CN111453805B - Process for reducing total nitrogen of methylamine wastewater, device and application thereof - Google Patents
Process for reducing total nitrogen of methylamine wastewater, device and application thereof Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention relates to the technical field of methylamine wastewater treatment, in particular to a process for reducing total nitrogen of methylamine wastewater, a device and an application thereof, wherein the process comprises the following steps: sequentially carrying out adsorption treatment on wastewater generated in methylamine production through a first-stage resin and a second-stage resin in a first treatment system to obtain purified water for output; meanwhile, the first-stage resin of the second treatment system is subjected to resin regeneration treatment by adopting methanol until the requirement is met, and the second-stage resin of the second treatment system is subjected to resin regeneration treatment by adopting hydrochloric acid until the requirement is met; the methanol obtained after the resin regeneration treatment is distilled and condensed in sequence and then is used for the first-stage resin regeneration; and (4) distilling and condensing hydrochloric acid obtained after resin regeneration treatment in sequence, and then using the distilled and condensed hydrochloric acid for second-stage resin regeneration. The technical scheme of the invention solves the problem of difficult biochemical treatment of the wastewater generated in the preparation of methylamine, improves the utilization efficiency of water and reduces the energy consumption.
Description
Technical Field
The invention relates to the technical field of methylamine wastewater treatment, in particular to a process for reducing total nitrogen of methylamine wastewater, and a device and application thereof.
Background
The information disclosed in this background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Methylamine is an important chemical raw material. It is widely used in various departments of national economy, and is a basic raw material for the industries of pesticide, medicine, rubber, tanning, synthetic dye, synthetic resin, chemical fiber, solvent, surfactant, dye, photographic material and the like. The production method of methylamine includes several kinds, but at present, the method generally adopted at home and abroad is the methanol gas-phase catalytic ammoniation process, the methanol ammoniation process uses methanol and ammonia as raw materials, and under the action of catalyst and according to a certain proportion, the methanol ammoniation process can obtain mono-, di-and trimethylamine at the same time, and has a series of reactions:
(1)
(2)
(3)
as can be seen from the above methylamine reaction equation: 1mol of water is generated when 1mol of methanol is consumed, and if the generated water of methylamine cannot be recycled, a large amount of wastewater needs to be discharged, so that a great load is brought to a subsequent wastewater treatment device. Therefore, the treatment and the recycling of the methylamine wastewater can not only reduce the resource waste, but also bring considerable economic benefits. However, the methylamine wastewater is complex in composition, and some nitrogen-containing heterocyclic organic matters are inevitably generated in the catalyst synthesis process, such as: the methylamine wastewater is characterized by high total nitrogen content and difficult biochemical treatment due to the refractory biological substances such as pyrrole, pyridine, thiophene, aniline and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a process for reducing total nitrogen in methylamine wastewater, a device and an application thereof. Specifically, the present invention is realized by the following technical solutions.
In a first aspect of the invention, a device for reducing total nitrogen in methylamine wastewater is disclosed, comprising: the first-stage purification tower A, the second-stage purification tower A, the first-stage purification tower B and the second-stage purification tower B are all filled with adsorption resin so as to carry out adsorption purification treatment on the wastewater.
All be provided with methyl alcohol import, methylamine waste water import on one-level purifying column A, the one-level purifying column B, all be provided with the hydrochloric acid import on second grade purifying column A, the second grade purifying column B, and all set up the water purification export on second grade purifying column A, the second grade purifying column B to the purified water that obtains after the discharge treatment.
And the water outlet of the primary purification tower A is connected with the water inlet of the secondary purification tower A. Namely, the first-stage purification tower A and the second-stage purification tower A are connected in series to carry out secondary treatment on the wastewater, so that the treatment effect is ensured.
And the water outlet of the primary purification tower B is connected with the water inlet of the secondary purification tower B. Namely, the first-stage purification tower B and the second-stage purification tower B are connected in series to carry out secondary treatment on the wastewater, so that the treatment effect is ensured.
