CN207933311U - A kind of purification devices of chromatographically pure Loprazolam - Google Patents
A kind of purification devices of chromatographically pure Loprazolam Download PDFInfo
- Publication number
- CN207933311U CN207933311U CN201721510157.4U CN201721510157U CN207933311U CN 207933311 U CN207933311 U CN 207933311U CN 201721510157 U CN201721510157 U CN 201721510157U CN 207933311 U CN207933311 U CN 207933311U
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- Prior art keywords
- threeway
- receiving bottle
- recipient
- bottle
- section door
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- UTEFBSAVJNEPTR-RGEXLXHISA-N loprazolam Chemical compound C1CN(C)CCN1\C=C/1C(=O)N2C3=CC=C([N+]([O-])=O)C=C3C(C=3C(=CC=CC=3)Cl)=NCC2=N\1 UTEFBSAVJNEPTR-RGEXLXHISA-N 0.000 title claims abstract description 18
- 229960003019 loprazolam Drugs 0.000 title claims abstract description 18
- 238000000746 purification Methods 0.000 title claims abstract description 14
- HWJPHQNEWARZLH-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5-decafluoro-6,6-bis(trifluoromethyl)cyclohexane Chemical compound FC(F)(F)C1(C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C1(F)F HWJPHQNEWARZLH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 8
- 210000000621 bronchi Anatomy 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 210000004916 vomit Anatomy 0.000 claims description 4
- 230000008673 vomiting Effects 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052753 mercury Inorganic materials 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 14
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000004255 ion exchange chromatography Methods 0.000 abstract description 4
- 239000003480 eluent Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 238000010977 unit operation Methods 0.000 abstract description 3
- 238000005530 etching Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 239000012982 microporous membrane Substances 0.000 abstract description 2
- 239000012264 purified product Substances 0.000 abstract description 2
- -1 rectifying bottle Chemical compound 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 abstract 1
- 238000006467 substitution reaction Methods 0.000 abstract 1
- 238000005070 sampling Methods 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DDKLZGLANVCKAZ-UHFFFAOYSA-N C.[S] Chemical compound C.[S] DDKLZGLANVCKAZ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model is related to a kind of purification devices of chromatographically pure Loprazolam, including rectifying bottle, rectifying column, Rectification head, foreshot receiving bottle, positive fraction receiving bottle, miillpore filter nutsch filter and nutsch filter receiving bottle.The present apparatus is in such a way that rectification under vacuum unit operation and filtering with microporous membrane unit operation are carried out continuously, the disposable requirement solved to purified product content, purity, again by the deep-etching of products substitution after purification and the sulfuric acid polluted by force, not only acquisition absorbing liquid can be used as but also ion chromatography eluent can be used as, the two uniformly makes analytic process more stablize, and analysis data reappearance is good.
Description
Technical field
The utility model belongs to environmental protection tests fine chemicals purifier apparatus field, especially a kind of chromatography pure methane sulphur
The purification devices of acid.
Background technology
When being measured to pollutants in air, since concentration is low, it is required to preenrichment.The enrichment of gas generally uses two kinds of sides
Formula：Passive sampling and actively sampling.Passive sampling and actively sampling are required for carrying out solvent absorption to the air sample adopted, and make
Solvent claims absorbing liquid, common absorbing liquid to be generally sulfuric acid.Sulfuric acid is strong corrosive acid, and sampling carrier filter paper can be made sour
Solution, and remaining sulfuric acid treatment is extremely difficult, can cause environment pollution.
Loprazolam is the successful substitute of sulfuric acid, has the characteristics that acid weak and corrosivity is weak, carrier filter paper when sampling
It is not acid hydrolysis, environmental pollution is small.
At present in determination of the environment (including big gas and water) metal ion generally with the simple chromatography of ions, as Na+, K+,
The leacheate of Mg2+, Ca2+, NH4+ etc., these cationic measurement are generally the inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, inorganic acid
Background conductance it is smaller, influence the detection sensitivity of the chromatography of ions, therefore the chromatography of ions of general complex sample is generally not
Make leacheate using inorganic acid, it is exactly Loprazolam to begin to use organic acid, preferred organic acid.
