactor to carry out esterification. For chemical reaction, the temperature of the reactor is gradually raised to about 75°C, and the vapor phase (methanol, water) coming out of the reactor directly enters the methanol rectification tower. After the reaction until the acid value dropped to 1mgKOH / g, the esterification reaction ended (about 0.5 hours), and the reaction solution settled for 4 hours to separate the lower layer of sulfuric acid catalyst and a small amount of impurities, and the upper layer was oil with an acid value of 0.92mgKOH / g.

[0017] Then, the clay oil after the esterification reaction is transesterified with methanol under the catalysis of the alkali catalyst, and settled f...

Embodiment 3

[0018] Example 3: In 3M 3 In the reactor, add 2000KG of refined waste oil (the main components are animal and vegetable oils, fatty acids, acid value 65.86mgKOH / g oil), and add solid catalyst Fe 2 o 3 / SO 4 2- / Carrier 40KG, stirring and heating at about 70°C, liquid phase methanol is continuously added from the bottom of the reactor for esterification reaction, the temperature of the reactor is gradually increased to about 100°C, and the vapor phase (methanol, water) coming out of the reactor is directly into the methanol distillation column. After reacting to the acid value and dropping to 2mgKOH / g, the esterification reaction ended (about 1.5 hours), and the reaction solution settled for 4 hours to separate the lower catalyst iron sulfate and a small amount of impurities, and the acid value of the upper layer reactant was 0.82mgKOH / g oil.

[0019] Then, the waste oil after the esterification reaction is transesterified with methanol under the catalysis of the alkali cat...

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Abstract

The improved continuous esterification process of waste animal and vegetable oil and grease with low carbon alcohol to prepare biodiesel oil features that liquid low carbon alcohol is introduced into the liquid comprising liquid waste animal and vegetable oil and grease in 95-99.9 wt% and acid catalyst in 0.1-5 wt% to produce esterification reaction at normal pressure and the temperature from vaporizing temperature to 95 deg.c while the vapor mixture comprising the resultant, water vapor and low carbon alcohol vapor is discharged from the top of the reactor and separated in a fractionating tower to obtain product, separated water and liquid low carbon alcohol for reuse. The process has high reaction speed, high reaction conversion rate and other advantages, and the product has acid value capable of being controlled below 2 mgKOH / g.

Description

technical field [0001] The invention relates to a method for preparing biodiesel, in particular to a method for preparing biodiesel by continuous esterification of low-carbon alcohols using waste animal and vegetable oils as raw materials. Background technique [0002] Biodiesel is a fatty acid ester (mixed fatty acid low-carbon alcohol ester) obtained by transesterifying animal and vegetable oils and low-carbon alcohols (such as methanol, ethanol, butanol, etc.) under the action of an alkali catalyst. It has the advantages of regeneration, easy biodegradation, non-toxicity, low sulfur content and small emission of harmful substances in the exhaust gas, and is an environmentally friendly fuel. [0003] Using waste animal and vegetable oils (acidified oil, gutter oil, hog oil, clay oil, etc.) as raw materials to prepare biodiesel can reduce costs and find a good disposal method for these waste oils. However, since the main components of waste oil include oil and fatty acid, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G3/00
CPCY02E50/13Y02E50/10Y02P30/20
Inventor 李为民许汉祥高琦
Owner JIANGSU ZHONGSHENG GAOKE ENVIRONMENTAL CO LTD
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