Background technology
Porous media is meant that inside contains the solid material of many small holes.Many materials of occurring in nature all have loose structure, such as soil, timber, vegetable drug and mineral etc.Along with popularizing and in-depth to the natural reproducible resource development and utilization, extraction as the Chinese medicine effective ingredient, particularly the needed energy of people and resource will come from natural porous material more and more, and development is applicable to that the efficient leaching method fast of porous media is of universal significance.
The principal element that influences the transmission of porous media quality is microcellular structure and the character of the fluid in the hole and the interaction between them of material.The existence of skeleton structure can not be strengthened the quality transfer behavior in the porous material by general method.The main at present method that adopts has two classes: a kind of is the method that reduces the macro-size of porous media, this method can suitably reduce the resistance to mass tranfer in the duct, but can not be from changing in the duct mode that flows in essence, and the size of material reduces to increase the difficulty of Separation of Solid and Liquid; Another kind is the method that applies the stronger outfield of penetration power, and as ultrasonic wave and microwave etc., these outfields can cause the activation and the disturbance of the solvent and the solute molecule of porous media inside.More than two kinds of methods can reach the purpose that improves the valuable constituent leaching efficiency, but also have the leaching that can increase invalid components (impurity), bring difficulty for the separation and purification in downstream; The fuel factor that the outfield causes can be destroyed temperature sensitive property solute, preliminary treatment cost height or process and amplify problems such as difficulty.Therefore, the method for development leaching reinforcement is extremely necessary.
Summary of the invention
The purpose of this invention is to provide a kind of leaching method that the porous media solute leaches fast that is used for, promptly utilize the interaction between solvent preferably of mutual solubility property to strengthen the leaching method that solute transmits in the porous media, this method has not only that leaching speed is fast, yield is high, and mild condition, expense are low, easy to implement.
Technical scheme of the present invention is as follows: be used for the leaching method that the porous media solute leaches fast, it is characterized in that this method comprises the steps:
(1) selects extracting solvent A and dissolve each other with A or be soluble in A and can dissolve the secondary solvent B of solute in the porous media;
(2) in porous media, add earlier secondary solvent B, and be retained to porous media reach swelling saturated till;
(3) the porous media external solvent is switched to A, leach.
Described extracting solvent A or secondary solvent B are the mixed solutions of a kind of solvent or several solvents.
Switching mode described in the step of the present invention (3) has two kinds: a kind of is directly to append solvent orange 2 A in container; Another kind is earlier with filtering or centrifugal mode adds solvent orange 2 A after will being in the solvent B removal of porous media outside again.
Porous media of the present invention mainly comprises the particle that natural economic plants, tcm and herbal slice and they obtain after roughing, requiring does not have chemical bond closely between solute and matrix.
Principle of the present invention is: one, the phase counterdiffusion meeting of the inside and outside solvent of porous media drives solute migration; Two, the course of dissolution between solvent makes and forms between two parts main body solvent by forming unstable solvent turbulence district of causing, and this regional solute transmission is the convection current diffusion.
The present invention compared with prior art, have the following advantages and the high-lighting effect: the present invention is applied to the leaching of solute in the porous media, it is fast to have leaching speed, leaches fully characteristics that are easy to realize, and can implementing under room temperature or the temperature near room temperature.Switch the requirement of method to porous media itself itself and internal and external environment based on solvent, the present invention is very suitable for leaching the medicinal plant that the active ingredient in the natural plants, particularly target are the multicomponent extract.Utilize the present invention, the effective mass tranfer coefficient in the porous media duct can be by 10
-9m
2/ s rises to 10
-7m
2/ s, the effective diffusion cofficient in the fine and close hole wall also can have the raising of 1~2 order of magnitude.
The specific embodiment
Further specify the present invention below in conjunction with drawings and Examples.
The present invention can implement in static or dynamic mode under normal pressure, and implementation step comprises:
(1) according to porous media and wherein the physicochemical properties of solute determine extracting solvent A, select to dissolve each other or be soluble in A and can dissolve the secondary solvent B of solute among the porous media C with A;
(2) adding secondary solvent B is saturated to reaching swelling in porous media C;
(3) external solvent with porous media C switches to extracting solvent A, leaches.
Wherein, select the standard of secondary solvent B to be:
A.B is soluble in A or can be miscible with A.
B.B is the good solvent of main valuable constituent among the porous media C.
C.A is very fast to the course of dissolution of B.
Implementation process is described:
Porous media material C is placed in the container, add B and be retained to porous media C reach swelling saturated till.
