CN206103912U - Reaction unit of glyoxal oxidation glyoxalic acid - Google Patents
Reaction unit of glyoxal oxidation glyoxalic acid Download PDFInfo
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- CN206103912U CN206103912U CN201620590509.0U CN201620590509U CN206103912U CN 206103912 U CN206103912 U CN 206103912U CN 201620590509 U CN201620590509 U CN 201620590509U CN 206103912 U CN206103912 U CN 206103912U
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- biformyl
- reaction unit
- reaction
- oxidation
- glyoxalic acid
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Abstract
The utility model discloses a reaction unit of glyoxal oxidation glyoxalic acid. It includes: pipe, fluid distribution ware, circulating pump, external heat exchanger, direct condenser, sample connection, glyoxalic acid export, the tower of absorb the remnant air etc. Are added to reation kettle, centrifugal blower, nitric acid. The utility model discloses a reaction unit of synthetic glyoxalic acid has that the investment is little, the installation is easy, the temperature is easily controlled, energy consumption low grade advantage the utility model discloses a reaction unit passes through the close cooperation that incoming air participated in the reaction, passed through reation kettle, external heat exchanger for the glyoxal obtains great improvement to the conversion rate and the glyoxalic acid quality of glyoxalic acid.
Description
Technical field
This utility model belongs to technical field of chemical, is related to a kind of reaction unit of Biformyl oxidation synthesis glyoxylate,
More particularly to a kind of Biformyl nitric acid oxidation method, air participate in the reaction unit of the synthesizing glyoxalic acid of oxidation.
Background technology
Glyoxalic acid is important fine chemical material, is widely used in the industries such as spice, pharmacy, pesticide, chemical industry.
Biformyl nitric acid oxidation method synthesizing glyoxalic acid is the technique of the production glyoxalic acid that most domestic enterprise adopts.The work
The advantage of skill is that the little, cost of investment is relatively low.
The chemical equation of Biformyl nitric acid oxidation method synthesizing glyoxalic acid is as follows：
3CHO-CHO + 2HNO3 → 3CHOCOOH + 2NO↑+ H2O。
At present, the open defect of Biformyl nitric acid oxidation method synthesizing glyoxalic acid technique shows as following several respects.
The Biformyl of about equivalent 17 ± % is excessively oxidated to be converted into our unwanted oxalic acid, its chemical reaction
Equation is as follows：
3CHOCOOH + 2HNO3 →3COOH-COOH + NO↑+H2O 。
During tail gas absorption, due to the effect of vacuum and entrained liquid, the equivalent 4-6% Biformyls that there are about enter absorption
Tower is consumed by nitric acid.
The reaction of Biformyl nitric acid oxidation method synthesizing glyoxalic acid is strong exothermal reaction, and the heat exchange area of reacting kettle jacketing only has
15m2 or so, cooling-down effect can not meet the needs of oxidation reaction heat release. therefore, reaction temperature is wayward.
Air has been only involved in tail gas absorption reaction, is not engaged in the oxidation reaction of Biformyl, and this objectively increased nitre
The consumption of acid, increases the quantum of output of by-product oxalic acid.
For the defect in current Biformyl nitric acid oxidation method synthesizing glyoxalic acid technique, we pass through further investigation, into
Work(develops a kind of Biformyl oxidation technology technology and oxidation unit that can reduce disadvantages described above.
The content of the invention
This utility model provides a kind of reaction unit of oxidation of glyoxal synthesizing glyoxalic acid, it is characterised in that 1. energy
Reaction temperature is precisely controlled enough, 2. air can participate in the oxidation reaction of Biformyl, 3. Biformyl is obtained to the conversion ratio of glyoxalic acid
To larger lifting.
This utility model provides a kind of reaction unit of Biformyl oxidation synthesis glyoxylate, it is characterised in that include：Instead
Kettle, nitric acid is answered to add pipe, centrifugal blower, fluid at the uniform velocity distributor, circulating pump, external heat exchanger, circulation water entrance, backflow
Condenser, cool brine import and export, sample tap, glyoxalic acid outlet, tail gas absorber etc..
Preferably, the reacting kettle jacketing described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model
Only it is connected with jet chimney, in reaction of the present utility model, it is only used for heating.
Preferably, the nitric acid described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model adds pipe
Port adds homemade at the uniform velocity Dropping feeder.
Preferably, the centrifugal blower described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model
For intermediate pressure centrifugal blower, operating pressure is 1.5-3.0kpa.
Preferably, the air intlet described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model connects
Connect self-control air filter.
Preferably, the air outlet slit described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model connects
It is connected to gas uniform speed distributor.
Preferably, the external heat exchanger described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model
For graphite heat exchanger or glass material heat exchanger, heat exchange area is 10-80m2.Its circulation water entrance is connected with 25 °C of ± circulations
Water.
