CN103252166B - Absorption and desorption device and desorption method of Chinese medicine volatile oil film - Google Patents
Absorption and desorption device and desorption method of Chinese medicine volatile oil film Download PDFInfo
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Abstract
The invention discloses an absorption and desorption device and a desorption method of a Chinese medicine volatile oil film. The device comprises a film component, a circulation pump, a double-layer storage tank, a permeation liquid storage tank, a pressure gauge, a flowmeter, a constant-temperature water bath, a peristaltic pump and stainless steel pipelines. The desorption method comprises the following steps of: under 0.25MPa and at constant temperature, ultra-filtering and absorbing the volatile oil through the film and simulating a solution for 24 hours, calculating the absorption amount of the volatile oil, and arranging the film after the absorption on the desorption device; taking an ethanol alkali solution as a strippant, keeping the temperature to be at 1 DEG C, desorbing for 30 minutes to 1.5 hours under the conditions that the pressure is less than 0.05MPa and the film surface flow velocity is within 0.1-1m/s; and taking a desorption liquid sample and obtaining the desorption rate of 90-95%. The method and the device are applicable to the film fining process of the components of the Chinese medicine volatile oil, in particular the process that the injection liquid pyrogen and resins are removed by using a film method and the process that the Chinese medicine volatile oil is enriched through the film, the loss ratio of the active components is greatly reduced, the transferring rate is improved, and the film is well regenerated.
Description
One. technical field
The present invention relates to a kind of sorption and desorption device and desorption method of Chinese medicine volatile oil film.The method is applicable to the Chinese medicinal film subtractive process into volatile oil component, greatly can reduce the loss late of volatile oil, improve its rate of transform.The invention belongs to the Extraction and separation technical field of Chinese medicine preparation.
Two. background technology
There is in Chinese medicine system relative to traditional isolation and purification method application of membrane separation technology the advantage of its uniqueness: separation process is low without phase transformation, normal-temperature operation, energy consumption, not with an organic solvent, the production cycle can be shortened, reduce loss of effective components, be beneficial to environmental protection and safety in production; Select suitable membrane material can obtain higher separation selectivity, keep the corresponding traits of former side thus the curative effect of guarantee finished product; Good impurity removing effect, can remove bacterium and pyrogen while of extending the Chinese medicine storage time; Be specially adapted to the separation of heat-sensitive ingredients in Chinese medicine, concentrate; Can realize serialization, automation mechanized operation, technological parameter is stablized controlled, and easy and other PROCESS COUPLING, meet the requirement of Chinese medicine production modernization.Since the eighties, UF membrane starts the production being applied to Chinese medicine preparation.Receive much attention.Wherein maximum with the application of milipore filter, relate generally to the following aspects: the extraction of (1) Effective Component of Chinese Medicine.(2) production of oral liquid.(3) preparation of medicinal extract preparation.(4) removal of thermal source.(5) from pharmacy waste water, effective ingredient is reclaimed.
Volatile oil be the class be present in plant have volatility, can with the general name of steam distillation oily liquids out.Chinese medicine is comparatively common in the sections such as composite family, Rutaceae, Umbelliferae, Zingiber belong to; Volatile oil is as the main body of Chinese medicine volatile materials, although amount is few, curative effect is given prominence to, and is the important substance basis that Chinese medicine plays a role.Effect is quite extensive, comprises anti-inflammatory, antiallergy, antimicrobial, anti-sudden change and antitumaous effect etc.Constantly there are the effect that various volatile oil is new and report in recent years.In addition, volatile oil is also in the ascendant in the application of spices, food and cosmetics industry.
Film enrichment traditional medicine volatile oil process (obtain Chinese medicine oil aqueous emulsion by steam distillation, then adopt membrane technology to carry out water-oil separating) environmental protection, practical, effectively can overcome the drawback of traditional handicraft, and obtain higher oil-collecting ratio and active ingredient retention rate.
Employing membrane technology replaces the pyrogen in traditional absorption and heating removal parenteral solution, effectively can solve the medicine sex change that conventional method is brought, generate new sediment, the problems such as flow process is complicated, this all has very large meaning to the production of traditional Chinese medicine injection and new product development.In addition, be separated if having employed resin adsorption in technique early stage, after also can remain certain resin wear thing in parenteral solution.Need adopt during membrane separation technique and remove.
Especially in above two kinds of processes, separation membrane surface often adsorbs certain active ingredient of Chinese herbs makes its rate of transform low, and waste natural resources of Chinese medicinal materials, increases production cost.Therefore need to find suitable method to solve this problem produced in film application process.Do not find that pertinent literature is reported at present.
