CN101596394A - Tail gas circulation absorption plant and absorption process thereof in a kind of methylene reaction and the still-process - Google Patents
Tail gas circulation absorption plant and absorption process thereof in a kind of methylene reaction and the still-process Download PDFInfo
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- CN101596394A CN101596394A CNA2009100884730A CN200910088473A CN101596394A CN 101596394 A CN101596394 A CN 101596394A CN A2009100884730 A CNA2009100884730 A CN A2009100884730A CN 200910088473 A CN200910088473 A CN 200910088473A CN 101596394 A CN101596394 A CN 101596394A
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- formaldehyde
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Abstract
The invention provides tail gas circulation absorption plant in a kind of methylene reaction and the still-process, but it comprises successively tourie 1, circulating pump 2, condenser 3 and the eluting column 4 of the separatory that links to each other by pipeline.MEA in the tourie has absorbed the formaldehyde tail gas in the eluting column 4 by the conveying of pipe circle pump 2 after condenser 3 coolings, further reaction generates required intermediate.The use of device for absorbing tail gas of the present invention has reduced production cost, has improved product purity, makes that production Technology is more green, environmental protection.
Description
Technical field
The present invention relates to a kind of tail gas circulation absorption plant, specifically, relate to circulation absorption plant and absorption technique thereof at tail gas in the Acetochlor production.
Background technology
In the methene method production technology of Acetochlor, paraformaldehyde and 2-methyl-6-MEA (MEA) reaction at first generates hydroxymethyl derivative, generate N-methylene-2-methyl-6-MEA (hereinafter to be referred as methene) through dehydration again, be used for further preparing Acetochlor.
The synthetic route of methene is as follows:
The preparation process of methene should just can react completely under the excessive situation of formaldehyde, and excessive paraformaldehyde is easy to distillation, condensing unit and plumbing installation are stopped up, production is caused potential safety hazard, also directly influence the purity of Acetochlor product on the other hand.
In the present methylene reaction production technology, the methods such as filtration or distillation that adopt are removed the intact paraformaldehyde of unreacted more from reactant mixture, caused the waste of paraformaldehyde, have increased production cost.
Summary of the invention
The purpose of this invention is to provide formaldehyde tail gas circulation absorption plant in a kind of methylene reaction process and the still-process, it absorbs the formaldehyde in the waste water effectively, and formaldehyde is recycled and absorbs and utilization again, has improved the utilization rate of formaldehyde.
Another object of the present invention provides formaldehyde tail gas circulation absorption process in a kind of methylene reaction process and the still-process, and it has reduced the content of formaldehyde in the waste water by the extraction of MEA to the waste water of reaction generation, has avoided the formaldehyde pollution on the environment.
In order to realize the object of the invention, formaldehyde tail gas circulation absorption plant in a kind of methylene reaction of the present invention and the still-process, but it comprises successively the tourie of the separatory that links to each other by pipeline, circulating pump, condenser and eluting column, described eluting column also have a tail gas import.
Wherein, described tourie is the taper tank body, and it also has a wastewater outlet, absorbs EO in circulation, and standing demix is told water and 2-methyl-6-MEA (MEA) absorption liquid that reaction generates.It not only is used for the storage of circulating absorption solution, has the effect of phase-splitter simultaneously concurrently.
Described condenser is used for the cooling of water, formaldehyde and MEA, is beneficial to increase the absorption rate and the absorbability of formaldehyde tail gas.
Formaldehyde tail gas circulation absorption process in a kind of methylene reaction process of the present invention and the still-process, it comprises the steps:
1) negative pressure (0.08～-0.095MPa) under the condition, water that the methene synthetic reaction produces and the formaldehyde that steams enter eluting column by the tail gas import of eluting column;
2) methyl of the 2-in the tourie-6-MEA (MEA) is carried through pipeline and by circulating pump, by entering eluting column after the condenser cooling, mixes with the mixture of formaldehyde and water;
3) enter tourie after the mixing, and then according to step 2) circulate and carry out;
4) after circulation absorbed the formaldehyde end, material carried out standing demix in the tourie, and water is discharged, and organic facies is used for following batch methene synthetic reaction.
After the condenser cooling of the present invention, its Controllable Temperature is built in 20～25 ℃.
The amount of substance (mole) of the MEA in the tourie of the present invention and tail gas to be absorbed is than being 15: 1～1: 1.This moment, the consumption of MEA can be used as down the inventory of criticizing MEA.
