RU2385900C1 - Method of preparing liquid biofuel - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: method involves preparation of raw material, heating with subsequent treatment and obtaining fuel. The prepared material is heated at 55-60°C, with subsequent separation of moisture and impurities, and the material is treated in a reaction vessel through simultaneous esterification and trans-esterifiction while mixing the material with alcohol in ratio 5:1-7:1 respectively and addition of a heterogeneous acid catalyst in amount of 5-10% to the mass. The process is carried out at 120-150°C for 60-120 minutes with turbulent stirring at 1200-1500 rpm and at atmospheric pressure. 5% glycerin is added 15 minutes before the end of the process. The process is stopped and the heterogeneous catalyst is extracted. The obtained substrate is put into a settling tank and kept for 6 hours. Biodiesel and glycerin in the settling tank are separated by draining the formed bottom glycerin phase. Excess alcohol is distilled off. The biodiesel is purified with magnesium silicate for 30 minutes. Magnesium silicate is extracted and reduced. The raw material used is raw fat containing 10-100% free fatty acids and/or plant material of oil-bearing crops, and the heterogeneous acid catalyst used is lanthanum diphosphate and/or magnesium silicate and/or aluminium diphosphate and/or sulphated zirconium.

EFFECT: invention increases output of the product with improved ecological index.

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Description

The invention relates to the field of processing industrial waste, in particular the food industry, livestock processing, and can be used in the production of liquid biofuels for agricultural and domestic needs.

A known method of producing fuel for a diesel engine, comprising: the step of first cleaning waste oil containing fish oil (unused oil or waste fish oil) or a filtered mixture of fish oil and vegetable oil (unused oil or waste vegetable oil) (hereinafter referred to as "starting material" ), with purification with stirring with the introduction of ozone for separation, the composition of the specified starting material and fine atomization of the starting material, the step of filtering the material obtained in the first treatment, step c the second purification of the mixture of the filtered material with the introduction of ozone for further fine atomization of the filtrate and the step of introducing the anti-crystallization agent into the material obtained in the second purification step, in which the redox and polymerization inhibitor are added at the first purification step, as a result of which the starting material is not oxidized so much (see RF application 2003113558, C10L 1/08, 2003).

A known method of converting a feedstock into at least one useful material, comprising preparing a suspension from said feedstock, introducing a suspension into a first reaction to obtain a reaction raw material comprising at least one solid reaction product, at least one liquid a reaction product and water, separating said at least one solid product, said water and said at least one liquid product from said reaction raw material and converting said at least of at least one liquid reaction product, for example, one liquid product includes at least one fat derivative or one fatty acid in at least one useful material in the second reaction (see application 2005133203, C05G 1/00, 2006 .).

Closest to the claimed method is known for processing animal fats and / or other raw materials into liquid fuel, which includes the following stages: feeding material including animal fats in liquid form to a distillation cube, extracting a volume of material from the distillation cube, heating the extracted material to a splitting temperature, returning the extracted material to a distillation cube, separation of compounds with a lower molecular weight from the cleaved material into a small fraction of volatile overheads and a secondary liquid fuel mixture on a distillation column, collecting a secondary liquid fuel mixture using a condenser (see application 2006120083, C10G 9/00, 2006).

Known methods allow to obtain liquid fuel, however, the methods are laborious.

The technical task of the claimed invention is to increase the yield of the product with improved environmental performance, reducing the cost of cleaning biodiesel and glycerin.

The problem is solved in a method for producing liquid biofuel, including the preparation of raw materials, heating, followed by processing and obtaining fuel, characterized in that the heating of the prepared raw materials is carried out at a temperature of 55-60 ° C, followed by separation of moisture and impurities, and the processing of the prepared raw materials is carried out in the reaction boiler by the simultaneous reaction of esterification and transesterification by mixing the feed with alcohol in a ratio of 5: 1-7: 1, respectively, and by adding a heterogeneous acid catalyst in an amount of 5 -10% by weight, while the process is carried out at a temperature of 120-150 ° C for 60-120 minutes with turbulent stirring at 1200-1500 rpm and atmospheric pressure, 15% glycerol is added 15 minutes before the end of the process, the process is stopped and the heterogeneous catalyst is removed, the resulting substrate is placed in the settling tank for 6 hours, the biodiesel and glycerin are separated in the settling tank by draining the lower glycerol phase, the excess alcohol is distilled off, the biodiesel is purified with magnesium silicate for 30 minutes, magnesium silicate is recovered and restored they are used as raw materials, containing fatty raw materials with a free fatty acid content of 10-100% and / or vegetable raw materials of Pancake week crops, and as a heterogeneous acid catalyst, lanthanum diphosphate, and / or magnesium silicate, and / or aluminum diphosphate, and / or sulfated zirconium.

