CN114053836A - Device and method for recycling and treating oxidized tail gas absorption liquid in production of furan ammonium salt - Google Patents
Device and method for recycling and treating oxidized tail gas absorption liquid in production of furan ammonium salt Download PDFInfo
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- CN114053836A CN114053836A CN202111360061.5A CN202111360061A CN114053836A CN 114053836 A CN114053836 A CN 114053836A CN 202111360061 A CN202111360061 A CN 202111360061A CN 114053836 A CN114053836 A CN 114053836A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1425—Regeneration of liquid absorbents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/54—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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Abstract
The invention discloses a device for recovering and treating an absorption liquid of oxidation tail gas in the production of furan ammonium salt, which adopts the following equipment: pumping the oxidized tail gas absorption liquid into an absorption liquid freezing kettle by using a centrifugal pump, introducing cold water at the temperature of-2-0 ℃ into the tail gas absorption liquid in the absorption liquid freezing kettle through an inner coil pipe for cooling, simultaneously carrying out frequency conversion stirring and cooling to 0-5 ℃, pumping the tail gas absorption liquid after freezing into a two-stage plate-and-frame filter and a fine filter by using the centrifugal pump for filtering, primarily filtering most of sodium carbonate, feeding the filtered absorption liquid into an acid adjusting kettle, pumping hydrochloric acid with the concentration of 8-12% into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor, controlling the pressure of the pump to be 0.25-0.3MPa, and carrying out frequency conversion control on the acid adjusting kettle for stirring and acid adjustment at the frequency of 30-35 Hz. The method effectively reduces the content of sodium carbonate in the tail gas absorption liquid from 3-6% to 0.5-0.8%, so that the tail gas absorption liquid is completely applied to production, the requirements of an oxidation production process are met, and the complete application production of the oxidation tail gas absorption liquid is completely realized.
Description
Technical Field
The invention relates to the technical field of furan ammonium salt production, in particular to a device and a method for recovering and treating an absorption liquid of oxidation tail gas in furan ammonium salt production.
Background
Furanamine salt (British name: SMIA) is currently the main raw material for producing cefuroxime and cefuroxime axetil, which are cephalosporin antibiotics, cefuroxime is firstly developed successfully by the company Loran William, is firstly marketed in the United kingdom, Ireland, Germany and Italy and then sold in many countries all over the world in 1978, is sold under the trade name of "Western Europe", is marketed in the United states after approval by the American FDA in 1987, is widely used for resisting various infections caused by sensitive bacteria due to definite curative effect, and enters the 20 th century for 90 s, the medicine becomes a world-wide-selling anti-infective medicine and has good curative effect, and the furan ammonium salt as a novel medical intermediate is a key intermediate for synthesizing the second-generation cefuroxime medicine, the property state of the furan ammonium salt is white or white crystalline powder, the molecular weight is 186.17, the boiling point: at760mmHg at 284.7 ℃, trans isomer ≦ 0.5%, and the chemical name is (z) -2-methoxy methylamino-2- (furan-2-yl) ammonium acetate.
Ketonic acid is used as a key intermediate product in the production of furan ammonium salt, and is a cost core step in the whole production of furan ammonium salt.
In the industrial production of furan ammonium salt, whether a tail gas system can stably produce and operate is the key for determining the whole oxidation synthesis production step of ketoacid, and relates to the safety of the oxidation reaction of ketoacid synthesis, the quality of process yield and the risk of environmental protection control, in the industrial production of furan ammonium salt, the current absorption liquid of ketoacid synthesis oxidation tail gas contains a certain content of sodium carbonate, the content is about 3-6%, when the sodium nitrite aqueous solution of the oxidation tail gas absorption liquid is applied to the production oxidation reaction, sodium carbonate can be enriched in the system to generate a large amount of carbon dioxide gas to seriously threaten the pressure of the tail gas system, so that the tail gas system is fluctuated, the operation of the ketoacid synthesis oxidation reaction process can be seriously influenced, even threatened the safety and the environmental protection of the tail gas system, the production safety and the yield are influenced, so that the tail gas absorption liquid can not be completely applied, in actual production, a nitrous acid aqueous solution with new configuration is needed, so that the production cost is increased, the tail gas absorption liquid is increased, and the problems of environmental pollution and the like are caused, so that the oxidized tail gas absorption liquid is completely used;
according to the invention, after the oxidized tail gas absorption liquid is frozen and filter-pressed to remove most of the sodium carbonate in the tail gas absorption liquid, a small amount of hydrochloric acid is added dropwise during preparation to further remove the sodium carbonate in the tail gas absorption liquid, so that the content of the sodium carbonate in the sodium nitrite aqueous solution of the tail gas absorption liquid used again is 0.5-0.8%, the production process requirement is met, the oxidized tail gas absorption liquid is completely used for production, the cost consumption of the raw material for producing sodium sulfite is greatly reduced, new waste water is not produced, the yield of the ketonic acid synthesis oxidation reaction process is improved, the production is more stable, the production safety is better guaranteed, and good safety, environmental protection and economic benefits are obtained.
