CN113018969A - Method for treating emulsion polymerization resin wastewater by using ceramic membrane - Google Patents
Method for treating emulsion polymerization resin wastewater by using ceramic membrane Download PDFInfo
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- CN113018969A CN113018969A CN202110116327.5A CN202110116327A CN113018969A CN 113018969 A CN113018969 A CN 113018969A CN 202110116327 A CN202110116327 A CN 202110116327A CN 113018969 A CN113018969 A CN 113018969A
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Abstract
The invention relates to the technical field of methods for polymerizing resin wastewater, and provides a method for treating emulsion polymerization resin wastewater by using a ceramic membrane, which comprises the following steps: step one, collecting and storing wastewater; step two, demulsification and flocculation: quantitatively pumping the wastewater in the water collecting tank into a reaction tank, and automatically and quantitatively pumping a demulsifier at the stirring speed of 5-200 rpm; step three, solid-liquid separation: the wastewater in the reaction tank automatically flows into a sedimentation tank, the retention time of the wastewater is 0.5-3h, and the upper layer liquid automatically flows into a transfer tank; and step four, filtering by using a ceramic membrane. The invention overcomes the defects of the prior art, has reasonable design and compact structure, and solves the problems of difficult separation and difficult biodegradation of the emulsion polymerization resin wastewater. The invention adopts the ceramic membrane filtration process, has high automation degree, stable equipment operation, high treatment efficiency and simple and quick process flow, and the separated clear liquid can directly reach the standard for recycling.
Description
Technical Field
The invention relates to the technical field of methods for polymerizing resin wastewater, in particular to a method for treating emulsion polymerization resin wastewater by using a ceramic membrane.
Background
Water-soluble emulsion polymerization is an important synthetic resin production method, and is also a mainstream production process of synthetic resins such as ABS resin, polymerized acrylate, styrene-acrylic resin, acrylate-vinyl acetate copolymer and the like. In the production process of the emulsion polymerization resin and the use process of a client, the cleaning of equipment such as a reaction kettle, a pipeline, a container and the like is involved, and a large amount of waste water is generated, wherein the waste water contains high-concentration difficultly-degradable polymers, high-toxicity polymer monomers, emulsion with high dispersity and good stability and a great amount of oily substances. The CODcr of the wastewater is hundreds of thousands or even millions of ppm, and the B/C is lower than 0.1, so the treatment difficulty is very large.
The patent (CN105712432A) proposes source emission reduction and tail end wastewater treatment, and the adopted processes are emulsion breaking, flotation, coagulation, air flotation and biochemical treatment processes. The patent (CN109111031A) adopts the steps of flocculation, precipitation, air flotation, moving bed biofilm reaction, terminal flocculation precipitation, terminal air flotation, Fenton oxidation reaction and the like, and the treatment process is complex. The fluctuation of the quality (pH, temperature, CODcr and the like) of the inlet water can greatly reduce the efficiency of biochemical treatment, and the quality of the outlet water is unstable.
Therefore, the invention provides the method for purifying the wastewater generated in the emulsion polymerization resin production, which has the advantages of stable operation, good treatment effect and high automation degree.
Therefore, a method for treating emulsion polymerization resin wastewater by using a ceramic membrane is provided.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for treating emulsion polymerization resin wastewater by using a ceramic membrane, which overcomes the defects of the prior art, has reasonable design and compact structure, and solves the problems of difficult separation and difficult biodegradation of the emulsion polymerization resin wastewater. The invention adopts the ceramic membrane filtration process, has high automation degree, stable equipment operation, high treatment efficiency and simple and quick process flow, and the separated clear liquid can directly reach the standard for recycling.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for treating emulsion polymerization resin wastewater by using a ceramic membrane is characterized by comprising the following steps: comprises the following steps:
step one, wastewater collection and storage:
collecting waste water generated in the production and use processes of the emulsion polymerization resin, and storing the waste water in a water collecting tank.
Step two, demulsification and flocculation:
quantitatively pumping the wastewater in the water collecting tank into a reaction tank, automatically and quantitatively pumping a demulsifier at a stirring speed of 5-200 rpm, wherein 0-5 kg of demulsifier is used in each ton of wastewater, and the reaction time is 5-60 min; after 5-60 min, automatically and quantitatively pumping a flocculating agent at the stirring speed of 1-50 rpm, wherein 0-5 kg of flocculating agent is used in each ton of wastewater, and the reaction time is 5-60 min;
step three, solid-liquid separation:
the wastewater in the reaction tank automatically flows into a sedimentation tank, the retention time of the wastewater is 0.5-3h, and the liquid on the upper layer automatically flows into a transfer tank. And (3) discharging the bottom sediment periodically, allowing the separated liquid to enter a water collecting tank through solid-liquid separation equipment, and treating the separated solid waste as hazardous waste.
Step four, ceramic membrane filtration:
the transfer pond waste water is automatic to be gone into ceramic membrane filtration equipment, separates out the clear liquid retrieval and utilization up to standard, separates out the concentrate pump and goes into the catch basin.
