UA28197U - Process for preparation of carboxylic esters - Google Patents

Abstract

A process for preparation of carboxylic esters involves esterification of oil and fat components of spent filter powder of plant oil production by compounding with alcohol in the presence of catalyst, isolation of final product from the reaction mixture.

Description

Description of the invention

The useful model refers to the field of fat processing, in particular to the technology of obtaining esters of carboxylic 2 acids by esterification of fats of biological origin, which are used as biological fuel for internal combustion engines, called in international practice as biodiesel.

Biodiesel or biodiesel fuel is an environmentally friendly type of fuel, an alternative to mineral fuels obtained from vegetable oils and used to replace conventional diesel fuel. The raw material for the production of biodiesel in different countries is the oil of different plants, for example: USA - soybean; Canada - canola; 70 | Indonesia - palm oil; Philippines - coconut oil; India - jatropha (daiornpa); Africa - soy, jatropha;

Brazil - castor oil. In European countries, rapeseed is the main source of vegetable oil for biodiesel production. About 8,095% of European biodiesel is produced from rapeseed oil, with around a third of the rapeseed crop used for biodiesel production.

Ukraine shows significant interest in the development of biodiesel production The development of biodiesel 712 fuel production in Ukraine is fully in line with the main principles of state policy in the field of alternative types of fuel, set out in the Law of Ukraine "On Alternative Types of Liquid and Gaseous Fuels" Мо1391-ХИ dated January 14, 2000 and in Decree of the President of Ukraine "On measures to develop fuel production from biological raw materials" Mo1094/2003 dated September 26, 2003). The Cabinet of Ministers of Ukraine approved the concept of the Program for the Development of Diesel Biofuel Production by 2010. 20 It is important to note that when the yield of rapeseed falls below a certain level, the production of biodiesel fuel from rapeseed oil becomes unprofitable. It is not always possible to ensure the appropriate yield of rape on the earthen lands of the European territory. That is, it is urgent to expand the raw material base for the production of biodiesel fuel while meeting the conditions of production profitability.

Known methods of obtaining esters of carboxylic acids, as a rule, are based on the reaction of esterification of 25 oil and fat components of biological origin by combining them with monohydric alcohol in the presence of a catalyst.

Thus, there is a known method of obtaining esters of carboxylic acids (patent of Ukraine Mo44931, IPC: С07С67/03, priority from 23.11.1998), in which the initial product in the form of fatty substances of plant or animal origin is combined with methanol and potassium hydroxide and conditions are created for obtaining chemical equilibrium by emulsifying the reaction mixture in 30 with a phase separation area, where the fat is subjected to esterification to obtain Ge"! carboxylic acid methyl ether followed by purification of the latter. When chemical equilibrium is reached, the glycerol phase and other precipitates are removed from the reaction mixture. The esterification reaction begins to be carried out at -- high pressure. During the process, the pressure is reduced. Gee)

The general features of the known method and the proposed solution are the method of obtaining esters of 35 carboxylic acids, which includes the esterification of oil and fat components of raw materials by combining them with alcohol in the presence of a catalyst, followed by the separation of the finished product from the reaction mixture.

The raw material base for the implementation of the specified method is limited to fats (oils) of vegetable or animal origin. "

Also known is the method of obtaining esters of carboxylic acids according to |(US patent Mo5354878, IPC: СО7С67/03, - 50 priority from 03.26.1993|. The method includes the combination of animal fat and/or vegetable fat (oil) with monoatomic alcohol, as which methanol is used in the presence of a catalyst - sodium hydroxide at

From" the reaction temperature to 1002С. Esterification is carried out in stages in serially connected reactors. The starting fat and/or oil of biological origin is fed into the first reaction apparatus, into which methyl alcohol and sodium hydroxide are introduced and esterification is performed with the movement of the reaction mixture into the next reactor, into which alcohol and a catalyst are added. The glycerol phase is removed from the reaction mixture of each reactor. From the last reactor, a finished product is obtained - methyl ether, which is subjected to purification. (ee) The general features of the known method and the proposed solution are the method of obtaining carboxylic esters from acids, which includes the esterification of the fatty components of the raw material by combining them with alcohol in the presence of a catalyst, followed by the separation of the finished product from the reaction mixture. (Se) 50 The raw material base for the implementation of the specified method is limited to fats (oils) of vegetable or animal origin.