The methanol outlets of the first-stage purifying tower A and the first-stage purifying tower B are connected with the regenerated methanol tank, and the regenerated methanol tank, the gas phase outlet of the methanol rectifying tower, the methanol condenser and the refined methanol tank are sequentially connected.
Hydrochloric acid outlets of the second-stage purification tower A and the second-stage purification tower B are connected with a regenerated hydrochloric acid tank, and the regenerated hydrochloric acid tank, a gas phase outlet of the hydrochloric acid rectifying tower, a hydrochloric acid condenser and a hydrochloric acid storage tank are sequentially connected.
Further, the waste liquid outlets of the methanol rectifying tower and the hydrochloric acid rectifying tower are connected with a waste liquid tank, and the residual waste liquid after the methanol and the hydrochloric acid are rectified is discharged from the waste liquid outlets and then enters the waste liquid tank to be collected uniformly.
Further, the methanol inlet is connected with a refined methanol tank so as to recycle the rectified and regenerated methanol.
Further, the hydrochloric acid inlet is connected with a refined alcohol tank so as to recycle the rectified and regenerated hydrochloric acid.
Furthermore, the resins filled in the first-stage purification tower A and the first-stage purification tower B are XDA-1G.
Furthermore, the resins filled in the secondary purification tower A and the secondary purification tower B are LXD-010.
Furthermore, the methanol condenser and the hydrochloric acid condenser are both heat exchange type condensers, and the main function of the condenser is to condense gas-phase methanol and gas-phase hydrochloric acid in the corresponding distillation device into liquid phase, and then collect and recycle the liquid phase.
The second aspect of the invention discloses a process for reducing total nitrogen in methylamine wastewater, which comprises the following steps:
and (3) sequentially carrying out adsorption treatment on the wastewater generated in methylamine production through a first-stage resin and a second-stage resin in a first treatment system to obtain purified water for output.
Meanwhile, the first-stage resin of the second treatment system is subjected to resin regeneration treatment by adopting methanol until the requirement is met, and the second-stage resin of the second treatment system is subjected to resin regeneration treatment by adopting hydrochloric acid until the requirement is met.
And the methanol obtained after the resin regeneration treatment is distilled and condensed in sequence and then is used for the first-stage resin regeneration.
And (4) distilling and condensing hydrochloric acid obtained after resin regeneration treatment in sequence, and then using the distilled and condensed hydrochloric acid for second-stage resin regeneration.
Further, the mass concentration of the methanol regenerated by the first-stage resin is not less than 95%.
Further, the mass concentration of the hydrochloric acid for regenerating the second-stage resin is 2-4.5%.
Further, when the total nitrogen content in the second-stage resin discharge purified water in the first treatment system is higher than a set value, the wastewater treatment is switched to the second treatment system, and the first treatment system starts the regeneration treatment of the resin, so that the regenerated resin meets the set adsorption requirement. The two treatment systems are mutually standby and are circularly transported to perform uninterrupted treatment on the wastewater.
The third aspect of the invention discloses the application of the process and the device for reducing the total nitrogen of methylamine wastewater in the fields of chemical industry, environment and the like, such as the reduction of organic matters in wastewater and the like, and the process and the device can play roles in purifying wastewater and recycling the wastewater.
Compared with the prior art, the invention has the following beneficial effects:
(1) the methylamine wastewater has the characteristics of complex components and containing organic substances such as nitrogen heterocycles and the like, so that the methylamine wastewater is integrally high in total nitrogen content and difficult in biochemical treatment.
(2) According to the invention, two groups of treatment systems are arranged, one group is used for treating wastewater, the other group is used for regenerating resin, and the regeneration of methanol and hydrochloric acid can be realized by a subsequent distillation device and the like after the resin is regenerated, so that the waste of methanol and hydrochloric acid is avoided to a great extent, and the problem of difficult waste liquid treatment caused by resin regeneration is also avoided.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are included to illustrate an exemplary embodiment of the invention and not to limit the invention.
Fig. 1 is a schematic structural diagram of a device for reducing total nitrogen in methylamine wastewater in the embodiment of the invention.
