CN104014161A - Bulk pharmaceutical chemical extraction liquid separation method - Google Patents
Bulk pharmaceutical chemical extraction liquid separation method Download PDFInfo
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- CN104014161A CN104014161A CN201310067029.7A CN201310067029A CN104014161A CN 104014161 A CN104014161 A CN 104014161A CN 201310067029 A CN201310067029 A CN 201310067029A CN 104014161 A CN104014161 A CN 104014161A
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- liquid
- hollow cavity
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Abstract
The invention relates to a bulk pharmaceutical chemical extraction liquid separation method and mainly solves the problem that the position of a separation layer of light-phase liquid and heavy-phase liquid after standing of extraction liquid cannot be quickly determined in the prior art. The method comprises the following steps: (a) arranging a buoyant liquid extraction device in an extraction tank, wherein the buoyant liquid extraction device comprises a hollow cavity and a liquid extraction pipe, the lower half part of the hollow cavity is concave, a concave space is formed, the liquid extraction pipe penetrates through the hollow cavity and is fixed with the hollow cavity through threads, and the length of the liquid extraction pipe extending into the concave space is adjusted through the threads; (b) connecting a flexible liquid extraction pipe to the liquid extraction pipe of the buoyant liquid extraction device, wherein the flexible liquid extraction pipe extends out of a tank from the position higher than the buoyant liquid extraction device; (c) when the light-phase liquid is siphoned, descending the buoyant liquid extraction device along with the descent of the liquid level of the light-phase liquid, and when the position of the buoyant liquid extraction device is fundamentally kept stationary, reaching an interface of the light-phase liquid and the heavy-phase liquid to stop extracting liquid. According to the technical scheme, the problem is well solved. The method can be applied to industrial production for bulk pharmaceutical chemical extraction liquid separation.
Description
Technical field
Originally the present invention relates to a kind of bulk drug extract separation method.
Background technology
Extraction is to use liquid extractant to process immiscible bi-component or Multi component with it, realizes the mass transfer separation process of component separation.The extraction process of bulk drug belongs to liquid-liquid extraction process.Certain component in selected separated from solvent liquid mixture for liquid-liquid extraction, solvent must be immiscible with the mixture liquid being extracted, there is optionally solvability, and the heat endurance that must have and chemical stability, and have less toxicity and corrosivity.
In traditional extraction and separation technology, for determining that extract gently divides aspect position with heavy phase, the layering situation and the color and luster thereof that need operating personnel by glass visor, to examine liquid at drain hole place change, and control by hand-guided baiting valve, thereby reach separated object.Obviously, this method, owing to entirely determining laminated fluid level position by artificial visual, for the unconspicuous extract of two-phase liquid shade deviation, will increase separated difficulty, likely produces mixed liquid phenomenon.
Summary of the invention
Technical problem to be solved by this invention is the problem that prior art cannot be determined the standing rear light phase liquid of extract and heavy phase liquid separating layer position fast, and a kind of new bulk drug extract separation method is provided.The method can be determined the separating layer position of the standing rear light phase liquid of extract and heavy phase liquid easily easily, thereby has facilitated operation, has improved separative efficiency, has reduced operate miss, has alleviated operating personnel's labour intensity.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of bulk drug extract separation method, comprising:
A) in extractor, be provided with buoyancy liquid taking device; Described buoyancy liquid taking device comprises hollow cavity 1 and liquid flowing tube 2; Hollow cavity 1 Lower Half is concavity, forms concavity space 23; Liquid flowing tube 2 is through hollow cavity 1; Liquid flowing tube 2 is fixing by screw thread 22 with hollow cavity 1, and regulates liquid flowing tube 2 to stretch into the length in concavity space 23 by screw thread 22;
B) on the liquid flowing tube 2 of buoyancy liquid taking device, be connected with and get liquid flexible pipe, get liquid flexible pipe from stretching out outside tank higher than buoyancy liquid taking device;
C), when the light phase liquid of siphon, buoyancy liquid taking device position is along with light phase liquid levels declines and declines; When buoyancy liquid taking device position keeps motionless substantially, arrive the interface of weight two-phase liquid, now can stop getting liquid.
In technique scheme, liquid flowing tube 2 preferred versions are for to pass from hollow cavity 1 center.Hollow cavity 1 preferred version is hollow semielliptical shape cavity or the hollow cylinder cavity with concavity space 23.The length L that the depth H in concavity space 23, liquid flowing tube 2 stretch into concavity space 23 is related to L=H – h – x, the height h three of buoyancy liquid taking device immersion liquid meets, and wherein x is adjustment coefficient, x=1～5mm, and preferable range is 2～4mm.