Three. summary of the invention
, problem of resource waste low for the rate of transform occurred in the pyrogen adopted in membrane technology removal parenteral solution and resin process and Chinese medicine volatile oil film enrichment process, technical problem to be solved by this invention is just to provide a kind of sorption and desorption device and desorption method of Chinese medicine volatile oil film.The method is applied to ultrafiltrationmembrane process depyrogenation and resin process, and Chinese medicine volatile oil film enrichment process, greatly can reduce the loss late of traditional medicine volatile oil, improve its rate of transform, and film obtains regeneration preferably simultaneously.
the object of the invention is to be realized by following technical scheme:
A kind of sorption and desorption device of Chinese medicine volatile oil film, it is characterized in that this device is by membrane module 1, circulating pump 2, double-deck stock chest 3, penetrating fluid stock chest 4, Pressure gauge 5, flowmeter 6, water bath with thermostatic control 7, peristaltic pump 8, stainless steel pipes 9 is made, wherein double-deck stock chest 3 is connected with circulating pump 2 by stainless steel pipes 9, be connected with Pressure gauge 5 by stainless steel pipes 9 again, be connected with membrane module 1 by stainless steel pipes 9 again, again by stainless steel pipes 9 and Pressure gauge 5, again by stainless steel pipes 9 and flowmeter 6, be connected with double-deck stock chest 3 by stainless steel pipes 9 again, a penetrating fluid conveying stainless steel pipes 9 is had in membrane module 1 lower end, penetrating fluid stock chest 4 is placed below stainless steel pipes 9, water bath with thermostatic control 7 is connected with peristaltic pump 8 by silica gel hose 12, be connected by the chuck import 10 of silica gel hose 12 with double-deck stock chest 3 again, the JO 11 of double-deck stock chest 3 is connected with water bath with thermostatic control 7 by silica gel hose 12.
The sorption and desorption device of described Chinese medicine volatile oil film, it is characterized in that described membrane module 1 is divided into organic plate film assembly, ceramic film component or metal film assembly, wherein organic plate film assembly is clipped between upper steel plate 15 and lower steel plate 18 by organic film 13, wherein upper steel plate 15 is inverted plate-like, the Pan Bi of axis has two holes, the short steel pipes with screw thread mouth is welded respectively in the position in hole, for import 16 and outlet 17, be connected with stainless steel pipes 9 respectively, the surface design of lower steel plate 18 has 6-12 road cast groove, per pass cast groove is all designed with a permeate flow and portals, all stainless steel pipes 9 is carried to be connected with the penetrating fluid bottom lower steel plate 18, upper and lower two steel plates add tightening seal by circular iron hoop 19, ceramic film component or metal film assembly be by tubular ceramic film or tubular metal film 14 by upper-lower seal circle vertical seal in stainless steel enrichment case, stainless steel enrichment case upper and lower side is equipped with screw thread mouth, be connected with stainless steel pipes 9, there is a penetrating fluid delivery outlet lower end, side of stainless steel enrichment case, penetrating fluid, by stainless steel pipes 9, flows in penetrating fluid stock chest 4.
The sorption and desorption device of described Chinese medicine volatile oil film, is characterized in that described organic film is polyether sulfone (PES) film, Kynoar (PVDF) film; Ceramic membrane is silicon oxide film, oxidation titanium film; Metal film is SUS316 film, SLS316L film.
The sorption and desorption device of described Chinese medicine volatile oil film carries out the method for sorption and desorption, it is characterized in that sorption and desorption method step is as follows:
A. get appropriate volatile oil to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is the simulated solution 10L of the volatile oil of 1-8g/L;
B. the simulated solution of step a is placed in the double-deck stock chest (3) of sorption and desorption device, by water bath with thermostatic control (7) by a certain value within the scope of the simulated solution constant temperature in double-deck stock chest (3) 10-60 DEG C;
C. organic film (13) is clipped in up and down between two block plates of organic film assembly, separately by tubular ceramic film or tubular metal film (14) vertical seal in stainless steel enrichment case, by screw thread mouth, stainless steel enrichment case upper and lower side is connected with stainless steel pipes (9);
D. ON cycle pump (2), by stainless steel pipes (9) and Pressure gauge (5), simulated solution is transported to membrane module to adsorb, solution after absorption is by stainless steel pipes (9), Pressure gauge (5) and flowmeter (6) are transported in double-deck stock chest (3), the pressure regulating Pressure gauge (5) is 0.25Mpa, crossflow velocity is adsorb under 2m/s condition, every 10min, the penetrating fluid in penetrating fluid stock chest (4) is poured in double-deck stock chest (3) in adsorption process, after circulation 24h, volatile oil absorption reaches balance;
E. from double-deck stock chest (3), sample 10ml, adopt the solution concentration after gas chromatography determination absorption, compare with the concentration of absorption front simulation solution, obtain adsorbance;
F. organic film, ceramic membrane or metal film after absorption are taken off, with distilled water, sorption and desorption device is cleaned up, the film after absorption is reinstalled on sorption and desorption device;
G. be that the 10-20% ethanol alkaline solution of 0.1-0.5mol/L loads in double-deck stock chest (3) as strippant using concentration, got a certain value constant temperature in 10-60 DEG C of temperature range by water bath with thermostatic control (7);
H. at constant temperature, pressure is less than 0.05MPa and crossflow velocity carries out desorb 30min-1.5h under 0.1-1m/s range of condition, in stripping liquid, the concentration of volatile oil is constant;
I. from double-deck stock chest (3), get stripping liquid sample, measure the concentration of stripping liquid according to the assay method in step e, obtain desorption efficiency 90%-95%.
