RU2598263C2 - Method and apparatus for processing by-products of mustard and oil processing production (versions) - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: group of inventions relates to food industry. Apparatus contains a hydrolyzer reactor installed in horizontal position and equipped with a jacket, mixer and remote-controlled valve, device to create vacuum in the reactor, which is a drier, and a system for removal of hydrolysate volatile compounds with capacitors and a condensate phases separator. device to create vacuum is placed in a hydrolysate volatile compounds removal system. There is an ultrasonic generator in a hydrolyzer reactor. Method, carried out on the said apparatus, where during constant mixing by-products mass is added with enzymes in the amount of 2-5 % of the by-products content, said enzymes are used as catalysts, not more than 30 % water is added. Obtained mass is heated to 45-50 °C hydrolyzing in the presence of a catalyst. Obtained hydrolysate is dehydrated under vacuum till forming a vapor phase and a dry residue with moisture content of not more than 13 %, vapor phase is removed on condensation and after separation of condensate the essential mustard oil is produced, and the dry residue is delivered as a feed supplement. Another version of the apparatus contains a hydrolyzer reactor installed in horizontal position and equipped with a jacket, mixer and remote-controlled valve, device to create vacuum in the reactor, which is a drier, a mixer installed in front of the reactor and a system for removal of hydrolysate volatile compounds with capacitors and a condensate phases separator. Device to create vacuum is placed in a hydrolysate volatile compounds removal system, a mixer comprises a loading hatch at the inlet, and mixing device and orifice grid at the outlet. There is an ultrasonic generator in a hydrolyzer reactor. Method, carried out on the said apparatus, where during constant mixing by-products mass is added with enzymes in the amount of 2-5 % of the by-products content, said enzymes are used as catalysts. Not more than 30 % water is added, the obtained mass is compacted to paste state, then it is heated to 45-50 °C hydrolyzing in the presence of a catalyst. Obtained hydrolysate is dehydrated under vacuum till forming a vapor phase and a dry residue with moisture content of not more than 13 %. Vapor phase is removed on condensation and after separation of condensate the essential mustard oil is produced, and the dry residue is delivered as a feed supplement.

EFFECT: group of inventions is aimed at reducing time of hydrolysis, obtaining a high quality product and larger amount of essential oil.

6 cl, 2 dwg

Description

The invention relates to the food industry and can be used in the processing of by-products of mustard and oil production to obtain essential mustard oil and feed additives.

It is known that to obtain essential mustard oils from by-products of mustard and oil production, a unit containing a jacketed reactor, a filter, a hydrolyzer and a condenser is used (see RF patent No. 2196811, IPC СВВ 13/00, publ. 2003). The reactor is equipped with a mixer, which is mixed by-products (cake) in the process of preparing an aqueous suspension. The filter is included in the installation for washing and separating the solid phase of the suspension. The hydrolyzer, like the reactor, is equipped with a stirrer and a jacket for hydrolysis with parameters of mixing and heating to a temperature of 40-60 ° C. At the same time, the liquid phase of the suspension, selected on the filter, with the attached products of processing mustard seeds (mustard powder, crushed mustard seeds) is sent to the hydrolyzer for enzymatic hydrolysis. When direct steam is fed into the hydrolyser, isothiocyanates (essential oils) are released from the hydrolyzate, which together with the steam are sent to the condenser to complete the steam distillation.

However, this installation does not allow to ensure the quality of the finished product. When direct steam is fed into the hydrolyzer, isothiocyanates are exposed to high temperature (100 ° C), which is why isothiocyanates undergo partial decomposition and are unstable during storage (3 months without stabilizers). In addition, the disadvantage of the installation is its energy intensity, due to both the need for 30-minute heating of the reactor to maintain the temperature of the water in it within 75-90 ° C during the preparation of the suspension, and the need to bring the temperature in the hydrolyzer to 100 ° C for a start evaporation of water from the hydrolyzate. At the same time, the installation incorporates several units of additional equipment.

So in addition to a reactor equipped with a stirrer and a jacket, in which an aqueous suspension of by-products is prepared, it is equipped with a filter designed for repeated washing of the solid phase.