This technological scheme has several advantages from traditional well-known technologies as follows:

- the use of any lipid raw material with any% FFA;

- carrying out reactions of ethefirization and transesterification at the same time;

- the use of a heterogeneous catalyst that increases the level of conversion of ethers, eliminating the formation of by-products of the reaction and pollution, allows you to use it repeatedly, reduces the cost of reagents;

- complex glycerol purification is not required;

- purification of the resulting esters is minimized;

- the use of a wider range of alcohols;

- more economical and energy-intensive processing of raw materials using silica gel, etc.

The scheme of the method is presented in the drawing.

Examples of the method

Example 1

100 kg of fatty raw materials with an acid number of 40 mg KOH / g are heated to 60 ° C, moisture and impurities are removed. Simple alcohol and a heterogeneous catalyst are added to the processed fatty raw materials.

The number of ingredients per batch is presented:

Ingredients amount Raw materials 100 kg Methanol 20 kg SO ₄ / ZrO ₂ (sulfated zirconium) 5 kg (Mg ₂ SiO ₄ ) Magnesium Silicate 2 kg

The esterification and transesterification reaction is carried out in a reaction boiler at 150 ° C. for 60 minutes at 1500 rpm (revolutions per minute) at atmospheric pressure. 5% glycerol is added to the reaction mixture obtained from the last batch and the process is continued for 15 minutes. Stopping the process and removing the heterogeneous catalyst. Place the resulting substrate in a settling tank for 6 hours. Separation of biodiesel and glycerol in a settling tank by draining the resulting lower phase of glycerol. Distillation of excess alcohol. Purification of biodiesel with magnesium silicate for 30 minutes Extraction of magnesium silicate and its recovery.

Example 2

100 kg of vegetable oil with an acid number of 2 mg KOH / g is heated to 55 ° C, moisture and impurities are removed.

Simple alcohol and a heterogeneous catalyst are added to the processed fatty raw materials.

The number of ingredients per batch is presented:

Ingredients amount Raw materials 100 kg Isopropyl 14.3 kg AlP (aluminum diphosphate) 7 kg (Mg ₂ SiO ₄ ) Magnesium Silicate 2 kg

An esterification and transesterification reaction is carried out at 120 ° C. for 60 minutes at 1200 rpm at atmospheric pressure. 5% glycerol is added to the reaction mixture and the process is continued for 15 minutes. Stopping the process and removing the heterogeneous catalyst. Place the resulting substrate in a settling tank for 6 hours. Separation of biodiesel and glycerol in a settling tank by draining the resulting lower phase of glycerol. Distillation of excess alcohol. Purification of biodiesel with magnesium silicate for 30 minutes Extraction of magnesium silicate and its recovery.

Example 3

50 kg of animal fat with an acid number of 150 mg KOH / g and 50 kg of vegetable oil with an acid number of 15 mg KOH / g are heated to 55 ° C, moisture and impurities are removed.

Simple alcohol and a heterogeneous catalyst are added to the processed fatty raw materials.

The number of ingredients per batch is presented:

Ingredients amount Raw materials 100 kg Ethanol 20 kg LaP (lanthanum diphosphate) 5 kg (Mg ₂ SiO ₄ ) Magnesium Silicate 2 kg

The esterification and transesterification reaction is carried out at 140 ° C. for 60 minutes at 1500 rpm at atmospheric pressure. 5% glycerol is added to the reaction mixture obtained from the last batch and the process is continued for 15 minutes. Stopping the process and removing the heterogeneous catalyst. Place the resulting substrate in a settling tank for 6 hours. Separation of biodiesel and glycerol in a settling tank by draining the resulting lower phase of glycerol. Distillation of excess alcohol. Purification of biodiesel with magnesium silicate for 30 minutes Extraction of magnesium silicate and its recovery.

Claims (1)

A method of producing liquid biofuel, including preparation of raw materials, heating, followed by processing and obtaining fuel, characterized in that the heating of the prepared raw materials is carried out at a temperature of 55-60 ° C, followed by separation of moisture and impurities, and the processing of prepared raw materials is carried out in a reaction boiler by simultaneous reaction esterification and transesterification by mixing raw materials with alcohol in a ratio of 5: 1-7: 1, respectively, and by adding a heterogeneous acid catalyst, in an amount of 5-10% by weight, while the process is t at a temperature of 120-150 ° C for 60-120 minutes with turbulent stirring at 1200-1500 rpm and atmospheric pressure, 15% glycerol is added 15 minutes before the end of the process, the process is stopped and the heterogeneous catalyst is removed, the resulting substrate is placed in settling tank for 6 hours, separate biodiesel and glycerin in the settling tank by draining the lower glycerol phase, distill excess alcohol, clean the biodiesel with magnesium silicate for 30 minutes, extract magnesium silicate and restore it, using fats as raw material raw materials with a free fatty acid content of 10-100% and / or vegetable raw materials of Pancake week crops, and as a heterogeneous acid catalyst, lanthanum diphosphate and / or magnesium silicate, and / or aluminum diphosphate, and / or sulfated zirconium.