As a prototype, the method of obtaining esters of carboxylic acids according to the declaration patent of Ukraine for the utility model Ke 23270, IPC: СО7С67/03, priority from 03.05.2007) was chosen. The method of obtaining a carboxylic acid ester includes esterification of the initial product in the form of fat and/or oil of biological origin by mixing it with monohydric alcohol in the presence of a catalyst in a technological chain with successively connected reactors, removing the glycerol phase from the reaction mixture, obtaining the finished product from the last reactor product and its purification, while the initial product is subjected to preliminary treatment in an additional reactor installed in front of the first reactor of the technological chain with the glycerol phase removed from other reactors, after which the glycerol phase is taken from the additional reactor for processing, and the reaction mixture from the additional reactor is sent to the first reactor of the technological chain.

The starting product, which is fat or oil of biological origin, is heated in a heat exchanger to 55-602C and fed to the first reactor of the technological chain through an additional reactor, which is installed in front of the first reactor. At the same time, monoatomic alcohol in the form of methanol or ethanol is fed into the cavity of the first reactor together with a catalyst, which is potassium hydroxide. After b5 20-25 minutes, the glycerol phase formed as a result of the esterification reaction is removed from the reaction mixture of the first reactor, which is directed into the cavity of the additional reactor, and the reaction mixture from the first reactor is moved through the sump to the second reactor, in which the operations performed in the first reactor are repeated , and so on along the technological chain. Thus, the glycerol phase, which contains a part of the alcohol and catalyst in its mass, from all reactors without exception, starting with the first one, falls into the mass of biological fat or oil contained in the cavity of the additional reactor, which allows to reuse previously used ones for the esterification reaction in other reactors, alcohol and a catalyst, thereby reducing the consumption of these components.

General features of the prototype and the proposed solution are the method of obtaining esters of carboxylic acids, which 7/0 includes the esterification of oil and fat components of raw materials by combining them with alcohol in the presence of a catalyst, followed by the separation of the finished product from the reaction mixture.

The raw material base for the implementation of the specified method, as well as the above-mentioned analogs, is limited to fats (oils) of vegetable or animal origin.

The basis of a useful model is the task of expanding the raw material base for the production of esters /5 of carboxylic acids.

The problem is solved by the fact that in the method of obtaining esters of carboxylic acids, which includes the esterification of oil and fat components of the raw material by combining them with alcohol in the presence of a catalyst, followed by the separation of the finished product from the reaction mixture, according to a useful model, the spent filter powder of the production is used as a raw material vegetable oil.

The listed features are essential features of a useful model.

It is advisable to use monoatomic alcohol as an alcohol, and to use potassium hydroxide as a catalyst.

It is expedient to isolate the finished product by centrifuging the reaction mixture or pressing the reaction mixture with its preliminary packing in filter material, followed by separation of the obtained liquid fraction into carboxylic acid esters and glycerin solution by settling or by centrifugation of the liquid fraction.

The essential features of a useful model are in a causal relationship with the achieved result. t

Thus, the production of carboxylic acid esters by esterification of oil and fat components of raw materials by combining them with alcohol in the presence of a catalyst followed by the separation of the finished product from the reaction mixture, when used as a raw material of spent filter powder from the production of vegetable oil, provides an opportunity to expand the raw material base for carboxylic acid esters and disposal of production waste.

The content of oil and fat components in spent filter powders from vegetable oil production ranges from 20 to 70,905 Me. They include light fat fractions (oils), as well as heavier fractions - waxes. "-

It has been experimentally confirmed that spent filter powders from the production of vegetable oil can be used as raw materials for the production of carboxylic acid esters. At the same time, there is no need to pre-separate the oil and fat components contained in the spent filter powder. with

Fatty components of the spent filter powder undergo an esterification reaction with the formation of carboxylic acid esters when alcohol and a catalyst are added directly to the spent filter powder. This makes it possible to use spent filter powders from the production of vegetable oil directly as raw materials for the production of carboxylic acid esters and utilization of production waste. Below is a description of the method of obtaining esters of carboxylic acids with examples of its specific implementation. ;" The method of obtaining esters of carboxylic acids is based on the reaction of esterification of fatty components of the spent filter powder of vegetable oil production by combining them with monoatomic bpyrt in the presence of a catalyst in a technological reactor. The spent filter powder from the production of vegetable oil is heated to a temperature of 50-609C and loaded into a technological reactor. Next, an alcohol, such as methanol, is added to the reactor in the amount of 10-2095, and a catalyst, for example, a ten-fifteen percent solution of potassium hydroxide, in the amount of 8-1595 relative to the weight of the oil and fat components contained in the spent filter powder. The mixture is stirred

In the reactor for 10-15 hours at a temperature of 50-6020. The finished product is isolated from the resulting reaction mixture. To do this, the reaction mixture is packed in bags of "I" filter material and pressed in this form in a suitable press with the removal of the liquid fraction.