The closest analogue of the claimed installation is the installation, the technological scheme of which is presented in the monograph "Comprehensive processing of mustard seeds" under the general editorship of Doctor of Pedagogical Sciences. G.G. Rusakova - IPK "Niva", Volgograd, 2009, p. 149 (prototype). This installation contains a reactor with a loading hatch, a stirrer and a steam jacket, a separator-condenser with a system for removing volatile compounds of the hydrolyzate and a device for dewatering the remainder of the hydrolyzate, which is made in the form of a spray dryer. The reactor is designed to prepare a suspension, while the reactor is filled with water heated to 35-50 ° C and with the stirrer loaded, by-products of the oil production (cake) are loaded. At the end of loading, steam is supplied to the reactor jacket, bringing the temperature of the suspension to 40-55 ° C, at which hydrolysis begins. In the process of hydrolysis carried out for 30-45 minutes at the indicated temperature, stirring of the reaction mixture is continued. After the time of hydrolysis for the distillation of volatile ether compounds open the supply of sharp steam into the reactor, while the temperature in the reactor reaches 96-103 ° C. From the reactor, pairs of volatile compounds enter the condenser, which is a heat exchanger. The condensation of essential oil vapors occurs due to the supply of cooling water into the annular space of the heat exchanger. Non-condensing vapors of volatile compounds enter the adjacent condenser, also cooled by water, and then the ether vapors as a finished product enter the packaging through the separator. After distillation of the ether compounds, the remaining hydrolyzate from the reactor is transferred to an intermediate tank, and then to a spray dryer for the subsequent production of a feed additive.

The known installation for processing by-products of mustard and oil production also does not allow to ensure the quality of the finished product, since when blowing hot steam through the reactor, the isothiocyanates have a temperature effect of 100 ° C, partial decomposition of isothiocyanates occurs, as a result of which they become unstable during storage. In addition, the installation is characterized by high energy intensity, since already at the stage of preparing the suspension it is necessary to fill the reactor with water heated to 35-50 ° С and load the by-products of the oil production (cake) with the mixer working. The energy intensity of equipment increases significantly at the stages of hydrolysis and distillation of volatile compounds of oils in connection with the heating of the suspension, both through the jacket of the reactor and by blowing hot steam. High energy consumption requires dehydration on the spray dryer of the hydrolyzate residue after distillation of essential oils, which is characterized by a high water content, therefore, instead of obtaining a feed additive, it is more advisable to discharge the remainder of the liquid phase into waste.

A known method of producing essential mustard oils (isothiocyanates) from by-products of mustard and oil production described in the patent of the Russian Federation No. 2196811, IPC СВВ 13/00, publ. 2003. In the known method, first, an aqueous suspension is prepared on the basis of by-products, while in a ratio of 1: 6 water is added to the by-products for extraction, which is carried out for 30 minutes at a water temperature of 75-90 ° C. After that, phase separation is carried out. The solid phase is washed, and in the liquid phase, the enzymatic hydrolysis of thioglycosides is carried out at a temperature of 40-60 ° C. The hydrolyzate is subjected to steam treatment to recover isothiocyanates.

Among the disadvantages of the method it should be noted that the formation of the vapor phase after hydrolysis is carried out at a temperature of 100 ° C, at this temperature exposure, partial decomposition of isothiocyanates occurs, and as a result, the obtained essential mustard oil is unstable during storage (3 months without stabilizers). In addition, after the preparation of the aqueous suspension, the synigrin dissolved in water is “washed” from the solid, moreover, the washing of the solid phase is carried out at least 6 times. The complexity of this stage, the extraction carried out for 30 min with heating at a water temperature of 75-90 ° C, as well as the high energy consumption during the distillation of isothiocyanates with hot steam, reduce the efficiency of processing by-products of mustard and butter production in order to obtain essential mustard oil. Obtaining a feed additive in a known manner is impractical, since it is necessary to drain the solid phase, which is characterized by a high moisture content (about 85% water) with the indicated ratio of by-products and water 1: 6, which entails high energy costs. The removal of the solid phase into waste for disposal is also accompanied by high transportation costs due to the high moisture content.

