CN114713600A - Treatment method of rectification residues - Google Patents
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- CN114713600A CN114713600A CN202210113430.9A CN202210113430A CN114713600A CN 114713600 A CN114713600 A CN 114713600A CN 202210113430 A CN202210113430 A CN 202210113430A CN 114713600 A CN114713600 A CN 114713600A
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- 238000000034 method Methods 0.000 title claims abstract description 40
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 72
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000004202 carbamide Substances 0.000 claims abstract description 33
- 235000013877 carbamide Nutrition 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 239000007791 liquid phase Substances 0.000 claims abstract description 14
- 239000007790 solid phase Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 230000008569 process Effects 0.000 claims description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 239000002585 base Substances 0.000 claims description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 238000004064 recycling Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002699 waste material Substances 0.000 description 13
- 239000002244 precipitate Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000004821 distillation Methods 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 239000006228 supernatant Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003245 coal Substances 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000003917 carbamoyl group Chemical class [H]N([H])C(*)=O 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010819 recyclable waste Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/78—Recycling of wood or furniture waste
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a rectification residue treatment method, which comprises the following steps: mixing a carbamide aqueous solution and an alkali aqueous solution to obtain a treatment solution; adding the treatment liquid into the rectification residues, uniformly stirring, adjusting the pH value of a system to 7-9, keeping, adding a loosening agent, and uniformly stirring; after standing, carrying out solid-liquid separation, purifying a liquid phase to recover dimethylformamide in the rectification residues, and incinerating a solid phase. The rectification residue treatment method of the invention mixes the rectification residue with the solution containing the carbamide and the alkaline substance, and adds the dispersant, and the mixture is layered after standing, so that the solid phase and the liquid phase are separated, and the liquid phase is further purified and refined by a recovery device to obtain the DMF, thereby realizing the recycling of resources and reducing the secondary pollution.
Description
Technical Field
The invention belongs to the technical field of waste treatment, and particularly relates to a rectification residue treatment method.
Background
With the rapid development of the textile industry, the pollution problem caused by three wastes (waste gas, waste water and waste residue) generated in the industrial development process is getting more serious and the social high attention is also attracted. In recent years, industrial waste gas and waste water problems have been greatly improved in terms of treatment. Waste gas generated in the process of the textile printing and dyeing after-finishing industry is treated by the recyclable waste gas, so that the problem of environmental pollution is solved, and good economic benefit can be obtained from the treatment process of recycling.
However, the disposal of the rectification residue after the recovery treatment is still not well solved. For example, in the coating after-finishing industry, a large amount of DMF (dimethyl formamide) solvent is used as a raw material diluent, waste gas generated after production and drying is treated by a treatment process mode of circulating spraying to obtain organic solvent waste liquid, the organic solvent waste liquid is rectified and purified, secondary hazardous waste of rectification residues can be formed in the rectification process, the characteristics of the DMF after-finishing industry are special, firstly, the rectification residues are evaporated at high temperature to form viscous oily waste residues, the main components of the rectification residues comprise formic acid, polyurethane, color paste, an active agent, a chemical auxiliary agent and wood powder, and calcium bicarbonate, cloth wool, residual dimethyl formamide and the like, and the DMF belongs to a severe pollution source and is greatly harmful to the environment, the ecology and the human bodies of operators; secondly, the oily waste residue contains about 10 percent of dimethyl formamide, and if the oily waste residue is directly disposed, the resource waste is caused.
For the above rectification residue, the conventional operations in the industry at present include the following: firstly, pouring residues into coal by adopting a combustion disposal method, and putting the residues into a boiler together for direct combustion; it has the following disadvantages: the coal is not completely combusted, the chain is easy to block, air cannot be blown, the coal is not breathable, the coal and the air are mixed together, the stirring is not uniform, blocks are formed, the coal is not completely combusted, the environment is not protected, and the energy consumption is wasted. Secondly, adopting a water adding dilution and air-entraining spraying method for combustion; it has the following disadvantages: in the process of spray combustion, a large amount of dense smoke and harmful gas substances are generated, and air and surrounding environment are seriously polluted; and during combustion, tar-like substances are released and can be deposited on the periphery of a boiler furnace and the inner wall of an air duct of the boiler, so that the corrosion is serious, and the danger coefficient is large.
For the above reasons, a method for performing physicochemical treatment of distillation residue relatively environmentally friendly is needed to realize resource recycling.
