Method of controlling processes of obtaining and drying enzyme preparations

FIELD: chemistry.

SUBSTANCE: enzyme preparations are obtained using a fermenter with a heating jacket for submerged culturing of microorganisms of the enzyme preparations with continuous aeration with compressed air and mechanical agitation at culturing temperature of 30…32°C on the entire volume of the fermenter; the culture liquid obtained in the fermenter is cultured to remove the residue and the filtrate of the culture liquid with moisture content of 92…95% is fed into a vacuum-sublimation drier, in which the desublimator used is a two-section evaporator of a vapour compression refrigerating machine, the working and spare section of which alternately operate in condensation and regeneration modes, respectively; wherein "hot" water is obtained by heating thereof in the condenser of the refrigeration machine using condensation heat of the coolant to temperature of 68…73°C, one part of which is fed into the heating jacket of the fermenter and the other is first fed for thawing the evaporator section operating in regeneration mode, and then the water cooled to temperature of 5…7°C is then removed from the evaporator section into a storage tank together with the liquid formed from the ice cover thawed on the surface of the cooling element in an amount of moisture evaporated from the enzyme preparation, and further, in closed cycle mode, fed in two streams, one of which is mixed with waste water after the fermenter before the condenser, and the second with "hot" water before the fermenter, wherein excess water from the recirculation loop is removed through the storage tank, followed by measurement of the culturing temperature in the fermenter, the flow rate and temperature of the water at the inlet of the heating jacket of the fermenter, the flow rate and moisture content of the filtrate of the culture liquid, residual pressure in the working volume of the vacuum-sublimation drier, the moisture content of the dried enzyme preparation, the flow rate and temperature of water vapour removed from the vacuum-sublimation drier into the working section of the evaporator, the boiling point of the coolant in the working section of the evaporator, the temperature of uncondensed vapour at the outlet of the working section of the evaporator and the level of water in the storage container; mass and heat flow of the mixture of cooled and "hot" water into the heating jacket of the fermenter is established by changing the ratio of flow rates thereof with adjustment of the culturing temperature in the fermenter; the measured values of moisture content and flow rate of the filtrate of the culture liquid are used to determine the power of the drive of the compressor of the refrigeration machine and the required residual pressure in the working volume of the sublimation drier by action on the power of the controlled drive of the vacuum pump with adjustment of the residual pressure on the final moisture content of the enzyme preparation; the flow rate and temperature of water vapour removed from the vacuum-sublimation drier into the working section of the evaporator, the temperature of uncondensed vapour at the outlet of the working section of the evaporator and the boiling point of the coolant in the working section of the evaporator are used to determine the current value of the coefficient of heat transfer from the water vapour to the coolant on the cooled surface of the working section of the evaporator, and upon achieving minimum permissible value of the coefficient of heat transfer, power of the drive of the compressor of the refrigeration machine is increased first, and the working section of the evaporator is then switched from condensation mode to regeneration mode while simultaneously switching to condensation mode the section operating in regeneration mode.

EFFECT: improved quality of enzyme preparations by increasing accuracy and reliability of controlling the process parameters, high energy efficiency and environmental safety of production processes and vacuum-sublimation drying.

1 dwg

 

The invention relates to automation of technological processes and can be used for automation of processes of production and vacuum freeze-drying of enzyme preparation in microbiological, medical, pharmaceutical and food industries.

The known method for automatic process control vacuum freeze-drying on the principle of heat pump [U.S. Pat. RF 2255279, F26B 25/22, 2005], which use the hot refrigerant as a heat source for the direct process vacuum freeze-drying products. When the condenser of the heat pump in the form of a coil is placed in a layer of frozen particles (granules) of the product, and the heat of condensation of the refrigerant through the tubes of the coil transfer of frozen particles (granules) of the product and is heated at least to a temperature of 70-80°C.

The disadvantage of this method is that it is not applicable to the drying of enzyme preparations. When the heating temperature of the overwhelming number of enzyme preparations above 32...40°C, as a rule, is inevitable inactivation of biologically valuable substances, loss of heat stability to the complete destruction of enzymes. In addition, the coil layer of the frozen particles of the product will prevent movement of the product in the internal volume of the freeze chamber and reduce the efficiency of the destruction layer, and consequently the nutrient, and the performance gain powder enzyme preparation.

The closest in technical essence and the achieved effect to the present invention is a method of automatic control of the drying process of the product in the freeze-dryer chamber connected with sectional desublimation and vacuum pump [U.S. Pat. RF 2108523, CL F26B 5/06, 1998], providing for the stabilization of the residual pressure in the freeze-drying chamber effect on the flow released from the freeze chamber water vapor correction on the final moisture content of the enzyme preparation, and regulation costs released from the freeze chamber water vapor and refrigerant in desublimator on the current value of the heat flow is diverted from the surface of the cooling element desublimator, disable regeneration of the previous section and connecting the following when reaching the current value of the heat flow very minimum value.

The disadvantages of the method:

- does not take into account the mechanism of heat transfer between the refrigerant and water vapor through the separating wall desublimator in terms of the increasing time the thickness of the ice crust on its surface, which can lead to lower quality enzyme preparation due to the variation in moisture from the set value;

- not provided used the e heat of condensation of the refrigerant in the condenser of the refrigeration machine to stabilize the temperature regime of the fermentation process for submerged cultivation of microorganisms enzyme preparation, that are not conducive to conserve heat and energy costs and does not give rise to fully consider the technology of production and drying of enzyme preparations of energy-saving;

- lack of training system hot water in closed circuit to defrost sectional desublimator does not allow to consider this method as energy efficient and environmentally friendly, and a lack of operational management of material and energy flows does not create conditions for increasing the accuracy and reliability of control of technological parameters at all stages of the process of obtaining high-quality enzyme products.

