CN208517315U - DMAc waste liquid treatment system containing acetic acid - Google Patents

DMAc waste liquid treatment system containing acetic acid Download PDF

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CN208517315U
CN208517315U CN201820899517.2U CN201820899517U CN208517315U CN 208517315 U CN208517315 U CN 208517315U CN 201820899517 U CN201820899517 U CN 201820899517U CN 208517315 U CN208517315 U CN 208517315U
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tower
dmac
acetic acid
pipeline
treatment system
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吴杨
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Tianjin Jingfen Technology Development Co ltd
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Tianjin Jingfen Technology Development Co ltd
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Abstract

The utility model provides a DMAc waste liquid treatment system containing acetic acid, which comprises a pretreatment tower, a low-pressure tower and a high-pressure tower; the top of the pretreatment tower is connected with the material inlet of the low-pressure tower through a pipeline, and the tower kettle of the pretreatment tower is connected with the top of the pretreatment tower in a reflux manner through a pipeline; the top of the low-pressure tower is connected with a DMAc post-treatment device through a pipeline, and the bottom of the low-pressure tower is connected with a material inlet of the high-pressure tower through a pipeline; the tower top of the high-pressure tower is connected with an acetic acid post-treatment device through a pipeline, and the tower kettle of the high-pressure tower is connected with the material inlet of the low-pressure tower through a pipeline. The utility model discloses equipment is simple, can improve the DMAc rate of recovery, reduce treatment cost, need not to add the characteristics that the DMAc circulated use can be guaranteed to the third component.