Disclosure of Invention
In view of the above, in order to overcome the defects of the prior art, the present invention aims to provide a method for treating rectification residues, which can realize the recovery of dimethylformamide in the rectification residues.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for treating rectification residues comprises the following steps: mixing a carbamide aqueous solution and an alkali aqueous solution to obtain a treatment solution; adding the treatment liquid into the rectification residues, uniformly stirring, adjusting the pH value of a system to 7-9, keeping, adding a loosening agent, and uniformly stirring; after standing, carrying out solid-liquid separation, purifying a liquid phase to recover dimethylformamide in the rectification residues, and incinerating a solid phase.
According to some preferred aspects of the invention, the concentration of the aqueous carbamide solution is 8-12%, preferably 10%. The aqueous solution of carboxamide is preferably at 10% concentration, primarily because this concentration range works synergistically with sodium hydroxide to create a slightly alkaline reaction environment, which optimizes the effect of the relaxer.
According to some preferred embodiments of the invention, the base is sodium hydroxide.
According to some preferred aspects of the invention, the aqueous solution of the base has a concentration of 8% to 12%, preferably a concentration of 10%. Preferably, when the concentration of the sodium hydroxide aqueous solution is about 10%, the distillation residue is layered obviously and is convenient to separate, when the concentration is over 10%, the mixed solution is in a relatively obvious mixed state, and relatively clear supernatant liquid does not exist, and in addition, if the concentration of the alkali liquor is too high, the supernatant liquid returns to the distillation and purification system, so that the process is not convenient to control, and when the concentration is about 10%, the supernatant liquid returns to the recovery and purification system, so that the neutral state of the waste liquid is convenient to maintain, and the purification quality is promoted to control.
According to some preferred embodiments of the invention, the mass ratio of the carbonic amide to the alkali in the treatment solution is 1: 0.8-1.2, and the mass ratio of the urea to the alkali is preferably 1:1. the pH value of the mixed solution is taken as an adjustment reference, the mixed solution is wholly controlled to be alkalescent (the pH value is about 8), and the above mass mixing ratio is used according to the blending to achieve the most effective effect.
According to some preferred embodiments of the invention, the distillation residue and the treatment liquid are mixed according to a mass ratio of 1: 1.5-3, and the mass ratio of the distillation residue to the treatment liquid is preferably 1: 2. Because the distillation residues have different viscosities and are rare and thick, the uniform mixing state is maintained according to the final mixed liquid, and the loosening agent is convenient to react and contact with the mixed liquid more fully.
According to some preferred aspects of the invention, the mass ratio of the rectification residue to the carbamide and the alkali is 1: 0.08-0.12: 0.08 to 0.12. Namely, the mass ratio of the rectification residue to the urea is 1: 0.08-0.12, preferably 1: 0.1; the mass ratio of the rectification residue to the alkali is 1: 0.08-0.12, preferably 1: 0.1; and preferably the mass ratio between urea and base is 1:1.
According to some preferred embodiments of the invention, the relaxer is polyacrylamide. The addition amount of the loosening agent is 2.5-3.5% and preferably 3% of the mixed treatment liquid by mass ratio, and the loosening agent has the main functions of mixing and flocculating oily substances in the mixed liquid and separating solid from liquid.
According to some preferred aspects of the invention, the content of formic acid in the rectification residue is 3% to 5%.
According to some preferred embodiments of the invention, the concentration of dimethylformamide in the liquid phase is between 4% and 8%.
The method comprises the steps of controlling the mass ratio of urea to sodium hydroxide in a treatment solution, controlling the acidity and alkalinity of the treatment solution to be alkalescent, preparing the treatment solution in advance according to the mass ratio, loading the rectification residue by using a loading container, adding the calculated treatment solution into the rectification residue, synchronously uniformly mixing the treatment solution and the rectification residue by using stirring equipment, testing the pH value of a mixed solution, supplementing proper materials according to the dilution degree of the mixed solution when the pH value is within a set value range, gradually adding a loosening agent and stirring according to the mass ratio after the materials are in a relatively uniform state, standing the mixed solution after the mixed solution is uniformly mixed and stirred, pumping a supernatant into a storage system for reutilization according to solid-waste separation operation, and uniformly sealing and storing the solid waste for reprocessing.