FIG. 2 is a process flow diagram for reducing the total nitrogen in methylamine wastewater in the example of the present invention.
The designations in the above figures represent respectively: 1-first-stage purification tower A, 2-second-stage purification tower A, 3-first-stage purification tower B, 4-second-stage purification tower B, 5-regenerated methanol tank, 6-methanol rectifying tower, 7-methanol condenser, 8-refined alcohol tank, 9-regenerated hydrochloric acid tank, 10-hydrochloric acid rectifying tower, 11-hydrochloric acid condenser, 12-hydrochloric acid storage tank and 13-waste liquid tank.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
For convenience of description, the words "up", "down", "left" and "right" in the present invention, if any, merely indicate that the directions of movement are consistent with those of the drawings, and do not limit the structure, but merely facilitate the description of the invention and simplify the description, rather than indicate or imply that the referenced device or element needs to have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention.
The terms "mounted," "connected," "fixed," and the like in the present invention are to be understood in a broad sense, and for example, the terms "mounted," "connected," and "fixed" may be fixed, detachable, or integrated; the two components can be connected mechanically or electrically, directly or indirectly through an intermediate medium, or connected internally or in an interaction relationship, and the terms used in the present invention should be understood as having specific meanings to those skilled in the art.
As mentioned in the foregoing, the components of the methylamine wastewater are complex, and some nitrogen-containing heterocyclic organic matters are inevitably generated in the catalyst synthesis process, so that the methylamine wastewater is characterized by high total nitrogen content and difficult biochemical treatment as a whole. Therefore, the invention provides a process and a device for reducing the total nitrogen of methylamine wastewater; the invention will now be further described with reference to the drawings and detailed description.
First embodiment
Referring to fig. 1, an apparatus for reducing total nitrogen in methylamine wastewater, comprising: the system comprises a primary purification tower A1, a secondary purification tower A2, a primary purification tower B3 and a secondary purification tower B4, wherein XDA-1G resin is filled in the primary purification tower A1 and the primary purification tower B3; LXD-010 resin is filled in the secondary purification tower A2 and the secondary purification tower B4 to carry out adsorption purification treatment on the wastewater.
And the primary purification tower A1 and the primary purification tower B3 are both provided with a methanol inlet and a methylamine wastewater inlet. Hydrochloric acid inlets are formed in the secondary purification tower A2 and the secondary purification tower B, and purified water outlets are formed in the secondary purification tower A2 and the secondary purification tower B4 to discharge purified water obtained after treatment.
The water outlet of the primary purification tower A1 is connected with the water inlet of the secondary purification tower A2, and the water outlet of the primary purification tower B3 is connected with the water inlet of the secondary purification tower B4; namely, the first-stage purification tower and the second-stage purification tower are connected in series to carry out the second-stage treatment on the wastewater. Wherein: the first-stage purification tower A1 and the second-stage purification tower A2 are a group of purification treatment devices, and the first-stage purification tower B3 and the second-stage purification tower B4 are another group of purification treatment devices.
The methanol feeding aims at resin pretreatment and resin regeneration in the primary purification tower, and the hydrochloric acid feeding aims at resin pretreatment and resin regeneration in the secondary purification tower. Two sets of purification unit connect in parallel and set up, and each other is for subsequent use, and a set of purification unit carries out the processing of waste water, and the regeneration of resin in one-level purification tower, the second grade purification tower is carried out through methyl alcohol and hydrochloric acid respectively to another group, and two sets of purification unit circulation is transported in reverse, guarantees that the processing to waste water can incessant operation.