Description

A kind of DMAc liquid waste treatment system containing acetic acid
Technical field
The utility model belongs to industrial waste water treatment, and in particular to a kind of technique of spandex DMAc liquid waste processing Method separates the mixed solvent of acetic acid and DMAc containing high polymer by the way of variable-pressure rectification.
Background technique
In polyurethane fiber dry spinning technique, three polymerization, spinning and solvent recovery technical process are related generally to.Usual situation Under, DMAc will be used for the dispersion of polymer as solvent in the course of the polymerization process, and after being separated and collected during the spinning process, send To solvent recovery unit.In solvent recovery process, most of DMAc is able to recycle and be recycled, and small part contains high polymer Acetic acid and DMAc mixed solvent will be handled as dangerous waste product.With being gradually improved of environmentally friendly laws and regulations, greenization Work concept is by extensive recognition and acceptance, to acetic acid and DMAc mixed solvent containing high polymer, in a manner of a kind of economical and efficient Separate and recover and recycling design is used, reduces the discharge amount and treating capacity of dangerous waste product, enterprise will be significantly improved Economic benefit and social benefit.
Since DMAc and acetic acid can form maximum azeotrope object, which dictates that being difficult to by the way of conventional distillation that its is thorough Bottom separates.
There are three types of conventional separating technologies.First, by the way of batch fractionating, by DMAc and acetic acid containing high polymer Distillation still rectification process is added in mixed solvent, and tower top obtains a part of lower DMAc solvent of amount containing acetic acid and is recycled, big portion Dividing the mixed solvent of DMAc and acetic acid containing high polymer will discharge at distillation still bottom, and as dangerous waste processing, this leads to a large amount of DMAc Solvent is lost, and yield is low；Second, by the way of lye neutralization, to the in the mixed solvent of DMAc and acetic acid containing high polymer A certain amount of lye is added, the acetic acid of in the mixed solvent is neutralized, then by simple distillation, tower top obtain water and DMAc, distillation still bottom is the salinities such as high polymer and sodium acetate, though this process can significantly improve the DMAc rate of recovery, steam Consumption is big, needs additionally to be added lye, and the salinities such as sodium acetate of generation are difficult to handle, and it is excessively high to eventually lead to recovery cost, not It is economical.Third is the assembly of above two technique, however it remains the defect of above two technique.
Some emerging separating technologies are attempted to improve the recovery utilization rate of DMAc.A kind of method uses weak base resin class material Acetic acid is adsorbed, to achieve the purpose that separating acetic acid and DMAc, this process requirement is using a large amount of fresh production water, and generation largely has Machine waste water, this energy consumption in removal process are high.A kind of method is by being added third component into DMAc, acetic acid, and such as four Vinyl chloride, water etc., DMAc and acetic acid are separately recovered by the way of azeotropic distillation, and the introducing of third component leads to recycling DMAc contains third component impurity thing, influences spandex product quality during DMAc is recycled.
Summary of the invention
A kind of DMAc method for treating waste liquid the purpose of this utility model is to provide spandex containing acetic acid has technical process Simply, the DMAc rate of recovery is high, processing cost is low, is added without third component to guarantee the characteristics of DMAc can be recycled.
The DMAc method for treating waste liquid containing acetic acid of the utility model, separates DMAc and second by the way of variable-pressure rectification Acid, by changing the operating pressure of rectification system, the binary azeotrope for forming DMAc and acetic acid is under different operating pressures Different compositions is presented, achievees the purpose that recycle DMAc and high-purity acetic acid.Specifically include the following steps:
(1) the DMAc waste liquid containing acetic acid is sent into lower pressure column, and lower pressure column overhead extraction DMAc gas phase, lower pressure column tower reactor is formed The low pressure mixed liquor of acetic acid and DMAc azeotropic composition is sent into high-pressure tower；
(2) high-pressure tower overhead extraction acetic acid gas phase, high-pressure tower tower reactor form the high pressure mixing of acetic acid and DMAc azeotropic composition Liquid returns to lower pressure column.
Wherein, it is sent into the composition of the DMAc waste liquid containing acetic acid of lower pressure column are as follows: in mass, DMAc70%- 99.9%, acetic acid 0.1%-30%.The material of the composition can be by the conventional pre- of original solution (generally spandex waste liquid) Processing obtains.
Wherein, the operating pressure of the lower pressure column is 0.001MPaA-0.2MPaA, and the operating pressure of the high-pressure tower is The operating pressure difference of 0.05MpaA-1.0MPaA, lower pressure column and high-pressure tower is not less than 0.05MPaA.The operating pressure difference of two towers Control further improves the composition difference of two tower binary azeotropes, is conducive to the smoothly extraction respectively of DMAc and acetic acid pure phase.
Wherein, the full pressure tower drop of the lower pressure column is no more than 0.005MPaA, and the full pressure tower drop of high-pressure tower is no more than 0.05MPaA advantageously reduces system energy consumption.