Isolation of the liquid fraction is also possible by centrifugation of the reaction mixture using known centrifuges. The liquid fraction includes esters of carboxylic acids and glycerin. To isolate the finished product, the resulting liquid fraction is allowed to stand for 4-6 hours. At the same time, carboxylic acid esters float to the top.

An aqueous solution of glycerin is collected at the bottom. After the settling of the liquid fraction, esters of carboxylic acids are merged to obtain the finished product. Isolation of the finished product is also possible by centrifugation of the liquid fraction using known centrifuges.

Example 1. 60 Raw material: spent filter powder from the production of sunflower oil at the "YUG RUSYA" enterprise, Rostov-on-Don, Russian Federation.

Characteristics of raw materials: - base - mineral kieselguhr brand "Sylayt-545"; organoleptic characteristics - non-homogeneous mass with fractional composition with a smell characteristic of 65 sunflower oil, white color; - content of oil and fat components - 6595.

The specified filter powder in the amount of 5Okg was heated to 55923 and loaded into a technological reactor with a mechanical paddle stirrer. Next, 4.9 kg of monoatomic alcohol - methanol SNZON (from the calculation of 1595 relative to the mass of oil and fat components in the spent filter powder) was added to the reactor and

2.2 kg of a twelve percent solution of potassium hydroxide KOH (based on the calculation of 1095 relative to the mass of oil and fat components in the spent filter powder). The mixture was stirred in the reactor for 12 hours at a temperature of 5590. The esterification reaction of the oil and fat components of the spent filter powder took place in the reactor.

The resulting reaction mixture, which includes filter powder, carboxylic acid esters, glycerin and water 70, was discharged from the reactor, packed into filter fabric bags and pressed in this form with a gradual increase in pressure to 250-300 atm. Upon reaching the indicated pressure value, pressing was held for 10-12 minutes at constant pressure. As a result of pressing, a liquid fraction was isolated from the reaction mixture, which includes esters of carboxylic acids, glycerin and water.

The liquid fraction was settled for 5 hours, after which the upper layer of the sediment was drained to obtain the finished product 75 in the form of carboxylic acid esters. The output of the finished product is 17.5 kg of carboxylic acid esters.

Example 2

Raw materials, operations, modes of operations, ratio of components are the same as in example 1. In addition, water in the amount of 95 liters was added to the mixture of spent filter powder, methanol and potassium hydroxide in the reactor (based on the calculation of three parts by weight of water to one part by weight oil and fat components contained in the used filter powder). The yield of the finished product in this example was 18.5 kg of carboxylic acid esters. The increase in the yield of the finished product is explained by the improvement of the contact of methanol with oil and fat components in the presence of water.

Thus, the method claimed as a useful model provides an expansion of the raw material base for the production of carboxylic acid esters due to the use of spent filter powder as a raw material, as a waste product of vegetable oil production. The output of the finished product is about 3595 from the mass of spent filter powder. in

Claims (4)

Formula of the invention "a 1. The method of obtaining esters of carboxylic acids, which includes the esterification of oil and fat components of Me. raw materials by combining them with alcohol in the presence of a catalyst with subsequent separation of the finished product from the 4-/s pe reaction mixture, which differs in that the used filter powder from the production of vegetable oil is used as a raw material. co 2. The method according to claim 1, which differs in that monohydric alcohol is used as alcohol. with C. The method according to claim 1, which differs in that potassium hydroxide is used as a catalyst. 4. The method according to claim 1, which differs in that the separation of the finished product is carried out by centrifuging the reaction mixture or pressing the reaction mixture with its preliminary packing in filter material, followed by the separation of the obtained liquid fraction into carboxylic acid esters and "glycerol solution by settling or centrifugation liquid fraction. shsh - Official Bulletin "Industrial Property". Book 1 "Inventions, useful models, topographies of integrated microcircuits", 2007, M 19, 26.11.2007. State Department of Intellectual Property of the Ministry of Education and Science of Ukraine. ime) (ee) - about 50 that with 60 b5