Preferably, the reflux condenser described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model
For coil pipe type glass condenser, for 1.5-15.0m2., which condenses the cool brine that water entrance is connected with 5-15 °C to area.
Preferably, the tail gas absorber described in a kind of reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model
For PP materials, built-in spherical PE fillers or the series connection of ripple packing .2-8 platforms absorption tower become an absorption tower combination.
A kind of reaction unit of Biformyl oxidation synthesis glyoxylate that this utility model is provided and Biformyl oxidation before
Reaction unit compares, with following clear advantage.
The at the uniform velocity addition of nitric acid, it is to avoid hot-spot phenomenon.
Reactant liquor is heated by reacting kettle jacketing, reactant liquor is lowered the temperature by external heat exchanger, cold point of heat
The control of temperature is more conducive to from operation.
Intermediate pressure centrifugal blower can make air continuously enter the oxidation reaction that reactant liquor participates in Biformyl, Jin Erhui
Nitric acid unit consumption is reduced, and Biformyl is improved to the conversion ratio of glyoxalic acid.
By increasing reflux condenser heat exchange area, to the method for the logical cool brine of reflux condenser so that solution-air entrainment
Biformyl and glyoxalic acid drop and return to reactor, meanwhile, the reaction end gas Jing after cooling are more beneficial for absorption tower and reclaim dust technology.
So device, a kind of reaction unit of Biformyl oxidation synthesis glyoxylate that this utility model is provided, are causing instead
While answering easily controllable temperature, air participation oxidation reaction, additionally it is possible to make nitric acid unit consumption decrease, Biformyl is to glyoxalic acid
Conversion ratio improve a lot.
Description of the drawings
In order to be illustrated more clearly that technical scheme in this utility model embodiment or prior art, below will to embodiment or
Needed for description of the prior art, accompanying drawing to be used is briefly described, it should be apparent that, drawings in the following description are only
Some embodiments of the present utility model, for those skilled in the art, can be obtaining which according to these accompanying drawings
Its accompanying drawing.
Fig. 1 is a kind of schematic diagram of the reaction unit of Biformyl oxidation synthesis glyoxylate of the present utility model
In Fig. 1：01- reactor main bodies, 02- steam inlets, 03- hot water outlets, 04- centrifugal blowers, the dilute nitre of 05-
Sour import, 06- reactor bottom valves, 07- circulating pumps, 08- external heat exchangers, 09- circulating water intakes, 10- circulating water outlets,
11- reflux condensers, 12- cool brine imports, the outlet of 13- cool brines, sample tap, the outlet of 15- transferred product, 16- are controlled in 14-
Absorption tower combination, 17- can emission outlets.
Specific embodiment
To make device of the present utility model, technical scheme clearly express, below in conjunction with the accompanying drawings to this utility model
Carry out in detail, be fully described by. obviously, described embodiment is a part of embodiment of the present utility model, and not all.
This specific embodiment embodiment provides a kind of reaction unit of oxidation of glyoxal synthesizing glyoxalic acid, its feature
It is, including：01 reactor main body, 02 steam inlet, 03 hot water outlet, 04 centrifugal blower, 05 dust technology import, 06 reaction
Bottom valve, 07 circulating pump, 08 external heat exchanger, 09 circulating water intake, 10 circulating water outlets, 11 reflux condensers, 12 cool brines
Sample tap is controlled in import, the outlet of 13 cool brines in 14, the outlet of 15 transferred product, 16 absorption towers are combined, and 17 can emission outlet.
The detailed process of this specific embodiment embodiment is as follows：First the Biformyl needed for reaction, composite catalyst are pressed
Ratio adds reactor -01, starts stirring, starts circulating pump -07, makes reactant liquor in reactor -01, reacting pipe, outer displacement
Hot device -09, between circulate. steam is passed through into reacting kettle jacketing, during uniform temperature reaction start, it is certain density being configured to
Dust technology by nitric acid add pipe -03 and nitric acid dropping port A at the uniform velocity add -01. reaction end gas Jing reflux condensers of reactor -
After 12 condensations, a part condenses back into reactor, and another part changes into dust technology into absorption tower combination -16, after absorption
Tail gas Jing offgas outlets -17 are discharged. and in reactant liquor cyclic process, air continuously enters reactant liquor by centrifugal blower
Participate in the oxidation reaction of Biformyl. it is after being reacted to certain hour, remaining from the sampling quick detection Biformyl of sample tap -14, work as second
When dialdehyde remnants reach requirement, product Jing products export -15 is transferred to product storage tank.
Such device, a kind of reaction dress of Biformyl oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Put, by the feed postition for improveing nitric acid, nitric acid is at the uniform velocity added, it is to avoid hot-spot phenomenon, and then reduce pair
The yield of product oxalic acid.
Such device, a kind of reaction dress of Biformyl oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Put, only for heating to reactant liquor, external heat exchanger is only for lowering the temperature to reactant liquor, warm for described reacting kettle jacketing
, cold lock out operation be more beneficial for the control of temperature, it is to avoid the fluctuation bounce of temperature, this is highly beneficial to oxidation reaction.