An object of the invention is to improve the quality of enzyme preparations by improving the accuracy and reliability of control of technological parameters, as well as energy efficiency and environmental safety processes of their production and vacuum freeze drying.

To solve the technical problem of the invention, a method for managing the processes of obtaining and drying of enzyme preparations, characterized in that to obtain the enzyme preparations used fermenter with a heating jacket for submerged cultivation of microorganisms enzyme preparations with continuous aeration of sterile the air and mechanical agitation at a temperature of cultivation 30...32°C throughout the volume of the fermenter; obtained in the fermenter culture liquid was filtered to remove the precipitate and the filtrate of the culture fluid with a humidity of 92...95% served in a vacuum freeze-dryer, which as desublimator use two-evaporator vapor compression refrigerating machine, the working and backup sections which alternately operate respectively in the modes of condensation and regeneration; thus receive hot water by means of its heat in the condenser of the refrigeration machine due to the heat of condensation of the refrigerant to a temperature of 68...73°C, one part of which is directed in the heating jacket of the fermenter, and the other first guide for defrosting the evaporator sector, working in the regeneration mode, and then cooled to a temperature of 5...7°C water away from the evaporator section in a cumulative collection together with the liquid formed from thawed on the surface of a cooling element of ice crust in the amount evaporated from the enzyme preparation of the moisture, and then in closed loop mode serves two streams, one of which is mixed with the waste water after the fermenter before the capacitor, and the second hot water before fermenter, while the excess water from the recirculation circuit is brought out through the cumulative collection, measures the temperature of the cultivation of the enzyme is ora, the flow rate and inlet water temperature in the heating jacket of the tank, flow rate and humidity of the culture filtrate of the liquid, the residual pressure in the working volume of the vacuum freeze-drying, humidity-dried enzyme preparation, consumption, and the temperature of the water vapor discharged from the vacuum-freeze dryer in the working section of the evaporator, the boiling temperature of the refrigerant in the working section of the evaporator, the temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator, the water level in the cumulative collection; set of mass and heat flow of the mixture chilled and hot water in the heating jacket of the tank by varying the ratio of their expenditures with correction for temperature cultivation in the fermenter; on the measured values of moisture content and flow rate of the filtrate of the culture fluid set the drive power of the compressor of the refrigeration machine and the required residual pressure in the working volume of freeze drying effect on power adjustable drive vacuum pump with correction of residual pressure on the final moisture content of the enzyme preparation; flow rate and the temperature of the water vapor discharged from the vacuum-freeze dryer in the working section of the evaporator, the temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator and the fact is the boiling temperature value of the refrigerant in the working section of the evaporator determine the current value of the transfer coefficient of water vapor to the refrigerant for cooling the surface of the working section of the evaporator and the highest the minimum value of heat transfer coefficient first increases the drive power of the compressor of the refrigerating machine, and then switch the working section of the evaporator with the mode of condensation on the regeneration mode with simultaneous inclusion on the mode of condensation section, who worked in the regeneration mode.

The technical result of the invention is to improve the quality of enzyme preparations by improving the accuracy and reliability of control of technological parameters, as well as in energy efficiency and environmental safety of fermentation processes and vacuum freeze drying.

In Fig. the circuit that implements the proposed method of control the processes of production and drying of enzyme preparations.

The schema contains the fermenters 1 with a heating jacket 2; filter 3; freeze dryer with 4 feeder-granulator 5, vacuum stopper 6 and the heater 7; compressor refrigeration machine 8; capacitor 9; working 10 and back 11 sections of the evaporator; an expansion valve 12; a vacuum pump 13; water collection 14; mixers 15, 16; distributors threads 17, 18, 19; pumps 20, 21; microprocessor 22; sensors: FE - flow, THE temperature, ME is the humidity, RE - pressure, LE - level; And enforcement mechanisms; line material flow: 1.0 - chilled water; 1.1 - hot the odes; 1.2 - a mixture of hot and chilled water; 1.3 - waste water; 2.0 - steams; 2.1 - main washing nscontainerbox vapor; 2.2 - sterile air; 3.0 - nutrient medium; 3.1 - inoculum; 3.2 - culture liquid; 3.3 / o sediment; 3.4 - cultural filtrate liquid; 3.5 - dried enzyme preparation; 4.0 - recycling refrigerant.

The method is as follows.

In fermenters 1 with a heating face 2 by the method of deep fermentation aerobic exercise training culture liquid at a temperature of 30...32°C during the creation of optimum conditions for cultivation due to intensive mass and energy exchange between the cells of the microorganism culture medium and inoculum (inoculum)is supplied through lines 3.0 and 3.1. When this exercise aeration of the nutrient medium flow of sterile air supplied to the fermenter along the line 2.2, and its continuous mechanical stirring throughout the volume of the fermenter.

Using multiple fermenters will ensure the continuity of the vacuum freeze-drying, as the time of cultivation is significantly greater than the drying time.

Obtained in the fermenter culture fluid fed into the filter 3 for separating the solid phase, which is output on line 3.3, and the filtrate of the culture fluid with humidity 93 which is 95% through the vacuum gate 5 via line 3.4 served in a vacuum freeze-dryer 4, where as desublimator use two-evaporator vapor compression refrigerating machine, working 10 and back sections 11 which alternately operate respectively in the modes of condensation and regeneration.