The method of above-mentioned sorption and desorption, is characterized in that the volatile oil described in step a is divided into light oil and heavy oil.
The method of above-mentioned sorption and desorption, is characterized in that light oil is Herba Schizonepetae volatile oil, rascal volatile oil, Rhizoma Cyperi volatile oil; Heavy oil is volatile clove oil, Essential Oil of Acorus tatarinowii.
The method of above-mentioned sorption and desorption, is characterized in that the alkaline strippant described in step g is NaOH.
The invention has the beneficial effects as follows:
Effectively can solve film refines in Chinese traditional medicine water extract process, especially the volatile oil active ingredient rate of transform occurred in the process of parenteral solution pyrogen and resin and in film enrichment traditional medicine volatile oil process is low, problem of resource waste to adopt membrane technology to remove, the rate of recovery can reach 95%, and film obtains regeneration preferably simultaneously.The method was both applicable to small-scale production, also met the demand of large scale business enterprise.In addition the method flow process is short, simple to operate, and according to the size of membrane module, desorption apparatus is easy to amplify, and also can echo on original production line, realize online desorb and recovery.For the large-scale promotion adopting embrane method to remove traditional medicine volatile oil parenteral solution pyrogen and resin process and Chinese medicine volatile oil film process of enriching provides technical guarantee.
four. accompanying drawing explanation
fig. 1 is the structural representation of organic film sorption and desorption device;
fig. 2 is the structural representation of ceramic membrane or metal film sorption and desorption device;
fig. 3 is organic film assembly front view.
reference numeral:1-membrane module; 2-circulating pump; 3-double-deck stock chest; 4-penetrating fluid stock chest; 5-pressure gauge; 6-flowmeter; 7-water bath with thermostatic control; 8-peristaltic pump; 9-stainless steel pipes; The import of 10-chuck; 11-JO; 12-rubber tubing; 13-organic film; 14-tubular ceramic film or tubular metal film
15-upper metallic plate; 16-import; 17-outlet; 18-lower metallic plate; 19-circular stirrup.
five. detailed description of the invention
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1: a kind of sorption and desorption device of Chinese medicine volatile oil film, it is characterized in that this device is by membrane module 1, circulating pump 2, double-deck stock chest 3, penetrating fluid stock chest 4, Pressure gauge 5, flowmeter 6, water bath with thermostatic control 7, peristaltic pump 8, stainless steel pipes 9 is made, wherein double-deck stock chest 3 is connected with circulating pump 2 by stainless steel pipes 9, be connected with Pressure gauge 5 by stainless steel pipes 9 again, be connected with membrane module 1 by stainless steel pipes 9 again, again by stainless steel pipes 9 and Pressure gauge 5, again by stainless steel pipes 9 and flowmeter 6, be connected with double-deck stock chest 3 by stainless steel pipes 9 again, a penetrating fluid conveying stainless steel pipes is had in membrane module 1 lower end, penetrating fluid stock chest 4 is placed below stainless steel pipes, water bath with thermostatic control 7 is connected with peristaltic pump 8 by silica gel hose 12, be connected by the import 10 of the chuck of silica gel hose 12 and extract or the double-deck stock chest 3 of stripping liquid again, the outlet 11 of the chuck of double-deck stock chest 3 is connected with water bath with thermostatic control 7 by silica gel hose 12.
The sorption and desorption device of described Chinese medicine volatile oil film, it is characterized in that described membrane module 1 is divided into organic plate film assembly, ceramic film component and metal film assembly, wherein organic plate film assembly is clipped between upper steel plate 15 and lower steel plate 18 by organic film 13, wherein upper steel plate 15 is inverted plate-like, the Pan Bi of axis has two holes, the short steel pipes with screw thread mouth is welded respectively in the position in hole, for import 16 and outlet 17, be connected with stainless steel pipes 9 respectively, the surface design of lower steel plate 18 has 6-12 road cast groove, per pass cast groove is all designed with a permeate flow and portals, all stainless steel pipes 9 is carried to be connected with the penetrating fluid bottom lower steel plate 18, upper and lower two steel plates add tightening seal by circular iron hoop 19, ceramic film component or metal film assembly be by tubular ceramic film or tubular metal film 14 by upper-lower seal circle vertical seal in stainless steel enrichment case, stainless steel enrichment case upper and lower side is equipped with screw thread mouth, be connected with stainless steel pipes 9, there is a penetrating fluid delivery outlet lower end, side of stainless steel enrichment case, penetrating fluid, by stainless steel pipes 9, flows in penetrating fluid stock chest 4.
Wherein:
Circulating pump: the happy chemical pumping of German prestige, model PM-100PE, power output 100W; H-Max: 4.5m; Flow: 2.7m
3/ h.
Peristaltic pump: German Thomas's peristaltic pump, model 20251352, maximum pressure: 2.0bar; Flow: 5m
3/ h.