Wherein, described 60-185 DEG C of low pressure column overhead temperatures, described 85-230 DEG C of high pressure column overhead temperatures.
Wherein, the lower pressure column overhead reflux ratio is 0.1-6, and the high-pressure tower overhead reflux ratio is 2-35.Improve reflux Than being conducive to improve extraction feed purity.
It wherein, further include handling original solution in pretreater before the DMAc waste liquid containing acetic acid is sent into lower pressure column Process, DMAc gas phase of the overhead extraction of pretreater containing acetic acid form the DMAc waste liquid containing acetic acid, tower reactor after temperature adjustment Extraction is mainly containing the raffinate of high polymer, and high polymer content is preferably no more than 1% in DMAc gas phase of the tower top containing acetic acid.Pretreatment The effect of tower is to remove the high polymer in original solution, the target material composition of acquisition feeding lower pressure column.
Further, the composition of the original solution are as follows: in mass, DMAc 70%-99%, acetic acid 0.1%-30% are high Polymers 0.001%-20%.Original solution composition meets the conventional composition of general spandex waste liquid.
Further, the operating pressure of the pretreater is 0.001MPaA-0.2MPaA, and full tower pressure drop is no more than 0.005MPaA, 105-200 DEG C of tower top temperature, overhead reflux ratio is 0.05-2.The above-mentioned preferred operations condition of pretreater is advantageous In the removal rate of raising high polymer, while reducing energy consumption.
The utility model additionally provides the DMAc liquid waste treatment system containing acetic acid, including pretreater, lower pressure column and high pressure Tower；The tower top of the pretreater is connect by pipeline with the material inlet of the lower pressure column, and the tower reactor of the pretreater is logical Piping is connect with overhead reflux；The tower top of the lower pressure column is connected by the after-treatment device of pipeline and DMAc, the low pressure The tower reactor of tower is connect by pipeline with the material inlet of the high-pressure tower；After the tower top of the high-pressure tower is by pipeline and acetic acid The tower reactor of processing unit connection, the high-pressure tower is connect by pipeline with the material inlet of the lower pressure column.After-treatment device is Refer to other aftertreatment device equipment not contacted directly with the utility model treatment process system, it is also possible to be only conventional Some storage tanks, the system for indicating that the material is sent the utility model enter among other process flows or equipment；For example, conduct The DMAc product of recycling from after the overhead extraction of lower pressure column, the after-treatment device of the DMAc of entrance can be recycled for DMAc storage tank or DMAc recovery and processing system.
Wherein, the pipeline of the reflux connection of the tower reactor of the pretreater and tower top is equipped with the first register, is used for Phegma is heated up, which can be heat exchanger.
Wherein, it is connected with raffinate extraction pipeline on the pipeline that the tower reactor of the pretreater is connect with overhead reflux, is used for Produce the raffinate containing high polymer.Wherein, the connecting tube between the tower top of the pretreater and the material inlet of the lower pressure column Road is equipped with feed surge tank, and for the adjustment and buffering before feeding, the second temperature adjustment dress is additionally provided with before the feed surge tank It sets, for the temperature adjustment before feeding to material, which can be heat exchanger, condenser etc..
Wherein, the tower top of the lower pressure column and/or high-pressure tower has been sequentially connected in series third register and return tank, and described time The discharge port for flowing tank connects two branches a: tower top as lower pressure column or high-pressure tower where reflux branch and the return tank Connection, one connects with the after-treatment device of the connection of the after-treatment device of corresponding DMAc or acetic acid.
Wherein, material conveying power is provided by pump in the system.
Wherein, the tower bottom of the lower pressure column and high-pressure tower is respectively equipped with reboiler.
The utility model removes the high polymer of DMAc and acetic acid in the mixed solvent by pretreater, using variable-pressure rectification method Isolation technics, by changing lower pressure column and high-pressure tower operating pressure respectively, so that the mixed solvent for changing DMAc and acetic acid exists Azeotropic forms in two towers, achievees the purpose that be completely separated two kinds of solvents.The variable-pressure rectification method that the utility model uses can be effective The azeotropic for breaking DMAc and acetic acid, obtains high-purity DMAc and acetic acid, low pressure column overhead DMAc mass fraction up to 99.5% or more, High pressure column overhead quality of acetic acid score is up to 99% or more.Third component need not be added in the utility model into system, to protect Card DMAc will not influence spandex product quality during recycling, and it is generally existing containing high polymer to solve PU Fiber Industry Acetic acid and DMAc liquid waste processing problem improve the rate of recovery of DMAc while significantly reducing spandex factory waste liquid discharging amount, DMAc primary recovery is not less than 90%, and under the premise of guaranteeing spandex product quality, DMAc can be recycled, and looks forward to for spandex Industry creates good economic benefit and social benefit.In addition, optimization design of the utility model by operating condition, Neng Goujin One step reduces energy consumption, and DMAc recovered steam unit consumption can reduce by 25% or more compared with traditional handicraft.