The closest analogue in relation to the proposed method is a method of processing waste mustard and oil production described in the patent of the Russian Federation No. 2360432, IPC A23K1 / 00, publ. 07/10/2009 (prototype). The known method includes combining waste with water, mixing, heating to 45-50 ° C for at least 15 minutes, obtaining a dry product under vacuum, while the mixture heated to 50 ° C is held for 20 minutes at a pressure of 0.1 atm. After that, water vapor with mustard essential oils is removed, and the resulting residue is granulated as a feed supplement.

Despite the fact that the known method allows to obtain a feed additive, the description of the method does not say about the qualitative characteristics of the obtained product, the achievement of which is important in view of the fact that the content of sinigrin in the resulting product is above the standard value, not only reduces the quality of the feed additive, but makes unsuitable for animal feed. Among the disadvantages of this method it should be noted that the need to heat the mass obtained by mixing the by-products with water for 15 minutes, affects the duration of the whole process and indicates high energy consumption.

The objective of the group of inventions is to develop an installation and method for producing essential mustard oil and feed additives from waste mustard and oil production, which reduce energy costs and improve product quality.

EFFECT: obtaining qualitative characteristics of waste products from mustard and oil mill production (essential oil and feed supplement).

The specified technical result is achieved by the fact that the installation for processing by-products of mustard and oil production (option 1) contains a horizontally mounted reactor-hydrolyzer equipped with a jacket, mixer and a remote-controlled valve. In addition, the installation contains means for creating a vacuum in the reactor, which in this case is a dryer and a system for removing volatile compounds of the hydrolyzate with condensers and a phase separator of the condensate, and the means for creating a vacuum is placed in the system for removing volatile compounds of the hydrolyzate.

In this case, an ultrasonic generator can be installed in the hydrolyzer reactor.

Comparative analysis with the prototype shows that the inventive installation, unlike the prototype, is equipped with a means for creating a vacuum in the reactor, which is installed in a horizontal position and equipped with a remote-controlled valve.

In the particular case of the installation for processing by-products, an ultrasonic generator is installed in the hydrolysis reactor.

Equipped with a stirrer and a steam jacket, the reactor, as in the prototype, is designed for hydrolysis, but when creating a vacuum, the hydrolyzer reactor equipped with a remote valve is a vacuum dryer. In addition, the horizontal position of the reactor allows for uniform mixing of a thick viscous mass of moistened cake. It is important that the uniform mixing of such a mass contributes to the full hydrolysis. The distillation of the essential oil from the mixture of by-products with water is carried out not at 100 ° C, which takes place during steam distillation, but at a temperature of 50 ° C, at which hydrolysis is carried out, which helps prevent overheating of the reaction mixture and decomposition of its protein components, as well as get a more stable product for storage (essential oil). It is important that the reactor designed for hydrolysis, due to the means of creating a vacuum, functionally provides dehydration of the hydrolyzate. Thus, in the process of processing by-products of production by one unit of equipment instead of two used in the prototype (reactor and spray dryer), the production and quality of high-protein feed additives can be ensured, which indicates the efficiency of use of the equipment and its economy in terms of reducing energy consumption. Moreover, in addition to the feed additive, the inventive installation allows not only to obtain essential mustard oil, but also to increase its quantitative yield by ensuring uniform mixing of a thick viscous mass of moistened cake.

In the particular case of execution by means of an ultrasonic generator, finely dispersed spraying of water can be carried out to ensure uniform moistening of the cake with a small amount of water up to 30% and intensification of mixing, and when dehydrated, eliminating burning of the cake on the heated walls of the hydrolyzer to improve heat transfer, which generally contributes to the energy efficiency of the installation.