Further, the demulsifier is one or more of sodium chloride, aluminum nitrate, SP type, AP type, AE type and AR type.
Further, the flocculating agent is one or more of polyaluminium chloride, polyaluminium sulfate, polyferric chloride, polyferric sulfate and polyacrylamide.
Further, the solid-liquid separation equipment is one of a plate-and-frame filter press, a centrifugal machine, a vacuum suction filter machine and a screw stacking machine.
Furthermore, the ceramic film is made of one or more of Al2O3, SiO2, TiO2 and ZrO 2.
Furthermore, the average pore diameter of the ceramic membrane is 0.1-1000 nm.
(III) advantageous effects
The embodiment of the invention provides a method for treating emulsion polymerization resin wastewater by using a ceramic membrane. The method has the following beneficial effects:
1. the method has good treatment effect on the wastewater generated in the production and use processes of the emulsion polymerization resin, and the wastewater has high purification degree and reaches the recycling standard. The wastewater treatment process is simple, the automation degree is high, and the manual operation cost is reduced.
2. The method for treating the emulsion polymerization resin wastewater by using the ceramic membrane solves the problems that the emulsion polymerization resin wastewater is difficult to separate and biodegrade, and realizes resource utilization of the emulsion polymerization resin wastewater.
3. The clear liquid after the ceramic membrane treatment can reach the first grade A standard in DB31-2018 Integrated wastewater discharge Standard, and the CODcr standard value is less than or equal to 50 mg/L.
Drawings
FIG. 1 is a flow chart of the wastewater treatment process of the present invention in FIG. 1.
FIG. 2 is a comparison between before and after the purification of wastewater in example 1 of the present invention.
FIG. 3 shows the mixture after the demulsification and flocculation reactions of example 1 of the present invention.
In the figure: the No. 1 is a waste water stock solution, the No. 2 is a concentrated solution, the No. 3 is a penetrating fluid, and the No. 4 is a mixed solution after demulsification and flocculation reaction.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the attached drawings 1-3, a method for treating emulsion polymerization resin wastewater by using a ceramic membrane,
example 1
A method for treating emulsion polymerization resin wastewater by using a ceramic membrane comprises the following steps:
step one, wastewater collection and storage:
collecting the reaction kettle washing wastewater generated in the production process of the polymerized acrylic ester emulsion, and storing the reaction kettle washing wastewater in a water collecting tank.
Step two, demulsification and flocculation:
quantitatively pumping the wastewater in the water collecting tank into a reaction tank, and automatically and quantitatively pumping a sodium chloride solution with the solid content of 10% under the condition of the stirring speed of 200rpm, wherein the using amount of sodium chloride is 0.5 kg/ton of wastewater, and the reaction time is 5 min; after 5min, automatically and quantitatively pumping 10 percent of polyaluminium chloride mixed solution under the condition of stirring speed of 20rpm, wherein the dosage of the polyaluminium chloride is 0.5 kg/ton of wastewater, and the reaction time is 5 min.
Step three, solid-liquid separation:
the wastewater in the reaction tank automatically flows into a sedimentation tank, the retention time of the wastewater is 2 hours, and the liquid on the upper layer automatically flows into a transfer tank. And (3) periodically discharging the bottom sediment, allowing the separated liquid to enter a water collecting tank through plate-and-frame filter pressing equipment, and treating the separated solid waste as hazardous waste.
Step four, ceramic membrane filtration:
the wastewater in the transfer pool is automatically pumped into TiO2 ceramic membrane filtering equipment with the average aperture of 1nm, and the CODcr of the separated clear liquid is 35mg/L, which can reach the standard for recycling; the separated concentrated liquid is pumped into a water collecting tank.
Example 2
A method for treating emulsion polymerization resin wastewater by using a ceramic membrane comprises the following steps:
step one, wastewater collection and storage:
and collecting the washing wastewater of the reaction kettle generated in the production process of the resin emulsion, and storing the washing wastewater in a water collecting tank.
Step two, demulsification and flocculation:
quantitatively pumping the wastewater in the water collecting tank into a reaction tank, and automatically and quantitatively pumping 10% of aluminum nitrate solution under the condition of stirring speed of 100rpm, wherein the using amount of aluminum nitrate is 5 kg/ton of wastewater, and the reaction time is 60 min; after the interval of 60min, under the condition of stirring speed of 1rpm, 10% of polyaluminium sulfate mixed liquor is automatically and quantitatively pumped in, the dosage of the polyaluminium sulfate is 2 kg/ton of waste water, and the reaction time is 30 min.
Step three, solid-liquid separation:
the wastewater in the reaction tank automatically flows into a sedimentation tank, the retention time of the wastewater is 3h, and the liquid on the upper layer automatically flows into a transfer tank. And (3) discharging the bottom sediment periodically, allowing the separated liquid to enter a water collecting tank through centrifugal machine equipment, and treating the separated solid waste as hazardous waste.
Step four, ceramic membrane filtration:
automatically pumping the wastewater in the transfer pool into ZrO2 ceramic membrane filtering equipment with the average pore diameter of 100nm, and separating clear liquid, wherein the CODcr of the clear liquid is 250 mg/L; the separated concentrated liquid is pumped into a water collecting tank.