In the inventive method, because the light phase liquid of different material medicine extract is different from the proportion of heavy phase liquid, the degree of depth that liquid flowing tube 1 stretches into concavity space 23 can the buoyancy difference theory at light phase liquid and heavy phase liquid calculate by hollow cavity, and can regulate height by screw thread 22, thereby simple and easy definite two-phase interface.
The inventive method, by utilizing buoyancy liquid taking device different with suffered buoyancy in heavy phase liquid at light phase liquid, can go out separating layer position by simple judgment.When the light phase liquid of siphon, the hollow cavity body position of buoyancy liquid taking device is along with liquid level declines rapidly, when hollow cavity body position keeps motionless substantially, (hose length no longer changes, when supernatant flow is zero simultaneously), arrive the parting surface of light phase liquid and heavy phase liquid, now can stop getting liquid.Like this, without operating personnel, by blowing visor, observe parting liquid color and luster and change to judge whether weight liquid obtains separation, has both improved separative efficiency, has reduced operate miss, has alleviated again operating personnel's labour intensity, has obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the separated schematic diagram of prior art bulk drug extract.
Fig. 2 is the inventive method schematic diagram.
Fig. 3 is the sectional structure chart of one embodiment of the invention buoyancy liquid taking device used, and its hollow cavity is hollow cylinder cavity.
Fig. 4 is the sectional structure chart of another embodiment of the invention buoyancy liquid taking device used, and its hollow cavity is hollow semielliptical shape cavity.
In Fig. 1 and Fig. 2,4 is extract, and 5 is extractor, and 6 is heavy phase flow container, 7 is light phase flow container, 8 is buoyancy liquid taking device, and 9 and 13 is all glass visor, and 10,11 and 12 is all valve, 14 is light phase liquid, 15 is heavy phase liquid, and 16 is the parting surface of light phase liquid and heavy phase liquid, 81 for buoyancy liquid taking device with flexible pipe.
In Fig. 3 and Fig. 4,1 is hollow cavity, and 2 is liquid flowing tube, and 23 is concavity space, 22 is screw thread, and h is the height that buoyancy liquid taking device immerses liquid, and H is the height in concavity space 23, L is the length that liquid flowing tube 2 stretches into concavity space 23, the external diameter that R is hollow cavity, the internal diameter that r is hollow cavity.
In Fig. 1, extract 4 enters after extractor 5, and after being uniformly mixed and having staticly settled, weight two-phase liquid is according to density natural layering, then open light liquid outlet valve 10, light phase liquid 14 is put into light phase tank 7, pay close attention to the liquid color situation of change in visor 9 simultaneously, until weight two-phase liquid interface in extractor 16, arrive after visor, close immediately light liquid outlet valve 10, open heavy-fluid outlet valve 11, heavy-phase liquid 15 is put into heavy phase tank 6, thereby reach the separation of extract.
In Fig. 2, use buoyancy liquid taking device 8, utilize hollow cavity different with suffered buoyancy in heavy phase liquid at supernatant (light phase) parting surface, can go out separating layer position by simple judgment.When operation starts, the vacuum of opening light phase tank 7, light phase liquid is retracted to light phase tank 7 from buoyancy sampler 8 by flexible pipe 81.Along with the decline of extractor 5 interior liquid levels, buoyancy liquid taking device also constantly declines, and the length of flexible pipe 81 is elongated gradually.Now in visor 13, can be observed passing through of light phase liquid.When light phase Liquid extracting complete, when buoyancy liquid taking device 8 arrives two-phase interface 16, because the buoyancy of heavy phase liquid is greater than the gravity of buoyancy sampler 8, cause it no longer to decline, the length that now can be observed flexible pipe 81 no longer changes, no longer include liquid in visor 13 passes through, and can judge light phase liquid and extract completely, now can close light phase liquid outlet valve 12, open heavy-phase liquid outlet valve 13, the heavy-phase liquid in extractor 5 flows into heavy phase flow container 6.So far separated complete.
Buoyancy liquid taking device shown in Fig. 3 and Fig. 4 comprises hollow cavity 1 and liquid flowing tube 2, and hollow cavity 1 Lower Half is concavity, forms concavity space 23; Liquid flowing tube 2 is through hollow cavity 1; Liquid flowing tube 2 is fixing by screw thread 22 with hollow cavity 1, and regulates liquid flowing tube 2 to stretch out the length in concavity space 23 by screw thread 22.
Liquid flowing tube 2 stretches into the length in concavity space 23 and can determine according to the density of supernatant and heavy phase liquid.
