CN108947848A - A kind of nitrification installation and nitration processes method of o-nitrobenzaldehyde preparation - Google Patents
A kind of nitrification installation and nitration processes method of o-nitrobenzaldehyde preparation Download PDFInfo
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- CN108947848A CN108947848A CN201810891727.1A CN201810891727A CN108947848A CN 108947848 A CN108947848 A CN 108947848A CN 201810891727 A CN201810891727 A CN 201810891727A CN 108947848 A CN108947848 A CN 108947848A
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- pipeline
- reactant
- nitrobenzaldehyde
- spiral tube
- magnetic stirring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of nitrification installations of o-nitrobenzaldehyde preparation, including first flow pump, pipeline one, magnetic stirring apparatus, second flow pump, pipeline two, pipeline three, spiral tube exchanger, pipeline four and fluid reservoir, the first flow pump is connected to magnetic stirring apparatus by pipeline one；The second flow pump is connected to magnetic stirring apparatus by pipeline two；The magnetic stirring apparatus is connected to spiral tube exchanger by pipeline three；The spiral tube exchanger is connected to fluid reservoir by pipeline four.The invention also discloses a kind of nitration processes methods of o-nitrobenzaldehyde preparation.The present invention has the advantages that improving starting reaction speed；Continuous feed；Reaction time is short, and it is few to participate in reaction mass total amount；When occurring to have a power failure, cut off the water, stop the factors such as stirring, since reaction mass total amount is less in reaction unit, therefore risk of explosion will not occur；Pipeline reactor takes inline process, and device is small, and yield is big.
Description
Technical field
The present invention relates to a kind of pharmaceutical-chemical intermediates, and in particular to a kind of nitrification installation of o-nitrobenzaldehyde preparation and
Nitration processes method.
Background technique
O-nitrobenzaldehyde is yellowish solid, 41-43 DEG C of fusing point, not soluble in water, is soluble in alcohol, ether, aromatic hydrocarbons, halogenated
The organic solvents such as hydrocarbon, ester.O-nitrobenzaldehyde molecular formula is C7H5NO3, relative molecular mass 151.1.O-nitrobenzaldehyde
Chemical structural formula are as follows:
O-nitrobenzaldehyde is a kind of important pharmaceutical intermediate organic functional material, is mainly used as preparing nifedipine etc.
Prevent and treat hypertension and cardiovascular disease medicine, and as preparing the eliminating the phlegm anti-inflammation drugs such as Ambroxol.O-nitrobenzaldehyde is also
The important source material of synthesizing new plant growth regulator ' Inshuzhi ', and for synthesizing ortho-nitrophenyl vinyl and adjacent nitro meat
The series of products such as cinnamic acid class.O-nitrobenzaldehyde may further be used to as four porphyrin of synthesising racemation, which can be made abzyme
Add halogen enzyme to substitute.Therefore, o-nitrobenzaldehyde high selectivity has environmental economy social benefit.
The traditional preparation process of o-nitrobenzaldehyde carries out nitro alcohol plus nitric acid (70%) in reaction kettle
Oxidation prepares o-nitrobenzaldehyde.Traditional preparation process has the disadvantage in that starting reaction is slow, with nitric acid additional amount
Increasing, reaction speed is accelerated, and reaction belongs to exothermic reaction, when occurring to have a power failure, cut off the water or reactor agitator breaks down,
The heat that reaction generates can not be taken away in time, and the enrichment of simultaneous reactions raw material is more, and reaction speed can increase in geometry speed, generate quick-fried
Fried risk.
Summary of the invention
Technical problem to be solved by the present invention lies in the nitrification process that traditional technique prepares o-nitrobenzaldehyde
In, nitration reaction is a kind of dangerous technique, and strict control nitrification temperature and nitration reaction speed are wanted in nitrifying process, works as generation
Have a power failure, cut off the water with consersion unit stirring etc. elements break down when, when reacting the thermal energy of generation cannot be quickly moved out, temperature is sharply
Rise, so that risk of explosion can occurs, and current o-nitrobenzaldehyde process units volume is big, deposits during nitration reaction
The uncontrollable problem of security risk.