Stainless steel pipes: wall thickness: 1cm, internal diameter: 3cm; Stainless steel tube and circulating pump, pressure gauge, membrane module, flowmeter and peristaltic pump are all with being threaded;
Double-deck stock chest: material: stainless steel, internal layer groover rot diameter: 20cm; Outer groover rot diameter 26cm; Groove is high: 40cm;
Water bath with thermostatic control: U.S. PolyScience freezes hot type circulator bath, operating temperature :-40 DEG C of ∽ 200 DEG C.
Penetrating fluid stock chest: material: stainless steel, wall thickness: 1cm, internal diameter: 20cm, groove is high: 40cm;
Pressure gauge: pressure vacuum meter YZ-100Z, measures pressure limit: 0 ~ 4Mpa;
Flowmeter: pipeline dobber flowmeter, model: LFS-15, measurement category: 6-60L/h;
Wherein membrane module:
Organic film assembly: organic film: poly (ether sulfone) film, polyvinylidene fluoride film, diameter: 20cm; Upper and lower two stainless steel clamp plates: diameter: 20cm; Thickness 1.5cm.Organic film is clipped between two clamping plate, then uses circular stirrup banding.
Ceramic membrane or metal film assembly: tubular ceramic film: silicon oxide film, oxidation titanium film, long: 22cm, internal diameter: 2cm, wall thickness: 0.15cm; Tubular metal film: SUS316 film, SLS316L film, long: 22cm, internal diameter: 2cm, wall thickness: 0.15cm; ; Cylindrical stainless steel enrichment case: wall thickness: 1cm; High: 20cm; Internal diameter: 4cm; Tubular ceramic film or tubular metal film are sealed in cylindrical stainless steel enrichment case, each 1cm in upper and lower two ends.
Embodiment 2: sorption and desorption method and the concrete steps of the sorption and desorption device of Chinese medicine volatile oil film are as follows:
The first step is be taken at the Herba Schizonepetae volatile oil 0.25g that Nanjing Ze Lang Pharmaceuticals Ltd purchases to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is the Herba Schizonepetae volatile oil simulated solution 10L of 1.0g/L;
Second step is the double-deck stock chest 3 above-mentioned simulated solution being placed in organic film sorption and desorption device, by water bath with thermostatic control 7 by simulated solution constant temperature to 10 DEG C;
3rd step is for being 70,000 by molecular cut off, and diameter is that the poly (ether sulfone) film of 20cm is arranged on up and down between two block plates of membrane module 1, and by two steel plates, with circular stirrup 19 banding, two ends are connected with stainless steel pipes 9;
4th step ON cycle pump 2, regulate Pressure gauge 5, pressure is adjusted to 0.25Mpa, circulate under crossflow velocity is 2m/s and 10 DEG C condition, every 10min in the process of circulation, by the penetrating fluid in penetrating fluid stock chest 4 down in double-deck stock chest 3, after circulation 24h, the absorption of Herba Schizonepetae volatile oil solution reaches balance;
5th step for sample 10ml from double-deck stock chest 3, and extraction into ethyl acetate, measures according to following chromatographic condition: chromatographic column is XE-60 fused-silica capillary column (20% cyanoethyl silicon rubber, 20.0 m × 0.53 mm, 0.25 μm); Detector: hydrogen flame ionization detector (FID); Detector temperature: 180 DEG C; Carrier gas is gas, flow rate of carrier gas: 1.0mL/min; Split ratio is 25:1; Temperature programming: 40 DEG C continue 3 min, then rise to 180 DEG C with the speed of 20 DEG C/min, continue 1 min, sampling volume: 1 μ L at 180 DEG C.Adopt finger-print peak area method, the Herba Schizonepetae volatile oil concentration calculated in the rear sample solution of absorption is 0.8g/L, and adsorbance is 2g;
Organic film sorption and desorption device, for be taken off by poly (ether sulfone) film, cleans up with distilled water by the 6th step, is reinstalled on organic film sorption and desorption device by the poly (ether sulfone) film after absorption;
7th step is be that the ethanolic sodium hydroxide stripping workshop 2 liters of 20% of 0.5mol/L is placed in the double-deck stock chest 3 of organic film sorption and desorption device by water bath with thermostatic control 7 constant temperature to 25 DEG C by concentration;
8th step is at 25 DEG C, and 0.03MPa and crossflow velocity are carry out desorb 30min under the condition of 0.8m/s, and in stripping liquid, the concentration of Herba Schizonepetae volatile oil remains unchanged;
9th step for get stripping liquid 10ml from double-deck stock chest 3, and according to the assay method in above-mentioned steps five, the concentration measuring Herba Schizonepetae volatile oil in stripping liquid is 0.95g/L, and desorption efficiency is 95%.