The present invention adopts the eluting column in formaldehyde tail gas circulation absorption plant, be MEA drip washing formaldehyde tail gas with low temperature, formaldehyde is absorbed by MEA and flow in the tourie that contains MEA, thereby effectively improved formaldehyde absorption efficiency and utilization rate, reduce of the pollution of formaldehyde tail gas atmosphere; And the extraction of formaldehyde has reduced the content of formaldehyde in the waste water in the waste water that eluting column produces reaction by MEA, has avoided the formaldehyde pollution on the environment.
In order to guarantee the purity of product, reduce production costs, when hydroxymethyl derivative is produced in first step reaction, need to steam except that formaldehyde.Therefore, formaldehyde tail gas circulation absorption plant passes through verification experimental verification repeatedly in methylene reaction of the present invention and the still-process, compares traditional handicraft in the past, has following remarkable advantage:
1) avoids the paraformaldehyde that distils in the course of reaction to the gathering and stopping up of condensing unit and pipeline, guaranteed production safety;
2) in the reaction under condition of negative pressure, in time removed the water that reaction generates, shortened the reaction time, guaranteed that methylene reaction can carry out more fast;
3) handle by the absorption of circulation absorption system, excessive paraformaldehyde and MEA are further reacted, thereby effectively improved the utilization rate of formaldehyde, saved production cost greatly, reduced the waste of resource;
4) absorb and utilization again by circulation, ensured production safety, reduced production cost, improved the purity of product methanal as tail gas
5) by the extraction of MEA, reduced the content of formaldehyde in the waste water, avoided the formaldehyde pollution on the environment the waste water of reaction generation.
Description of drawings
Fig. 1 is the structural representation of formaldehyde tail gas circulation absorption plant in methylene reaction process of the present invention and the still-process.
Among the figure:
1 tourie, 11 wastewater outlets
2 circulating pumps, 3 condensers
4 absorption towers, 41 exhaust gas inlet
5MEA measuring tank 6 reactors
The specific embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Among the embodiment, symbol kg=kilogram, the L=liter, the mol=mole, ℃=degree centigrade, MPa=MPa, Pa=handkerchief.
As shown in Figure 1, formaldehyde tail gas circulation absorption plant in methylene reaction of the present invention and the still-process, but it comprises successively tourie 1, circulating pump 2, condenser 3 and the eluting column 4 of the separatory that links to each other by pipeline.
Eluting column 4 also has a tail gas import 41, feeds the water of methylene reaction generation and excessive formaldehyde, and it enters eluting column 4 by the spray mode.
Tourie 1 is the taper tank body, and it also has a wastewater outlet 11, is used to discharge waste water.
In the methylene reaction process, use formaldehyde tail gas circulation absorption plant in methylene reaction of the present invention and the still-process, its detailed process is: add 99% MEA 302kg, 99% polymerization inhibitor 7.80kg, 93% paraformaldehyde 108.7kg and 99% triethylamine 1.35kg in the methene synthesis reactor 6 of 500L, after opening electric mixer, utilize reacting kettle jacketing steam to begin slow heating, control reactor internal temperature is between 70～80 ℃, and under this temperature insulation reaction, dissolve fully until material.Then start device for absorbing tail gas.At first open vavuum pump, Adjustment System vacuum is about 0.04MPa, then open the pipe circle pump 2 supporting with MEA tourie 1, make the MEA in the MEA tourie 1 between tubing pump 2, condenser 3, absorption tower 4 and MEA tourie 1, circulate, utilize the MEA (temperature of condenser cooling back MEA generally can be controlled in 20～25 ℃) that circulates to absorb the formaldehyde steam in distilled water and the formaldehyde process.The amount of substance (mole) of the MEA in the tourie and tail gas to be absorbed is than being 4: 1.
After device for absorbing tail gas operation is normal, slowly gas clean-up and be controlled between 0.080～0.085MPa (be negative pressure-0.080～-0.085MPa), decompression steams water; Then again between gas clean-up to 0.090～0.095MPa (be negative pressure-0.090～-0.095MPa), decompression steams excessive formaldehyde.
After the formaldehyde distillation finishes, stop vacuum pump system earlier, utilize the broken sky of nitrogen, then closing MEA circulating pump 2, stop the operation of tail gas absorption system device to normal pressure.
Material is through behind the standing demix in the MEA tourie 1, and lower layer of water is discharged into the wastewater treatment center processing by wastewater outlet, and upper organic phase is delivered in the MEA measuring tank 5 through circulating pump 2, uses as following batch raw material.
Open high-vacuum pump at last, the vacuum of Adjustment System is to 200Pa, and high vacuum state distillation down obtains methene 324.0kg; The content 98.4% of methene, yield 97.91%.