Such device, a kind of reaction dress of Biformyl oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Put, described centrifugal blower can make air continuously enter the oxidation reaction that reactant liquor participates in Biformyl, and then can temperature
With reaction condition, reduction nitric acid unit consumption, Biformyl is improved to the conversion ratio of glyoxalic acid.
Such device, a kind of reaction dress of Biformyl oxidation synthesis glyoxylate that this specific embodiment embodiment is provided
Put, by increasing reflux condenser heat exchange area, to the method for the logical cool brine of reflux condenser so that solution-air carries Biformyl secretly
Dropping with glyoxalic acid and return to reactor, while the reaction end gas Jing after cooling are more conducive to absorption tower reclaims dust technology. this is to reducing
Biformyl loss, it is highly beneficial to the absorption of nitric acid.
As preferably and citing, involved by the reaction unit of the Biformyl oxidation synthesis glyoxylate that this specific embodiment is provided
And the cooling water that is passed through of external heat exchanger can be 25 °C ± recirculated water, but, the drop is passed through by reflux condenser
Temperature water must be less than 15 °C of cool brine.
As preferred and citing, the reaction dress of the Biformyl oxidation synthesis glyoxylate that this specific embodiment is provided
As preferably and citing, involved by the reaction unit of the Biformyl oxidation synthesis glyoxylate that this specific embodiment is provided
And tail gas absorber combination is made up of 2-8 platforms absorption tower.The vacuum pump of its end only plays drainage and can not show negative pressure.
The implementation result of reaction unit of the Biformyl oxidation synthesis glyoxylate that this utility model is provided is：Causing reaction
While temperature is easily controllable, additionally it is possible to make nitric acid unit consumption decrease, the conversion ratio of Biformyl to glyoxalic acid reaches 83.0-
86.0%. simultaneously as the reduction of oxoacetic acid product mesoxalic acid and other organic by-products amounts, highly beneficial to follow-up operation.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or use that this practicality is new
Type. various modifications that these embodiments are carried out, will be apparent for professional and technical personnel, it is determined herein
The General Principle of justice can be realized in the case of without departing from spirit or scope of the present utility model in other embodiments.Cause
This, this utility model will not be limited to the embodiments shown herein, every within this utility model spirit and principle,
Any modification, equivalent substitution and improvements made etc., should be included within protection domain of the present utility model.This utility model
Institute's protection domain is to fit to the most wide scope consistent with principles disclosed herein and features of novelty.
Claims (7)
1. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate, it includes：Reactor, centrifugal blower, nitric acid add pipe,
Fluid distributor, circulating pump, external heat exchanger, reflux condenser, sample tap, glyoxalic acid outlet, tail gas absorber, its feature exist
In, in reactor bottom, external heat exchanger one end is by circulating pump, reactor bottom valve and reaction for the air outlet slit of centrifugal blower
Kettle connects, and the other end enters reactor by reactor top charging aperture.
2. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate according to claim 1, it is characterised in that described nitre
It is F4 enamels or PP materials that acid adds tubing matter, and its port is connected with homemade nitric acid at the uniform velocity Dropping feeder.
3. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate according to claim 1, it is characterised in that it is described from
Heart aerator is intermediate pressure centrifugal blower, and operating pressure is 1.5-3.0kpa.
4. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate according to claim 1, it is characterised in that described is outer
It is graphite or glass material heat exchanger to put heat exchanger, and heat exchange area is 10-80m2。
5. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate according to claim 1, it is characterised in that described returns
Flow condenser is coil pipe type glass condenser. area is 1.5-15m2。
6. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate according to claim 1, it is characterised in that described sky
Feed channel is PP materials, and air outlet slit adds fluid at the uniform velocity distributor.
7. a kind of reaction unit of Biformyl oxidation synthesis glyoxylate according to claim 1, it is characterised in that described tail
Aspiration tower is PP materials, built-in spherical PE fillers or ripple packing, and 2-8 platforms absorption tower is connected becomes an absorption tower combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620590509.0U CN206103912U (en) | 2016-06-17 | 2016-06-17 | Reaction unit of glyoxal oxidation glyoxalic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620590509.0U CN206103912U (en) | 2016-06-17 | 2016-06-17 | Reaction unit of glyoxal oxidation glyoxalic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106215830A (en) * | 2016-07-23 | 2016-12-14 | 河南新天地药业股份有限公司 | A kind of reaction unit of Biformyl oxidation synthesis glyoxylate |
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2016
- 2016-06-17 CN CN201620590509.0U patent/CN206103912U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106215830A (en) * | 2016-07-23 | 2016-12-14 | 河南新天地药业股份有限公司 | A kind of reaction unit of Biformyl oxidation synthesis glyoxylate |
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