CN101844063A - Mass continuous safe production diazomethane reactor and working method thereof - Google Patents
Mass continuous safe production diazomethane reactor and working method thereof Download PDFInfo
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- CN101844063A CN101844063A CN201010207615.3A CN201010207615A CN101844063A CN 101844063 A CN101844063 A CN 101844063A CN 201010207615 A CN201010207615 A CN 201010207615A CN 101844063 A CN101844063 A CN 101844063A
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Abstract
The invention relates to a mass continuous safe production diazomethane reactor, which consists of a cavity body, a reaction center I, a reaction center II, a raw material A dripping port, a raw material B dripping port, a N2 air suction bubbling tube, a diazomethane discharging tube, a cooling jacket, a cooling medium inlet, a cooling medium outlet and a waste liquid discharging tube, wherein the cavity body consists of an upper seal end a reactor wall and a lower seal end. Working method comprises the following steps that: (1) diazald and NaOH enter the reaction center I inside the cavity body of the reactor respectively through the raw material A dripping port and the raw material B dripping port to be contacted and reacted with each other to generate diazomethane; (2) reaction liquid inside the reaction center I slowly flows into the reaction center II from an overflow port above the reaction center I, the raw materials which are not completely reacted are continuously reacted with each other to generate the diazomethane gas during the process. The reactor has the advantages that: under the condition that the explosion danger is reduced, the device has simple structure, mass and continuous production of the diazomethane can be realized, and the diazomethane is free from being stored and can be directly used.
Description
(1) technical field:
The present invention relates to a kind of diazomethane reaction device, particularly a kind of mass continuous safe production diazomethane reactor and method of work thereof.
(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 objective of the invention is to design a kind of mass continuous safe production diazomethane reactor and method of work thereof, its diazomethane gas of keeping the safety in production continuously, in enormous quantities, and diazomethane gas need not to store and directly use.
Technical scheme of the present invention: a kind of mass continuous safe production diazomethane reactor 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.
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 method of work of mass continuous safe production diazomethane reactor is characterized in that:
(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 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.
Inventive principle of the present invention is:
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 among the reaction center II.Include the diazomethane of few raw material, solvent, dissolving, another product of this reaction in the reaction residue, the present invention 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 invention 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 among the present invention 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 mass continuous safe production diazomethane reactor of the present invention.
Wherein, 1 is reaction center I, and 2 is 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 mass continuous safe production diazomethane reactor and method of work (see figure 1) thereof is characterized in that dripping mouth 3, raw material B dropping mouth 4, N by cavity 10, reaction center I1, reaction center II2, 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 I1, reaction center II2 are in cavity 10, and wherein reaction center I1 is positioned at cavity 10 internal upper parts, and reaction center II2 is positioned at cavity 10 inner bottom parts; Said reaction center II2 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 I1 in the said cavity 10.
Said reaction center I1 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 method of work of mass continuous safe production diazomethane reactor is characterized in that:
(1) diazald from raw material A drip mouthful, NaOH drips from raw material B that mouth enters in the reaction center I1 in the reactor cavity contact and reaction generates diazomethane;
(2) reactant liquor in the reaction center I1 slowly flows into reaction center II2 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 I1 and reaction center II2 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 among the reaction center II2.Include the diazomethane of few raw material, solvent, dissolving, another product of this reaction in the reaction residue, the present invention 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 (8)
1. a mass continuous safe production diazomethane reactor 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.
2. according to a kind of mass continuous safe production diazomethane reactor described in the claim 1, it is characterized in that 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.
3. according to a kind of mass continuous safe production diazomethane reactor described in the claim 1, it is characterized in that said raw material A is diazald (diazald), raw material B is NaOH.
4. according to a kind of mass continuous safe production diazomethane reactor described in the claim 1, it is characterized in that comprising at least in the said cavity reaction center I.
5. according to a kind of mass continuous safe production diazomethane reactor described in the claim 1, it is characterized in that said reaction center I connects a N at least
2The air inlet bubbling pipe.
6. according to a kind of mass continuous safe production diazomethane reactor 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.
7. according to a kind of mass continuous safe production diazomethane reactor described in the claim 1, the rate of addition that it is characterized in that said raw material A Diazald is 10～300ml/min, the diazomethane gas that generates 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%.