The technical solution adopted by the present invention to solve the technical problems is: providing a kind of nitrification of o-nitrobenzaldehyde preparation
Device, including first flow pump, pipeline one, magnetic stirring apparatus, second flow pump, pipeline two, pipeline three, spiral tube exchanger,
Pipeline four and fluid reservoir, the first flow pump are connected to magnetic stirring apparatus by pipeline one；The second flow pump passes through pipe
Road two is connected to magnetic stirring apparatus；The magnetic stirring apparatus is connected to spiral tube exchanger by pipeline three；The helix tube changes
Hot device is connected to liquid storage kettle by pipeline four.
It is as above-mentioned technical proposal to further describe: ball valve one is housed on heretofore described pipeline one.
It is as above-mentioned technical proposal to further describe: ball valve two is housed on heretofore described pipeline two.
It is as above-mentioned technical proposal to further describe: heretofore described pipeline one, pipeline two, pipeline three, pipeline four
UsingRound tube
It is as above-mentioned technical proposal to further describe: heretofore described spiral tube exchanger include reaction-ure inlet,
Reactant exit, hot water inlet, hot water outlet.
As above-mentioned technical proposal to further describe: the hot water inlet side of heretofore described spiral tube exchanger is equipped with
Water inlet pipe, hot water outlet side are equipped with outlet pipe.
The present invention also provides a kind of nitration processes method of o-nitrobenzaldehyde preparation, the first flow pump is controlled
First reactant enters the flow of magnetic stirring apparatus；The second flow pump controls the second reactant and enters magnetic stirring apparatus
Flow；After first reactant and the second reactant are thoroughly mixed in magnetic stirring apparatus, it is delivered to by pipeline three
Spiral tube exchanger；The spiral tube exchanger is passed through circulating hot water by water inlet pipe, and pipeline three continues to spiral tube exchanger
Convey the first reactant and the second reactant of mixing, the heat of hot water passes to the first of mixing instead by spiral tube exchanger
Object and the second reactant are answered, the first reactant and the second reactant mixed in spiral tube exchanger is just completed in the shorter time
Reaction accumulates the first reactant of mixing and the second reactant not in spiral tube exchanger；Reaction product adjacent nitro
Benzaldehyde is delivered in liquid storage kettle by pipeline four.
It is as above-mentioned technical proposal to further describe: the first reaction mixed in heretofore described spiral tube exchanger
Object and the second reactant walk tube side, and hot water walks shell side.
It is as above-mentioned technical proposal to further describe: mixed in the tube side of heretofore described spiral tube exchanger
One reactant and the second reactant are contrary with the hot water flowing in shell side, are in counterflow heat exchange.
It is as above-mentioned technical proposal to further describe: heretofore described first reactant be nitrobenzyl alcohol, second
Reactant is nitric acid.
Compared with prior art, beneficial effect possessed by the present invention is:
1, starting reaction speed is improved；
2, continuous feed；
3, the reaction time is short, and it is few to participate in reaction mass total amount；
4, raw material is not enriched with；
5, device is small, and yield is big；
6, when unpredictalbe burst factor such as have a power failure, cut off the water occurs, the security risks such as explosion will not be generated.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the nitrification installation of o-nitrobenzaldehyde preparation of the embodiment of the present invention.
1: first flow pump, 2: pipeline one, 3: magnetic stirring apparatus, 4: second flow pump, 5: pipeline two, 6: pipeline three, 7:
Spiral tube exchanger, 8: pipeline four, 9: liquid storage kettle, 10: ball valve one, 11: ball valve two, 12: water inlet pipe, 13: outlet pipe, 71: anti-
Answer object import, 72: reactant exit, 73: hot water inlet, 74: hot water outlet.
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched
The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
As shown in Figure 1, the present invention provides a kind of nitrification installation of o-nitrobenzaldehyde preparation, including first flow pump 1,
Pipeline 1, magnetic stirring apparatus 3, second flow pump 4, pipeline 25, pipeline 36, spiral tube exchanger 7, pipeline 48 and liquid storage kettle
9。
The first flow pump 1 is connected to magnetic stirring apparatus 3 by pipeline 1.
The second flow pump 4 is connected to magnetic stirring apparatus 3 by pipeline 25.
The magnetic stirring apparatus 3 is connected to spiral tube exchanger 7 by pipeline 36.
The spiral tube exchanger 7 is connected to liquid storage kettle 9 by pipeline 48.
Ball valve 1 is housed on the pipeline 1.
Ball valve 2 11 is housed on the pipeline 25.