Disclosure of Invention
The invention aims to solve the problems of safe and stable operation of the oxidized tail gas system and ensure safe, efficient, continuous and stable production of oxidized ketoacid in the key core reaction step of the furan ammonium salt, and provides a device and a method for recovering and treating oxidized tail gas absorption liquid in the production of the furan ammonium salt.
The utility model provides an oxidation tail gas absorption liquid recovery processing device in furan ammonium salt production, adopts following equipment: pumping the oxidized tail gas absorption liquid into an absorption liquid freezing kettle by using a centrifugal pump, introducing cold water at the temperature of-2-0 ℃ into the tail gas absorption liquid in the absorption liquid freezing kettle through an inner coil pipe for cooling, simultaneously carrying out frequency conversion stirring and cooling to 0-5 ℃, pumping the tail gas absorption liquid after freezing into a two-stage plate-and-frame filter and a fine filter by using the centrifugal pump for filtering, primarily filtering most of sodium carbonate, feeding the filtered absorption liquid into an acid adjusting kettle, pumping hydrochloric acid with the concentration of 8-12% into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor, controlling the pressure of the pump to be 0.25-0.3MPa, and carrying out frequency conversion control on the acid adjusting kettle for stirring and acid adjustment at the frequency of 30-35 Hz.
Preferably, the device also comprises a pressure gauge, a temperature measuring instrument, a variable frequency regulation controller, a pump and a cold water inlet pipeline and a cold water outlet pipeline.
A method for recycling and treating an absorption liquid of oxidation tail gas in production of furan ammonium salt comprises the following steps:
step S1: cooling the oxidized tail gas absorption liquid to 0-5 ℃ in an absorption liquid freezing kettle by using cold water with the temperature of-2-0 ℃ for an inner coil pipe;
step S2: the absorption liquid freezing kettle adopts variable frequency stirring, the variable frequency is controlled at 20-25Hz, the stirring speed is controlled to cool and grow the crystal, and more sodium carbonate is precipitated and filtered;
step S3: freezing the absorption liquid to 0-5 deg.C, and filtering with two-stage plate-and-frame filter and fine filter;
step S4: the filtered absorption liquid is sent to an acid adjusting kettle, and hydrochloric acid with the concentration of 8-12% is pumped into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor.
Preferably, in the step S4, the pump pressure is controlled to be 0.25 to 0.3Mpa, the frequency conversion of the acid adjusting kettle is controlled to be 30 to 35Hz, and the frequency conversion speed is controlled not to be too fast, so that the hydrochloric acid is brought out along with carbon dioxide gas generated by the reaction in the hydrochloric acid reaction process, thereby affecting the utilization rate of the acid.
In the invention, oxidized tail gas absorption liquid is pumped into an absorption liquid freezing kettle by a centrifugal pump, the tail gas absorption liquid in the absorption liquid freezing kettle is pumped into a two-stage plate-and-frame filter and a fine filter by an inner coil pipe to be cooled down, and simultaneously is stirred and cooled to 0-5 ℃ in a variable frequency manner, the tail gas absorption liquid after freezing is pumped into a two-stage plate-and-frame filter and the fine filter by the centrifugal pump to filter out most of sodium carbonate primarily, the filtered absorption liquid enters an acid adjusting kettle, hydrochloric acid with the concentration of 8-12% is pumped into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor, the pressure of the pump is controlled to be 0.25-0.3Mpa, the frequency conversion of the acid adjusting kettle is controlled to be 30-35Hz to stir and adjust the acid, the content of the sodium carbonate in the absorption liquid after analysis and detection is 0.5-0.8% and is completely applied to the oxidation production reaction, the requirement of the production process is met, thereby completely realizing the application production of the oxidized tail gas absorption liquid, not only greatly reduces the cost consumption of raw materials for producing sodium nitrite, but also does not generate new waste water, improves the yield of the ketonic acid synthesis oxidation reaction process, ensures more stable production, better ensures the production safety, and obtains good safety, environmental protection and economic benefit.
