Method for preparing concentrated sapropel

FIELD: medicine.

SUBSTANCE: invention refers to medicine, particularly to experimental balneology, and concerns a method for preparing concentrated sapropel. A method for preparing concentrated sapropel, involving recovering and concentrating easily disaggregating water-soluble components of sapropel by placing native sapropelinto a vacuum evaporator, which is exhausted and heated; a heating procedure is combined with exposing to ultrasound with measuring an ultrasound rate continuously or intermittently and accelerating ultrasound by differentiating the ultrasound rate on time; the above measurement procedure is repeated until the ultrasound acceleration gets equal to zero; the procedure of recovering the easily disaggregating water-soluble components of sapropel and the concentration procedure is terminated, and a dry residue is solubilised in the concentrated easily disaggregating water-soluble components in certain circumstances.

EFFECT: method enables reducing the time of concentrated sapropel production and improving the product quality.

1 dwg, 1 ex

 

The method applies to balneology, more precisely to a method of obtaining concentrates of sapropel, preserving the main biologically active components.

Known methods for producing extracts from sapropel, characterized in that the extracts contain one of the biologically active components or a group of similar components. Thus, each of these extracts is deprived of a significant part of the components inherent in the whole of the sapropel.

There is a way to obtain concentrates of sapropel, which is carried out by pre-treatment of native mud alcoholic solution of alkali to pH (8,5÷9,0) and extraction of the treated raw water at the ratio of raw materials-extractant 1:(10÷12) under vigorous stirring (1500 rpm) for 15 min at 50-60°C, separating the extract from the precipitate, evaporation in vacuum [1].

However, this method is complex, requires the use of chemicals, and the obtained target product contains only legkodelimae water-soluble components of the mud in an amount equal to about half the volume of the original mud.

Also known is a method of obtaining mud centrifugate based on the use of centrifugal force for separation of the liquid phase of the mud [2].

According to this method sapropel centrifuged with acceleration 600g for 1 h, separated adosados, apolnet them three-liter bottles and rolled for transportation. The resulting product is used in local applications with paraffin in the treatment of arthritis, arthrosis, sciatica, gynecological diseases.

The disadvantage is that centrifugal contains only legkodelimae water-soluble components of the mud in an amount equal to about half the volume of the original mud.

There is a way, in addition to those. The product obtained with it, is called "Palidin". According to this method, the sapropel is poured into a porcelain capacity 5-fold volume of physiological solution, insist (3-4) days while stirring, allow the mixture to settle and merge sucks. After filtration of sludge is sterilized and poured for transportation in glass containers. The scope is the same as for mud centrifugate, from which palidin increased 5 times by volume and the fact that it contains more water-soluble components due to prolonged infusion of saline mud.

There is a way to obtain humic complex sapropel, based on the precipitation of sodium humates from alkaline extract dirt [2]. To obtain humic acids sapropel pour 10-fold volume of a 2% aqueous solution of sodium hydroxide, heated (4-6) hours at the boiling point, cooled and diluted with water 2 times, defend 24 h, siphoninus and filtered, the filtrate add 20% sulfuric acid to pH 1,0, defend until complete precipitation, adosados discarded, and the precipitate washed with water and dried at 60°C. the resulting product is a complex of humic acid - used for medicinal purposes, including for conditions that are treated by centrifugation dirt and plaidinum.

The disadvantage of this method is that the target product contains only one useful component of whole sapropel - humic acid.

There is a way to obtain a product containing lipid complex from whole sapropel [2].

To obtain drug dirt fill in an organic solvent or mixture of solvents, maintained at a constant stirring 6-12 h, decanted solvent, filtered, the filtrate is evaporated to small volume and transferred to the oil solution, removing traces of solvent.

The product contains high-molecular fatty acids, phytosterols, chlorophyll, carotene and oxidized carotenoids. The downside of it is the complete absence of water-soluble components and humic acids present in the whole sapropel.

A known method of obtaining a concentrate of the sapropel, including removing lipid complex organic solvents. In this advance of sapropel consistently remove water-soluble matter and humic acids. Then ex is ract, containing water-soluble substances, concentrated by evaporation in 25 to 30 times, and in the resulting concentrate solubilizing pre-selected complexes of humic acids and lipids [3].

The sequence of operations in the above-mentioned method is as follows:

from a single product sapropel extracted water-soluble compounds by infusing it with a 5-fold volume of water and separation of the extract;

the rest of the sapropel, obtained after extraction of water-soluble components, is used for separation of complex humic acids, which get in the form of dry individual product;

the rest of the sapropel after removing from it the water-soluble compounds and humic complex, is used for extraction of the lipid complex is obtained in the form of a dry product.