The pipeline 1, pipeline 25, pipeline 36, pipeline 48 useRound tube
The spiral tube exchanger 7 includes reaction-ure inlet 71, reactant exit 72, hot water inlet 73, hot water outlet 74.
73 side of hot water inlet of the spiral tube exchanger 7 is equipped with water inlet pipe 12, and 74 side of hot water outlet is equipped with outlet pipe 13.
The present invention also provides a kind of nitration processes methods of o-nitrobenzaldehyde preparation, include the following steps:
The first flow pump 1 controls the flow that the first reactant enters magnetic stirring apparatus 3；The second flow pump 4
Control the flow that the second reactant enters magnetic stirring apparatus 3；First reactant and the second reactant are in magnetic stirring apparatus 3
In be thoroughly mixed after, spiral tube exchanger 7 is delivered to by pipeline 36；The spiral tube exchanger 7 passes through water inlet pipe 12
It is passed through circulating hot water, pipeline 36 continues the first reactant and the second reactant to the conveying mixing of spiral tube exchanger 7, hot water
Heat the first reactant and the second reactant of mixing are passed to by spiral tube exchanger 7, mixed in spiral tube exchanger 7
The first reactant and the second reactant just complete to react in the shorter time, make mixing the first reactant and the second reactant
It is not accumulated in spiral tube exchanger 7；Reaction product o-nitrobenzaldehyde is delivered in kettle 9 by pipeline 48.
The first reactant and the second reactant mixed in the spiral tube exchanger 7 walks tube side, and hot water walks shell side.
The hot water stream in the first reactant and the second reactant and shell side mixed in the tube side of the spiral tube exchanger 7
Move it is contrary, be in counterflow heat exchange.
First reactant is nitrobenzyl alcohol, and the second reactant is nitric acid.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of nitrification installation of o-nitrobenzaldehyde preparation, including first flow pump (1), pipeline one (2), magnetic stirring apparatus
(3), second flow pump (4), pipeline two (5), pipeline three (6), spiral tube exchanger (7), pipeline four (8) and fluid reservoir (9), institute
It states first flow pump (1) and magnetic stirring apparatus (3) is connected to by pipeline one (2)；The second flow pump (4) passes through pipeline two
(5) magnetic stirring apparatus (3) are connected to；The magnetic stirring apparatus (3) is connected to spiral tube exchanger (7) by pipeline three (6)；Institute
It states spiral tube exchanger (7) and liquid storage kettle (9) is connected to by pipeline four (8).
2. a kind of nitrification installation of o-nitrobenzaldehyde preparation according to claim 1, it is characterised in that: the pipeline one
(2) ball valve one (10) is housed on.
3. a kind of nitrification installation of o-nitrobenzaldehyde preparation according to claim 1, it is characterised in that: the pipeline two
(5) ball valve two (11) is housed on.
4. a kind of nitrification installation of o-nitrobenzaldehyde preparation according to claim 1, it is characterised in that: the pipeline one
(2), pipeline two (5), pipeline three (6), pipeline four (8) useRound tube.
5. a kind of nitrification installation of o-nitrobenzaldehyde preparation according to claim 1, it is characterised in that: the helix tube
Heat exchanger (7) includes reaction-ure inlet (71), reactant exit (72), hot water inlet (73), hot water outlet (74).
6. a kind of nitrification installation of o-nitrobenzaldehyde preparation according to claim 5, it is characterised in that: the helix tube
Hot water inlet (73) side of heat exchanger (7) is equipped with water inlet pipe (12), and hot water outlet (74) side is equipped with outlet pipe (13).
7. a kind of nitration processes method prepared using o-nitrobenzaldehyde as claimed in any one of claims 1 to 6, feature
It is, the first flow pump (1) controls the flow that the first reactant enters magnetic stirring apparatus (3)；The second flow pump
(4) flow that the second reactant enters magnetic stirring apparatus (3) is controlled；First reactant and the second reactant are stirred in magnetic force
It mixes after being thoroughly mixed in device (3), spiral tube exchanger (7) is delivered to by pipeline three (6)；The spiral tube exchanger
(7) it is passed through circulating hot water by water inlet pipe (12), it is anti-that pipeline three (6) continues mix to spiral tube exchanger (7) conveying first
Object and the second reactant are answered, the heat of hot water passes to the first reactant and second of mixing instead by spiral tube exchanger (7)
Object is answered, the first reactant and the second reactant mixed in spiral tube exchanger (7) is just completed to react in the shorter time, makes to mix
The first reactant and the second reactant closed is not accumulated in spiral tube exchanger (7)；Reaction product o-nitrobenzaldehyde
It is delivered in liquid storage kettle (9) by pipeline four (8).