Compared with the prior art, the invention has the beneficial effects that:
1. the oxidized tail gas absorption liquid is cooled to 0-5 ℃ in an absorption liquid freezing kettle by using cold water at the temperature of-2-0 ℃ through an inner coil pipe, most of sodium carbonate in the tail gas absorption liquid can be well frozen and separated out at the temperature, and the content of the sodium carbonate is reduced from 3-6% to 1.0-1.5%;
2. the absorption liquid freezing kettle adopts variable frequency stirring, the variable frequency is controlled at 20-25Hz, the crystallization granularity of the sodium carbonate can be well ensured, and favorable conditions are provided for the next filtration;
3. the filtered absorption liquid is sent to an acid adjusting kettle, hydrochloric acid with the concentration of 8-12% is pumped into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor, the pressure of the pump is controlled to be 0.25-0.3Mpa, the frequency conversion of the acid adjusting kettle is controlled to be 30-35Hz, the hydrochloric acid well reacts to remove sodium carbonate in the hydrochloric acid, and further the content of the sodium carbonate is reduced from 1-1.5% to 0.5-0.8%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, an oxidized tail gas absorption liquid recovery processing device in furan ammonium salt production adopts the following equipment: pumping the oxidized tail gas absorption liquid into an absorption liquid freezing kettle by a centrifugal pump, introducing the tail gas absorption liquid in the absorption liquid freezing kettle into cold water at the temperature of-2-0 ℃ through an inner coil pipe for cooling, simultaneously adopting a variable frequency regulation controller to control frequency conversion stirring and cooling to 0-5 ℃, pumping the tail gas absorption liquid after freezing into a two-stage plate frame filter and a fine filter by the centrifugal pump for filtering, primarily filtering most of sodium carbonate, enabling the filtered absorption liquid to enter an acid regulation kettle, pumping hydrochloric acid with the concentration of 8-12% from two sides of the bottom of the acid regulation kettle into the acid regulation kettle through a hydrochloric acid distributor, controlling the pump pressure to be 0.25-0.3MPa, and adopting the variable frequency regulation controller to control the frequency conversion to stir and regulate the acid at the speed of 30-35 Hz.
The device also comprises a pressure gauge, a temperature measuring instrument, a variable frequency regulation controller, a pump and a cold water inlet pipeline and a cold water outlet pipeline.
A method for recycling and treating an absorption liquid of oxidation tail gas in production of furan ammonium salt comprises the following steps:
step S1: cooling the oxidized tail gas absorption liquid to 0-5 ℃ in an absorption liquid freezing kettle by using cold water with the temperature of-2-0 ℃ for an inner coil pipe;
step S2: the absorption liquid freezing kettle is stirred by adopting variable frequency, and the variable frequency is controlled at 20-25 Hz;
step S3: freezing and cooling the absorption liquid to 0-5 ℃, and filtering by adopting a two-stage plate-and-frame filter and a fine filter to obtain 365 kg of sodium carbonate;
step S4: and (3) pumping the filtered absorption liquid into an acid adjusting kettle from two sides of the bottom of the acid adjusting kettle by a hydrochloric acid distributor with the concentration of 8-12% hydrochloric acid, controlling the pressure of the pump to be 0.25-0.3Mpa, controlling the frequency conversion of the acid adjusting kettle to be 30-35Hz, consuming 650L of hydrochloric acid, and detecting the content of sodium carbonate in the absorption liquid to be 0.61%.
Continuously and stably running for 3 months, and treating tail gas absorption liquid 580 m3The content of sodium carbonate in the absorption liquid is 0.53 percent, the production process requirement is met, so that the oxidation tail gas absorption liquid is completely produced in a recycling way, the cost consumption of raw materials for producing sodium sulfite is greatly reduced, new waste water is not produced, the content of sodium carbonate is low, the tail gas impurity gas is less, and the ketonic acid synthesis oxidation reaction process can be used for collectingThe rate is improved, the production is more stable, the content of the ketonic acid is increased from the original average 74-75% to 76-78%, the production safety is better ensured, and good safety, environmental protection and economic benefits are obtained.
