Summary of the invention
The object of the present invention is to provide a kind of cryoconcentration method of Chinese medicine extraction liquid;
Another object of the present invention is to provide the device of realizing said method.
The cryoconcentration method of Chinese medicine extraction liquid of the present invention, be that can the flow technology of ice crystal or ice slurry is applied in the low-temperature concentration process of herb liquid, and generate continuously, automatically or the herb liquid extract at low temperature concentration systems technology of continuous production type such as the automatic discharging of discontinuous centrifugal force in conjunction with ice crystal, replace original multiple-effect evaporation herb liquid concentration technique, solve the technical problem that exists in the prior art, final tcm product quality and the Chinese medicine extraction yield of improving reduces the product energy resource consumption.
Method of the present invention makes Chinese medicine extraction liquid reach supercooling temperature, makes over-cooled solution generate ice crystal continuously with physical means then, separates with solute by the centrifugal solvent of carrying secretly in the ice crystal that makes.
Above-mentioned supercooling temperature is determined according to the concentration of Chinese medicine extraction liquid and the dependence of its phase transition temperature by temperature-controlling system, is carried out by refrigeration system.
Above-mentioned physical means is passive or active method, as collision or ultrasound wave.
Method of the present invention can be applicable to the separation of soluble component, as desalinization, wastewater treatment etc.
A kind of device of realizing the cryoconcentration method of Chinese medicine extraction liquid of the present invention mainly comprises 3 loops:
(1) dress flow container, pump, effusion meter, cooling heat exchanger, the continuous generation of ice slurry and whizzer are in turn connected into the loop; Part connecting pipe in this loop connects heater;
(2) adorn flow container, quality inspection and cryogenic temperature control system, refrigeration system, computer temperature measurement and refrigeration system temperature control system, the continuous generation of ice slurry and whizzer and be in turn connected into the loop;
(3) cooling heat exchanger and refrigeration system connect into the loop;
Wherein adorn medicine liquid outlet is arranged on the flow container, ice slurry generates continuously and there is the ice cube outlet upper end of whizzer.
Above-mentioned pump is a centrifugal water pump.
Above-mentioned refrigeration system for well, be similar to the refrigerator refrigeration, but the cold that provides is based on mobile refrigerating medium with handpiece Water Chilling Units; Computer temperature is measured and is adopted temperature data collecting system, generally adopts T type thermocouple that measurement point is carried out temperature survey; Temperature control system can adopt the temperature-sensitive bag of feedback usefulness in the general refrigeration system, and also available temperature control software system is controlled.
The continuous production technical matters that the present invention mainly adopts outer circulation heat exchange cooling, the continuous nucleus generation of subcooled liquid, centrifugal force centrifugal separation technology to combine.According to the dependence of the concentration of wanting concentrated traditional Chinese medicine liquid and its phase transition temperature, determine the operative temperature of refrigeration system in the system, make herb liquid in flow process, be cooled to degree of supercooling.By specific nucleus production technology, make the moisture in the supercool medicinal liquid in liquid bath, generate the ice crystal that flows as methods such as vibrations or ultrasound wave, system accurately controls the growth rate and the wafer size of ice crystal by chilling temperature, with solid ice crystal and separating liquid medicine, and by centrifugal method with the separating liquid medicine of carrying secretly in the solid ice crystal.The concentration change of on-site measurement herb liquid, and control the temperature of refrigeration system successively.The sample medicinal liquid is extracted in requirement according to product design, detects the control ability of quality of liquid medicine quantizating index.The final accounting and the energy conversion efficiency of the system of improvement optimized the technological level of whole system according to the production capacity of system.
Utilize method of the present invention, can bring following beneficial effect.
(1) environmental friendliness.Because medicinal liquid is at low temperatures the moisture crystallization to be separated out, the abnormal smells from the patient that does not have evaporation and brought; And water of crystallization separates fully clean, no waste water handling problem;
(2) retention rate of effective ingredient improves 20%, and particularly volatile substances is able to complete reservation;
(3) do not have albumen, the polyreaction of polysaccharide thing concentrates the back runny plaste and is easy to drying; The acidification reaction that does not have the saccharide thing, the final products mouthfeel is good;
(4) energy-conservation: the latent heat energy of water crystallization is 1/7th of an evaporation latent heat, and the crystallization concentration technique itself is exactly a power-saving technology.
(5) this low-temperature concentration process and apparatus structure compactness are simple to operate, produce continuously, and the working environment close friend, the GMP authentication of being convenient to production technology is passed through.
The specific embodiment
The cryoconcentration process of embodiment 1 experiment medicinal liquid
The experiment medicinal liquid contains ethanol 7%, and ethylene glycol 7%, sodium chloride 1%, polyvinyl alcohol 0.01% (mass percent), molecular weight are that 90000 polyvinyl alcohol is equivalent to hmw protein, and the solution concentration of so initial medicinal liquid is about 15%.Along with concentrating of medicinal liquid, pure ice crystal is separated, and liquor strength is increased gradually, and crystallization temperature reduces, and its corresponding relation is as shown in table 1.The concentration of medicinal liquid increases with crystallization temperature decline linear substantially as can be seen from Figure 2.
Among Fig. 1, medicinal liquid is packed in the flow container 4, make medicinal liquid reach messenger drug liquid by cooling heat exchanger 9 by centrifugal water pump 7 and effusion meter 8 and be cooled to supercooled effect, the low temperature of cooling heat exchanger 9 is supplied with by refrigeration system 10; When supercool medicinal liquid arrives continuous generation of ice slurry and whizzer 3, make supercool medicinal liquid generate ice crystal continuously by passive, active methods such as collision or ultrasound wave, ice crystal further filters in 3, separates, and by centrifugal force the solvent of carrying secretly in the ice crystal is separated with solute.Purified ice cube is separated by ice cube outlet 2, and the medicinal liquid after concentrating flows in the dress flow container 4.The herb liquid product of certified concentration enters next stage product program by medicine liquid outlet 6 packings.By the concentration in quality inspection and the cryogenic temperature control system 5 on-site measurement herb liquid containers, when concentration does not also reach the ultimate density requirement, concentration for this moment, running temperature according to the dependence between the Pressure, Concentration, Temperature of specific medicinal liquid (Fig. 2) field control refrigeration system meets final requirement up to concentration.Computer temperature is measured and refrigeration system temperature control system 1, the temperature of on-site measurement system medicinal liquid in service and the operational factor of feedback control refrigeration system.The process repetitive cycling reaches the concentrated effect that needs until final this stove herb liquid as described above.On the connecting pipe of this device, connect one or more heaters 11, occur the situation that system can not run well when preventing because of the ice crystal blocking pipe.
The relation of table 1 liquor strength and crystallization temperature
Liquor strength (%) | The medicinal liquid crystallization temperature (℃) |
15 | -2.4 |
20 | -3.2 |
25 | -4.1 |
30 | -4.9 |
35 | -5.7 |
40 | -6.5 |
45 | -7.3 |
50 | -8.1 |
55 | -8.9 |
60 | -9.7 |
65 | -10.6 |
70 | -11.4 |
75 | -12.2 |
80 | -13.0 |
85 | -13.8 |
90 | -14.6 |