This sequence of operations instead of three volumes of sapropel, which are necessary to obtain a water-soluble component, humic and lipid complexes according to known methods, to use only one volume, i.e., provides for the preparation of biologically active components of sapropel to use 3 times less than the target sapropel;

simultaneously with the extraction of humic and lipid complexes extract containing water-soluble concentrates you what Arianism, to reduce its original volume in 25-30 times;

in a concentrated extract solubilizer obtained earlier complex of humic acids, and then the obtained lipid complex.

The result of these actions is to obtain the target product, which contains the main biologically active components of whole sapropel (water-soluble compounds, humic acids and complex lipids) in volume, less than 25-30 times than in the method-analogue.

All actions in the sequence provides the 3-fold decrease in the original sapropel while maintaining the composition of the target product main component of whole sapropel, as well as reducing the amount of the target product in 25-30 times, which makes it easy to transport.

However, this method is complex, as it consists of many stages, energy-consuming, requires the use of additional organic solvents, and extraction with water, and in the process of getting concentrate loose some nutrients available in native sapropel. Obtained in this way sapropel has a low biological activity.

Disadvantages ways equivalents:

using the first and second way of analog receive the aqueous phase of the sapropel, containing only the easily soluble compounds, the volume of the target is on the product 2 times less than the volume of the original sapropel;

using the third method is similar to getting a product containing water-soluble components of sapropel more fully, however, the amount of the target product increases against the amount of the original sapropel 3-4 times, in addition, as in the first case, the target product does not contain such biologically important components such as humic and lipid complexes;

using the fourth method is similar to get the target product that does not contain water-soluble compounds and lipid complex, which is the most important biologically active component of sapropel;

using the fifth method-analogue receive a product containing only lipid complex and does not contain water-soluble components and humic acids;

with all the way of analog part of the sapropel, preserving the uncovered components, is lost, as each method provides for obtaining the target product using the original sapropel;

the sixth way is similar complex since it consists of many stages, energy-consuming, requires the use of additional organic solvents and extraction with water, and in the process of getting concentrate loose some nutrients available in native sapropel, and obtain in this way the sapropel has a low biological activity.

Nai is more close to the claimed method is a method of obtaining a concentrate of sapropel[4].

Prototype method involves dividing a native of sapropel on the dry residue and the liquid fraction, concentrated liquid fraction, and solubilization in the resulting concentrate the solids and native sapropel divided into the dry residue and the liquid fraction by placing it in a vacuum evaporation apparatus, within which generate a vacuum of 50-60 Torr, heated native sapropel up to 30-40°C, concentrated legkodelimae water-soluble components of the sapropel, then after separation and preconcentration lightdesign water-soluble components from sapropel make final drying and grinding of solids, for which the dry residue is placed in a vacuum drying drum, inside which again generate a vacuum of 50-60 Torr, and heated dry residue sapropel up to 30-40°C, and ground to particle size of 20-40 microns, followed by the solubilization of the obtained dry residue in concentrate lightdesign water-soluble components.

However, in the method prototype there is no control of the separation process native sapropel on dry and liquid fraction. The absence of such control is not possible to accurately determine the time of completion of the process of separation of the liquid fraction, which leads either to unnecessary prolongation of the process of separation native sapropel the dry and the liquid fraction, or to premature interruption of this process that has a negative impact on the quality of the product. In addition, the process of separating native sapropel on the dry and the liquid fraction is insufficient and increases the duration of the process and leads to unnecessary expenditure of energy.

The technical problem of the invention is to develop a control process of separating native sapropel into fractions that can accurately determine the time of completion of the process of separation of the liquid fraction, creating the possibility of reducing the time of the above process and improve the quality of the product, as well as to increase the intensity of the separation process native sapropel into fractions and reduce energy consumption.

The problem is solved in that in the method of obtaining a concentrate of the sapropel, including the extraction and preconcentration lightdesign water-soluble components of sapropel by placing native sapropel in the vacuum evaporation apparatus, in which creates a vacuum of 50-60 Torr and heating sapropel up to 30-40°C, subsequent solubilization in the resulting concentrate the solids in the heating process of sapropel he is under the influence of ultrasound, the frequency of which is higher than the frequency of the cavitation threshold in the low frequency range from 20 kHz to 100 is Hz, and the intensity of the above-mentioned ultrasound lies in the area of stable cavitation from 1.5 W/cm2up to 2.5 W/cm2while continuously or periodically measure the speed of ultrasound and its acceleration by differentiation of the velocity of ultrasound in time, and this procedure is repeated as long as the acceleration of the ultrasound will be equal to zero, then the process branches lightdesign water-soluble components from sapropel and their concentration, stop, and perform the solubilization of solids in the resulting concentrate lightdesign water-soluble components.

