CN201815300U - Reactor for producing diazomethane in batch continuously and safely - Google Patents
Reactor for producing diazomethane in batch continuously and safely Download PDFInfo
- Publication number
- CN201815300U CN201815300U CN2010202348666U CN201020234866U CN201815300U CN 201815300 U CN201815300 U CN 201815300U CN 2010202348666 U CN2010202348666 U CN 2010202348666U CN 201020234866 U CN201020234866 U CN 201020234866U CN 201815300 U CN201815300 U CN 201815300U
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- Prior art keywords
- diazomethane
- reaction
- reaction center
- cavity
- reactor
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- 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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- YXHKONLOYHBTNS-UHFFFAOYSA-N Diazomethane Chemical compound C=[N+]=[N-] YXHKONLOYHBTNS-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000002826 coolant Substances 0.000 claims abstract description 18
- 239000002699 waste material Substances 0.000 claims abstract description 18
- 230000005587 bubbling Effects 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 22
- 230000008676 import Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000004880 explosion Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 239000007789 gas Substances 0.000 description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002777 nucleoside Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- -1 diazomethane-O methyl Chemical group 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 230000005195 poor health Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a reactor for producing diazomethane in batch continuously and safely, which comprises a cavity, a reacting center I, a reacting center II, materials A and B, a dripping port, an N2 inlet air bubbling tube, a diazomethane outlet tube, a cooling jacket, a cooling medium inlet, a cooling medium outlet, a waste liquor draining tube, wherein the cavity comprises an upper seal head, a reactor wall and a lower seal head. The reactor for producing diazomethane in batch continuously and safely has the advantages of having simple structure, being capable of realizing continuous mass production, and directly using diazomethane without storage in the premise of reducing potential explosion risks.
Description
(1) technical field:
The utility model relates to a kind of chemical reactor, particularly a kind of mass continuous safe production diazomethane reactor.
(2) background technology:
The diazomethane chemical formula is CH
2N
2, character is very active, and polytype reaction can take place, and is important reagent in organic synthesis, is mainly used in organic synthesis intermediate (methyl substituted agent), also is used to produce the methylene Cabbeen.The boiling point of liquid diazomethane is-23 ℃, and diazomethane can be dissolved in ether, and its diethyl ether solution is more stable, the normal diethyl ether solution that uses diazomethane on synthesizing.
Owing to diazomethane severe toxicity and blast easily, therefore when preparing and using it, pay special attention to safety.The obstacle of industrial production diazomethane is:
1. diazomethane instability, explosive can not long preservation, should drop into next reaction after the preparation immediately, meets light, meets acid, meets matsurface, excessive concentration all can set off an explosion.
2. diazomethane is poisonous can be carcinogenic, sucks diazomethane, and skin or eye contact diazomethane all be poisonous (TLV 0.2ppm), symptom comprise heart discomfort, headache, in poor health, be short of physical strength, can cause the people when serious and faint.Its harmfulness assessment is as follows:
| The gas title | LD50(mg/kg) | LC50(mg/m 3) | Maximum permissible concentration (mg/m in the air 3) | Remarks |
| Diazomethane | 380 (rat orals) | 200 | (0.4 the former Soviet Union) | Carcinogenic, teratogenesis |
Point out among the patent US5459243, utilize the preliminary Synthetic 2 of diazomethane-O methyl (or ethyl)-1,3,5-tri-benzoyl-α-D-ribose, and then Synthetic 2-O-methyl-pyridine nucleosides.Because the demand to 2-O-methyl-pyridine nucleosides grows with each passing day, this just needs the large-scale production diazomethane, to satisfy the demands.But the output of this device diazomethane is about 0.1mol (4.2g), can not satisfy industrial production and use, and be difficult to produce continuously.
Point out among the patent US5817778A, with the diethylene glycol ether of 40%-50%KOH as raw material A, the ether mixture of diazald is as raw material B, at 45 ℃ of-55 ℃ of following prepared in batches diazomethanes, by pipeline the gas diazomethane is transferred in-30 ℃ the condenser, collect the diazomethane liquid that condensation is got off with the container that diethyl ether solution is housed again, finally, obtain the ether mixture of diazomethane, and it is stored under-30 ℃ the temperature conditions, produce in the reactor of 12L～300 gallon, the output of every batch of diazomethane is 2.1 kilograms to 42.1 tons.But because the highly purified diazomethane liquid of this prepared in reaction, and need under the temperature of strictness, store, for having increased potential safety hazard in the industrial processes.
(3) summary of the invention:
The purpose of this utility model is to design a kind of diazomethane reaction device, its diazomethane gas of keeping the safety in production continuously, in enormous quantities, and diazomethane gas need not to store and directly use.
The technical solution of the utility model: a kind of diazomethane reaction device is characterized in that dripping mouth, N by cavity, reaction center I, reaction center II, raw material A, B
2Air inlet bubbling pipe, diazomethane escape pipe, cooling jacket, cooling medium import and export, waste liquid discharge pipe are formed, and said cavity is made up of upper cover, reactor wall, low head.