Example 3
A method for treating emulsion polymerization resin wastewater by using a ceramic membrane comprises the following steps:
step one, wastewater collection and storage:
collecting the reaction kettle washing wastewater generated in the production process of the polymerized acrylic ester emulsion, and storing the reaction kettle washing wastewater in a water collecting tank.
Step two, demulsification and flocculation:
quantitatively pumping the wastewater in the water collecting tank into a reaction tank, and automatically and quantitatively pumping 3% of SP type demulsifier under the condition of stirring speed of 5rpm, wherein the dosage of the SP type demulsifier is 2.5 kg/ton of wastewater, and the reaction time is 30 min; after the interval of 30min, 5% of polymeric ferric sulfate mixed solution is automatically and quantitatively pumped in under the condition of stirring speed of 50rpm, the dosage of the polymeric ferric sulfate is 5 kg/ton of wastewater, and the reaction time is 60 min.
Step three, solid-liquid separation:
the wastewater in the reaction tank automatically flows into a sedimentation tank, the retention time of the wastewater is 0.5h, and the upper layer liquid automatically flows into a transfer tank. And (3) periodically discharging bottom sediment, allowing the separated liquid to enter a water collecting tank through vacuum filtration equipment, and treating the separated solid waste as hazardous waste.
Step four, ceramic membrane filtration:
automatically pumping the wastewater in the transfer pool into ZrO2/TiO2 ceramic membrane filtering equipment with the average pore diameter of 1000nm, and separating clear liquid, wherein CODcr is 450 mg/L; the separated concentrated liquid is pumped into a water collecting tank.
The samples before and after wastewater purification in example 1 of the present invention were analyzed and the results are shown in Table 1.
TABLE 1 comparison of test results before and after purification of wastewater samples
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A method for treating emulsion polymerization resin wastewater by using a ceramic membrane is characterized by comprising the following steps: the method comprises the following steps:
step one, wastewater collection and storage:
collecting waste water generated in the production and use processes of the emulsion polymerization resin, and storing the waste water in a water collecting tank;
step two, demulsification and flocculation:
quantitatively pumping the wastewater in the water collecting tank into a reaction tank, automatically and quantitatively pumping a demulsifier at a stirring speed of 5-200 rpm, wherein 0-5 kg of demulsifier is used in each ton of wastewater, and the reaction time is 5-60 min; after 5-60 min, automatically and quantitatively pumping a flocculating agent at the stirring speed of 1-50 rpm, wherein 0-5 kg of flocculating agent is used in each ton of wastewater, and the reaction time is 5-60 min;
step three, solid-liquid separation:
the wastewater in the reaction tank automatically flows into a sedimentation tank, the retention time of the wastewater is 0.5-3h, and the liquid on the upper layer automatically flows into a transfer tank. The sediment at the bottom layer is periodically discharged, the separated liquid enters a water collecting tank through solid-liquid separation equipment, and the separated solid waste is treated as hazardous waste;
step four, ceramic membrane filtration:
the transfer pond waste water is automatic to be gone into ceramic membrane filtration equipment, separates out the clear liquid retrieval and utilization up to standard, separates out the concentrate pump and goes into the catch basin.
2. The demulsifier of claim 1, wherein the demulsifier is one or more of sodium chloride, aluminum nitrate, SP type, AP type, AE type, and AR type.
3. The flocculant of claim 1, wherein the flocculant is one or more of polyaluminium chloride, polyaluminium sulfate, polyferric chloride, polyferric sulfate and polyacrylamide.
4. The solid-liquid separation device according to claim 1, wherein the solid-liquid separation device is one of a plate-and-frame filter press, a centrifuge, a vacuum filter press, and a stack screw machine.
5. The ceramic membrane of claim 1, wherein the ceramic membrane is made of one or more of Al2O3, SiO2, TiO2, and ZrO 2.
6. The ceramic membrane of claim 1, wherein the ceramic membrane has an average pore size of 0.1 to 1000 nm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526476A (en) * | 2019-09-25 | 2019-12-03 | 北京华电利源科技有限公司 | The method for handling comprehensive heavy metal wastewater thereby |
| CN211470893U (en) * | 2019-08-16 | 2020-09-11 | 乐陵思盛聚合物材料有限公司 | Waterborne polyurethane sewage treatment recovery unit |
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- 2021-01-28 CN CN202110116327.5A patent/CN113018969A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN211470893U (en) * | 2019-08-16 | 2020-09-11 | 乐陵思盛聚合物材料有限公司 | Waterborne polyurethane sewage treatment recovery unit |
| CN110526476A (en) * | 2019-09-25 | 2019-12-03 | 北京华电利源科技有限公司 | The method for handling comprehensive heavy metal wastewater thereby |
Non-Patent Citations (2)
| Title |
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| 张朝升: "《给水排水工程设备基础》", 31 December 2004, 高等教育出版社 * |
| 黄仲涛: "《无机膜技术及其应用》", 31 March 1999, 中国石化出版社 * |
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Application publication date: 20210625 |