The specified technical result is achieved when implementing on the installation described above (option 1) a method for processing by-products of mustard and oil production. In this method (option 1), enzymes in the amount of 2-5% of the content of by-products are added to the mass of by-products with constant stirring as catalyst, not more than 30% water is added and hydrolysis is carried out in the presence of a catalyst, heating the resulting mass to a temperature of 45 -50 ° C, the hydrolyzate obtained in this case is dehydrated under vacuum until a vapor phase and a dry residue with a moisture content of not more than 13% are formed, the vapor phase is allowed to condense and after separation of the condensate an essential mustard oil is obtained, and with hoi residue shipped as feed supplements.

In the inventive method, in contrast to the prototype, the catalyst is first added to the by-products in the form of enzymes, and then water is added, the amount of enzymes being 2-5% of the content of by-products, and the amount of water not exceeding 30%. As in the prototype, in the claimed technical solution, hydrolysis takes place with heating with stirring. But unlike the prototype, at the stage of hydrolysis, heating of the hydrolysis mixture for 15 minutes to 45-50 ° C is excluded, since in the presence of a catalyst, hydrolysis takes place in the process of wetting by-products with water.

The presence of a catalyst in the inventive method allows not only to increase the rate of hydrolysis. The enzymes used as a catalyst allow for the complete hydrolysis reaction to take place, which is important for improving the quality of the final product, since the content of residual synigrin in the feed additive corresponds to the normative allowable value, while providing a larger amount of essential oil. In accordance with the claimed method, the amount of water can be taken no more than 30% of the content of by-products, which allows to reduce the energy consumption when stirring, heating and dehydrating the hydrolysis mass. The water content in such a quantity is optimal, since a lower value will not allow to evenly mix and distribute water in the mass of by-products and will be insufficient for hydrolysis.

The specified technical result is also achieved by the fact that the installation for processing by-products of mustard and oil production (option 2) contains a horizontally installed hydrolyzer reactor equipped with a jacket, mixer and a remote-controlled valve. In addition, the installation contains a mixer installed in front of the reactor, means for creating a vacuum in the reactor, which is also a dryer, and a system for removing volatile compounds of the hydrolyzate with condensers and a condenser phase separator. Moreover, the means for creating a vacuum is placed in the system for removing volatile compounds of the hydrolyzate, and the mixer contains a loading hatch at the inlet, a mixing device and a die plate at the outlet.

In this case, an ultrasonic generator can be installed in the hydrolyzer reactor.

Comparative analysis with the prototype shows that the inventive installation, made in the second embodiment, has the same differences from the prototype as in the first embodiment, except that it is equipped with a mixer that contains a loading hatch at the inlet, a mixing device and a die plate at the exit. The unit is equipped with a mixer in order to ensure uniform wetting of the cake with a small amount of water (30% of the amount of by-products).

Moreover, the installation for processing by-products in a particular embodiment comprises a hydrolyzer reactor in which an ultrasonic generator is installed.

In the installation according to the second embodiment, as in the first embodiment, it is essential that the horizontal position of the reactor provides uniform mixing, and the reactor itself, designed for hydrolysis, is a dryer by means of creating a vacuum. However, in the installation according to the second embodiment, it is important that with the help of a mixer equipped with a spinneret grate at the outlet, a uniform distribution of water in the mass of by-products during the preparation of the hydrolysis mass is ensured. This preparation of the reaction mixture contributes to the implementation of hydrolysis in full, due to which the normative allowable content of residual synigrin in the feed additive and the amount of essential oil obtained are ensured. It is also important that essential mustard oil and a high protein feed additive can be obtained with one piece of equipment instead of the two used in the prototype (reactor and spray dryer), which indicates the efficiency of use of the equipment and its economy in terms of reducing energy consumption.

In the particular case, when performing the installation according to the second variant, finely dispersed spraying of water can be carried out by means of an ultrasonic generator to ensure uniform moistening of the cake with a small amount of water up to 30% and intensification of mixing, and during dehydration, eliminating burning of the cake on the heated walls of the hydrolyzer to improve heat transfer, which generally contributes to the energy efficiency of the installation.