The vapor compression refrigerating machine comprising a working 10 and back 11 sections of the evaporator, the compressor 8, a condenser 9, thermostatic expansion valve 12, works in heat pump mode at the following thermodynamic cycle.

The refrigerant sucked by the compressor 8, is compressed to a pressure of condensation and closed-loop 4.0 is supplied to the condenser 9. Then, the refrigerant is sent to thermostatic expansion valve 12, where the coolant is expanded to a predetermined pressure corresponding to the boiling point of the refrigerant. With this pressure, the refrigerant enters the working section 10 of the evaporator and evaporates emitting cold. A pair of refrigerant along the contour 4.0 going into the compressor 8, is compressed until the condensing pressure, and thermodynamic cycle repeats.

In the condenser 9 of the refrigeration machine due to the heat of condensation of the refrigerant receive hot water with a temperature of 68...73°C available on line 1.1 and using the flow distributor 18 is divided into two streams. One stream of hot water mixed with cold water in the mixer 15 and the resulting mixture is hot and chilled water is with a temperature of 55...65°C is sent to a heating jacket 2 of the tank 1 through line 7.2, and another thread "hot water" is first sent to defrost the evaporator section 11 operating in the regeneration mode, and then cooled to a temperature of 5...7°C water away on lines 1.0 from sections of the evaporator 11 in cumulative collection of 14 together with the liquid formed from thawed on the surface of a cooling element of ice crust in the amount evaporated from the enzyme preparation of the moisture, and then in closed loop mode using the pump 20 serves two streams 1.0 mixers 15 and 16; the excess water from the recirculation circuit is brought out through the cumulative collection 14.

Information about the temperature of culturing in the fermenter 1; the flow rate and the temperature of the mixture of hot and chilled water in line 1.2 input in the heating jacket 2 of the tank 1; the flow rate and humidity of the filtrate of the culture fluid in the line 3.4; residual pressure in the working volume of the vacuum-freeze dryer 4; humidity dried enzyme preparation in line 3.5; the boiling temperature of the refrigerant in the working section of the evaporator 10, flow rate and temperature of water vapor supplied from the vacuum-freeze dryer in the working section of the evaporator through line 2,0; temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator in the line of evacuation down 2.1; the water level in a cumulative collection of 14 using sensors transmission is carried out in the microprocessor 22, which embedded programmable logic algorithm provides operational control of technological parameters, taking into account overlayed limitations as the finished product of high quality, and economic viability.

The microprocessor sets the mass and heat flow of the mixture chilled and hot water with a temperature of 55...65°C in a heating jacket 2 of the tank 1 through the mixer 15 in line 1.2 impact on the cost of chilled and hot water through distributors threads 17 and 18 by changing the power frequency drives of the pumps 20 and 21 with the correction of this ratio on the temperature of culturing in the fermenter 1. This provides stabilization of the fermentation temperature 30...32°C and the rational use of the heat of condensation of the refrigerant in the condenser of the refrigerating machine when you receive the "hot water" with a temperature of 68...73°C.

For measured values of moisture content and flow of cultural filtrate of the fluid supplied in a vacuum-freeze dryer line 3.4, microprocessor 22 sets the drive power of the compressor 8 of the refrigerating machine and the required residual pressure in the working volume of the freeze dryer 4 impact on power adjustable drive the vacuum pump 13. When you reject the scientific research Institute final moisture content of the dried enzyme preparation in line 3.5 from the setpoint, the microprocessor adjusts the residual pressure in the working volume of the vacuum-sublimation drying by changing the power adjustable drive the vacuum pump 13.

The temperature and flow rate of water vapor removed from the freeze dryer line 2.0 in the working section of the evaporator 10, the temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator in line 2.1, the boiling temperature of the refrigerant in the working section of the evaporator 10, the microprocessor continuously calculates the current value of the transfer coefficient on the cooling surface of the evaporator section.

The heat transfer coefficient determines the amount of heat that is transferred from one fluid to another (from water vapor to the refrigerant or refrigerant water vapor) through a unit area between them a cooling surface of the working section of the evaporator per unit of time when the temperature difference between fluids 1 grad:

,

where Q=Vcρ(t1-t2- the quantity of heat from the water vapor coming from the vacuum-freeze dryer in the working section of the evaporator vapor compression refrigerating machine, refrigerant, kJ/h; c, ρ - average values of heat capacity, kJ/(kg·K), and density, kg/m3, water vapor; V - volume flow of water vapor, m3/h; F is the surface area of the cooling element of the evaporator, m2; ∆ Tcf=(t1-t2)/ln[(t1-t3)/(t2-t3)] - the average is temperatury head, °C; t1- temperature water vapor supplied from the vacuum-freeze dryer in the working section of the evaporator °C, t2- temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator, °C, t3- boiling point refrigerant in the evaporator, °C.

The microprocessor continuously produces a signal deviation of the current value of the transfer coefficient from the reference value, which affects the ratio of costs "water vapor refrigerant" by changing the refrigerant flow in the recirculation line 4.0 impact on the drive power of the compressor 8. When the deviation of the current value of the transfer coefficient from the set downward, the microprocessor increases the cooling capacity of the refrigeration machine.

If the increase in the cooling capacity (flow rate of the refrigerant in line 4.0) does not allow to display the current value of the coefficient of heat transfer to the preset value, the microprocessor disables the working section of the evaporator 10 of the recirculation line of the refrigerant 4.0 refrigerating machine and connects the back section 11 by means of synchronous operation of the Executive mechanisms.

