CN110237715B - Membrane flux recovery method after PCB wastewater filtration by separation membrane - Google Patents
Membrane flux recovery method after PCB wastewater filtration by separation membrane Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/164—Use of bases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/168—Use of other chemical agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Hydrology & Water Resources (AREA)
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Abstract
The invention relates to a membrane flux recovery method after PCB wastewater is filtered by a separation membrane, which comprises one-time physical cleaning and three-time chemical cleaning. According to the membrane flux recovery method after PCB wastewater is filtered by the separation membrane, only isobaric flushing is used in the cleaning process, and a back flushing device is not needed; the cleaning water is clean RO product water which is free of hardness, metal ions and residual chlorine, so that secondary pollution of the membrane element is avoided; the cleaning working pressure is lower than or equal to 4bar, the energy consumption is low, and the operation is simple. The flux of the special separation membrane polluted by the PCB wastewater is completely recovered by combining physical cleaning and chemical cleaning and selecting a specific cleaning agent, so that the use cost of the membrane component is greatly reduced, the service life of the membrane component is prolonged, and the application market of the membrane component is expanded.
Description
Technical Field
The invention relates to a membrane flux recovery method after PCB wastewater is filtered by a separation membrane.
Background
With the rapid development of industrialization, the problem of water pollution brought by the rapid development of industrialization seriously affects the living environment of people and restricts the development of social economy, so that the membrane separation technology is rapidly developed and widely applied as a high and new separation technology in the field of water treatment. The membrane separation is to realize the separation, purification and concentration of different components of feed liquid by utilizing the selective permeability of a membrane, and the membrane separation is different from the traditional filtration in that the membrane can carry out separation in a molecular range, and the process is a physical process, does not generate phase change and does not need to add an auxiliary agent. The membrane separation technology is a high-tech engineering technology for solving major problems of energy, resources, environment and the like by human beings at present, but in practical engineering application, two major factors of concentration polarization and membrane pollution restrict the popularization and application of the membrane separation technology. After membrane fouling, membrane flux decreases, separation efficiency decreases, losses increase, and membrane elements are expensive to replace, and it is necessary to find an efficient membrane cleaning solution. Due to the complexity of the various fluid components and the variability in membrane material properties, there has not been a specific targeted cleaning protocol to date. Often the fouling is progressive, if not controlled as early as possible, and the fouling will damage the membrane elements in a relatively short time, so that the membrane elements must be cleaned in time. Therefore, whether the membrane pollution problem can be solved, and whether the membrane can be effectively cleaned and the performance of the membrane can be better and quickly recovered is one of the key factors of whether the membrane technology can be widely applied in industrialization. At present, Printed Circuit Board (PCB) market greatly increased, however, can produce a large amount of copper-containing waste water in the PCB production process, quality of water is complicated, and the main pollutant in the waste water has: acid-base, suspended matters, copper, nickel, ammonia nitrogen, a comprehensive agent NH4OH, EDTA and other organic matters; the membrane separation technology is used for treating the PCB wastewater, so that the use of an extracting agent and the discharge of pollutants are reduced, the copper recovery rate is high, the effluent is easier to treat and can be recycled or discharged in zero, and the energy-saving, low-consumption and cost-saving effects are achieved. However, in the actual operation process of treating PCB wastewater by the membrane separation technology, because the PCB wastewater contains a large amount of sludge and runs for a long time, the PCB wastewater is polluted by suspended matters or indissolvable salts in inlet water, membrane blockage is inevitable, membrane flux is reduced by about 20%, membrane elements need to be cleaned at the moment, and the membrane flux cannot be recovered by adopting conventional physical cleaning.
Disclosure of Invention
The invention aims to provide a membrane flux recovery method after PCB wastewater is filtered by a separation membrane.
The invention discloses a membrane flux recovery method after PCB wastewater is filtered by a separation membrane, which comprises the following steps: s101: introducing washing water into a washing water tank of separation equipment, starting the washing equipment to carry out low-pressure circulating washing, measuring the conductivity of water at a discharge port by using a conductivity meter, and stopping washing when the conductivity of the water at the discharge port is 10-20% of the conductivity of water inlet; s102: adding sodium hydroxide powder into water, adjusting the pH value to 11.5-12.5 to obtain a first cleaning solution, starting cleaning equipment for circular cleaning, sampling and detecting the conductivity of the first cleaning solution at a discharge port after cleaning, then draining a cleaning tank, cleaning with water at low pressure, and filling the cleaning tank with water; s103: adding sodium dodecyl sulfate powder into water, then adding sodium hydroxide to adjust the pH value of the solution to 10.5-11.5 to obtain a second cleaning solution, then starting cleaning equipment to carry out circulating cleaning, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the mass ratio of the sodium dodecyl sulfate powder to the water is 1: 1000; s104: adding disodium citrate powder into water, then adding sodium hydroxide to adjust the pH value of the disodium citrate powder to 9.0-11.0 to obtain a third cleaning solution, then starting cleaning equipment to carry out circulating cleaning, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the weight ratio of the water to the disodium citrate powder is 2000: 1; s105: starting cleaning equipment to carry out low-pressure circulating cleaning, then operating the separation equipment under the condition that a cleaning water discharge valve is opened, measuring the conductivity of water at a discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 10-20% of the conductivity of water inlet.
According to the membrane flux recovery method after PCB wastewater is filtered by the separation membrane, only isobaric flushing is used in the cleaning process, and a back flushing device is not needed; the cleaning water is clean RO product water which is free of hardness, metal ions and residual chlorine, so that secondary pollution of the membrane element is avoided; the cleaning working pressure is lower than or equal to 4bar, the energy consumption is low, and the operation is simple. The flux of the special separation membrane polluted by the PCB wastewater is completely recovered by combining physical cleaning and chemical cleaning and selecting a specific cleaning agent, so that the use cost of the membrane component is greatly reduced, the service life of the membrane component is prolonged, and the application market of the membrane component is expanded.