Embodiment 3: sorption and desorption method and the concrete steps of the sorption and desorption device of Chinese medicine volatile oil film are as follows:
The first step is be taken at the rascal volatile oil 0.5g that Nanjing Ze Lang Pharmaceuticals Ltd purchases to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is the rascal volatile oil simulated solution 10L of 2.0g/L;
Second step is the double-deck stock chest 3 above-mentioned simulated solution being placed in organic film sorption and desorption device, by water bath with thermostatic control 7 by simulated solution constant temperature to 60 DEG C;
3rd step is for being 140,000 by molecular cut off, and diameter is that Kynoar (PVDF) film of 20cm is arranged on up and down between two block plates of membrane module 1, and by two steel plates, with circular stirrup 19 banding, two ends are connected with stainless steel pipes 9;
4th step ON cycle pump 2, regulate Pressure gauge 5, pressure is adjusted to 0.25Mpa, circulate under crossflow velocity is 2m/s and 60 DEG C condition, every 10min in the process of circulation, by the penetrating fluid in penetrating fluid stock chest 4 down in double-deck stock chest 3, after circulation 24h, the absorption of rascal volatile oil solution reaches balance;
5th step for sample 10ml from double-deck stock chest 3, and extraction into ethyl acetate, measures according to following chromatographic condition: chromatographic column is XE-60 fused-silica capillary column (20% cyanoethyl silicon rubber, 20.0 m × 0.53 mm, 0.25 μm); Detector: hydrogen flame ionization detector (FID); Detector temperature: 180 DEG C; Carrier gas is gas, flow rate of carrier gas: 1.0mL/min; Split ratio is 25:1; Temperature programming: 40 DEG C continue 3 min, then rise to 180 DEG C with the speed of 20 DEG C/min, continue 1 min at 180 DEG C, sampling volume: 1 μ L, adopt finger-print peak area method, the rascal volatile oil concentration calculated in the rear sample solution of absorption is 1.7g/l, and adsorbance is 3.0g;
Organic film sorption and desorption device, for be taken off by polyvinylidene fluoride film, cleans up with distilled water by the 6th step, is reinstalled on organic film sorption and desorption device by the polyvinylidene fluoride film after absorption;
7th step is be that the ethanolic sodium hydroxide stripping workshop 2 liters of 10% of 0.2mol/L is placed in the double-deck stock chest 3 of organic film sorption and desorption device by water bath with thermostatic control 7 constant temperature to 35 DEG C by concentration;
8th step is at 35 DEG C, and 0.05MPa and crossflow velocity are carry out desorb 30min under the condition of 1m/s, and in stripping liquid, the concentration of rascal volatile oil remains unchanged;
9th step for get stripping liquid 10ml from double-deck stock chest 3, and according to the assay method in above-mentioned steps five, the concentration measuring rascal volatile oil in stripping liquid is 1.38g/L, and desorption efficiency is 92%.
Embodiment 4: sorption and desorption method and the concrete steps of the sorption and desorption device of Chinese medicine volatile oil film are as follows:
The first step is be taken at the volatile clove oil 1.25ml that Nanjing Ze Lang Pharmaceuticals Ltd purchases to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is the volatile clove oil simulated solution 10L of 5.0g/L;
Second step is the double-deck stock chest 3 above-mentioned simulated solution being placed in ceramic membrane or metal film sorption and desorption device, by water bath with thermostatic control 7 by simulated solution constant temperature to 25 DEG C;
3rd step is for being 70,000 by molecular cut off, and length is the TiO of 22cm
2film is arranged on being sealed in cylindrical stainless steel enrichment case of membrane module 1, and stainless steel enrichment case two ends are connected with stainless steel pipes;
4th step ON cycle pump 2, regulate Pressure gauge 5, pressure is adjusted to 0.25Mpa, circulate under crossflow velocity is 2m/s and 25 DEG C condition, every 10min in the process of circulation, by the penetrating fluid in penetrating fluid stock chest 4 down in double-deck stock chest 3, after circulation 24h, volatile clove oil absorption reaches balance;
5th step for sample 10ml from double-deck stock chest 3, and extraction into ethyl acetate, measures according to following chromatographic condition: chromatographic column is XE-60 fused-silica capillary column (20% cyanoethyl silicon rubber, 20.0 m × 0.53 mm, 0.25 μm); Detector: hydrogen flame ionization detector (FID); Detector temperature: 180 DEG C; Carrier gas is gas, flow rate of carrier gas: 1.0mL/min; Split ratio is 25:1; Temperature programming: 40 DEG C continue 3 min, then rise to 180 DEG C with the speed of 20 DEG C/min, continue 1 min, sampling volume: 1 μ L at 180 DEG C.Adopt finger-print peak area method, the volatile clove oil concentration calculated in the rear sample solution of absorption is 3.0g/l, and adsorbance is 2g;
6th step is by TiO
2film takes off, and ceramic membrane or metal film sorption and desorption device is cleaned up with distilled water, by the poly-TiO after absorption
2film is reinstalled on ceramic membrane or metal film sorption and desorption device;
7th step is be that the ethanolic sodium hydroxide stripping workshop 2 liters of 10% of 0.1mol/L is placed in the double-deck stock chest 3 of ceramic membrane or metal film sorption and desorption device by water bath with thermostatic control 7 constant temperature to 10 DEG C by concentration;
8th step is at 10 DEG C, and 0.01MPa and crossflow velocity are carry out desorb 60min under the condition of 0.5m/s, and in stripping liquid, the concentration of volatile clove oil remains unchanged;
9th step for get stripping liquid 10ml from double-deck stock chest 3, and according to the assay method in above-mentioned steps five, the concentration measuring volatile clove oil in stripping liquid is 0.90g/L, and desorption efficiency is 90%.