Said upper cover top is provided with raw material A, B drips mouth, N
2Air inlet bubbling pipe and diazomethane escape pipe; Said reaction center I, reaction center II are in cavity, and wherein the reaction center I is positioned at the cavity internal upper part, and the reaction center II is positioned at the cavity inner bottom part; Said reaction center II is connected with low head, and the low head place is provided with the waste liquid discharge pipe; Said reactor wall built-in cooling jacket, the chuck upper and lower part is provided with the cooling medium import and export respectively.
Said raw material A is diazald (diazald), and raw material B is NaOH.
At least comprise a reaction center I in the said cavity.
Said reaction center I connects a N at least
2The air inlet bubbling pipe.
Said waste liquid discharge pipe can be manually or is got rid of waste liquid automatically.
The rate of addition of said raw material A diazald is 10～300ml/min, and the diazomethane gas of generation is 1: 1 with raw material diazald mol ratio in theory, but is about 1: 2 in the actual production process; Rate of addition 100～300ml/min of said NaOH, the concentration of NaOH solution is 5～20%, the ratio that nitrogen adds is 80%～95%.
The course of work of the present utility model:
(1) diazald from raw material A drip mouthful, NaOH drips from raw material B that mouth enters in the reaction center I in the reactor cavity contact and reaction generates diazomethane;
(2) reactant liquor in the reaction center I slowly flows into the reaction center II from the top overfall, still continues between the uncompleted raw material of reaction to interact in this process to generate diazomethane gas.
The effect of reaction center I and reaction center II is to increase the catalytic time, guarantee that reaction is more abundant, in whole synthesis process, play continuous feed, discharging, make continuously preparation diazomethane gas of this device, and as the source of the gas of next step synthetic reaction.
Said N
2The air inlet bubbling pipe is a nitrogen inlet, plays bubbling and stirs, and nitrogen is sent as an envoy to the diazomethane gas safety belt of being produced simultaneously, and it carries out subsequent reactions.
Said cooling medium adds by the cooling medium inlet of cooling jacket, and the cooling medium outlet is discharged, thereby makes reaction maintain required temperature.
Show that by the experimental data that is accumulated unreacted material rate content is very little in the liquid in the reaction center II.Include the diazomethane of few raw material, solvent, dissolving, another product of this reaction in the reaction residue, the utility model directly enters this raffinate to destroy in the sealing waste liquid tank that acetate is housed by the waste liquid discharge pipe and handles.
Superiority of the present utility model is: reducing under the situation of hidden peril of explosion, apparatus structure is simple, and can realize in enormous quantities, the production of serialization, need not to store and directly use diazomethane.Through calculating, the reaction unit volume in the utility model is 20L, and diazomethane gas accounts for 5%～20%, and therefore, the instantaneous diazomethane gas flow that remains in this reactor has only 0.05～0.18mol, has increased security greatly.
(4) description of drawings:
Fig. 1 is the structural representation of the related a kind of diazomethane reaction device of the utility model.
Wherein, 1 is the reaction center I, and 2 is the reaction center II, and 3 for raw material A drips mouth, and 4 is that raw material B drips mouth, and 5 is the diazomethane escape pipe, and 6 is N
2The air inlet bubbling pipe, 7 is upper cover, and 8 is reactor wall, and 9 are the cooling medium outlet, and 10 is cavity, and 11 is the waste liquid discharge pipe, and 12 is low head, and 13 is cooling jacket, and 14 is cooling medium inlet, and the direction of arrow is the flooding process of reactant liquor.
(5) specific embodiment:
Embodiment: a kind of diazomethane reaction device (see figure 1) is characterized in that dripping mouth 3, raw material B dropping mouth 4, N by cavity 10, reaction center I 1, reaction center II 2, raw material A
2Air inlet bubbling pipe 6, diazomethane escape pipe 5, cooling jacket 13, cooling medium inlet 14, cooling medium outlet 9, waste liquid discharge pipe 11 are formed.
Said cavity 10 is made up of upper cover 7, reactor wall 8, low head 12, and said upper cover 7 tops are provided with raw material A and drip mouth 3, raw material B dropping mouth 4, N
2Air inlet bubbling pipe 6 and diazomethane escape pipe 5; Said reaction center I 1, reaction center II 2 are in cavity 10, and wherein reaction center I 1 is positioned at cavity 10 internal upper parts, and reaction center II 2 is positioned at cavity 10 inner bottom parts; Said reaction center II 2 is connected with low head 12, and low head 12 places are provided with waste liquid discharge pipe 11; Said reactor wall 8 built-in cooling jackets 13, chuck upper and lower part are provided with cooling medium inlet 14, cooling medium outlet 9 respectively.
Said raw material A is diazald (diazald), and raw material B is NaOH.
At least comprise a reaction center I 1 in the said cavity 10.
Said reaction center I 1 connects a N at least
2The air inlet bubbling pipe.
Said waste liquid discharge pipe 11 can be manually or is got rid of waste liquid automatically.