Detailed description of the invention
The attached drawing for constituting a part of the utility model is used to provide a further understanding of the present invention, this is practical new The illustrative embodiments and their description of type are not constituteed improper limits to the present invention for explaining the utility model.? In attached drawing:
Fig. 1 is the flow diagram of the utility model.
Wherein, 1- pretreater；2- lower pressure column；3- high-pressure tower；4- heat exchanger；5- condenser A；6- feed surge tank；7- Reboiler；8- condenser B；9- lower pressure column return tank；10- condenser C；11- high-pressure tower return tank.
Specific embodiment
In order to better understand the utility model, the utility model is described in detail with reference to the accompanying drawing.
Embodiment 1
By taking the waste liquid of spandex manufacturing enterprise discharge as an example, original solution is sent into pretreater 1, each component in original solution Mass fraction is respectively 85%DMAc, 12% acetic acid, 3% high polymer, inlet amount 500Kg/h.1 operating pressure of pretreater 0.02MPaA, full pressure tower drop 0.002MPaA, 130 DEG C of tower top temperature, reflux ratio 0.1.Tower top material is through 5 temperature adjustment of condenser A After be temporarily stored into feed surge tank 6, material group become 87%DMAc, 13% acetic acid.1 tower reactor of pretreater is produced containing high polymer Raffinate, by returning to 1 tower top of pretreater as phegma after 4 temperature adjustment of heat exchanger, a part produces a part as raffinate.
Material in feed surge tank 6 is by being pumped into lower pressure column 2,2 operating pressure 0.02MPaA of lower pressure column, full pressure tower Drop 0.004MPaA, 115 DEG C of tower top temperature, reflux ratio 4.High-purity DMAc gas phase of overhead extraction enters after the condensation of condenser B 8 Then lower pressure column return tank 9 is divided into two: one as phegma and returns to 2 tower top of lower pressure column, the DMAc of another Zhi Zuowei recycling Product extraction.2 column bottom temperature of lower pressure column is 132 DEG C, and 2 kettle liquid of lower pressure column is sent by pumping to high-pressure tower 3.
0.008MPaA drops in 3 operating pressure 0.25MPaA of high-pressure tower, full pressure tower, and 150 DEG C of tower top temperature, reflux ratio 25.Tower Top extraction high purity acetic acid gas phase enters high-pressure tower return tank 11 after the condensation of condenser C 10, is then divided into two: one conducts Phegma returns to 3 tower top of high-pressure tower, an acetic acid product extraction as recycling.3 column bottom temperature of high-pressure tower is 215 DEG C, through height Press 3 kettle liquid kettle liquid of tower by being pumped back to lower pressure column 2.
In above-described embodiment system, low pressure column overhead DMAc mass fraction >=99.5%, DMAc primary recovery >=90%, High pressure column overhead quality of acetic acid score >=99%, DMAc recovered steam unit consumption is 1.15 tons of steam/ton DMAc finished product.
Embodiment 2
By taking the waste liquid of spandex manufacturing enterprise discharge as an example, original solution is sent into pretreater 1, each component in original solution Mass fraction is respectively 94%DMAc, 4% acetic acid, 2% high polymer, inlet amount 1000Kg/h.1 operating pressure of pretreater 0.01MPaA, full pressure tower drop 0.002MPaA, 125 DEG C of tower top temperature, reflux ratio 0.1.Tower top material is through 5 temperature adjustment of condenser A After be temporarily stored into feed surge tank 6, material group become 95.5%DMAc, 4.5% acetic acid.The extraction of 1 tower reactor of pretreater is containing high poly- The raffinate of object, a part by returning to 1 tower top of pretreater as phegma after 4 temperature adjustment of heat exchanger, adopt as raffinate by a part Out.
Material in feed surge tank 6 is by being pumped into lower pressure column 2,2 operating pressure 0.01MPaA of lower pressure column, full pressure tower Drop 0.003MPaA, 88 DEG C of tower top temperature, reflux ratio 2.High-purity DMAc gas phase of overhead extraction enters after the condensation of condenser B 8 Then lower pressure column return tank 9 is divided into two: one as phegma and returns to 2 tower top of lower pressure column, the DMAc of another Zhi Zuowei recycling Product extraction.2 column bottom temperature of lower pressure column is 110 DEG C, and 2 kettle liquid of lower pressure column is sent by pumping to high-pressure tower 3.
0.008MPaA drops in 3 operating pressure 0.3MPaA of high-pressure tower, full pressure tower, and 165 DEG C of tower top temperature, reflux ratio 18.Tower Top extraction high purity acetic acid gas phase enters high-pressure tower return tank 11 after the condensation of condenser C 10, is then divided into two: one conducts Phegma returns to 3 tower top of high-pressure tower, an acetic acid product extraction as recycling.3 column bottom temperature of high-pressure tower is 220 DEG C, through height Press 3 kettle liquid kettle liquid of tower by being pumped back to lower pressure column 2.
In above-described embodiment system, low pressure column overhead DMAc mass fraction >=99.8%, DMAc primary recovery >=92%, High pressure column overhead quality of acetic acid score >=99.2%, DMAc recovered steam unit consumption is 0.98 ton of steam/ton DMAc product.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this Within the spirit and principle of utility model, any modification, equivalent replacement, improvement and so on should be included in the utility model Protection scope within.