The control mode of the invention is automatically controlled by the controller, the control circuit of the controller can be realized by simple programming of a person skilled in the art, the supply of the power supply also belongs to the common knowledge in the field, and the invention is mainly used for protecting mechanical devices, so the control mode and the circuit connection are not explained in detail in the invention.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. The utility model provides an oxidation tail gas absorption liquid recovery processing device in furan ammonium salt production which characterized in that adopts following equipment: pumping the oxidized tail gas absorption liquid into an absorption liquid freezing kettle by using a centrifugal pump, introducing cold water at the temperature of-2-0 ℃ into the tail gas absorption liquid in the absorption liquid freezing kettle through an inner coil pipe for cooling, simultaneously carrying out frequency conversion stirring and cooling to 0-5 ℃, pumping the tail gas absorption liquid after freezing into a two-stage plate-and-frame filter and a fine filter by using the centrifugal pump for filtering, primarily filtering most of sodium carbonate, feeding the filtered absorption liquid into an acid adjusting kettle, pumping hydrochloric acid with the concentration of 8-12% into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor, controlling the pressure of the pump to be 0.25-0.3MPa, and carrying out frequency conversion control on the acid adjusting kettle for stirring and acid adjustment at the frequency of 30-35 Hz.
2. The device for recovering and treating the absorption liquid of the oxidation tail gas in the production of the furan ammonium salt according to claim 1, characterized in that: the device also comprises a pressure gauge, a temperature measuring instrument, a variable frequency regulation controller, a pump and a cold water inlet pipeline and a cold water outlet pipeline.
3. A method for recycling and treating an absorption liquid of an oxidation tail gas in the production of furan ammonium salt, which is characterized in that the recycling and treating device of the absorption liquid of the oxidation tail gas in the production of furan ammonium salt according to any one of claims 1-2 is adopted, and comprises the following steps:
step S1: cooling the oxidized tail gas absorption liquid to 0-5 ℃ in an absorption liquid freezing kettle by using cold water with the temperature of-2-0 ℃ for an inner coil pipe;
step S2: the absorption liquid freezing kettle is stirred by adopting variable frequency, and the variable frequency is controlled at 20-25 Hz;
step S3: freezing the absorption liquid to 0-5 deg.C, and filtering with two-stage plate-and-frame filter and fine filter;
step S4: the filtered absorption liquid is sent to an acid adjusting kettle, and hydrochloric acid with the concentration of 8-12% is pumped into the acid adjusting kettle from two sides of the bottom of the acid adjusting kettle through a hydrochloric acid distributor.
4. The method for recycling and treating the absorption liquid of the oxidation tail gas in the production of the furan ammonium salt according to claim 3, which is characterized in that: in the step S4, the pump pressure is controlled to be 0.25-0.3Mpa, and the frequency conversion of the acid adjusting kettle is controlled to be 30-35 Hz.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111360061.5A CN114053836A (en) | 2021-11-17 | 2021-11-17 | Device and method for recycling and treating oxidized tail gas absorption liquid in production of furan ammonium salt |
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| CN202111360061.5A CN114053836A (en) | 2021-11-17 | 2021-11-17 | Device and method for recycling and treating oxidized tail gas absorption liquid in production of furan ammonium salt |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247748A (en) * | 2011-06-30 | 2011-11-23 | 湖北省宏源药业有限公司 | Treatment method and treatment system of tail gas from glyoxylic acid production by nitric acid oxidation of glyoxal |
| CN108273367A (en) * | 2018-04-04 | 2018-07-13 | 烟台国邦化工机械科技有限公司 | A kind of gas cleaning desalination process and system |
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- 2021-11-17 CN CN202111360061.5A patent/CN114053836A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247748A (en) * | 2011-06-30 | 2011-11-23 | 湖北省宏源药业有限公司 | Treatment method and treatment system of tail gas from glyoxylic acid production by nitric acid oxidation of glyoxal |
| CN108273367A (en) * | 2018-04-04 | 2018-07-13 | 烟台国邦化工机械科技有限公司 | A kind of gas cleaning desalination process and system |
Non-Patent Citations (1)
| Title |
|---|
| 继红主编: "《抗性淀粉生产技术及其应用》", 郑州：河南科学技术出版社, pages: 324 - 325 * |
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