In Fig. 1 shows graphs of the dependence of ultrasonic velocity on the time separation of native sapropel liquid and dry fractions.

The invention consists in the following. Native sapropel is placed in a vacuum evaporation apparatus, and create it in a vacuum of 50-60 Torr. Creating a vacuum inside the vacuum evaporation apparatus is necessary in order to implement effective vaporization mode of boiling water, to ensure allocation, concentrated and save in a concentrated form lightdesign water-soluble components of the sapropel. The range of dilution in 50-60 Torr in the vacuum evaporation apparatus due to the following reasons. It is known that the lower the value of the bit is the or the lower the temperature of boiling water. For example, when the pressure of 10 Torr water boils at 18°C. However, for low temperatures, boiling water is required to tighten the requirements to tightness of the vacuum evaporation apparatus to the booster pump, which complicates the application of the method in practice and leads to increased cost of manufacture of the vacuum apparatus. When the pressure of 50 Torr, the water begins to boil at a relatively low temperature is 30°C. Obtaining dilution in 50 Torr simply is relatively cheap booster pumps and can be obtained without particularly strict requirements to ensure the integrity of the vacuum evaporation apparatus. Relatively low boiling temperature of water at a pressure of 50 Torr, the possibility of obtaining the specified dilution cheaper booster pumps and exceptions excessive demands for tightness of the vacuum evaporation apparatus indicate the inappropriateness by evaporation and the concentration of applying a lower vacuum than 50 Torr. When the negative pressure 60 Torr water boils at a temperature of 40°C. Therefore, when creating rarefaction more than 60 Torr will be required to provide boiling water to raise the temperature of the heating native sapropel, which results in obtaining a concentrate of sapropel to increase e ergetically costs and to the destruction of biologically active substances. The choice of a similar range of exhaustion and temperature of heating of the sapropel in the vacuum drum dryer caused by the same reasons, the selection of these modes in the vacuum evaporation unit. The premise of dry residue after extraction and concentration lightdesign water-soluble components from native sapropel in the vacuum drum drier carry out in order to produce the final drying and grinding of dry residue. Grinding the dry residue is carried out in order to increase the active surface interaction of the particles of the dry residue of the sapropel, which leads to an increase in its chemical and biological activity.

It is known that many processes " when exposed to the process object by the ultrasound.

In the present method by ultrasound significantly increases the intensity of the process of separation of native sapropel on dry and liquid fractions.

By their physical nature ultrasound is an elastic wave, and in this he is no different from the sound.

It is considered that the ultrasonic range includes frequencies in the range from 20 kHz to 1 GHz. Frequency in the range from 16 kHz to 20 kHz, refer to audible sound.

Frequencies below 16 kHz are infrasound and frequency, lojasiewicz 1 GHz are called supersonic.

The frequency range of the ultrasound can be divided into three sub-regions:

- ultrasound low frequency (2×104-105Hz) - ULF;

- ultrasound medium frequency (105-107Hz) - USC;

- ultrasound-high frequency (107-109Hz) - USVC.

In liquid medium under the action of ultrasound occurs and proceeds specific physical process of ultrasonic cavitation, providing maximum energy influence on the particles of the sapropel.

In an ultrasonic wave during the half-periods of depression occur cavitation bubbles, which abruptly shut after moving to an area of high pressure, giving rise to strong hydrodynamic disturbances in the sapropel, which significantly increases the amount of excretion of water-soluble substances and water from sapropel.

Cavitation is produced by the alternating waves of high and low pressure created by high-frequency sound (ultrasound).

Ultrasonic cavitation is the main initiator of physico-chemical processes occurring in the liquid under the action of ultrasound and, in particular, separation of sapropel on dry and liquid fractions.

Cavitation phenomena in a particular environment occur only when exceeding the ultrasound cavitation threshold.

The cavitation threshold is called the intensity of the ultrasound, the nether is not observed cavitation. The cavitation threshold depends on the parameters characterizing both the ultrasound and the liquid.

For water and aqueous solutions cavitation thresholds increase with increasing frequency ultrasound and reducing the time of exposure.

At frequencies above 20 kHz the threshold unstable cavitation is in the range from 0.3 W/cm2up to 1 W/cm2.