Claims (10)

1. a kind of DMAc liquid waste treatment system containing acetic acid, including pretreater, lower pressure column and high-pressure tower；It is characterized in that, institute The tower top for stating pretreater is connect by pipeline with the material inlet of the lower pressure column, and the tower reactor of the pretreater passes through pipeline It is connect with overhead reflux；The tower top of the lower pressure column is connected by the after-treatment device of pipeline and DMAc, the tower of the lower pressure column Kettle is connect by pipeline with the material inlet of the high-pressure tower；The tower top of the high-pressure tower is filled by the post-processing of pipeline and acetic acid Connection is set, the tower reactor of the high-pressure tower is connect by pipeline with the material inlet of the lower pressure column.
2. the DMAc liquid waste treatment system according to claim 1 containing acetic acid, which is characterized in that the tower of the pretreater The pipeline of the reflux connection of kettle and tower top is equipped with the first register.
3. the DMAc liquid waste treatment system according to claim 2 containing acetic acid, which is characterized in that first register For heat exchanger.
4. the DMAc liquid waste treatment system according to claim 1 containing acetic acid, which is characterized in that the tower of the pretreater Raffinate extraction pipeline is connected on the pipeline that kettle is connect with overhead reflux.
5. the DMAc liquid waste treatment system according to claim 1 containing acetic acid, which is characterized in that the tower of the pretreater Connecting pipe between top and the material inlet of the lower pressure column is equipped with feed surge tank, also sets before the feed surge tank There is the second register
6. the DMAc liquid waste treatment system according to claim 5 containing acetic acid, which is characterized in that second register For heat exchanger.
7. the DMAc liquid waste treatment system according to claim 5 containing acetic acid, which is characterized in that second register For condenser.
8. the DMAc liquid waste treatment system according to claim 1 containing acetic acid, which is characterized in that the lower pressure column and/or The tower top of high-pressure tower has been sequentially connected in series third register and return tank, discharge port two branches of connection of the return tank: one Item is connect as reflux branch with the tower top of lower pressure column or high-pressure tower where the return tank, one with the rear place of corresponding DMAc Manage device connection or the after-treatment device connection of acetic acid.
9. the DMAc liquid waste treatment system according to claim 1 containing acetic acid, which is characterized in that material is defeated in the system Power is sent to be provided by pump.
10. the DMAc liquid waste treatment system according to claim 1 containing acetic acid, which is characterized in that the lower pressure column and height The tower bottom of pressure tower is respectively equipped with reboiler.
CN201820899517.2U 2018-06-11 2018-06-11 DMAc waste liquid treatment system containing acetic acid Active CN208517315U (en)

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Publication Number Publication Date
CN208517315U true CN208517315U (en) 2019-02-19

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