Compared with the prior art, the invention has the advantages that: the rectification residue treatment method of the invention mixes the rectification residue with the solution containing the carbamide and the alkaline substance, and adds the dispersant, and the mixture is layered after standing, so that the solid phase and the liquid phase are separated, and the liquid phase is further purified and refined by a recovery device to obtain the DMF, thereby realizing the recycling of resources and reducing the secondary pollution.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
The rectification residue treatment method mainly comprises the following steps:
1) dissolving carbamide (urea) in water to prepare a carbamide water solution (with the concentration of 10 percent) for later use; dissolving sodium hydroxide in water to obtain a sodium hydroxide aqueous solution (with the concentration of 10%) for later use; mixing and stirring the carbamide aqueous solution and the sodium hydroxide aqueous solution to form a treatment solution, and cooling to the normal temperature. The carbamide aqueous solution and the alkaline solution are respectively prepared, so that the respective concentration and the added mass ratio can be conveniently controlled, the preparation is more sufficient in the synchronous shunting and mixing process, and the preparation and classified storage are convenient in advance.
2) The distillation residue was placed in a reaction tank (about 5 m)3) Because the viscosity of the rectification residue is high, the treatment solution is added according to the mass ratio of the residue to the treatment solution of 1:2, the treatment solution is uniformly stirred, the pH value of the system is adjusted to be about 8, the loosening agent is added, the mixture is stirred to form a suspension, the suspension is kept stand, solid-liquid separation is carried out, a liquid phase is purified to recover dimethylformamide, and a solid phase is burnt. In actual operation, the solid phase which is primarily separated is subjected to standing and draining operation, then is incinerated, and the liquid obtained by draining is purified and recovered together with the liquid phase which is separated previously.
Wherein the main components in the solid-phase flocculation precipitate are solid in residue, wood powder, cloth hair, CaCO3And part of small molecular PU, auxiliaries, carbides and polymers thereof, the content is about 30 percent; dissolving DMF in the rectification residue in water by utilizing the hygroscopicity of DMF; due to formic acid in the rectification residueThe content is high (about 3% -5%), and the pH value is controlled to be about 8 strictly because the urea is decomposed and ammonia smell overflows due to overhigh pH value, so that the urea can exert greater effect, and the dosage of the urea is generally controlled to be about 0.8Kg for 1T rectification residue.
The rectification residue has complex components, has high content of formic acid except DMF and high-boiling-point auxiliary agent, and can be recycled after dilution and neutralization. Adding urea as catalyst and stirring to promote the reaction of urea, sodium hydroxide and solid in the residue, and the formed floc has relatively slow settling speed (about 3 hr).
Experiments prove that the urea serving as a catalyst has more remarkable treatment effect on the rectification residues after purification of organic wastewater such as printing and dyeing and the like, the removal rate of suspended matters and chromaticity is higher, a large amount of organic solvent (DMF) in the rectification residues can be separated out, and floc precipitates are changed from black to yellow, are non-viscous and dispersed, so that the problems of adhesion and blockage of a feeding mechanism finally entering an incinerator for treatment are reduced and avoided, and the safety of the incinerator is ensured. And the separation ratio can reach: about 60% solid phase and about 40% liquid phase. The treated wastewater has clear water quality, the concentration of DMF in the liquid phase is about 4-8%, and the wastewater can be recycled and purified again, so the economic benefit is considerable. Meanwhile, the smell of the rectification residue is reduced, and the secondary pollution is reduced. The point treatment method has the characteristics of small urea consumption, strong flocculation capacity, small volume of generated precipitates, high separation efficiency and the like, does not need temperature regulation, and has mild reaction conditions, excellent settling property and low comprehensive treatment cost.
Example 1
The rectification residue treatment method in the embodiment comprises the following steps:
1) preparing 10% carbamide water solution.
2) A 20% sodium hydroxide aqueous solution was prepared.
3) And mixing the carbamide aqueous solution and the sodium hydroxide aqueous solution according to the mass ratio of 1:1 to form a treatment solution.
4) Adding a treatment liquid into the rectification residues, and stirring, wherein the mass ratio of the rectification residues to the treatment liquid is 1: 2; and the pH value of the system is controlled to be 8.
Stirring for 20min, adding loosening agent, and stirring for 5 min.
And (4) after the loosening agent is uniformly mixed, sealing the system. Standing for 5h, and pouring out the supernatant after the upper and lower layers are separated.
5) And purifying the supernatant to recover the dimethylformamide, and sending the precipitate into an incinerator for incineration.
Examples 2 to 4
The steps of examples 2 to 4 are substantially the same as those of example 1, and the difference is that the concentrations and the addition amounts of the urea aqueous solution and the alkaline solution are different, and specific reference can be made to the parameters in table 1.
