CN106496160A - A kind of synthesis technique of N methyl nafoxidine - Google Patents
A kind of synthesis technique of N methyl nafoxidine Download PDFInfo
- Publication number
- CN106496160A CN106496160A CN201610912962.3A CN201610912962A CN106496160A CN 106496160 A CN106496160 A CN 106496160A CN 201610912962 A CN201610912962 A CN 201610912962A CN 106496160 A CN106496160 A CN 106496160A
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- catalyst
- ceramic ring
- synthesis technique
- methyl nafoxidine
- reactor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/023—Preparation; Separation; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/027—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring
- C07D295/03—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring with the ring nitrogen atoms directly attached to acyclic carbon atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of synthesis technique of N methyl nafoxidine, fixed bed reactors are heated to 300～400 DEG C, catalyst and ceramic ring are alternately stacked to reactor head, reactant tetrahydrofuran and monomethyl amine are passed through reactor from reactor head pipeline, and product N methyl nafoxidine is collected from reactor bottom pipeline.The invention has the advantages that：Catalyst and ceramic ring are alternately stacked air penetrability height, and porosity is good, is fully contacted can reactant and catalyst；Reduced by reactor resistance after material gasification, contacted fully with catalyst；Reduce reaction temperature.
Description
Technical field
The present invention relates to field of fine chemical, specifically a kind of synthesis technique of N- methyl nafoxidine.
Background technology
The conventional synthetic method of N- methyl nafoxidine be in the reactor directly loading catalyst to reactor head, with
Tetrahydrofuran and monomethyl amine are reactant, are heated to more than 400 DEG C, are passed directly in reactor and are reacted with catalyst.By
Directly stacked in catalyst in the reactor, when the gasification of reactant mixed material gas is by reactor, one is that resistance is big, and two are
Mixed material gas is insufficient contact with catalyst, is also easy to produce channeling；So that reaction temperature is improved, the conversion ratio of reaction
Reduce, increase production cost.
Therefore, the production of current N- methyl nafoxidine, the reaction temperature insufficient contact with catalyst that be faced with reactant
High, the low problem of reaction yield.
Content of the invention
For the problems referred to above, the present invention proposes a kind of synthesis technique of N- methyl nafoxidine, can make reactant and urge
Agent is fully contacted, and improves reaction yield.
The present invention is by the following technical programs, solves above-mentioned technical problem：
Fixed bed reactors are heated to 300～400 DEG C, and catalyst and ceramic ring are alternately stacked to reactor head, reactant
Tetrahydrofuran and monomethyl amine are passed through reactor from reactor head pipeline, and product N- methyl nafoxidine is from reactor bottom
Pipeline is collected.
Further, ceramic ring is laid on the reactor bottom, and catalyst is laid in ceramic ring, and the ceramic ring and catalyst are handed over
For stacking.
Further, bottom ceramic ring is laid on above flase floor.
Further, in order that product gasifies, and reaction temperature is reached, fixed bed reactors are preferably heated to 350
℃.
Further, the gas permeability of reactant gas, in order that reactant and catalyst fully react, is improved, and catalyst is every
Layer 40～60cm of stack thickness, every layer of 20～40cm of stack thickness of ceramic ring.
Further, per layer of catalyst preferably stack thickness 50cm, per layer of ceramic ring preferably stack thickness 30cm.
Further, in order that reactant reaction is complete, the mol ratio of reactant tetrahydrofuran and monomethyl amine is：1:1～
1:2.
Further, in order to improve the heat resistance and gas permeability of ceramic ring, ceramic ring is microporous activated ceramic ring.
Further, in order to improve reactivity, catalyst is metal type oxide or rare metal oxide catalyst.
Compared with prior art, the invention has the advantages that：Catalyst and ceramic ring are alternately stacked air penetrability height, and porosity is good,
It is fully contacted can reactant and catalyst；Reduced by reactor resistance after feed vaporization, contacted fully with catalyst；Drop
Low reaction temperature.