Embodiment 5: sorption and desorption method and the concrete steps of the sorption and desorption device of Chinese medicine volatile oil film are as follows:
The first step is be taken at the grass leaf sweetflag rhizome volatile oil 1.25ml that Nanjing Ze Lang Pharmaceuticals Ltd purchases to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is the volatile oil simulated solution 10L of 5g/L;
Second step is the double-deck stock chest 3 said extracted liquid being placed in ceramic membrane or metal film sorption and desorption device, by water bath with thermostatic control 7 by simulated solution constant temperature to 25 DEG C;
3rd step is for being 70,000 by molecular cut off, and length is the SiO of 22cm
2film be sealed in membrane module 1 in cylindrical stainless steel enrichment case, stainless steel enrichment case two ends are connected with stainless steel pipes 9;
4th step ON cycle pump 2, regulate Pressure gauge 5, pressure is adjusted to 0.25Mpa, circulate under crossflow velocity is 2m/s and 25 DEG C condition, every 10min in the process of circulation, by the penetrating fluid in penetrating fluid stock chest 4 down in double-deck stock chest 3, after circulation 24h, Essential Oil of Acorus tatarinowii absorption reaches balance;
5th step for sample 10ml from double-deck stock chest 3, and extraction into ethyl acetate, measures according to following chromatographic condition: chromatographic column is XE-60 fused-silica capillary column (20% cyanoethyl silicon rubber, 20.0 m × 0.53 mm, 0.25 μm); Detector: hydrogen flame ionization detector (FID); Detector temperature: 180 DEG C; Carrier gas is gas, flow rate of carrier gas: 1.0mL/min; Split ratio is 25:1; Temperature programming: 40 DEG C continue 3 min, then rise to 180 DEG C with the speed of 20 DEG C/min, continue 1 min, sampling volume: 1 μ L at 180 DEG C.Adopt finger-print peak area method, the Essential Oil of Acorus tatarinowii concentration calculated in the rear sample solution of absorption is 2.0g/l, and adsorbance is 3g;
6th step is by TiO
2film takes off, and ceramic membrane or metal film sorption and desorption device is cleaned up with distilled water, by the TiO after absorption
2film is reinstalled on ceramic membrane or metal film sorption and desorption device;
7th step is be that the ethanolic sodium hydroxide stripping workshop 2 liters of 10% of 0.2mol/L is placed in the double-deck stock chest 3 of ceramic membrane or metal film sorption and desorption device by water bath with thermostatic control 7 constant temperature to 20 DEG C by concentration;
8th step is at 20 DEG C, and 0.02MPa and crossflow velocity are carry out desorb 10min under the condition of 0.7m/s, and in stripping liquid, the concentration of Essential Oil of Acorus tatarinowii remains unchanged;
9th step for get stripping liquid 10ml from double-deck stock chest 3, and according to the assay method in above-mentioned steps five, the concentration measuring Essential Oil of Acorus tatarinowii in stripping liquid is 1.425g/L, and desorption efficiency is 95%.
Embodiment 6: sorption and desorption method and the concrete steps of the sorption and desorption device of Chinese medicine volatile oil film are as follows:
The first step is be taken at the Rhizoma Cyperi volatile oil 1gl that Nanjing Ze Lang Pharmaceuticals Ltd purchases to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is the Rhizoma Cyperi volatile oil simulated solution 10L of 4g/L;
Second step is the double-deck stock chest 3 above-mentioned simulated solution being placed in ceramic membrane or metal film sorption and desorption device, by water bath with thermostatic control by simulated solution constant temperature to 25 DEG C;
3rd step is for being 70,000 by molecular cut off, and the long SUS316 film for 22cm is sealed in the cylindrical stainless steel enrichment case of ceramic membrane or metal film assembly, and stainless steel enrichment case two ends are connected with stainless steel pipes 9;
4th step ON cycle pump 2, regulate Pressure gauge 5, pressure is adjusted to 0.25Mpa, circulate under crossflow velocity is 2m/s and 25 DEG C condition, every 10min in the process of circulation, by the penetrating fluid in penetrating fluid stock chest 4 down in double-deck stock chest 3, after circulation 24h, Rhizoma Cyperi volatile oil absorption reaches balance;
5th step for sample 10ml from double-deck stock chest 3, and extraction into ethyl acetate, measures according to following chromatographic condition: chromatographic column is XE-60 fused-silica capillary column (20% cyanoethyl silicon rubber, 20.0 m × 0.53 mm, 0.25 μm); Detector: hydrogen flame ionization detector (FID); Detector temperature: 180 DEG C; Carrier gas is gas, flow rate of carrier gas: 1.0mL/min; Split ratio is 25:1; Temperature programming: 40 DEG C continue 3 min, then rise to 180 DEG C with the speed of 20 DEG C/min, continue 1 min, sampling volume: 1 μ L at 180 DEG C.Adopt finger-print peak area method, the Rhizoma Cyperi volatile oil concentration calculated in the rear sample solution of absorption is 3.8g/L, and adsorbance is 2g;
Ceramic membrane or metal film sorption and desorption device, for be taken off by SUS316 film, clean up with distilled water by the 6th step, are reinstalled on ceramic membrane or metal film sorption and desorption device by the SUS316 film after absorption;
7th step is be that the ethanolic sodium hydroxide stripping workshop 2 liters of 15% of 0.4mol/L is placed in the double-deck stock chest 3 of ceramic membrane or metal film sorption and desorption device by water bath with thermostatic control 7 constant temperature to 30 DEG C by concentration;
8th step is at 30 DEG C, and 0.03MPa and crossflow velocity are carry out desorb 60min under the condition of 0.8m/s, and in stripping liquid, the concentration of Rhizoma Cyperi volatile oil remains unchanged;
9th step for get stripping liquid 10ml from double-deck stock chest 3, and according to the assay method in above-mentioned steps five, measuring Rhizoma Cyperi volatile oil concentration in stripping liquid is 0.95g/L, and desorption efficiency is 95%.