The specified technical result is achieved when the method for processing by-products of mustard and oil production is implemented on the installation described above according to option 2. This method (option 2) is carried out in the following sequence. To the mass of by-products with constant stirring, first enzymes are added as a catalyst in the amount of 2-5% of the content of by-products, then 30% water is added. Next, the mass of moistened by-products is compacted to a pasty state and subjected to hydrolysis with heating to a temperature of 45-50 ° C. The resulting hydrolyzate is dehydrated under vacuum until a vapor phase and a dry residue with a moisture content of not more than 13% are formed. Further, according to the method, the vapor phase is diverted to condensation and after separation of the condensate an essential mustard oil is obtained, and the dry residue is shipped as a feed supplement.

Comparative analysis with the prototype shows that, unlike the prototype, in the method according to the second embodiment, enzymes are first attached to the by-products when they are mixed, and then mixed with water, the amount of enzymes being 2-5%, and the amount of water no more than 30% of the content of by-products. It is important that this mass is compacted, creating pressure, and then subjected to hydrolysis with heating and stirring.

In the inventive method according to the second embodiment, as in the first embodiment, in the presence of a catalyst, the hydrolysis takes place in full, which ensures a normative permissible content of residual synigrin in the feed additive to improve the quality of the final product. In addition, to undergo hydrolysis in full, the uniform distribution of water in the mass of by-products is important. Therefore, when implementing the method according to the second embodiment, to ensure uniform distribution of water in the mass of by-products, they are first mixed with water, then, creating pressure, the mass is compacted. It is important to note that the reaction mixture thus prepared during hydrolysis in the reactor determines the production of a larger amount of essential oil. In addition, as in the first embodiment, the inventive method allows you to enter into the technological cycle water in an amount of not more than 30% of the content of by-products, which helps to reduce energy consumption for mixing, heating and dehydration of the hydrolysis mass and to increase the efficiency of processing waste mustard and oil mill production.

The invention is illustrated by drawings, which schematically shows a plant for processing by-products of mustard and oil production. The figure 1 shows the installation diagram for option 1; in FIG. 2 - the same as in option 2.

Installation for processing by-products of mustard and oil production (option 1) contains a horizontally mounted reactor 1, intended for hydrolysis of sinigrin from a mixture of by-products with water. The reactor-hydrolyzer 1, equipped with a jacket and a stirrer, is connected to the condensers 2, 3 through a forced vapor recovery system of the hydrolyzate. The forced vapor recovery system of the hydrolyzate is equipped with a means for creating a vacuum in the reactor, for example, a vacuum pump 4 and a remote-controlled valve 5. Condensers 2, 3 are made in the form of heat exchangers and connected to a phase separator 6, from which essential mustard oil is shipped. A screw conveyor 7 is installed in front of the reactor 1 for loading by-products of oil production into it. The reactor-hydrolyzer 1 through the discharge hatch by a pipe 8 is connected to the hopper 9, intended for filling the feed additive.

The plant for processing by-products of mustard and oil production according to the second embodiment contains all the same constituent elements as in the first embodiment, with the exception that it is equipped with a mixer 10. The mixer 10 has a loading hatch at the inlet, a mixing device and a die outlet grille.

To implement the invention in both cases, the well-known structural components used in the art can be used, components, components and materials, including hydraulic elements, rubber products and fasteners.

Installation for processing by-products of mustard and oil production according to the first embodiment is as follows. Preliminarily, enzymes, for example, in the form of crushed seeds of white mustard, are attached to the by-products supplied on the conveyor 7 to the reactor 1 in an amount of not more than 2-5%. Then the resulting mass is placed through the loading hatch in the reactor-hydrolyzer 1, heated through the jacket to 50 ° C. In reactor 1, the mass of by-products with enzymes with a working stirrer is moistened with water to obtain a hydrolyzate. After all the necessary volume of water is introduced into the reactor 1 in the amount of 30% of the content of by-products, the loading door is closed. Next, in the reactor 1 using a remotely controlled valve 5 through a vacuum pump 4 create a vacuum to dehydrate the hydrolyzate. Vacuum treatment produces a vapor phase containing essential mustard oil vapors. The vapor phase is transported through a forced-exhaust system using a vacuum pump 4 to a condenser 2. In this case, the condensation of essential oil vapors occurs due to the supply of cooling water to the annular space of the heat exchanger, in the form of which a condenser 2 is made. 2 non-volatile vaporized compounds in the condenser enter condenser 3, which is similar to condenser 2 is cooled by water. Essential oils are separated by decantation from water in separator 6. Essential mustard oil is dispatched from separator 6. The dry hydrolyzate residue obtained by dehydration, characterized by a moisture content of 13%, is discharged from the reactor 1 and fed through the hopper 9 through the pipe 9 to the packaging as a high-protein feed additive.