Take hollow cylinder cavity as example, and in the time of among buoyancy liquid taking device is positioned at liquid, its volume of discharging liquid is: V=л * (R
2-r
2) * h, the quality of discharging liquid is: W=V* ρ=л * (R
2-r
2) * h* ρ (density that ρ is liquid, V is for discharging liquid volume, and g is acceleration of gravity, 9.8m/s
2).According to Archimedes' principle, the buoyancy F that object is subject in liquid equates with the gravity G that this object is discharged liquid, i.e. G=F=Wg=л * h* (R
2-r
2) * ρ * g, now reaching stress balance, this object will float on liquid.
From formula, when liquid taking device one timing, its weight W, inside and outside radius R and the r of hollow cavity are constant, and its height h that immerses liquid is relevant with the density p of this liquid.According to formula, convert known:
h＝G/л**(R
2-r
2)*ρ。
Be provided with the liquid of two kinds of different densities, light liquid and heavy-fluid, its density is respectively ρ 1 and ρ 2, and the immersion depth of liquid taking device in two kinds of liquid is respectively h1 and h2, as shown from the above formula, when ρ 2> ρ 1, because G is a constant,
h1>h2。
Hence one can see that, and the buoyancy size being subject in the liquid of two kinds of different densities by calculating buoyancy liquid taking device can calculate the height L that liquid flowing tube stretches out concavity space 23.Its correlation is L=H-h2-x.Wherein x is liquid level adjusted value, by minute performance of interlayer and the liquid fluctuating factor of two-phase liquid, determined, be the yield that guarantees separating effect and liquid, the span of x between 1～5mm, optimum range 2～4mm.
The advantage of hollow semielliptical shape cavity is to have adopted surface modeling, and liquid is difficult for residual, easy to clean.But the buoyancy calculations more complicated of hollow semielliptical shape cavity, Computing Principle is with hollow cylinder cavity.
Below by embodiment, the present invention is further elaborated.
The specific embodiment
[embodiment 1]
Adopt method raw materials for production medicine intermediate first semi-annular jade pendant acid esters shown in Fig. 2.Methyl semi-annular jade pendant acyl chlorides, triethylamine, triazole compounds fine work add retort, carry out the reaction of first semi-annular jade pendantization.Reacted mixed liquor adds water, then staticly settle, upper strata water discards, the organic heavy-phase liquid of lower floor adds crystallization under ethanol low temperature to obtain crude product again, through centrifugation, after dry, makes first semi-annular jade pendant acid esters crude product.
Adopt the buoyancy sampler shown in Fig. 3 to carry out separation.The upper light liquid of first semi-annular jade pendant acid esters layering liquid is water, density p 1=1000kg/m
3, the density p 2=1200kg/m of heavy-phase liquid
3, R=0.15m, r=0.05m, buoyant device weight W is 2kg, according to formula:
H=G/ л * * (R
2-r
2) * ρ is known:
h1=2/3.14*（0.15
2-0.05
2）*1000＝0.032m。
h2=2/3.14*（0.15
2-0.05
2）*1200＝0.027m。
Depth H=the 50mm in concavity space.Adjust coefficient x=2mm, liquid flowing tube stretches out the height L in concavity space and is:
L＝H–h2–x＝50–27–2＝21mm。
Liquid flowing tube 22 tops are connected with gets liquid flexible pipe, and when siphon supernatant, hollow cavity body position, along with liquid level declines rapidly, when hollow cavity body position keeps motionless substantially, arrives supernatant parting surface, now stops getting liquid.
Because methyl semi-annular jade pendant acyl chlorides is acid, the pH of whole reactant liquor is less than 7, so this buoyancy sampler and flexible pipe thereof are nonmetallic materials preparations (as ABS).
[embodiment 2]
Adopt the crude product of method raw materials for production medicine Itraconazole shown in Fig. 2.Intermediate hydroxylic species and and first semi-annular jade pendant acyl ester add respectively retort, under toluene, water, NaOH exist, carry out associated reaction, reactant liquor is divided into upper toluene Ceng He lower floor aqueous layer.Add after water washing toluene layer, lower floor's aqueous layer is emitted.Upper toluene layer to crystallizing tank carries out crystallization, separation, obtains the crude product of Itraconazole after dry.
Adopt the toluene layer that extracts upper strata shown in Fig. 4 with the buoyancy liquid taking device of oval cavity.The density p 1=800kg/m of toluene layer
3, the about ρ=1050kg/m of density of aqueous layer
3, R=0.15m, r=0.05m, the weight of buoyant device is 2kg, calculates h1=40mm, h2=30mm by above-mentioned same way.