Further increase in intensity of 1.5 W/cm2leads to the violation of the linearity of the oscillations of the walls of the bubbles. Stable cavitation stage begins. The range of intensities of stable cavitation lies in the area of 1.5 W/cm2up to 2.5 W/cm2. The bubble itself becomes a source of ultrasonic vibrations. On its surface waves occur, microcurrents, electrical discharges.

The increased intensity ultrasound for the value of 2.5 W/cm2leads again to the stage of unstable cavitation.

The most intense division of sapropel on dry and liquid fractions occurs in the range of stable cavitation occurring at low frequencies. Therefore dividing the sapropel liquid and dry faction of the best ultrasound low frequency. The choice of this frequency range due to the following factors.

First, the frequency of 20 kHz is taken as the lower boundary of occurrence of ultrasonic vibrations. At frequencies below 20 kHz is the area heard the Vuka and the process of cavitation in this region are not observed.

Secondly, in the low frequency range lying between 20 kHz to 100 kHz, the range of intensities of ultrasound, in which there is a stable cavitation, as it was mentioned above, lies in the field of 1.5 W/cm to 2.5 W/see

The frequency range above 100 kHz relates to the field of mid-frequency ultrasound. To ensure stable cavitation in the middle frequencies require more powerful irradiator than to create a named region in the low frequency range. This is due to the fact that the cavitation threshold increases with the frequency of the ultrasound. The necessity of a more powerful emitters in the midrange compared to the power of the emitters in the region of low frequencies, results in a complicated and expensive device for the separation of native sapropel on dry and liquid phase.

In the present method the most efficient use of the range of intensities of stable cavitation, which lies in the region from 1.5 W/cm to 2.5 W/see

The speed of ultrasound in different environments depends on their density. When the division of sapropel on liquid and dry fractions, removing from native sapropel water and water-soluble substances, the speed of ultrasound is continuously increasing (see Fig.1). The acceleration of ultrasound is also continuously changed. This change of acceleration ultrasound about what goes until while from sapropel will not stand out all the liquid phase. After evaporation of all liquid phase from sapropel speed of ultrasound in the remaining solid residue sapropel (meal) is stabilized and acceleration ultrasound ceases to change and becomes equal to zero. At this point in time, the process residue native sapropel stop. The selected liquid fraction from native sapropel concentrated by further evaporation and the resulting concentrate solubilizer obtained dry residue.

A specific example. Concentrated two parties sapropel mined at lake Karasev, located in kolachevska district Tomboy area. One batch of sapropel was concentrated in the prototype method, and the other by the present method. For the implementation of the prototype method used vacuum evaporation apparatus BBA-100 [3], with the evaporation capacity of 100 l/h Inside BBA-100 created a vacuum of 50 Torr. Native sapropel warmed to a temperature of 30°C, at which the water was boiling. After 12 hours the process of selection and concentration lightdesign water-soluble components of the sapropel was completed, and the dry residue of the sapropel was overloaded in a vacuum drum dryer of the type-25, with a capacity of 20 kg/hour for the evaporated moisture. In the vacuum drum dryer created once egenie 50 Torr and heated dry residue to a temperature of 30°C. The dryer drum is rotated at a speed of 2 rpm C. In the drying drum dryer balls dry residue was ground into a powder to the grain size of the powder 20-40 microns. Grind the dry residue to sizes less than 20 microns dryer drum does not allow. When the grain size of the powder is more than 40 μm falls chemical and biological activity of the powder. The process of drying and grinding was continued for 10 hours. Upon completion of the final drying and grinding the dry residue was solubilizers in the resulting concentrate lightdesign water-soluble components. Grinding the dry residue of sapropel increases its reactivity, which leads to a more intensive process of solubilization of solids in the resulting concentrate lightdesign water-soluble components and to increase the biological activity of the target product.

The concentration of the claimed method was carried out similarly as in the method prototype. The difference was only that in the process of evaporation native sapropel at him continuously affected by the ultrasound frequency was 20 kHz, and the intensity of the above-mentioned ultrasound lay in the field of stable cavitation and was equal to 2 W/cm2. While continuously measured speed (Fig.1) and the acceleration of ultrasound. In accordance with the inventive method is m for intensification of the process of separation of sapropel on dry and liquid fraction was applied industrial sound processor "Hielscher Ultrasound Technology UP" brand UIP 1000 hd [5], which was used as the cavitation activator. Sound velocities were determined by ultrasonic concentration meter substances I:PIOX® S [6].