Simultaneously, the microprocessor 22 carries out switching of a direction of movement of hot water through the dispenser flow 19 in the working section of the evaporator of the refrigeration machine is 10, which mode of condensation of water vapor on its cooling surface is switched to the regeneration mode, i.e. the mode defrost icy crust.

Chilled in the defrost water to a temperature of 5...7°C with liquid formed from thawed on the surface of a cooling element of the evaporator of the ice cover, is directed to a cumulative collection of 14 from which they excrete excess water from the recirculation circuit upon reaching its upper limit.

The microprocessor tracks the amount of hot water allowed for the regeneration of the cooling surface of the evaporator on line 1.1. How much hot water will be allocated for regeneration, the same amount of cold water is added through line 1.0 through the dispenser threads 17 in the mixer 16 of cumulative collector 14 by pump 20.

Examples of implementation of the method.

The fermentation process was carried out in aerobic fermenter deep fermentation with a combined supply of energy to the gas phase for aeration with sterile air through barbaterom and to the liquid phase by mixing with a mechanical stirrer, which was dosed to the feed flow of the nutrient medium, inoculum (inoculum), sterile air, hot water in the heating jacket to ensure high intensivnostyakh and metabolism of microbial cells inoculum with a nutrient medium due to the stabilization of process parameters on the level required for optimal development of producer and education of the target product. From the fermenter took the exhaust air, waste water and the culture fluid in the form of a mixture containing cells, extracellular metabolite and biomass residual concentration of the target product.

For separation of the target product from the culture liquid was subjected to filtration to remove sediment biomass and flow of the filtrate in a vacuum freeze-dryer continuous action [Nikolaenko SV, Antipov ST, Kretov IT Freeze dryer continuous // Refrigerating equipment. - 1993. No. 6, p.2-4] with the following technical characteristics:

remote
The capacity of the dryer on the dry product, kg/h2,8-3,2
The residual pressure in the freeze-drying chamber, PA62-70
The frequency of rotation of the perforated drum, with-10,1
The heating source is a quartz lamp type KG-220-1500-5, t2
The degree of filling of the drum product0,1-0,2
The type of evaporator (desublimator)
The cooling surface of desublimator, m28
Type compressor desublimatorpiston single stage
Cooling capacity, kW20
The refrigerant (freon 22)R 22
The mass flow rate of refrigerant at the entrance to desublimator, kg/s0,35-0,58
The heat capacity of the refrigerant, kJ/(kg·°C)2,09
The condensing temperature of the refrigerant in the condenser, °C75-80

For continuous input of the filtrate in vacuum sublimation chamber used feeder-granulator [U.S. Pat. RF 2053468, F26B 17/04, 1996], providing education and samozatachivanie pellet product with their subsequent destruction and receiving powder enzyme preparation.

Example No. 1.

As the object of a vacuum-freeze drying used enzyme preparation inulinase received in-depth way using producer micromycete Aspergillus awamori 2250 [Shevtsov A.A., Tertychnyy IV, Tertychnyy so-CALLED. // State, problems and prospects of production and processing of agricultural products: Materials international. nauch.-practical use. Conf., dedicated to the 10th anniversary of the faculty of food technology, 29-30 March 2011 - Ufa, 2011. - S-357].

Inulinase enzyme gidrolizuemye inulin in the Jerusalem artichoke, topin-sunflower, dandelion and chicory to fructose. Fructose 1.73 times sweeter than sucrose, it is less karyagina, and therefore finds increasing application as sugar-containing component in the diabetic diet.

The maximum activity of the target product in the culture fluid was achieved by the following mode of fermentation:

The pressure of sterile air
when filing in the fermenter, MPa0,02-0,03
The rotational speed of the stirrer, with-13,5-3,6
the pH of the liquid phase4,2
Fermentation temperature, °C31±0,5
The humidity of the cultural filtrate liquid
to the total product weight, %93±0,5
Activity inulinase, u/cm325±3
The asset is ity β-fructofuranosidase, u/cm3100±5

When entering the vacuum-freeze dryer enzyme samosobirayutsya to a temperature of 19±0.5°C, corresponding to the level of residual pressure 66...67 PA.

In accordance with this pressure, mass flow and temperature released from the freeze chamber to the evaporator water vapour in the steady state of the energy supply from the emitters (quartz lamps) is 3.2±0,05 kg/h and 8±0.5°C and the humidity and temperature of the drug at the outlet of the dryer are respectively equal to: 1.5% and 20°C, which meets the requirements of the standard quality of the finished powder. Activity inulinase is 250...285 IU/g of the drug, the activity of β-fructofuranosidase - 1000-1032 u/g product.

Given the operational characteristics of freeze-drying and refrigerating machines operating in heat pump mode, find the rational interval of values of heat transfer coefficient of water vapor to the refrigerant through the surface of the cooling element desublimator [Danilov G.N., The filatkin NR. and other collections of problems on heat transfer processes in the food and refrigeration industry. - M.: Agropromizdat, 1986. - 288 S.].

As desublimator used horizontal shell-and-tube evaporator with in-tube boiling of R22 refrigerant cooling capacity Qo =20 kW, made of copper tubes with a diameter of 20×2 mm with aluminum insert. In the annular space move water vapor and condenses on the surface of the tubes with the formation of ice crust. The temperature of the water vapor included in the evaporator, t1=-8°C, temperature neskondensirovannyh vapor leaving the evaporator, t2=-17°C, evaporating temperature of the refrigerant t3=-20°C.