Embodiment 7: sorption and desorption method and the concrete steps of the sorption and desorption device of Chinese medicine volatile oil film are as follows:
The first step is be taken at the rascal volatile oil 0.25g that Nanjing Ze Lang Pharmaceuticals Ltd purchases to add in the beaker that 250ml distilled water is housed, and magnetic stirring apparatus stirs 3h, and setting mixing speed is 350rpm, and compound concentration is the volatile oil simulated solution 10L of 1g/L;
Second step is the double-deck stock chest 3 said extracted liquid being placed in ceramic membrane or metal film sorption and desorption device, by water bath with thermostatic control 7 by simulated solution constant temperature to 25 DEG C;
3rd step is for being 140,000 by molecular cut off, and the long SLS316L film for 22cm is sealed in the cylindrical stainless steel enrichment case of membrane module 1, and stainless steel enrichment case two ends are connected with stainless steel pipes 9;
4th step is ON cycle pump 2, regulate Pressure gauge 5, pressure is adjusted to 0.25Mpa, circulate under crossflow velocity is 2m/s and 25 DEG C condition, every 10min in the process of circulation, by the penetrating fluid in penetrating fluid stock chest 4 down in double-deck stock chest 3, after circulation 24h, the absorption of rascal volatile oil reaches balance;
5th step for sample 10ml from double-deck stock chest 3, and extraction into ethyl acetate, measures according to following chromatographic condition: chromatographic column is XE-60 fused-silica capillary column (20% cyanoethyl silicon rubber, 20.0 m × 0.53 mm, 0.25 μm); Detector: hydrogen flame ionization detector (FID); Detector temperature: 180 DEG C; Carrier gas is gas, flow rate of carrier gas: 1.0mL/min; Split ratio is 25:1; Temperature programming: 40 DEG C continue 3 min, then rise to 180 DEG C with the speed of 20 DEG C/min, continue 1 min, sampling volume: 1 μ L at 180 DEG C.Adopt finger-print peak area method, the rascal volatile oil concentration calculated in the rear sample solution of absorption is 0.75g/L, and adsorbance is 2.5g;
Ceramic membrane or metal film sorption and desorption device 2, for be taken off by SLS316L film, clean up with distilled water by the 6th step, are reinstalled on ceramic membrane or metal film sorption and desorption device 2 by the SLS316L film after absorption;
7th step is be that the ethanolic sodium hydroxide stripping workshop 2 liters of 10% of 0.4mol/L is placed in the double-deck stock chest 3 of ceramic membrane or metal film sorption and desorption device by water bath with thermostatic control 7 constant temperature to 25 DEG C by concentration;
8th step is at 25 DEG C, and 0.002MPa and crossflow velocity are carry out desorb 60min under the condition of 0.1m/s, and in stripping liquid, the concentration of rascal volatile oil remains unchanged;
9th step for get stripping liquid 10ml from double-deck stock chest 3, and according to the assay method in above-mentioned steps five, the concentration measuring rascal volatile oil in stripping liquid is 1.16g/L, and desorption efficiency is 93%.
Claims (2)
1. the sorption and desorption device of a Chinese medicine volatile oil film, it is characterized in that this device is by membrane module (1), circulating pump (2), double-deck stock chest (3), penetrating fluid stock chest (4), Pressure gauge (5), flowmeter (6), water bath with thermostatic control (7), peristaltic pump (8), stainless steel pipes (9) is made, wherein double-deck stock chest (3) is connected with circulating pump (2) by stainless steel pipes (9), be connected with Pressure gauge (5) by stainless steel pipes (9) again, be connected with membrane module (1) by stainless steel pipes (9) again, be connected with Pressure gauge (5) and flowmeter (6) respectively by stainless steel pipes (9) again, be connected with double-deck stock chest (3) by stainless steel pipes (9) again, penetrating fluid conveying stainless steel pipes (9) is had in membrane module (1) lower end, penetrating fluid stock chest (4) is placed in stainless steel pipes (9) below, water bath with thermostatic control (7) is connected with peristaltic pump (8) by silica gel hose (12), be connected with the chuck import (10) of double-deck stock chest (3) by silica gel hose (12) again, the JO (11) of double-deck stock chest (3) is connected with water bath with thermostatic control (7) by silica gel hose (12).