In environmental analysis, Loprazolam is the absorbing liquid of sample collection, and is the leacheate of ion chromatography, therefore to first
The purity and content of alkyl sulfonic acid have high request, generally require chromatographically pure, and content is 99% or more, so preparing high-purity chromatography
Pure methane sulfonic acid is very important.
Utility model content
It is directly used as ion chromatography eluent for current general commercially available Loprazolam reagent, chromatogram spectrogram pole can be caused
The situation that limit is unstable, separation is deteriorated, impurity peaks are a lot of, the utility model provide a kind of purifying dress of chromatographically pure Loprazolam
It sets, the Loprazolam of the present apparatus after purification is chromatographically pure, effectively prevents the above problem.
The technical scheme adopted by the utility model is that：
A kind of chromatographically pure Loprazolam purification devices, including rectifying bottle, rectifying column, Rectification head, foreshot receiving bottle, just evaporate
Part receiving bottle, miillpore filter nutsch filter and nutsch filter receiving bottle；
The rectifying bottle is three-necked flask, and middle port connects rectifying column, and two side ports are respectively provided with the air inlet of regulating flow quantity
Pipe and the first thermometer, rectifying bottle are placed in heating mantle, Rectification head are terminated on rectifying column, Rectification head upper end is equipped with second temperature
Meter, Rectification head middle part are formed with the first connecting piece, and the mercury ball upper surface of second temperature meter is located at prolonging for the first connection tube hub line
On long line；
The first connecting piece other end is tightly connected a branch pipe of the first threeway distillation recipient, and the first threeway distillation receives
Branch pipe connects the first condenser above device, and the lower outlet of condenser extends in the first threeway distillation recipient；First threeway is distilled
Recipient lower branch line is connect with the second threeway distillation recipient, and centre is provided with section door；Recipient lower bottom part is distilled in second threeway
Center connects the second condenser；
Second condensator outlet is vertically downward, to connect 120 ° of threeway section doors, threeway section door one terminates foreshot receiving bottle, preceding
Fraction receiving bottle top has emptying section door, another termination vacuum reception pipe of threeway section door, the outlet of vacuum reception pipe to connect positive fraction and connect
Bottle is received, vacuum reception pipe is formed with a bronchus, and positive fraction receiving bottle top is provided with emptying section door, and bottom centre is provided with branch pipe
It is connect with miillpore filter nutsch filter, centre is provided with section door, and nutsch filter is connect with nutsch filter receiving bottle, nutsch filter receiving bottle top
It is provided with emptying section door, bottom centre is provided with the vomit pipe with section door；
The second connecting piece is connected between first condenser top and the second threeway distillation recipient, is made in the middle part of the second connecting piece
There are threeway section door, the second connecting piece lower part to be formed with a branch outlet, branch outlet and the bronchus vacuum of vacuum reception pipe are resistance to
Pressure pipe connects.
Moreover, being surrounded by heating and thermal insulation set outside filling glass θ annulated columns in the rectifying column.
Moreover, outlet is at the top of the first threeway distillation recipient under first condenser, slightly prominent Internal Spherical Surface, there are six
Spinule.
Moreover, the branch pipe one is protruded distills recipient inner top in the second threeway, it is punctured into and tilts down about 45 ° small
Mouth, direction distillate direction backwards to distillate.
Moreover, the miillpore filter nutsch filter is upper and lower two parts, centre is equipped with miillpore filter.
The advantages of the utility model and good effect:
1, the present apparatus organically combines rectification under vacuum unit operation and filtering with microporous membrane unit behaviour, can carry out continuously,
The disposable requirement solved to purified product content, purity, the present apparatus also have the advantages that easy to disassemble, cleaning, assembling.
2, the sulfuric acid that the chromatographically pure Loprazolam that the present apparatus obtains after purification is polluted instead of deep-etching and by force, can both make
Ion chromatography eluent, the two can be used as so that analytic process is more stablized, analyze data weight again for acquisition absorbing liquid
Existing property is good.
Description of the drawings
Fig. 1 is the structural schematic diagram of the utility model.
Specific implementation mode
It is described in further detail below in conjunction with the accompanying drawings and by specific embodiment to the utility model, following embodiment only describes
Property, it is not restrictive, protection scope of this utility model cannot be limited by this.