Srednetehnicheskih temperature pressure between the refrigerant and water vapor:

.

The heat transfer coefficient of the evaporator kNRas related to the overall surface of the pipes, find the equation of heat transfer from the vapor to the refrigerant:

.

Condensation of water vapor in the cooling element of the evaporator ice (frost) leads to a gradual reduction of the rate of heat transfer from the vapor to the refrigerant through the surface of the cooling pipes of the evaporator. As a result, the process of condensation of water vapor on the surface of the cooling pipes of the evaporator is slowed, reducing the consumption of water vapor in the vacuum line, increases the residual pressure in the freeze-drying chamber and, finally, decreases the rate of dehumidification.

Changing the operating conditions of the evaporator due to the formation of a layer of frost (ice) (ρin=200 kg/m3/sup> ), for example, the thickness δin=3 mm, will lead to an increase in temperature neskondensirovannyh vapor leaving the evaporator, with t2=-17°C to t2=-14°C, then

,

.

The influence of ice on the heat transfer process leads to a decrease of the heat flux of water vapor through the ice to the finned surface of the tubes of the evaporator. The mass of the drop-down frost when the formation of ice crust corresponds to the amount of moisture evaporated from the product, for example 3.2 kg/h (or 8.9×10-4kg/s). The amount of frost will be:

Formed per hour frost will have a thickness of

During the formation of a layer of frost to the maximum thickness, for example 3 mm, will be:

Therefore, in the drying process it is necessary to maintain the current value of the transfer coefficient not lower than 291,72 W/ (m2·°C).

By reducing the current value of the coefficient of heat transfer below 291,72 W/ (m2·°C), the microprocessor disables the working section of the evaporator recirculation line refrigerant and connects the backup partition.

At the same time in the condenser of the refrigeration machine get hot water with a temperature of 68...73°C is mixed with cold water and the resulting mixture is hot nd cold water with a temperature of 55±0.5°C is directed in the heating jacket of the fermenter, providing a given mode of fermentation of the drug.

Example No. 2.

The method of controlling the processes of obtaining and drying the enzyme preparation analogous to example 1.

Fermentation and subsequent vacuum freeze-drying was subjected to glucoamylase from Aspergillus awamori WUDT-2, which has been widely used as ocharovashka enzyme in alcohol and brewing industries [Yakovlev A.N., Stallions N.A., Grigorov B.C., shuvayeva G.P. Amylase thermotolerance micromycete A. amavori WUDT-2 preparative get // Biotechnology. - 1994. No. 3. - C.11-14; Yakovlev A.N., Tertychnyy T.N., Bakulin O.V. // Abstracts of international scientific-practical use. proc. "Scientific-technical progress in fermentation industries". - May 29-31, 1997 - Voronezh, 1997. - P.39].

The enzyme is sufficient to fully hydrolyze starch to glucose, necessary for the implementation of the digestion process and increase the yield of ethanol. The maximum activity of the target product in the culture fluid was achieved by the following mode of fermentation:

The pressure of sterile air
when filing in the fermenter, MPa0,025 0,005...
The rotational speed of the stirrer, with-1 3,8±0,5
the pH of the liquid phase4,5
Fermentation temperature, °C31±0,5
The humidity of the cultural filtrate liquid
to the total product weight, %95±0,5
The enzyme activity, IU/cm3195±5

The process of vacuum-sublimation drying of enzyme technician with minimum energy cost and high quality of the drug was provided with the following modes:

Temperature samozatachivanie enzyme °C17±0,5
Residual pressure in the vacuum freeze-drying chamber, PA66-67
Temperature released from the freeze camera
in the evaporator water vapor, °C- 8±0,5
The flow of water vapor, kg/h2,4±0,05
The moisture of the product at the outlet of the dryer, %, 1,5±0,5
The temperature of the drug at the outlet of the dryer, °C22±0,5
Activity glucoamylase, u/g2050-2085

Srednetehnicheskih temperature pressure between the refrigerant and water vapor at a given maximum thickness of the ice crust on the finned surface of the tubes of the evaporator, 5±0.3 mm, will be:

.

Maximum value of heat transfer coefficient of the evaporator kNRas related to the overall surface of the pipes:

.

When reaching the heat transfer coefficient maximum permissible values 343,88 W/(m·°C), the microprocessor disables the working section of the evaporator recirculation line refrigerant and connects the backup partition and creates the required temperature of fermentation due to the preparation of hot water in the condenser of the refrigeration machine and its supply in the heating jacket of the tank.

From the above examples that the proposed method of controlling the processes of production and drying of enzyme preparations with the use of refrigerating machines operating in heat pump mode, expands the boundaries of energy efficient pairing of objects of different temperature potentials based util is urbanized and recovery of waste energy. When fully implemented universal approach in creating competitive heat pump technology for the generation of heat and cold for the conjunction of the processes of fermentation and vacuum freeze drying.

In the proposed method, the setpoint of the heat transfer coefficient of the evaporator of the refrigeration machine is determined by the permissible thickness of ice on the cooling pipes. In this case, the heat transfer coefficient is the effective management of the refrigerating machine, providing timely switching sections of the evaporator with the mode of condensation on the regeneration mode and Vice versa, while maintaining the parameters of the continuous process, the vacuum freeze-drying to the extent necessary.