The methanol outlet 1 of the first-stage purification tower A1 and the methanol outlet of the first-stage purification tower B3 are connected with the inlet of the regenerated methanol tank 5, and the outlet of the regenerated methanol tank 5, the gas phase outlet of the methanol rectifying tower 6, the methanol condenser 7 and the refined methanol tank 8 are connected in sequence. Hydrochloric acid outlets of the second-stage purification tower A2 and the second-stage purification tower B are connected with an inlet of the regenerated hydrochloric acid tank 9, an outlet of the regenerated hydrochloric acid tank 9, a gas phase outlet of the hydrochloric acid rectifying tower 10, the hydrochloric acid condenser 11 and the hydrochloric acid storage tank 12 are connected in sequence, and the methanol condenser 7 and the hydrochloric acid condenser 11 are heat exchange type condensers. And the waste liquid outlets of the methanol rectifying tower 6 and the hydrochloric acid rectifying tower 10 are both connected with a waste liquid tank 13, and the residual waste liquid after the methanol and the hydrochloric acid are rectified is discharged from the waste liquid outlets and then enters the waste liquid tank 13 to be uniformly collected.
The methylamine wastewater enters a primary purification tower, enters a secondary purification tower after being subjected to primary adsorption, the total nitrogen content in the wastewater is reduced to be below a target value, and the obtained purified water enters a methylamine system for recycling. The methanol flowing through the first-stage purification tower enters a regenerated methanol tank for temporary storage, and waits for methanol regeneration in the methanol rectifying tower 6. The hydrochloric acid flowing through the secondary purification tower enters a regenerated hydrochloric acid tank and waits for hydrochloric acid regeneration in the hydrochloric acid rectification tower 10. Further, the methanol rectifying tower is used for treating the methanol from the regenerated methanol tank, and the methanol recovered from the tower top enters a refined alcohol tank for recycling by utilizing the principle that the boiling point of the methanol is lower than that of the organic by-product, and the waste liquid in the tower bottom enters a waste liquid tank.
After the methanol and the hydrochloric acid are used for resin regeneration treatment, a large amount of organic byproducts adsorbed and trapped by resin are dissolved, in order to recycle the methanol and the hydrochloric acid, the methanol and the hydrochloric acid from a regenerated methanol tank and a regenerated hydrochloric acid tank are respectively treated in a methanol rectifying tower and a hydrochloric acid rectifying tower by utilizing the principle that the boiling points of the methanol and the hydrochloric acid are lower than that of the organic byproducts, the gas-phase methanol and the hydrochloric acid recovered from the tower top enter a condenser to be condensed into liquid state and then enter a corresponding storage tank to be stored, and waste liquid (organic byproducts) remained after distillation in the methanol rectifying tower and the hydrochloric acid rectifying tower enter a waste liquid tank to be uniformly temporarily stored and finally sent to a waste water treatment part for centralized treatment.
Second embodiment
The difference from the first embodiment is that: the methanol inlet of the first-stage purification tower A1 and the methanol inlet of the first-stage purification tower B3 are both connected with the refined alcohol tank 8 so as to recycle the rectified and regenerated methanol. And a hydrochloric acid inlet on the secondary purification tower A2 and a hydrochloric acid inlet on the secondary purification tower B are both connected with the refined alcohol tank 8 so as to recycle the rectified and regenerated hydrochloric acid. By recycling the regenerated methanol and hydrochloric acid, the waste of the methanol and hydrochloric acid is avoided to a great extent, and the problem of large enterprise load caused by treatment of a large amount of waste liquid caused by resin regeneration is also avoided.
Third embodiment
A process for reducing total nitrogen in methylamine wastewater is carried out by adopting a device shown in figure 1, and comprises the following steps:
soaking XDA-1G resin in a first-stage purification tower A1 and a first-stage purification tower B3 for 4h by using a methanol solution with the mass concentration of 95%, discharging the methanol solution soaked with the resin into a regenerated methanol tank for temporary storage, enabling the XDA-1G resin to reach a standby state after soaking, and closing methanol feeding.
The LXD-010 resin in the secondary purification tower A2 and the secondary purification tower B4 is washed by hydrochloric acid solution with the mass concentration of 4 percent, and the flow rate of the hydrochloric acid solution is controlled to be 1BVm 3 And h, discharging the hydrochloric acid solution after washing the resin into a regenerated hydrochloric acid tank for temporary storage, enabling the LXD-010 resin to reach a standby state after the washing, and closing the hydrochloric acid feeding.