A kind of chromatographically pure Loprazolam purification devices, including rectifying bottle 1, rectifying column 2, Rectification head 3, foreshot receiving bottle 4,
Positive fraction receiving bottle 5, miillpore filter nutsch filter 6 and nutsch filter receiving bottle 7；
The rectifying bottle is three-necked flask, and middle port connects rectifying column, and two side ports are respectively provided with the air inlet of regulating flow quantity
Pipe 8 and the first thermometer 9, rectifying bottle are placed in heating mantle 25, and heating and thermal insulation set is surrounded by outside filling glass θ annulated columns in rectifying column
10, Rectification head 3 is terminated on rectifying column, Rectification head upper end is equipped with second temperature meter 12, the first connecting piece 11 is formed in the middle part of Rectification head,
The mercury ball upper surface of second temperature meter is located on the extended line of the first connection tube hub line, and pipe end is connected from first convenient for detection
The gas temperature that portion comes out.
The first connecting piece other end is tightly connected the branch pipe of the first threeway distillation recipient 13, and recipient is distilled in the first threeway
Top branch pipe connects the first condenser 14, and the lower outlet of condenser extends in the first threeway distillation recipient, slightly beyond interior ball
There are multiple spinules in face, is oozed convenient for condensed fluid dispersion；Recipient lower branch line is distilled in first threeway and the second threeway distillation receives
Device 15 connects, and centre is provided with section door 16；The lower branch line that recipient is distilled in first threeway is protruded in the second threeway distillation recipient
Inner top, is punctured into the smallmouth for tilting down about 45° angle, and direction distillates direction backwards to distillate；Second threeway distillation receives
Device lower bottom part center connects the second condenser 17, and the second condenser is tilted down with level about at 25 ° of angles.
Second condensator outlet is vertically downward, to connect 120 ° of threeway section doors 18, and threeway section door one terminates foreshot receiving bottle
4, foreshot receiving bottle top has emptying section door 19, another termination vacuum reception pipe 20 of threeway section door, the outlet of vacuum reception pipe to connect
Positive fraction receiving bottle, vacuum reception pipe are formed with a bronchus, and positive 5 top of fraction receiving bottle, which is provided with, is vented section door 21, in bottom
The heart is provided with branch pipe and is connect with miillpore filter nutsch filter 6, and centre is provided with section door 22, and miillpore filter nutsch filter is upper and lower two
Point, centre is equipped with miillpore filter.Miillpore filter nutsch filter lower part sub-export is up-small and down-big horn mouth, with nutsch filter receiving bottle
Connection, nutsch filter receiving bottle top are provided with emptying section door 23, and bottom centre is provided with the vomit pipe with section door 24, and vomit pipe connects
Enter in finished product receiving bottle.
The second connecting piece, the second connecting piece middle part are connected between first condenser top and the second threeway distillation recipient 15
It is formed with threeway section door 25, the second connecting piece lower part is formed with a branch outlet 26, and branch outlet and the bronchus of vacuum reception pipe are used
Vacuum pressure pipe 27 connects.
The operating procedure of the utility model is as follows：
1. closing all section doors of system, condenser (14) upper outlet is capped glass plug, condenser water flowing.
2. rectifying bottle (1) is added in industrial Loprazolam, threeway section door (18) leads to foreshot receiving bottle (4).Threeway section
Door (25) all-pass, accesses vacuum system.Air inlet pipe (8) charge flow rate is adjusted, bumping in bottle is prevented.
3. when system vacuum reaches 1.33kpa (10mmHg), rectifying bottle (1) heating.
4. infinite reflux 1 hour adjusts section door (16), between so that reflux ratio is kept 4.0-4.5, foreshot is collected.
5. when thermometer (12) reaches 165 DEG C, section door (18) is led into positive Fraction collection bottle (5) and collects positive fraction.
6. when the temperature varies, closing section door (16), threeway section door (18) leads to low fraction receiving bottle (4).
7. rectifying bottle (1) stops heating, 50 DEG C are cooled to hereinafter, increasing air inlet pipe (8) flow, detaches with vacuum system.
8. after positive fraction cooling, positive fraction receiving bottle (5) emptying section door (21) is opened, miillpore filter nutsch filter (6) is connect
Enter vacuum system, opens section door (22) and filter.
9. suction filtration terminates, detached with vacuum system.