Thus, the proposed method has the following advantages compared with prototype:

- improves the quality of the target product by improving the accuracy and reliability of control of technological parameters of production processes and drying of the enzyme preparation;

- allows to improve the energy efficiency of fermentation processes and vacuum-sublimation drying of enzyme preparation and to reduce the specific energy consumption for 5...7% due to the efficient use of the heat of condensation of the refrigerant in the condenser of the refrigerating machine when nahrawan the water and its subsequent flow into the heating jacket of the fermenter;

- reduces the range of variation final moisture content of the drug and the load on the drive of the vacuum pump due to the correction mode, the vacuum freeze-drying on the heat transfer coefficient of water vapor to the refrigerant through the finned surface of the tubes of the working section of the evaporator;

- improves environmental safety of production processes and drying of enzyme preparations due to closed recirculation schemes on material and energy flows.

The method of controlling the processes of production and drying of enzyme preparations, characterized in that to obtain the enzyme preparations used fermenter with a heating jacket for submerged cultivation of microorganisms enzyme preparations with continuous aeration with sterile air and mechanical agitation at a temperature of cultivation 30...32°C throughout the volume of the fermenter; received in fermenter culture liquid was filtered to remove the precipitate and the filtrate of the culture fluid with a humidity of 92...95% served in a vacuum freeze-dryer, which as desublimator use two-evaporator vapor compression refrigerating machine, the working and backup sections which alternately operate respectively in the modes of condensation and regeneration; get "hot water by means of its heat in the condenser of the refrigeration machine due to the heat of condensation of the refrigerant to a temperature of 68...73°C, one of which is directed in the heating jacket of the fermenter, and the other first guide for defrosting the evaporator sector, operating in the regeneration mode, and then cooled to a temperature of 5...7°C water away from the evaporator section in a cumulative collection together with the liquid formed from thawed on the surface of a cooling element of ice crust in the amount evaporated from the enzyme preparation of the moisture, and then in closed loop mode serves two streams, one of which is mixed with the waste water after the fermenter before the capacitor, and the second hot water before fermenter, while the excess water from the recirculation circuit is brought out through the cumulative collection, measure the temperature of culturing in the fermenter, the flow rate and inlet water temperature in the heating jacket of the tank, flow rate and humidity of the culture filtrate of the liquid, the residual pressure in the working volume of the vacuum freeze-drying, humidity-dried enzyme preparation, consumption, and the temperature of the water vapor discharged from the vacuum-freeze dryer in the working section of the evaporator, the boiling temperature of the refrigerant in the working section of the evaporator, the temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator, the water level in the cumulative collection; establish the mass and heat flow of the mixture chilled and hot water in the heating jacket of the tank by varying the ratio of their expenditures with correction for the temperature of cultivation in a fermenter; for measured values of moisture content and flow rate of the filtrate of the culture fluid set the drive power of the compressor of the refrigeration machine and the required residual pressure in the working volume of freeze drying effect on power adjustable drive vacuum pump with correction of residual pressure on the final moisture content of the enzyme preparation; flow rate and the temperature of the water vapor discharged from the vacuum-freeze dryer in the working section of the evaporator, the temperature neskondensirovannyh vapor at the outlet of the working section of the evaporator and the boiling temperature of the refrigerant in the working section of the evaporator determine the current value of the transfer coefficient of water vapor to the refrigerant for cooling the surface of the working section of the evaporator, and the highest minimum values the heat transfer coefficient first increases the drive power of the compressor of the refrigerating machine, and then switch the working section of the evaporator with the mode of condensation on the regeneration mode with simultaneous inclusion on the mode of condensation section, who worked in the regeneration mode.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to production of fluoropolymer powdered materials. A modified fluoropolymer powdered material is obtained. A suspension of solid fluoropolymer particles from a group comprising a fluoroethylenepropylene polymer and a polymer of perfluoroalkoxy compounds together with PTFE particles in an aqueous liquid carrier is obtained. The aqueous suspension is frozen. The frozen carrier is removed by sublimation at pressure below atmospheric pressure to obtain dry fluoropolymer particles, which are modified by presence of PTFE modifier in powder form.

EFFECT: method of obtaining fluoropolymer powdered materials is disclosed.

14 cl, 3 dwg, 1 ex

FIELD: food industry.

SUBSTANCE: one first performs the sections preliminary vacuum treatment using an ejector vacuum pump till residual pressure is equal to 610 Pa, then one cools the external surface of the profile drum acting as the desublimator with electric current supplied onto the groups of thermoelectric modules placed on the internal surface of the profile drum which creates the required temperature gradient for vapours movement to the desublimator surface; then one supplies heat energy to the product using heaters, as a result moisture evaporation takes place at a residual pressure lower than 610 Pa; part of the moisture evaporated from the product is removed from the chamber via the ejector vacuum pump, the other part is adsorbed by the desublimator surface represented by a nanomaterial layer; release of evaporated moisture molecules takes place after the desublimator turning due to the thermoelectric modules connection polarity changing. In the vacuum-and-sublimation drier using nanomaterials and thermoelectric modules, including a drying chamber consisting of sections equipped with a nipple with a locking valve installed with the possibility to connect to a vacuum pump, the vacuum pump, the desublimator placed between the sections and a heater. The drying chamber is made of two sealed sections connected to the vacuum pump and separated with a plate wherein a profile drum representing the desublimator is horizontally installed so that to enable rotation; a nanomaterial layer is applied onto the drum external surface while independent groups of thermoelectric modules are installed on the internal surface.