Comparative example 1
This comparative example was substantially identical to the procedure of example 1, except that the pH of the system in this comparative example was controlled to 6 by adjusting the concentrations and the amounts of the aqueous urea solution and the alkali solution.
Comparative example 2
This comparative example is substantially identical to the procedure of example 1, except that the pH of the system in this comparative example was controlled to 10 by adjusting the concentrations and the addition amounts of the aqueous urea solution and the alkali solution.
Comparative example 3
This comparative example is essentially identical to the procedure of example 1, with the difference that the mass ratio of the residue to urea and base in this comparative example is 1: 0.08:0.2, i.e. the addition of excess base.
Comparative example 4
This comparative example is essentially identical to the procedure of example 1, with the difference that the mass ratio of the residue to urea and base in this comparative example is 1: 0.16:0.12, i.e. urea addition excess.
Comparative example 5
This comparative example was substantially identical to example 2 except that the amount of the loosening agent added in this comparative example was 1.5% by mass of the treatment liquid.
Discussion of test and results
In the treatment processes of the above examples and comparative examples, the supernatant was sampled to test its DMF concentration and recorded; sampling the precipitate to test the weight of the precipitate, converting the weight into weight ratio, and calculating the removal rate of suspended matters; and (4) comparing the chroma of the precipitate by using a colorimeter, and confirming the chroma removal efficiency.
TABLE 1 Process parameters and test results
The results of the above table show that: according to the test of different mass ratios of the treatment solution and the adjustment of the mixed mass ratio of the rectification residue and the treatment solution, different pH values of the reaction system are set, the same mixing mode is used, and the condition setting of the embodiment 2 is finally used to confirm that the final treatment effect is optimal, a large amount of DMF solution in the rectification residue can be recycled, and solid and liquid can be separated more efficiently.
Compared with the traditional residue treatment mode, the treatment method is more reasonable, the harmful pollution components of the rectification residue are reduced, the dangerous solid waste is reduced into the common solid waste, and the resource recycling is facilitated.
The invention retreats the rectification residue generated by the rectification and purification of DMF (dimethyl formamide) waste liquid, adds urea aqueous solution and alkaline water into the rectification residue to form precipitate after being easily stirred, and finally achieves the layering of solid and liquid phases through standing for a certain time, the layered solution is transferred to a waste liquid storage tank, the layered aqueous solution contains dimethyl formamide, the concentration of the dimethyl formamide can reach 4-8%, and the partial solution is rectified again, so that the waste of dimethyl formamide can be reduced. The color of the layered solid phase residue turns from black to yellow without viscosity, the layered solid phase residue is scattered in appearance, the layered solid phase residue can be collected uniformly and stored reasonably, and a qualification unit is entrusted to dispose the layered solid phase residue. The invention has the advantages of low treatment cost and simple operation, and is beneficial to cyclic utilization of resources. The process route for treating the residues can realize the recycling of resources, reduce secondary pollution, have obvious social benefit and good economic benefit principle and can realize the recycling of the resources.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. The method for treating the rectification residue is characterized by comprising the following steps of: mixing a carbamide aqueous solution and an alkali aqueous solution to obtain a treatment solution; adding the treatment liquid into the rectification residues, uniformly stirring, adjusting the pH value of a system to 7-9, keeping, adding a loosening agent, and uniformly stirring; after standing, carrying out solid-liquid separation, purifying a liquid phase to recover dimethylformamide in the rectification residues, and incinerating a solid phase.
2. The treatment process according to claim 1, characterized in that the mass ratio of the rectification residue to carbamide and base is 1: 0.08-0.12: 0.08 to 0.12.
3. The treatment method according to claim 1, characterized in that the concentration of the carbamide aqueous solution is 8-12%.
4. The process of claim 1, wherein the base is sodium hydroxide.
5. The treatment method according to claim 3, wherein the concentration of the aqueous alkali solution is 8 to 12%.
6. The treatment method according to claim 1, wherein the mass ratio of the carbonic amide to the alkali in the treatment liquid is 1: 0.8-1.2.
7. The treatment method according to claim 1, wherein the rectification residue is mixed with the treatment liquid in a mass ratio of 1:1.5 to 3.
8. The process of claim 1 wherein the relaxer is polyacrylamide.
9. The treatment method according to claim 1, wherein the mass ratio of formic acid in the rectification residue is 3% -5%.
10. The process according to any one of claims 1 to 9, characterized in that the concentration of dimethylformamide in the liquid phase is between 4% and 8%.
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