Methylamine wastewater with total nitrogen of about 220mg/L is treated by the treatment of 20m 3 Flowing through a first-stage purification tower A1 at flow rate, adsorbing macromolecules such as pyridine in methylamine wastewater by XDA-1G resin in the first-stage purification tower A1 to make water enterAnd (3) performing primary adsorption, then enabling the wastewater to enter a secondary purification tower A2, adsorbing organic amines such as dimethylamine and the like in the wastewater by using LXD-010 resin in the secondary purification tower, further purifying the water quality, and reducing the total nitrogen content of the wastewater to be below 20ppm to obtain purified water, and enabling the purified water to enter a methylamine production system for recycling.
In the methylamine wastewater treatment process, the primary purification tower B3 and the secondary purification tower B4 are in a standby state and do not participate in wastewater treatment temporarily. When the total nitrogen content in the wastewater is more than 20ppm, the wastewater at the clean water outlet of the secondary purification tower A2 is sampled and analyzed, and the adsorption saturation of the resin in the primary purification tower A1 and the secondary purification tower A2 is proved. At the moment, the primary purification tower A1 and the secondary purification tower A2 stop wastewater treatment, the primary purification tower B3 and the secondary purification tower B4 start to participate in the wastewater treatment, and the wastewater sequentially passes through the primary purification tower B and the secondary purification tower B, and the wastewater is continuously treated by using the resin in the primary purification tower B and the secondary purification tower B.
And (3) starting regeneration of the resin in the first-stage purification tower A1 and the second-stage purification tower A2, and completely discharging wastewater in the first-stage purification tower A1 and the second-stage purification tower A2. Introducing a methanol solution with the mass concentration of 95% into a first-stage purification tower A1, regenerating the XDA-1G resin, and discharging the methanol solution soaked with the resin into a regenerated methanol tank for temporary storage. Introducing a hydrochloric acid solution with the mass concentration of 4% into a secondary purification tower A2 for washing, regenerating the LXD-010 resin, and discharging the hydrochloric acid solution washed with the resin into a regenerated hydrochloric acid tank for temporary storage; and (4) completely discharging residual solutions in the first-stage purification tower A1 and the second-stage purification tower A2 after the regeneration of the resin is finished, and achieving a standby state.
And (3) feeding the methanol in the regenerated methanol tank into a methanol rectifying tower for rectifying and purifying, condensing the methanol serving as a tower top product, recycling the methanol to a refined alcohol tank for recycling, and feeding residual waste liquid after rectification into a waste liquid tank for temporary storage. Meanwhile, the hydrochloric acid in the regenerated hydrochloric acid tank is sent to a hydrochloric acid rectifying tower for rectification and purification, the hydrochloric acid is condensed as a product at the top of the tower and then recycled to a hydrochloric acid storage tank for recycling, and the residual waste liquid after rectification is sent to a waste liquid tank for temporary storage.
In the embodiment, the methylamine wastewater is adsorbed by using the mode of series resin, the process is safe and environment-friendly, and the adsorption treatment is carried out according to 20m with reference to figure 2 3 Calculating the flow of wastewater inlet water to generate wasteThe liquid flow is about 0.004m 3 H is used as the reference value. The total nitrogen of the treated wastewater is reduced to below 20ppm, thereby reaching the recycling standard. The problem of difficult biochemical treatment of methylamine sewage is solved, the utilization efficiency of water is improved, and the energy consumption is reduced.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. An apparatus for reducing total nitrogen in methylamine wastewater, comprising:
a first-stage purification tower A, a second-stage purification tower A, a first-stage purification tower B and a second-stage purification tower B which are all filled with adsorption resin; the first-stage purification tower A and the second-stage purification tower A are connected in series, and the first-stage purification tower B and the second-stage purification tower B are connected in series;
the primary purification tower A and the primary purification tower B are both provided with a methanol inlet and a methylamine wastewater inlet;
the second-stage purification tower A and the second-stage purification tower B are both provided with a hydrochloric acid inlet and a purified water outlet;
the methanol outlets of the first-stage purification tower A and the first-stage purification tower B are connected with a regenerated methanol tank, and the regenerated methanol tank, the gas-phase outlet of the methanol rectifying tower, the methanol condenser and the refined methanol tank are sequentially connected;
the hydrochloric acid outlets of the second-stage purification tower A and the second-stage purification tower B are connected with the regenerated hydrochloric acid tank, and the regenerated hydrochloric acid tank, the gas phase outlet of the hydrochloric acid rectifying tower, the hydrochloric acid condenser and the hydrochloric acid storage tank are sequentially connected;
the resin filled in the first-stage purification tower A and the first-stage purification tower B is XDA-1G; and the resins filled in the secondary purification tower A and the secondary purification tower B are LXD-010.