8. the method for work of mass continuous safe production diazomethane reactor is characterized in that:
(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 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.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467278A (en) * | 2013-09-25 | 2013-12-25 | 威海韩孚生化药业有限公司 | Preparation method and device of 2,4-dichlorphenoxyacetic acid |
| CN104045777A (en) * | 2013-03-11 | 2014-09-17 | 中国石油化工集团公司 | Post-treatment system and post-treatment method for monomer removing and deodorization in production of polymer polyol |
| CN104557606A (en) * | 2013-10-18 | 2015-04-29 | 中国石油化工股份有限公司 | Methylation method achieved through diazomethane |
| CN105418452A (en) * | 2015-11-09 | 2016-03-23 | 宜宾久凌化学有限公司 | Method and equipment for preparing diazomethane |
| WO2020232625A1 (en) | 2019-05-21 | 2020-11-26 | 凯莱英医药集团（天津）股份有限公司 | Process of preparing diazomethane |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5459243A (en) * | 1994-03-10 | 1995-10-17 | Isis Pharmaceuticals, Inc. | Apparatus and processes for the large scale generation and transfer of diazomethane |
| US5817778A (en) * | 1997-11-13 | 1998-10-06 | Aerojet-General Corporation | Large scale batch process for diazomethane |
| US5854405A (en) * | 1997-11-13 | 1998-12-29 | Aerojet-General Corporation | Continuous process for diazomethane from an n-methyl-n-nitrosoamine and from methylurea through n-methyl-n-nitrosourea |
| CN201815300U (en) * | 2010-06-24 | 2011-05-04 | 凯莱英医药化学（天津）有限公司 | Reactor for producing diazomethane in batch continuously and safely |
-
2010
- 2010-06-24 CN CN201010207615.3A patent/CN101844063B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5459243A (en) * | 1994-03-10 | 1995-10-17 | Isis Pharmaceuticals, Inc. | Apparatus and processes for the large scale generation and transfer of diazomethane |
| US5817778A (en) * | 1997-11-13 | 1998-10-06 | Aerojet-General Corporation | Large scale batch process for diazomethane |
| US5854405A (en) * | 1997-11-13 | 1998-12-29 | Aerojet-General Corporation | Continuous process for diazomethane from an n-methyl-n-nitrosoamine and from methylurea through n-methyl-n-nitrosourea |
| CN201815300U (en) * | 2010-06-24 | 2011-05-04 | 凯莱英医药化学（天津）有限公司 | Reactor for producing diazomethane in batch continuously and safely |
Non-Patent Citations (1)
| Title |
|---|
| 《Organic Process Research & Development》 20021029 Lee D.Proctor等 Development of a Continuous Process for the Industrial Generation of Diazomethane 884－892 1－8 第6卷, 第6期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045777A (en) * | 2013-03-11 | 2014-09-17 | 中国石油化工集团公司 | Post-treatment system and post-treatment method for monomer removing and deodorization in production of polymer polyol |
| CN104045777B (en) * | 2013-03-11 | 2018-08-31 | 中国石油化工集团公司 | For taking off single and deodorization after-treatment system and method in polymer polyol alcohol production |
| CN103467278A (en) * | 2013-09-25 | 2013-12-25 | 威海韩孚生化药业有限公司 | Preparation method and device of 2,4-dichlorphenoxyacetic acid |
| CN103467278B (en) * | 2013-09-25 | 2015-04-08 | 威海韩孚生化药业有限公司 | Preparation method and device of 2,4-dichlorphenoxyacetic acid |
| CN104557606A (en) * | 2013-10-18 | 2015-04-29 | 中国石油化工股份有限公司 | Methylation method achieved through diazomethane |
| CN105418452A (en) * | 2015-11-09 | 2016-03-23 | 宜宾久凌化学有限公司 | Method and equipment for preparing diazomethane |
| WO2020232625A1 (en) | 2019-05-21 | 2020-11-26 | 凯莱英医药集团（天津）股份有限公司 | Process of preparing diazomethane |
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Address after: 300457, No. six Dongting street, Seventh Street, Tianjin economic and Technological Development Zone Applicant after: Asymchem Medical Group (Tianjin) Inc. Address before: 300457, No. six Dongting street, Seventh Street, Tianjin economic and Technological Development Zone Applicant before: Kailaiying Medical Chemical (Tianjin) Co., Ltd. |
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