EFFECT: evaporated moisture vapours capture effectiveness is enhanced; desublimation surface regeneration is ensured during the drier operation in a continuous mode; workload onto the vacuum pump is reduced due to depressurisation in the vacuum-and-sublimation chamber.

2 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: method for freeze drying an erythrocyte diagnosticum involves deep freezing the preparation, putting into a freeze drying chamber and further sublimation thereof in vacuum conditions with subsequent formation of a lyophilisate. At the preparatory step after deposition by centrifuging, separations of the supernatant fluid of erythrocytes are diluted in ratio of 1:9 by a drying medium consisting of a solution of 15 wt % rheopolyglucin and 7.5 wt % saccharose in distilled water, and shelf temperature and pressure in the sublimation chamber is not changed for the first 8 hours and maintained at -15°C and 30 Pa, respectively, and then for the next 14 hours, gradually varied at a rate of (2.6±0.4)°C/h and (2±0.1) Pa/h to 22°C and 3 Pa, respectively, and said parameters are maintained for at least 3 hours.

EFFECT: owing to the disclosed method of drying labile erythrocyte diagnosticums in maximally gentle conditions, activity thereof virtually does not change after prolonged storage and rehydration.

1 tbl, 2 dwg

FIELD: chemistry.

SUBSTANCE: method of obtaining a lyophilisate of a pharmaceutical preparation involves immersing a cellular carrier into the solution of the pharmaceutical preparation to form films of the solution in cells of the carrier, putting the carrier into a freezing zone and then into a heating zone where the solution is dried, with subsequent removal of the lyophilisate of the pharmaceutical preparation, wherein moisture content is controlled in each cell in the heating zone by positioning a fibre-optic sample of a transmission-type spectrophotometer operating in the near-infrared range or which detects Raman shift.

EFFECT: simple process of production, high output of the end product, enabling automation of the process, low cost of the product, enabling inspection of moisture of the end product, high quality of the end product.

8 cl

FIELD: food industry.

SUBSTANCE: cryogenic vacuum-and sublimation installation with complex usage of inert gas includes a device for preliminary freezing of the product, a vacuum-and sublimation drier with a sealed drying chamber wherein a perforated drum and a heating element are positioned; the element is designed in the form of a coil installed in the bottom zone of the drum, its cross-section having the form of a segment; the heating element is the cooling agent cooler and is designed with the spacing between the tubes amounting to no more than 15 mm; the element inlet nipple is connected to the pump line of the desublimator cooling machine while the outlet nipple is connected to the low-pressure line of the cooling agent feed into the cooling machine; the drier chamber is connected to the vacuum-pumping system via the desublimator; the novelty is in the following: the device for preliminary freezing of the product is represented by a tunnel-type cryogenic fast-freezing aggregate (its frozen product feeding conveyor connected to the vacuum-and-sublimation drier doser, the drier heating element made of a material with high heat-conduction coefficient or a semi-permeable material) while the desublimator cooling machine is represented by a gas liquefaction machine working according to the Stirling reverse cycle principle; the machine nipple for feeding liquefied gas is connected to the desublimator represented by a nitrogen trap and to the fast-freezing aggregate nozzles; the nitrogen trap is installed between the vacuum-and- sublimation drier chamber and the vacuum pump; the exhaust gas outlet nipple of the cryogenic fast-freezing aggregate and the outlet nipple of the vacuum pump are connected to the inlet nipple of a membrane apparatus while its outlet nipple for inert gas cleared of impurities is connected to the automatic packaging device.

EFFECT: product fast freezing with cells preservation taking place within the whole bulk, enhancement of the sublimation process intensity due to ensuring highly efficient combined energy input to the product by varied methods.

2 cl, 2 dwg

FIELD: chemistry.

SUBSTANCE: suspension of solid particles of a fluorine-containing polymer in a liquid carrier, preferably water, is frozen and the frozen carrier is then removed via sublimation at subatmospheric pressure to obtain dry powder of fluorine-containing polymer particles.

EFFECT: method enables to obtain powdered materials from a liquid suspension of solid particles of a fluorine-containing polymer which, at normal conditions, cannot be pumped by a pump due to fibrillation capacity.

13 cl

FIELD: medicine.

SUBSTANCE: glass reservoirs with flat bottom, containing biopreparations, are placed into tray with low-temperature medium. Low-temperature layer in tray is, as minimum, twice as thick as layer of frozen biopreparation in reservoir. As medium water solution of calcium chloride is used. Freezing and further sublimation drying are carried out.

EFFECT: reduction of time for process carrying out and obtaining product with developed capillary-porous structure.

2 tbl, 4 ex, 1 dwg

FIELD: food industry.

SUBSTANCE: installation contains a cryogenic freezing chamber, a separation chamber containing a device for cleaning fruits of crystalline hydrates and a device for cleaning inert gas of crystalline hydrates, a drying chamber with an US radiation source and an inert gas inlet, a gas chilling machine with a vertical tube. The cryogenic freezing chamber, the separation chamber and the drying chamber are tightly connected and included into one main with the compressor.

EFFECT: invention enables production of a high quality product.

1 dwg, 1 tbl

FIELD: medicine.