Depth H=the 50mm in concavity space.Adjust coefficient x=2mm, liquid flowing tube stretches out the height L in concavity space and is:
L＝H–h2–x＝50–30–2＝18mm。
Due to reactant liquor meta-alkalescence, so make this buoyancy liquid taking device with stainless steel, joint face system is made curved surface, prevents fluid accumulation, is convenient to clean.
[comparative example 1]
Adopt the separated methyl semi-annular jade pendant acyl ester reactant liquor of method shown in Fig. 1 or Itraconazole associated reaction liquid, need operating personnel constantly to observe vomit pipe visor, in case light phase waste water layer enters heavy phase liquid, reduce separative efficiency, or carry heavy-phase liquid secretly while extracting light phase liquid and enter.And because reactant liquor shade deviation is not obvious, be difficult to judgement layering position, can cause unavoidably weight phase liquid batch mixing.And adopt the buoyancy liquid taking device shown in Fig. 3 or Fig. 4, after having staticly settled, buoyancy liquid taking device can rest in liquid interface automatically according to the difference of two-phase fluid density, thereby has avoided the phenomenon of batch mixing again after extract separation.
Claims (5)
1. a bulk drug extract separation method, comprising:
A) in extractor, be provided with buoyancy liquid taking device; Described buoyancy liquid taking device comprises hollow cavity (1) and liquid flowing tube (2); Hollow cavity (1) Lower Half is concavity, forms concavity space (23); Liquid flowing tube (2) is through hollow cavity (1); Liquid flowing tube (2) is fixing by screw thread (22) with hollow cavity (1), and regulates liquid flowing tube (2) to stretch into the length of concavity space (23) by screw thread (22);
B) on the liquid flowing tube of buoyancy liquid taking device (2), be connected with and get liquid flexible pipe, get liquid flexible pipe from stretching out outside tank higher than buoyancy liquid taking device;
C), when the light phase liquid of siphon, buoyancy liquid taking device position is along with light phase liquid levels declines and declines; When buoyancy liquid taking device position keeps motionless substantially, arrive the interface of weight two-phase liquid, now can stop getting liquid.
2. bulk drug extract separation method according to claim 1, is characterized in that liquid flowing tube (2) passes from hollow cavity (1) center.
3. bulk drug extract separation method according to claim 1, is characterized in that hollow cavity (1) is for having hollow semielliptical shape cavity or the hollow cylinder cavity in concavity space (23).
4. bulk drug extract separation method according to claim 1, it is characterized in that height h three that the depth H of concavity space (23), length L that liquid flowing tube (2) stretches into concavity space (23), buoyancy liquid taking device immerse liquid meets is related to L=H – h – x, wherein x is for adjusting coefficient, x=1～5mm.
5. bulk drug extract separation method according to claim 4, is characterized in that x=2～4mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310067029.7A CN104014161A (en) | 2013-03-01 | 2013-03-01 | Bulk pharmaceutical chemical extraction liquid separation method |
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|---|---|---|---|
| CN201310067029.7A CN104014161A (en) | 2013-03-01 | 2013-03-01 | Bulk pharmaceutical chemical extraction liquid separation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104623928A (en) * | 2015-02-10 | 2015-05-20 | 右江民族医学院 | Liquid-liquid separation chromatography device |
| CN105457340A (en) * | 2015-12-09 | 2016-04-06 | 榆林学院 | Device for extracting oil from oil-water mixture |
| CN107557150A (en) * | 2017-08-31 | 2018-01-09 | 贵州南方嘉木食品有限公司 | A kind of tea seed oil purifying technique |
| CN111467873A (en) * | 2020-05-26 | 2020-07-31 | 唐山三友硅业有限责任公司 | Methylsiloxane dewatering and impurity removing process and device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104623928A (en) * | 2015-02-10 | 2015-05-20 | 右江民族医学院 | Liquid-liquid separation chromatography device |
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| CN105457340A (en) * | 2015-12-09 | 2016-04-06 | 榆林学院 | Device for extracting oil from oil-water mixture |
| CN107557150A (en) * | 2017-08-31 | 2018-01-09 | 贵州南方嘉木食品有限公司 | A kind of tea seed oil purifying technique |
| CN107557150B (en) * | 2017-08-31 | 2021-02-02 | 贵州南方嘉木食品有限公司 | Tea seed oil purification process |
| CN111467873A (en) * | 2020-05-26 | 2020-07-31 | 唐山三友硅业有限责任公司 | Methylsiloxane dewatering and impurity removing process and device |
| CN111467873B (en) * | 2020-05-26 | 2024-05-24 | 唐山三友硅业股份有限公司 | Methyl siloxane dehydration and impurity removal process and equipment |
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Application publication date: 20140903 |