As follows from Fig.1, the speed of ultrasound in the vaporizing native sapropel continuously changed within 7 hours. After 7 hours the sound speed is stabilized, and its acceleration becomes zero. At the moment of equality of acceleration ultrasound zero separation process native sapropel on the dry and the liquid fraction was stopped. The liquid component of the sapropel was concentrated and solubilizers it dry the rest of the sapropel (meal).

Thus, the inventive method has the following advantages over the method of the prototype:

in the claimed method was developed process control division native sapropel into fractions that can accurately determine the time of completion of the process of separation of the liquid fraction, which enables to reduce the time of the above process and to improve the quality of the product;

in the present method due to the impact on the sapropel ultrasound process of separation of sapropel on the dry and liquid components is reduced in comparison with the prototype by 30% from 10 o'clock in the prototype up to 7 hours in the claimed method.

Sources

1. RF patent №1793578. The way to obtain substances with protiva sporitelny action. // Burkova C. N., Saratikov A. S., Pisarev, S. I., N. Yudina.In., Mathis E. J., Kurkalova E. A., Sibileva L. A., B. N. Moskvin, S. Banevich M/ Publ. 27.09.1996.

2. htt://www.ntpo.com/patents_medicine/ medicine_6/medicine-69/shtml.

3. RF patent №2005478. A method of obtaining a concentrate of the sapropel. // Byszewski A. W., A. Potapov P., Gembarzhevskii S. B., Chryatiev E. A. // Publ. 1994.01.15.

4. RF patent№2477140. A method of obtaining a concentrate of the sapropel. // Smirnov, C., Smirnov, D., Detenido A. N., Palason Y. R. // date of publication of application: 10.09.2012 bull.№25. Posted: 10.03.2013 - Bul. No. 7-(Prototype).

5. Inquiry from http://www.hielscher.com.

6.1:many cases it serves® S - ultrasonic concentration meter.mht.

A method of obtaining a concentrate of the sapropel, including the extraction and preconcentration lightdesign water-soluble components of sapropel by placing native sapropel in the vacuum evaporation apparatus, in which creates a vacuum of 50-60 Torr and heating sapropel up to 30-40°C and subsequent solubilization in the resulting concentrate of solids, characterized in that in the heating process of sapropel he is under the influence of ultrasound, the frequency of which is higher than the frequency of the cavitation threshold in the low frequency range from 20 kHz to 100 kHz, and the intensity of the above-mentioned ultrasound lies in the area of stable cavitation from 1.5 W/cm2up to 2.5 W/cm2while continuously or periodically measure the velocity ul is rasluka and its acceleration by differentiation of the velocity of ultrasound in time when the specified measurement procedure is repeated as long as the acceleration of the ultrasound will be equal to zero, then the process branches lightdesign water-soluble components from sapropel and their concentration stop and perform the solubilization of solids in the resulting concentrate lightdesign water-soluble components.



 

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7 cl, 1 tbl, 3 ex

FIELD: medicine, veterinary science.

SUBSTANCE: the present innovation refers to medicinal preparations obtained out of natural humificated materials, such as peat. One should carry out alkaline extraction of sodium humates with aqueous solution of caustic soda due to infusing at temperature up to 90°C in a closed reservoir at weight ratio of peat/water being 1:20...1:25, moreover, sieved peat and caustic soda should be separately packed into filtration parcels made out of air-tight material. Infusion should be continued during 6..12 h at the concentration of aqueous solution of caustic soda being 0.10...0.18 weight%. For storage and delivery to the distant place for extraction one should hermetically pack filtration parcels with peat and caustic soda into preventive membrane out of water- and air-tight material with the help of vacuum packaging equipment. The veterinary preparation suggested contains stock solution of sodium humates prepared due to the above-described technique, it has hydrogen value of pH 7...8 and the concentration of sodium humates being 2...5 weight%. It additionally contains in therapeutic dosages, at least, one macro- and/or micro-elements in water-soluble and/or easily hydrolyzed form chosen out of the following group: iron, iodine, calcium, cobalt, magnesium, manganese, copper, selenium, phosphorus and their combinations. As a result, macro- and micro-elements could be observed in the following total quantities, mg/l: iron 42.6...65.4; iodine 0.29...0.36; calcium 590...730; cobalt 0.24...0.30; copper 6.52...7.98; magnesium 15.1...18.5; manganese 13.2...16.2; selenium 0.10...0.13; total phosphorus 244...296. The innovation enables to obtain the product of increased content of macro- and micro-elements.

EFFECT: higher efficiency.

8 cl, 1 tbl

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