2. The apparatus for reducing the total nitrogen of methylamine wastewater as claimed in claim 1, wherein the waste liquid outlets of the methanol rectification tower and the hydrochloric acid rectification tower are connected with a waste liquid tank.
3. The apparatus for reducing the total nitrogen of methylamine wastewater as claimed in claim 1, wherein the methanol inlet is connected to a fine alcohol tank.
4. The apparatus for reducing the total nitrogen of methylamine wastewater as claimed in claim 1, wherein said hydrochloric acid inlet is connected to a fine alcohol tank.
5. The apparatus for reducing the total nitrogen of methylamine wastewater as claimed in claim 1, wherein the methanol condenser and the hydrochloric acid condenser are heat exchange type condensers.
6. A process for reducing the total nitrogen of methylamine wastewater by using the device for reducing the total nitrogen of methylamine wastewater in claim 5, which comprises the following steps:
sequentially carrying out adsorption treatment on wastewater generated in methylamine production through a first-stage resin and a second-stage resin in a first treatment system to obtain purified water for output;
meanwhile, the first-stage resin of the second treatment system is subjected to resin regeneration treatment by adopting methanol until the requirement is met, and the second-stage resin of the second treatment system is subjected to resin regeneration treatment by adopting hydrochloric acid until the requirement is met;
the methanol obtained after the resin regeneration treatment is distilled and condensed in sequence and then is used for the first-stage resin regeneration;
the hydrochloric acid obtained after resin regeneration treatment is distilled and condensed in sequence and then is used for second-stage resin regeneration;
wherein the mass concentration of the methanol regenerated by the first-stage resin is not less than 95 percent; the mass concentration of the hydrochloric acid for regenerating the second-stage resin is 2-4.5%.
7. The process for reducing the total nitrogen content of methylamine wastewater as claimed in claim 6, wherein when the total nitrogen content in the second stage resin effluent purified water in the first treatment system is higher than a set value, the wastewater treatment is switched to the second treatment system, and the first treatment system starts the regeneration treatment of the resin, so that the regenerated resin meets the set adsorption requirement.
8. The use of the apparatus for reducing the total nitrogen of methylamine wastewater as claimed in any one of claims 1 to 4 and/or the process for reducing the total nitrogen of methylamine wastewater as claimed in any one of claims 6 to 7 in chemical and environmental fields.
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| CN109912098A (en) * | 2019-04-01 | 2019-06-21 | 南京简迪环境工程有限公司 | A kind of resin adsorption treatment process of high-salt wastewater containing amine system |
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|---|---|---|---|---|
| US20110077144A1 (en) * | 2006-07-14 | 2011-03-31 | Rayne Dealership Corporation | Regeneration of ion exchange resin and recovery of regenerant solution |
| CN108840497A (en) * | 2018-06-04 | 2018-11-20 | 宿迁新亚科技有限公司 | A method of sewage middle and high concentration ammonia nitrogen is removed with large aperture synthetic resin |
| CN109437462A (en) * | 2018-12-24 | 2019-03-08 | 安徽国星生物化学有限公司 | A kind of processing method of pyridine waste water |
| CN109912098A (en) * | 2019-04-01 | 2019-06-21 | 南京简迪环境工程有限公司 | A kind of resin adsorption treatment process of high-salt wastewater containing amine system |
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