The rate of addition of said raw material A diazald is 100ml/min, and the diazomethane gas of generation and raw material diazald mol ratio are 1: 2; The rate of addition 150ml/min of said NaOH, the concentration of NaOH solution is 15%, the ratio that nitrogen adds is 90%.
The course of work of the present utility model:
(1) diazald from raw material A drip mouthful, NaOH drips from raw material B that mouth enters in the reaction center I 1 in the reactor cavity contact and reaction generates diazomethane;
(2) reactant liquor in the reaction center I 1 slowly flows into reaction center II 2 from the top overfall, still continues between the uncompleted raw material of reaction to interact in this process to generate diazomethane gas.
The effect of reaction center I 1 and reaction center II 2 is to increase the catalytic time, guarantee that reaction is more abundant, in whole synthesis process, play continuous feed, discharging, make continuously preparation diazomethane gas of this device, and as the source of the gas of next step synthetic reaction.
Said N
2The air inlet bubbling pipe is a nitrogen inlet, plays bubbling and stirs, and nitrogen is sent as an envoy to the diazomethane gas safety belt of being produced simultaneously, and it carries out subsequent reactions.
Said cooling medium adds by the cooling medium inlet of cooling jacket, and the cooling medium outlet is discharged, thereby makes reaction maintain required temperature.
Show that by the experimental data that is accumulated unreacted material rate content is very little in the liquid in the reaction center II 2.Include the diazomethane of few raw material, solvent, dissolving, another product of this reaction in the reaction residue, the utility model directly enters this raffinate to destroy in the sealing waste liquid tank that acetate is housed by the waste liquid discharge pipe and handles.
Claims (4)
1. a diazomethane reaction device is characterized in that dripping mouth, N by cavity, reaction center I, reaction center II, raw material A, B
2Air inlet bubbling pipe, diazomethane escape pipe, cooling jacket, cooling medium import and export, waste liquid discharge pipe are formed, and said cavity is made up of upper cover, reactor wall, low head; Said upper cover top is provided with raw material A, B drips mouth, N
2Air inlet bubbling pipe and diazomethane escape pipe; Said reaction center I, reaction center II are in cavity, and wherein reaction center I is positioned at the cavity internal upper part, and reaction center II is positioned at the cavity inner bottom part; Said reaction center II is connected with low head, and the low head place is provided with the waste liquid discharge pipe; Said reactor wall built-in cooling jacket, the chuck upper and lower part is provided with the cooling medium import and export respectively.
2. according to a kind of diazomethane reaction device described in the claim 1, it is characterized in that comprising at least in the said cavity reaction center I.
3. according to a kind of diazomethane reaction device described in the claim 1, it is characterized in that said reaction center I connects a N at least
2The air inlet bubbling pipe.
4. according to a kind of diazomethane reaction device described in the claim 1, it is characterized in that said waste liquid discharge pipe can be manually or get rid of waste liquid automatically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202348666U CN201815300U (en) | 2010-06-24 | 2010-06-24 | Reactor for producing diazomethane in batch continuously and safely |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202348666U CN201815300U (en) | 2010-06-24 | 2010-06-24 | Reactor for producing diazomethane in batch continuously and safely |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201815300U true CN201815300U (en) | 2011-05-04 |
Family
ID=43913272
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010202348666U Expired - Lifetime CN201815300U (en) | 2010-06-24 | 2010-06-24 | Reactor for producing diazomethane in batch continuously and safely |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201815300U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844063A (en) * | 2010-06-24 | 2010-09-29 | 凯莱英医药化学（天津）有限公司 | Mass continuous safe production diazomethane reactor and working method thereof |
-
2010
- 2010-06-24 CN CN2010202348666U patent/CN201815300U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844063A (en) * | 2010-06-24 | 2010-09-29 | 凯莱英医药化学（天津）有限公司 | Mass continuous safe production diazomethane reactor and working method thereof |
| CN101844063B (en) * | 2010-06-24 | 2013-09-25 | 凯莱英医药集团（天津）股份有限公司 | Mass continuous safe production diazomethane reactor and working method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: ASYMCHEM LABORATORIES (TIANJIN) CO., LTD. Free format text: FORMER NAME: KAILAIYING MEDICAL CHEMICAL(TIANJIN) CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 300457, No. six Dongting street, Seventh Street, Tianjin economic and Technological Development Zone Patentee after: Asymchem Medical Group (Tianjin) Inc. Address before: 300457, No. six Dongting street, Seventh Street, Tianjin economic and Technological Development Zone Patentee before: Kailaiying Medical Chemical (Tianjin) Co., Ltd. Address after: 300457, No. six Dongting street, Seventh Street, Tianjin economic and Technological Development Zone Patentee after: Asymchem Medical Group (Tianjin) Inc. Address before: 300457, No. six Dongting street, Seventh Street, Tianjin economic and Technological Development Zone Patentee before: Kailaiying Medical Chemical (Tianjin) Co., Ltd. |
|
| CX01 | Expiry of patent term |
Granted publication date: 20110504 |
|
| CX01 | Expiry of patent term |