Description of the drawings
Fig. 1 is a kind of synthesis technique figure of N- methyl nafoxidine of the invention.
Specific embodiment
Below in conjunction with the concrete technical scheme that Fig. 1 and specific embodiment further describe the present invention, in order to this area
Technical staff be further understood from the present invention, and do not constitute the restriction to its right.
Embodiment 1
Fixed bed reactors 6 heat 350 DEG C, and ceramic ring 3 is laid on flase floor 1, and the thickness of the laying of ceramic ring 3 is 30cm,
The thick catalyst 2 of 50cm is laid in ceramic ring 3, and then the thick catalyst 2 of the thick ceramic rings 3 of 30cm and 50cm is alternately stacked to reactor
Top.
It is 1 by mol ratio:1 tetrahydrofuran and monomethyl amine, are passed through fixed bed reactors 6 from reactor head pipeline 5, Gu
High temperature in fixed bed reactor 6 makes reactant rapidly gasify, and reacts with catalyst 2, product N- methyl nafoxidine
Collect from reactor bottom pipeline 4.
Less by reactor, resistance after reactant gasification, contribute to the abundant reaction with catalyst；Catalyst and ceramic ring
Be alternately stacked, voidage is good, and air penetrability is good, contributes to reactant complete with catalyst reaction.
Embodiment 2
Fixed bed reactors 6 are heated to 300 DEG C, and ceramic ring 3 is laid on flase floor 1, and the thickness of the laying of ceramic ring 3 is
40cm, the thick catalyst 2 of laying 40cm in ceramic ring 3, then the thick catalyst 2 of the thick ceramic rings 3 of 40cm and 40cm be alternately stacked to
Reactor head.
It is 1 by mol ratio:1.5 tetrahydrofuran and monomethyl amine, are passed through fixed bed reactors 6 from reactor head pipeline 5,
High temperature in reactor reaction device 6 makes reactant rapidly gasify, and reacts with catalyst 2, product N- methyl tetrahydrochysene pyrrole
Cough up and collect from reactor bottom pipeline 4.
Less by reactor, resistance after reactant gasification, contribute to the abundant reaction with catalyst；Catalyst and ceramic ring
Be alternately stacked, voidage is good, and air penetrability is good, contributes to reactant complete with catalyst reaction.
Embodiment 3
Fixed bed reactors 6 are heated to 400 DEG C, and ceramic ring 3 is laid on flase floor 1, and the thickness of the laying of ceramic ring 3 is
20cm, the thick catalyst 2 of laying 60cm in ceramic ring 3, then the thick catalyst 2 of the thick ceramic rings 3 of 20cm and 60cm be alternately stacked to
Reactor head.
It is 1 by mol ratio:2 tetrahydrofuran and monomethyl amine, are passed through fixed bed reactors 6 from reactor head pipeline 5, Gu
High temperature in fixed bed reactor 6 makes reactant rapidly gasify, and reacts with catalyst 2, product N- methyl nafoxidine
Collect from reactor bottom pipe 4.
Less by reactor, resistance after reactant gasification, contribute to the abundant reaction with catalyst；Catalyst and ceramic ring
Be alternately stacked, voidage is good, and air penetrability is good, contributes to reactant complete with catalyst reaction.
The conversion ratio of the N- methyl nafoxidine reaction prepared using this technique can bring up to 90% by original 50%, with
When reaction temperature be down to 300-400 DEG C, reduce production cost.
Presently preferred embodiments of the present invention is the foregoing is only, not in order to limit the present invention, all in essence of the invention
Any modification, equivalent and improvement that is made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of synthesis technique of N- methyl nafoxidine, it is characterised in that：Fixed bed reactors are heated to 300～400 DEG C, urge
Agent and ceramic ring are alternately stacked to reactor head, and reactant tetrahydrofuran and monomethyl amine are passed through reaction from reactor head pipeline
Device, product N- methyl nafoxidine are collected from reactor bottom pipeline.
2. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that the ceramic ring is laid on
The reactor bottom, the catalyst are laid in ceramic ring, and the ceramic ring and catalyst are alternately stacked.
3. a kind of synthesis technique of N- methyl nafoxidine according to claim 2, it is characterised in that the bottom ceramic ring
It is laid on above flase floor.
4. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that per layer of the catalyst
40～60cm of stack thickness, every layer of 20～40cm of stack thickness of the ceramic ring.
5. a kind of synthesis technique of N- methyl nafoxidine according to claim 4, it is characterised in that per layer of the catalyst
It is preferred that stack thickness 50cm, per layer of the ceramic ring preferably stack thickness 30cm.
6. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that the fixed bed reaction
Device is preferably heated to 350 DEG C.
7. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that the reactant tetrahydrochysene
The mol ratio of furans and monomethyl amine is：1:1～1:2.
8. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that the ceramic ring is micropore
Active ceramic ring.
9. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that the catalyst is gold
Category type oxide or rare metal oxide catalyst.
10. a kind of synthesis technique of N- methyl nafoxidine according to claim 1, it is characterised in that the fixed bed is anti-
Device is answered to be heated to 300 DEG C, the ceramic ring laying depth is, 40cm, the catalyst laying depth is 40cm, the tetrahydrofuran
Mol ratio with monomethyl amine is 1:1.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610912962.3A CN106496160A (en) | 2016-10-20 | 2016-10-20 | A kind of synthesis technique of N methyl nafoxidine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610912962.3A CN106496160A (en) | 2016-10-20 | 2016-10-20 | A kind of synthesis technique of N methyl nafoxidine |
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| CN106496160A true CN106496160A (en) | 2017-03-15 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3595626A (en) * | 1968-11-14 | 1971-07-27 | Du Pont | Ceramic fillers and covers for packed beds |
| GB1511514A (en) * | 1974-05-09 | 1978-05-17 | Shell Bv | Process and apparatus for hydrotreating a liquid petroleum fraction |
| CN201529518U (en) * | 2009-05-13 | 2010-07-21 | 中国石油化工股份有限公司 | Gas-liquid-solid three-phase fixed bubbling column reactor |
| CN101912779A (en) * | 2010-08-03 | 2010-12-15 | 河北工业大学 | Catalyst for catalytic synthesis of N-methylpyrrolidine and application thereof |
| CN103785331A (en) * | 2012-11-05 | 2014-05-14 | 中国石油化工股份有限公司 | Catalyst unloading component |
| CN204816456U (en) * | 2015-07-14 | 2015-12-02 | 中国石油天然气股份有限公司 | Catalyst loads component |
-
2016
- 2016-10-20 CN CN201610912962.3A patent/CN106496160A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3595626A (en) * | 1968-11-14 | 1971-07-27 | Du Pont | Ceramic fillers and covers for packed beds |
| GB1511514A (en) * | 1974-05-09 | 1978-05-17 | Shell Bv | Process and apparatus for hydrotreating a liquid petroleum fraction |
| CN201529518U (en) * | 2009-05-13 | 2010-07-21 | 中国石油化工股份有限公司 | Gas-liquid-solid three-phase fixed bubbling column reactor |
| CN101912779A (en) * | 2010-08-03 | 2010-12-15 | 河北工业大学 | Catalyst for catalytic synthesis of N-methylpyrrolidine and application thereof |
| CN103785331A (en) * | 2012-11-05 | 2014-05-14 | 中国石油化工股份有限公司 | Catalyst unloading component |
| CN204816456U (en) * | 2015-07-14 | 2015-12-02 | 中国石油天然气股份有限公司 | Catalyst loads component |
Non-Patent Citations (2)
| Title |
|---|
| 王一军: "固定床一步法连续合成N-甲基四氢吡咯与工艺改进", 《精细化工原料及中间体》 * |
| 郑旭煦等 主编: "《化工原理》", 31 January 2016 * |
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