8. a kind of nitration processes method of o-nitrobenzaldehyde preparation according to claim 7, it is characterised in that: the spiral shell
The first reactant and the second reactant mixed in coil heat exchanger (7) walks tube side, and hot water walks shell side.
9. a kind of nitration processes method of o-nitrobenzaldehyde preparation according to claim 8, it is characterised in that: the spiral shell
The first reactant and the second reactant mixed in the tube side of coil heat exchanger (7) is contrary with the hot water flowing in shell side,
In counterflow heat exchange.
10. a kind of nitration processes method of o-nitrobenzaldehyde preparation according to claim 7, it is characterised in that: described
First reactant is nitrobenzyl alcohol, and the second reactant is nitric acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810891727.1A CN108947848A (en) | 2018-08-07 | 2018-08-07 | A kind of nitrification installation and nitration processes method of o-nitrobenzaldehyde preparation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810891727.1A CN108947848A (en) | 2018-08-07 | 2018-08-07 | A kind of nitrification installation and nitration processes method of o-nitrobenzaldehyde preparation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112206739A (en) * | 2020-10-19 | 2021-01-12 | 蚌埠学院 | Device for nitrogen dioxide nitrification |
Citations (7)
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|---|---|---|---|---|
| CH438253A (en) * | 1963-10-07 | 1967-06-30 | Syntex Corp | Process for oxidizing primary and secondary alcohols |
| DE2708115A1 (en) * | 1976-03-11 | 1977-09-22 | Dresden Arzneimittel | (Ortho)-nitro-benzaldehyde prepn. - by hydrolysis of (ortho)-nitro-benzyl bromide to (ortho)-nitro-benzyl alcohol; followed by oxidation with nitric acid |
| JPS59212441A (en) * | 1983-05-17 | 1984-12-01 | Mitsubishi Chem Ind Ltd | Production of carbonyl compound |
| CN102060710A (en) * | 2010-12-10 | 2011-05-18 | 合肥工业大学 | High-selectivity synthesis method of O-nitrobenzaldehyde |
| CN105439867A (en) * | 2014-08-22 | 2016-03-30 | 南京理工大学 | A preparing method of 2-nitrobenzaldehyde |
| CN106928100A (en) * | 2015-12-29 | 2017-07-07 | 沈阳化工研究院有限公司 | A kind of continuous nitrification method of naphthalene sulfonic acids class compound |
| CN108164421A (en) * | 2017-12-01 | 2018-06-15 | 灌南伊斯特化工有限公司 | The preparation method of o-nitrobenzaldehyde |
-
2018
- 2018-08-07 CN CN201810891727.1A patent/CN108947848A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH438253A (en) * | 1963-10-07 | 1967-06-30 | Syntex Corp | Process for oxidizing primary and secondary alcohols |
| DE2708115A1 (en) * | 1976-03-11 | 1977-09-22 | Dresden Arzneimittel | (Ortho)-nitro-benzaldehyde prepn. - by hydrolysis of (ortho)-nitro-benzyl bromide to (ortho)-nitro-benzyl alcohol; followed by oxidation with nitric acid |
| JPS59212441A (en) * | 1983-05-17 | 1984-12-01 | Mitsubishi Chem Ind Ltd | Production of carbonyl compound |
| CN102060710A (en) * | 2010-12-10 | 2011-05-18 | 合肥工业大学 | High-selectivity synthesis method of O-nitrobenzaldehyde |
| CN105439867A (en) * | 2014-08-22 | 2016-03-30 | 南京理工大学 | A preparing method of 2-nitrobenzaldehyde |
| CN106928100A (en) * | 2015-12-29 | 2017-07-07 | 沈阳化工研究院有限公司 | A kind of continuous nitrification method of naphthalene sulfonic acids class compound |
| CN108164421A (en) * | 2017-12-01 | 2018-06-15 | 灌南伊斯特化工有限公司 | The preparation method of o-nitrobenzaldehyde |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112206739A (en) * | 2020-10-19 | 2021-01-12 | 蚌埠学院 | Device for nitrogen dioxide nitrification |
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