2. the sorption and desorption device of Chinese medicine volatile oil film according to claim 1, it is characterized in that described membrane module (1) is divided into organic plate film assembly, ceramic film component or metal film assembly, wherein organic plate film assembly is clipped between upper steel plate (15) and lower steel plate (18) by organic film (13), wherein upper steel plate (15) is inverted plate-like, the Pan Bi of axis has two holes, the short steel pipes with screw thread mouth is welded respectively in the position in hole, for import (16) and outlet (17), be connected with stainless steel pipes (9) respectively, the surface design of lower steel plate (18) has 6-12 road cast groove, per pass cast groove is all designed with a permeate flow and portals, all stainless steel pipes (9) is carried to be connected with the penetrating fluid of lower steel plate (18) bottom, upper and lower two steel plates add tightening seal by a circular iron hoop (19), ceramic film component or metal film assembly be by tubular ceramic film or tubular metal film (14) by upper-lower seal circle vertical seal in stainless steel enrichment case, stainless steel enrichment case upper and lower side is equipped with screw thread mouth, be connected with stainless steel pipes (9), there is a penetrating fluid delivery outlet lower end, side of stainless steel enrichment case, penetrating fluid, by stainless steel pipes (9), flows in penetrating fluid stock chest (4).
3. the sorption and desorption device of Chinese medicine volatile oil film according to claim 2, is characterized in that described organic film is poly (ether sulfone) film, PS membrane; Ceramic membrane is silicon oxide film, oxidation titanium film; Metal film is SUS316 film, SLS316L film.
4. use the sorption and desorption device of the Chinese medicine volatile oil film described in claim 1 to carry out a method for sorption and desorption, it is characterized in that sorption and desorption method step is as follows:
A. get appropriate volatile oil to add in the beaker that 250ml distilled water is housed, magnetic stirring apparatus stirs 3h, setting mixing speed is 350rpm, and compound concentration is 1-8g/L volatile oil simulated solution 10L;
B. the simulated solution of step a is placed in the double-deck stock chest (3) of sorption and desorption device, by water bath with thermostatic control (7) by a certain value within the scope of the simulated solution constant temperature in double-deck stock chest (3) 10-60 DEG C;
C. organic film (13) is clipped in up and down between two block plates of organic film assembly, separately by tubular ceramic film or tubular metal film (14) vertical seal in stainless steel enrichment case, by screw thread mouth, stainless steel enrichment case upper and lower side is connected with stainless steel pipes (9);
D. ON cycle pump (2), by stainless steel pipes (9) and Pressure gauge (5), simulated solution is transported to membrane module to adsorb, solution after absorption is by stainless steel pipes (9), Pressure gauge (5) and flowmeter (6) are transported in double-deck stock chest (3), the pressure regulating Pressure gauge (5) is 0.25Mpa, crossflow velocity is adsorb under 2m/s condition, every 10min, the penetrating fluid in penetrating fluid stock chest (4) is poured in double-deck stock chest (3) in adsorption process, after circulation 24h, volatile oil absorption reaches balance;
E. from double-deck stock chest (3), sample 10ml, adopt the solution concentration after gas chromatography determination absorption, compare with the concentration of absorption front simulation solution, obtain adsorbance;
F. organic film, ceramic membrane or metal film after absorption are taken off, with distilled water, sorption and desorption device is cleaned up, the film after absorption is reinstalled on sorption and desorption device;
G. be that the 10-20% ethanol alkaline solution of 0.1-0.5mol/L loads in double-deck stock chest (3) as strippant using concentration, got a certain value constant temperature in 10-60 DEG C of temperature range by water bath with thermostatic control (7);
H. at constant temperature, pressure is less than 0.05MPa and crossflow velocity carries out desorb 30min-1.5h under 0.1-1m/s range of condition, in stripping liquid, the concentration of volatile oil is constant;
I. from double-deck stock chest (3), get stripping liquid sample, measure the concentration of stripping liquid according to the assay method in step e, obtain desorption efficiency 90%-95%.
5. the method for sorption and desorption according to claim 4, is characterized in that the volatile oil described in step a is divided into light oil and heavy oil.
6. the method for sorption and desorption according to claim 5, is characterized in that light oil is Herba Schizonepetae volatile oil, rascal volatile oil, Rhizoma Cyperi volatile oil; Heavy oil is volatile clove oil, Essential Oil of Acorus tatarinowii.
7. the method for sorption and desorption according to claim 4, is characterized in that the strippant described in step g is NaOH.
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