Whole operation process, system's tail gas all have MEA absorption plant treatment and purification, have improved the utilization ratio of formaldehyde, have reduced the consumption of formaldehyde, have purified tail gas simultaneously, have reduced in formaldehyde tail gas and the waste water formaldehyde to the pollution of environment.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (7)
1. tail gas circulation absorption plant in methylene reaction and the still-process, it is characterized in that, but it comprises successively tourie (1), circulating pump (2), condenser (3) and the eluting column (4) of the separatory that links to each other by pipeline, and described eluting column (4) also has a tail gas import (41).
2. tail gas circulation absorption plant according to claim 1 is characterized in that described tourie (1) is the taper tank body, and it has a wastewater outlet (11).
3. formaldehyde tail gas circulation absorption process that adopts claim 1 or 2 described devices, it comprises the steps:
1) under condition of negative pressure, water that the methene synthetic reaction produces and the formaldehyde that steams enter eluting column (4) by the tail gas import (41) of eluting column (4);
2) the 2-methyl-6-MEA in the tourie (1) is carried through pipeline and by circulating pump (2), by entering eluting column (4) after condenser (3) cooling, mixes with the mixture of formaldehyde and water;
3) enter tourie (1) after the mixing, and then according to step 2) circulate and carry out;
4) after circulation absorbed the formaldehyde end, the interior material of tourie (1) carried out standing demix, and water is discharged, and organic facies is used for methylene reaction.
4. method according to claim 3 is characterized in that, the negative pressure in the step 1) is-0.08～-the 0.095MPa condition.
5. according to claim 3 or 4 described methods, it is characterized in that 2-methyl-6-MEA amount of substance in the tourie (1) and tail gas amount of substance ratio to be absorbed are between 15: 1～1: 1.
6. method according to claim 5 is characterized in that, the 2-methyl-molal quantity of 6-MEA in the tourie (1) is 4: 1 with the ratio of the molal quantity of absorbed formaldehyde.
7. method according to claim 3 is characterized in that, described condenser cooling is controlled at 20～25 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100884730A CN101596394B (en) | 2009-07-02 | 2009-07-02 | Tail gas circle absorber in methylene reaction and distillation process and absoption method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100884730A CN101596394B (en) | 2009-07-02 | 2009-07-02 | Tail gas circle absorber in methylene reaction and distillation process and absoption method thereof |
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| CN101596394A true CN101596394A (en) | 2009-12-09 |
| CN101596394B CN101596394B (en) | 2011-09-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114031519A (en) * | 2021-12-08 | 2022-02-11 | 浙江工业大学 | Method for synthesizing N-aryl imine |
| CN114768487A (en) * | 2022-05-07 | 2022-07-22 | 江苏凯美酷碳科技有限公司 | Circulating system for recycling solvent, performing gas-liquid separation and recycling wastewater and operating method thereof |
| CN115466198A (en) * | 2022-07-29 | 2022-12-13 | 南通江山农药化工股份有限公司 | Method for recovering formaldehyde in production of methylene amide pesticides and application thereof |
-
2009
- 2009-07-02 CN CN2009100884730A patent/CN101596394B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114031519A (en) * | 2021-12-08 | 2022-02-11 | 浙江工业大学 | Method for synthesizing N-aryl imine |
| CN114031519B (en) * | 2021-12-08 | 2024-04-26 | 浙江工业大学 | Method for synthesizing N-aryl imine |
| CN114768487A (en) * | 2022-05-07 | 2022-07-22 | 江苏凯美酷碳科技有限公司 | Circulating system for recycling solvent, performing gas-liquid separation and recycling wastewater and operating method thereof |
| CN114768487B (en) * | 2022-05-07 | 2023-11-21 | 江苏凯美酷碳科技有限公司 | Circulating system for solvent recovery gas-liquid separation and wastewater reuse and operation method thereof |
| CN115466198A (en) * | 2022-07-29 | 2022-12-13 | 南通江山农药化工股份有限公司 | Method for recovering formaldehyde in production of methylene amide pesticides and application thereof |
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| CN101596394B (en) | 2011-09-21 |
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Owner name: SHANGYU YINGTAI FINE CHEMICAL CO., LTD. Free format text: FORMER OWNER: BEIJING YINGTAI JIAHE SCIENCE AND TECHNOLOGY CO., LTD. Effective date: 20111031 |
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Effective date of registration: 20111031 Address after: 312369, No. nine, No. 9, Shangyu Industrial Zone, Hangzhou Bay, Zhejiang Patentee after: Shangyu Yingtai Fine Chemical Co., Ltd. Address before: 100085 B308 room, Zhongguancun biological medicine Park, No. 5, Pioneer Road, Beijing, Haidian District Patentee before: Nutrichem Laboratory Co., Ltd. |