CN106179150A - A kind of association response device of Biformyl oxidation synthesis glyoxylate - Google Patents
A kind of association response device of Biformyl oxidation synthesis glyoxylate Download PDFInfo
- Publication number
- CN106179150A CN106179150A CN201610582669.5A CN201610582669A CN106179150A CN 106179150 A CN106179150 A CN 106179150A CN 201610582669 A CN201610582669 A CN 201610582669A CN 106179150 A CN106179150 A CN 106179150A
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- CN
- China
- Prior art keywords
- biformyl
- association response
- response device
- gas
- oxidation synthesis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/23—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups
- C07C51/235—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups of —CHO groups or primary alcohol groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
- B01J2219/0277—Metal based
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
- B01J2219/0295—Synthetic organic materials
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to technical field of chemical, association response device particularly to a kind of Biformyl oxidation synthesis glyoxylate. it includes: reactor, nitric acid adds pipe, circulating pump, gas-liquid reactor, air intlet, reacting pipe, external heat exchanger, reflux condenser, sample tap, glyoxalic acid exports, tail gas absorber etc. the association response device of a kind of synthesizing glyoxalic acid of the present invention, there is investment little, install easily, easy temperature control system, low power consumption and other advantages. the association response device of the present invention participates in reaction by introducing air, pass through reactor, reacting pipe, gas-liquid reactor, the close fit of external heat exchanger, Biformyl is made to obtain bigger raising to conversion ratio and the glyoxalic acid quality of glyoxalic acid.
Description
Technical field
The invention belongs to technical field of chemical, relate to the reaction unit of a kind of Biformyl oxidation synthesis glyoxylate, especially
Relate to the association response device of the synthesizing glyoxalic acid of a kind of Biformyl nitric acid oxidation method, air participation 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 producing glyoxalic acid that most domestic enterprise uses.This work
The advantage of skill is that investment is little, cost 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 most about converting into that the Biformyl of 17 ± % is excessively oxidated is converted into our unwanted oxalic acid, its chemistry is anti-
Answer equation as follows:
3CHOCOOH + 2HNO3 →3COOH-COOH + NO↑+H2O
2., during tail gas absorption, due to vacuum and the effect of entrained liquid, the equivalent 4-6% Biformyl that there are about enters suction
Receive tower to be consumed by nitric acid.
3. the reaction of Biformyl nitric acid oxidation method synthesizing glyoxalic acid is strong exothermal reaction, and the heat exchange area of reacting kettle jacketing is only
Having about 15m2, cooling-down effect can not meet the needs of oxidation reaction heat release. and therefore, reaction temperature is wayward.
［ 4. air has been only involved in tail gas absorption reaction, is not engaged in the oxidation reaction of Biformyl, and this is objectively adding
The consumption of nitric 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 become through further investigation
Merit develops a kind of Biformyl oxidation technology technology that can reduce disadvantages described above and oxidation unit.
Summary of the invention
The invention provides the association response device of a kind of oxidation of glyoxal synthesizing glyoxalic acid, it is characterised in that 1. energy
Enough being precisely controlled reaction temperature, 2. air can participate in the oxidation reaction of Biformyl, and 3. Biformyl obtains to the conversion ratio of glyoxalic acid
To bigger lifting.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate that the present invention provides, it is characterised in that including: anti-
Answer still, nitric acid addition pipe, circulating pump, gas-liquid reaction device, air intlet, reacting pipe, external heat exchanger, recirculated water to import and export,
The import and export of reflux condenser, cool brine, sample tap, glyoxalic acid outlet, tail gas absorber etc..
Preferably, the reacting kettle jacketing described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention
Only being connected with jet chimney, in the reaction of the present invention, it is only used for heating.
Preferably, the nitric acid described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention adds pipe
Port adds homemade at the uniform velocity Dropping feeder.
Preferably, the gas-liquid reaction described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention
Device is enamel, PP or F4 material, and its main diameter is 80-200mm, and port connects fluid accelerating attachment.
Preferably, the air intlet described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention is even
Connect self-control air purifier.
Preferably, the reacting pipe described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention is
PP, F4 or enamel material, its a length of 5.0-25.0m.
Preferably, the external heat exchanger described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention
For graphite heat exchanger or glass material heat exchanger, heat exchange area is 10-80m2.Its recirculated water imports and exports connection 25 ° of C ± circulations
Water.
Preferably, the reflux condenser described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention
For coil pipe type glass condenser, area is that the import and export of its condensed water of 1.5-15.0m2. connect the cool brine having 5-15 ° of C.
Preferably, the tail gas absorber described in association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention
For PP material, built-in spherical PE filler or ripple packing. become an absorption tower combination by the series connection of 2-8 platform absorption tower.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate that the present invention provides and Biformyl oxidation before
Reaction unit compares, and has a following clear advantage:
1. the at the uniform velocity addition of nitric acid, it is to avoid hot-spot phenomenon.