10. opening the emptying section door (23) of nutsch filter receiving bottle (7), section door (24) is opened, releases finished product.
Claims (5)
1. a kind of purification devices of chromatographically pure Loprazolam, it is characterised in that：Including rectifying bottle, rectifying column, Rectification head, foreshot
Receiving bottle, positive fraction receiving bottle, miillpore filter nutsch filter and nutsch filter receiving bottle；
The rectifying bottle is three-necked flask, and middle port connects rectifying column, two side ports be respectively provided with regulating flow quantity air inlet pipe and
First thermometer, rectifying bottle are placed in heating mantle, and Rectification head is terminated on rectifying column, and Rectification head upper end is equipped with second temperature meter, essence
It evaporates centriciput and is formed with the first connecting piece, the upper surface of the mercury ball of second temperature meter is located at the extended line of the first connection tube hub line
On；
The first connecting piece other end is tightly connected a branch pipe of the first threeway distillation recipient, and the first threeway is distilled on recipient
Fang Zhiguan connects the first condenser, and the lower outlet of condenser extends in the first threeway distillation recipient；First threeway distillation receives
Device lower branch line is connect with the second threeway distillation recipient, and centre is provided with section door；Recipient lower bottom part center is distilled in second threeway
Connect the second condenser；
Second condensator outlet is vertically downward, to connect 120 ° of threeway section doors, and threeway section door one terminates foreshot receiving bottle, foreshot
Receiving bottle top has emptying section door, another termination vacuum reception pipe of threeway section door, the outlet of vacuum reception pipe to connect positive fraction receiving bottle,
Vacuum reception pipe is formed with a bronchus, and positive fraction receiving bottle top is provided with emptying section door, bottom centre be provided with branch pipe with it is micro-
Hole filter membrane nutsch filter connection, centre are provided with section door, and nutsch filter is connect with nutsch filter receiving bottle, the setting of nutsch filter receiving bottle top
There are emptying section door, bottom centre to be provided with the vomit pipe with section door；
The second connecting piece is connected between first condenser top and the second threeway distillation recipient, three are formed in the middle part of the second connecting piece
Logical section door, the second connecting piece lower part is formed with a branch outlet, the bronchus vacuum pressure pipe of branch outlet and vacuum reception pipe
Connection.
2. the purification devices of chromatographically pure Loprazolam according to claim 1, it is characterised in that：Filling in the rectifying column
It is surrounded by heating and thermal insulation set outside glass θ annulated columns.
3. the purification devices of chromatographically pure Loprazolam according to claim 1, it is characterised in that：Under first condenser
Outlet is at the top of the first threeway distillation recipient, and slightly prominent Internal Spherical Surface, there are six spinules.
4. the purification devices of chromatographically pure Loprazolam according to claim 1, it is characterised in that：The branch pipe one protrudes
Recipient inner top is distilled in second threeway, is punctured into and tilts down 45 ° of smallmouth, direction distillates direction backwards to distillate.
5. the purification devices of chromatographically pure Loprazolam according to claim 1, it is characterised in that：The miillpore filter filters
Device is upper and lower two parts, and centre is equipped with miillpore filter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721510157.4U CN207933311U (en) | 2017-11-14 | 2017-11-14 | A kind of purification devices of chromatographically pure Loprazolam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721510157.4U CN207933311U (en) | 2017-11-14 | 2017-11-14 | A kind of purification devices of chromatographically pure Loprazolam |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN207933311U true CN207933311U (en) | 2018-10-02 |
Family
ID=63644533
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721510157.4U Expired - Fee Related CN207933311U (en) | 2017-11-14 | 2017-11-14 | A kind of purification devices of chromatographically pure Loprazolam |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN207933311U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912580A (en) * | 2021-11-03 | 2022-01-11 | 瑞孚信江苏药业股份有限公司 | Method for purifying 4- (hydroxymethyl) -5-methyl- [1,3] dioxol-2-one |
-
2017
- 2017-11-14 CN CN201721510157.4U patent/CN207933311U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912580A (en) * | 2021-11-03 | 2022-01-11 | 瑞孚信江苏药业股份有限公司 | Method for purifying 4- (hydroxymethyl) -5-methyl- [1,3] dioxol-2-one |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181002 |
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| CF01 | Termination of patent right due to non-payment of annual fee |