The external solvent B of porous media C is switched to A two kinds of optional modes are arranged.
Mode 1: in container, directly append A.
Mode 2: earlier with filtering or centrifugal mode adds A after will being in the B removal of porous media outside again.
Handoff procedure had no special requirements for the time, allowed to finish as early as possible in the scope of equipment permission.
Mode 1 also can realize by dynamic mode: porous media C is placed fixed-bed type leacher (as percolation filter), make B slowly pass through bed according to certain orientation, switch to A quarter in due course and get final product.
Said process can carry out in room temperature or under near the temperature of room temperature.
Embodiment:
(1) with the acid chromium blue k is the solute tracer of holding concurrently, solvent B is water or methyl alcohol, consumption 0.4mL, extracting solvent A adopts methyl alcohol, acetone, ethanol or water respectively, consumption 20mL, B is full of the capillary of 20 internal diameter 0.5mm,, adds the mode of solvent orange 2 A after the switching mode of solvent adopts the solvent B with the outside to remove again with the solute in the A leaching capillary.
Experimental result is as shown in the table:
Solvent orange 2 A | Initial concentration Ppm | Solvent B | Mass transfer time S | Main body concentration ppm | Effective diffusion cofficient, D
eff????m
2/s
|
Water | ??1750 | Water | ??300 | ??0.464 | ????5.00×10
-9 |
Methyl alcohol | ??1750 | Methyl alcohol | ??120 | ??0.518 | ????1.55×10
-8 |
Ethanol | ??1750 | Water | ??60 | ??2.840 | ????9.00×10
-7 |
Methyl alcohol | ??1750 | Water | ??60 | ??1.850 | ????3.85×10
-7 |
Acetone | ??1750 | Water | ??60 | ??2.630 | ????7.70×10
-7 |
Can see that by table use the leaching velocity that the present invention can accelerate solute effectively, effective diffusion cofficient improves greatly.
(2) with the Chinese herb rhubarb be object, dried medicinal material consumption 1.0g, general anthraquinone is for investigating solute, and solvent orange 2 A is a water, and consumption 200mL, solvent B are ethanol, 60 ℃ of leaching temperatures, the switching mode of solvent adopts the mode of directly appending solvent orange 2 A.Experimental result sees the following form.
Directly leaching | Solvent switches |
Leaching time min | Leachate concentration ppm | Recovery rate 100 * g/g | Leaching time min | Leachate concentration ppm | Recovery rate 100 * g/g |
????1 | ??27.5 | ????0.55 | ????1 | ??31.6 | ????0.63 |
????2 | ??36.5 | ????0.73 | ????2 | ??37.4 | ????0.75 |
????6 | ??46.5 | ????0.93 | ????8 | ??52.8 | ????1.06 |
????16 | ??55 | ????1.1 | ????16 | ??63.2 | ????1.26 |
????32 | ??58.5 | ????1.17 | ????32 | ??65.2 | ????1.30 |
????64 | ??61 | ????1.22 | ????64 | ??63.4 | ????1.27 |
????120 | ??61.5 | ????1.23 | ????120 | ??71.8 | ????1.44 |
Can see by table, use the present invention when reaching same recovery rate required time short, the recovery rate height in the identical time.
(3) with the Chinese herb rhubarb be object, dried medicinal material consumption 1.0g, general anthraquinone is for investigating solute, and solvent orange 2 A is an ethanol, and consumption 200mL, solvent B are water, and 60 ℃ of leaching temperatures add the mode of solvent orange 2 A again after the switching mode of solvent adopts the solvent B with the outside to remove.Experimental result sees the following form.
Directly leaching | Solvent switches |
Leaching time min | Leachate concentration ppm | Recovery rate 100 * g/g | Leaching time min | Leachate concentration Ppm | Recovery rate 100 * g/g |
????1 | ??23.5 | ????0.47 | ????1 | ??40.0 | ????0.8 |
????8 | ??28.0 | ????0.56 | ????2 | ??52.5 | ????1.05 |
????16 | ??35.5 | ????0.71 | ????4 | ??103.0 | ????2.06 |
????32 | ??39.5 | ????0.79 | ????16 | ??106.5 | ????2.13 |
????64 | ??49.5 | ????0.99 | ????32 | ??102.5 | ????2.05 |
????120 | ??54.5 | ????1.09 | ????120 | ??110.0 | ????2.2 |
Can be seen that by table the recovery rate when using 2min of the present invention is suitable when directly leaching 120min, strengthening effect is obvious.