2. being heated reactant liquor by reacting kettle jacketing, lowered the temperature reactant liquor by external heat exchanger, heat is cold
Lock out operation is more conducive to the control of temperature.
3. gas-liquid reaction device can make air enter reactant liquor continuously and participate in the oxidation reaction of Biformyl, Jin Erhui
Mild reaction conditions, reduction nitric acid unit consumption, it is possible to increase the conversion ratio of Biformyl to glyoxalic acid.
4. the reaction in the reacting pipe of relative closure of the reactant liquor after accelerating can be more abundant, and this is to improving Biformyl
Conversion ratio is highly beneficial.
5. by increasing reflux condenser heat exchange area, the method leading to cool brine to reflux condenser so that solution-air is carried secretly
Biformyl and glyoxalic acid drop and return to reactor, meanwhile, through cooling after reaction end gas be more beneficial for absorption tower reclaim dilute nitre
Acid.
So device, the association response device of a kind of Biformyl oxidation synthesis glyoxylate that the present invention provides, making instead
While answering temperature easily controllable, additionally it is possible to make nitric acid unit consumption decrease, the conversion ratio of Biformyl to glyoxalic acid has and carries more greatly
High.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the association response device of a kind of Biformyl oxidation synthesis glyoxylate of the present invention.
Claims (7)
1. an association response device for Biformyl oxidation synthesis glyoxylate, it includes: reactor, nitric acid add pipe, circulating pump,
The import and export of gas-liquid reaction device, air intlet, reacting pipe, external heat exchanger, recirculated water, reflux condenser, cool brine turnover
The outlet of mouth, sample tap, glyoxalic acid, tail gas absorber, it is characterised in that circulating pump and reactor are passed through in gas-liquid reaction device one end
Bottom is connected, and the other end of gas-liquid reaction device is connected with reactor top by external heat exchanger, the side of gas-liquid reaction device
Import and air communication, it is anti-to the conversion of glyoxalic acid that reactor, gas-liquid reaction device composition association response device realizes Biformyl
Should.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate the most as claimed in claim 1, it is characterised in that described
Nitric acid add tubing matter be F4 or enamel material, its port connect have homemade nitric acid at the uniform velocity Dropping feeder.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate the most as claimed in claim 1, it is characterised in that described
Gas-liquid reaction device be enamel, PP, F4 material, its port connect have fluid accelerating attachment.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate the most as claimed in claim 1, it is characterised in that described
External heat exchanger be graphite heat exchanger or glass material heat exchanger. heat exchange area is 10-80m2.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate the most as claimed in claim 1, it is characterised in that described
Reflux condenser be coil pipe type glass condenser or graphite condenser, area is 1.5-15.0m2.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate the most as claimed in claim 1, it is characterised in that described
Air line be PP material, air intlet installs purifier additional.
The association response device of a kind of Biformyl oxidation synthesis glyoxylate the most as claimed in claim 1, it is characterised in that described
Tail gas absorber be PP material, built-in spherical PE filler or ripple packing, by 2-8 platform absorption tower series connection become an absorption
Tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610582669.5A CN106179150A (en) | 2016-07-23 | 2016-07-23 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610582669.5A CN106179150A (en) | 2016-07-23 | 2016-07-23 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106179150A true CN106179150A (en) | 2016-12-07 |
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ID=57492487
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610582669.5A Pending CN106179150A (en) | 2016-07-23 | 2016-07-23 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
Country Status (1)
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| CN (1) | CN106179150A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203448102U (en) * | 2013-08-29 | 2014-02-26 | 黄冈师范学院 | Gas-liquid spraying circulating reaction device for preparing glyoxylic acid by oxygen oxidization method |
| CN203741248U (en) * | 2014-03-17 | 2014-07-30 | 湖北省宏源药业有限公司 | Improved oxidation reaction and tail gas adsorption device for synthesizing glyoxylic acid |
| CN206276369U (en) * | 2016-06-17 | 2017-06-27 | 河南新天地药业股份有限公司 | A kind of association response device of glyoxal oxidation synthesis glyoxylate |
-
2016
- 2016-07-23 CN CN201610582669.5A patent/CN106179150A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203448102U (en) * | 2013-08-29 | 2014-02-26 | 黄冈师范学院 | Gas-liquid spraying circulating reaction device for preparing glyoxylic acid by oxygen oxidization method |
| CN203741248U (en) * | 2014-03-17 | 2014-07-30 | 湖北省宏源药业有限公司 | Improved oxidation reaction and tail gas adsorption device for synthesizing glyoxylic acid |
| CN206276369U (en) * | 2016-06-17 | 2017-06-27 | 河南新天地药业股份有限公司 | A kind of association response device of glyoxal oxidation synthesis glyoxylate |
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Application publication date: 20161207 |
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| RJ01 | Rejection of invention patent application after publication |