The plant for processing by-products of mustard and butter production according to the second embodiment works in the same way as in the first embodiment, except that by-products (oil cake) with attached enzymes are loaded into mixer 10 before being fed to reactor 1. In mixer 10 the by-products are mixed with water, added in an amount of 30% of the by-products content, and with the aid of a mixing device are advanced to the exit equipped with a spinneret grate. When passing through the spinneret grating, the mass is compressed to a pasty state, which is then loaded into the hydrolysis reactor 1, heated to a temperature of 50 ° C. Immediately after loading, the loading hatch of the reactor 1 is closed and a vacuum is created by means of a remote control valve 5 by means of a vacuum pump 4 to dehydrate the hydrolyzate in the reactor 1.

The claimed technical solutions are implemented in an industrial environment at the enterprise LLC “Volgograd mustard creamery“ SAREPTA ”. Essential mustard oil obtained in the processing of waste mustard and oil production is a certified product, which issued the relevant documents and certificates. Technological and quality indicators of this product, in particular, are reflected in the "Chemical Safety Data Sheet".

Claims (6)

1. Installation for processing by-products of mustard and oil production, containing a horizontal reactor-hydrolyzer equipped with a jacket, mixer and a remote-controlled valve, means for creating a vacuum in the reactor, which is then a dryer, and a system for removing volatile compounds of the hydrolyzate with capacitors and a phase separator of the condensate, while the means for creating a vacuum is placed in the removal system of volatile compounds of the hydrolyzate. 2. Installation according to claim 2, characterized in that an ultrasonic generator is installed in the hydrolyzer reactor. 3. The method of processing by-products of mustard and oil production, carried out on the apparatus according to claim 1, in which, with constant mixing of the by-products, enzymes in the amount of 2-5% of the content of by-products are added to their mass as a catalyst, and no more than 30% water, the resulting mass is heated to a temperature of 45-50 ° C, subjected to hydrolysis in the presence of a catalyst, the resulting hydrolyzate is dehydrated under vacuum to form a vapor phase and a dry residue with a moisture content of not more than 13%, steam the phase is allowed to condense and after separation of the condensate an essential mustard oil is obtained, and the dry residue is shipped as a feed supplement. 4. Installation for processing by-products of mustard and oil production, containing a horizontal hydrolyzer reactor equipped with a jacket, a stirrer and a remote-controlled valve, means for creating a vacuum in the reactor, which is a dryer, a mixer and an exhaust system installed in front of the reactor volatile compounds of the hydrolyzate with capacitors and a separator of the phases of the condensate, while the means for creating a vacuum is placed in the removal system of volatile compounds of the hydrolyzate a mesitel comprises charging port inlet, a stirring device and a die at the outlet grille. 5. Installation according to claim 5, characterized in that an ultrasonic generator is installed in the hydrolysis reactor. 6. A method for processing by-products of mustard and oil production, carried out on the apparatus according to claim 4, in which, with constant mixing of the by-products, enzymes in the amount of 2-5% of the content of by-products are added to their mass as a catalyst, and no more than 30% water, compact the resulting mass to a pasty state, and then it is heated to a temperature of 45-50 ° C, subjected to hydrolysis in the presence of a catalyst, the resulting hydrolyzate is dehydrated under vacuum until a vapor phase is formed and dry of residue with a moisture content not exceeding 13%, the vapor phase is withdrawn to the condensation and separation of condensate is obtained after the etheric oil of mustard, and the dry residue was shipped as feed supplements.

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