SUBSTANCE: method for preparing a frozen-dried material involves the use of a container enclosed by a capsule, has a permeable area, and contains a dispersed material in a carrier fluid, and said capsule having the permeable area is permeated with a penetrator to form a channel through the capsule to connect an internal part and an external part of the container when the penetrator has passed through the permeable area, evaporation of the carrier fluid from the container through said channel and removal of the penetrator from the permeable area. The penetrator contains an integrally tapered element with a hole adjacent to its top, an open base or a hole adjacent to its base, and with a channel passing through the penetrator, connecting these two holes so that the top of the penetrator can pass through the permeable area, and the carrier fluid vapour can be supplied into the top, pass through the hollow internal part of the taper and escape. Said method is implemented inside a sterile cover which temperature can be changed between ambient temperature and temperature whereat the carrier fluid freezes, and which atmospheric pressure can be changed between environment pressure and lowered atmospheric pressure.

EFFECT: simplification of the method.

21 cl, 27 dwg

FIELD: heating.

SUBSTANCE: during vacuum-sublimation drying process the product is pre-frozen in trays with transverse partitions for increasing the heat exchange surface, at double bottoms of which made from material with high heat conductivity coefficient there installed are thermoelectric modules the operating principle of which is based on Peltier effect. Trays in lower part have finning serving for desublimation of steam of below located cascade. Heat generated with hot ends of thermoelectric modules is used for supply of energy to the product. Drying chamber (sublimator) has cylindrical shape with the flap cover made in the form of semi-cylinder with inspection hole. Along the perimeter of inner surface of sublimator there installed is desublimator for additional condensation (desublimation) of steam.

EFFECT: reduction of specific energy consumption, improvement of product quality, simplifying the drier design, multi-cascade location of trays on the support allows increasing the volume of loaded product.

4 dwg

FIELD: chemistry.

SUBSTANCE: when culturing phototrophs, the culture fluid is stirred and aerated through agitation by moving cultivators back and forth in the horizontal plane at given temperature and pH values. The cultivators are illuminated with a pulsed light source with pulse duration of 0.00001-0.001 s and pulse spacing of 0.01-0.1 s. In the apparatus used, the culture fluid is illuminated with diodes located under transparent bottoms of vessels of the same geometric shape and powered by a pulse generator with controlled frequency and light pulse duration.

EFFECT: group of inventions enables to reduce power consumption when culturing phototroph biomass.

2 cl, 2 dwg, 2 ex

FIELD: chemistry; biochemistry.

SUBSTANCE: device for speeding up reproduction, through faster reproduction and/or increased reproduction output of living cells in a suspension or any cultured organisms through a natural selection process has a flexible sterile pipe 7 with culture medium. A system of movable clamping apparatus 3, 4, 5 divides the pipe 7 into separate zones, containing spent culture (downstream zone), growing culture (growth compartment) and fresh growth medium (upstream zone). In the device there is an apparatus 13 for moving gates and the pipe such that, part of the growth compartment and the culture associated with it can be shut off by clamping apparatus and separated from the growth compartment. That way, part of the pipe which contains unused medium can be linked with part of the culture and medium associated with it, already present in the growth compartment.

EFFECT: realising a method with high reproduction output of living cells or cultured organisms.

36 cl, 10 dwg

FIELD: biochemistry, in particular, methods and devices for producing coloring substances, possible use in food and cosmetic industry, and also during various biological research.

SUBSTANCE: phycoerythrin protein pigment is produced by extraction from seaweed. It is extracted from seaweed, selected from a group including Galaxaura oblongata, Halymenia ceylanica, Helminthocladia australis and Porphyra dentate.

EFFECT: phycoerythrin has high optical density.

2 cl, 27 dwg, 2 tbl

FIELD: equipment for growing plant tissues.

SUBSTANCE: in accordance to the invention, unit for accelerating growth of plant tissues contains a set of boards, forming matrices of holes. Each hole contains a tissue sample. Support for boards is provided by a rack which contains a set of vertically stacked shelves, containing one or more holding recesses, which forcedly move boards to given positions. Light for tissue samples is provided by a set of matrices of light diodes, mounted on mounting plates. Light diodes emit white light. Each mounting plate is supported by corresponding end comber-type rack connector, so that light diodes are close to boards, supported by shelves, positioned lower. Matrix of light diodes preferably matches matrix of holes, supported by a lower positioned shelf in fixed position, so that each light diode is centered above a corresponding hole.

EFFECT: creation of high capacity system for processing samples of tissues which require light for supporting cell reproduction.

7 cl, 7 dwg

FIELD: biotechnology, in particular biopreparation production.

SUBSTANCE: claimed method includes feeding of sterilized broth into presterilized inoculator or bioreactor equipped with means for redox-potential (eH) controlling, including eH electrode and microprocessor unit for controlling and adjustment of eH and pH measurement of redox potential value for 1 h under stirring and comparison of steady-state eH values with steady-state values. When redox-potential value deviates from steady-state value of broth redox-potential by 10 % said broth is recognized as non-sterile one.

EFFECT: process of decreased cost.

4 tbl, 4 ex

The invention relates to the field of purification of gases and can be used for exhaust gas cleaning in microbiological, paint, chemical, food, petroleum refining, and processing of agricultural products

The invention relates to biotechnology, namely biotechnologische equipment used in the processes of cultivation of microorganisms

FIELD: oil and gas industry.

SUBSTANCE: invention relates to the method to produce oil fuel, in which mixing is carried out and reaction of hydrolysis is done with water containing a ferment, which a hydrocarbon oil product, besides, water containing a ferment, is produced by means of mixing of a natural vegetable ferment, containing, at least lipase, in water. The natural vegetable ferment may additionally contain cellulase. The invention also relates to a device for production of oil fuel.

EFFECT: increased efficiency of fuel, which is stable, and also suppression of hazardous substances formation.

10 cl, 11 dwg, 1 ex

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