In addition, the membrane flux recovery method after PCB wastewater is filtered by the separation membrane can also have the following additional technical characteristics:
further, in the step S101, the low-pressure circulation flushing time is 15min to 25min, and the water inlet pressure is 3bar to 4 bar.
Further, in the step S101, the low-pressure circulation washing is performed 2 to 3 times.
Further, in the step S102, the time of the circulation cleaning is 0.8h to 1.2 h.
Further, in the step S103, the time of the circulation cleaning is 0.8h to 1.2 h.
Further, in the step S104, the time of the circulation cleaning is 0.8h to 1.2 h.
Further, the water is product water or deionized water which is free of metal ions and residual chlorine and is subjected to hardness removal.
Further, the cleaning temperature is 25 ℃ to 30 ℃.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and not to be construed as limiting the invention.
Example 1
Embodiment 1 provides a membrane flux recovery method after PCB wastewater is filtered by a separation membrane, comprising the following steps:
(1) introducing the flushing water into a flushing water tank of the separation equipment, starting the flushing equipment to perform low-pressure circulating flushing, measuring the conductivity of the water at the discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 10% of the conductivity of the water at the inlet. Wherein the low-pressure circulating flushing time is 25min, the water inlet pressure is 3bar, and the low-pressure circulating flushing is carried out for 3 times. The water is product water which is free of metal ions and residual chlorine and has hardness removed, and the cleaning temperature is 25 ℃.
(2) Adding sodium hydroxide powder into water, adjusting the pH value to 12.5 to obtain a first cleaning solution, starting cleaning equipment for circular cleaning for 0.8h, sampling and detecting the conductivity of the first cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, cleaning with water at low pressure, and filling the cleaning tank with water.
(3) Adding sodium dodecyl sulfate powder into water, then adding sodium hydroxide to adjust the pH value to 11.5 to obtain a second cleaning solution, then starting cleaning equipment to carry out circulating cleaning for 0.8h, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the mass ratio of the sodium dodecyl sulfate powder to the water is 1: 1000.
(4) Adding disodium citrate powder into water, then adding sodium hydroxide to adjust the pH value to 9.0 to obtain a third cleaning solution, then starting cleaning equipment to carry out circulating cleaning for 1.2h, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the weight ratio of the water to the disodium citrate powder is 2000: 1.
(5) Starting a cleaning device to perform low-pressure circulation cleaning, then operating the separation device under the condition that a cleaning water discharge valve is opened, measuring the conductivity of the water at a discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 20% of the conductivity of the water at the inlet.
Example 2
Embodiment 2 provides a membrane flux recovery method after PCB wastewater is filtered by a separation membrane, which includes the following steps:
(1) introducing the washing water into a washing water tank of the separation equipment, starting the washing equipment to carry out low-pressure circulating washing, measuring the conductivity of the water at the discharge port by using a conductivity meter, and stopping washing when the conductivity of the water at the discharge port is 20% of the conductivity of the water at the inlet. Wherein the low-pressure circulating flushing time is 15min, the water inlet pressure is 4bar, and the low-pressure circulating flushing is carried out for 2 times. The water is deionized water which is used for removing hardness and does not contain metal ions and residual chlorine, and the cleaning temperature is 30 ℃.
(2) Adding sodium hydroxide powder into water, adjusting the pH value to 11.5 to obtain a first cleaning solution, starting cleaning equipment for circular cleaning for 1.2h, sampling and detecting the conductivity of the first cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, cleaning with water at low pressure, and filling the cleaning tank with water.
(3) Adding sodium dodecyl sulfate powder into water, then adding sodium hydroxide to adjust the pH value to 10.5 to obtain a second cleaning solution, then starting cleaning equipment to carry out circulating cleaning for 1.2h, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the mass ratio of the sodium dodecyl sulfate powder to the water is 1: 1000.
(4) Adding disodium citrate powder into water, then adding sodium hydroxide to adjust the pH value to 11.0 to obtain a third cleaning solution, then starting cleaning equipment to carry out circulating cleaning for 0.8h, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the weight ratio of the water to the disodium citrate powder is 2000: 1.
(5) Starting a cleaning device to perform low-pressure circulating cleaning, then operating the separation device under the condition that a cleaning water discharge valve is opened, measuring the conductivity of the water at a discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 10% of the conductivity of the water at the inlet.
Example 3
Embodiment 3 provides a membrane flux recovery method after PCB wastewater is filtered by a separation membrane, comprising the following steps:
(1) introducing the flushing water into a flushing water tank of the separation equipment, starting the cleaning equipment to perform low-pressure circulating flushing, measuring the conductivity of the water at the discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 15% of the conductivity of the water at the inlet. Wherein the low-pressure circulating flushing time is 20min, the water inlet pressure is 4bar, and the low-pressure circulating flushing is carried out for 2 times. The water is product water which is free of metal ions and residual chlorine and has hardness removal, and the cleaning temperature is 27 ℃.
(2) Adding sodium hydroxide powder into water, adjusting the pH value to 12 to obtain a first cleaning solution, starting cleaning equipment for circular cleaning for 1h, sampling and detecting the conductivity of the first cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, cleaning with water at low pressure, and filling the cleaning tank with water.
(3) Adding sodium dodecyl sulfate powder into water, then adding sodium hydroxide to adjust the pH value to 11 to obtain a second cleaning solution, then starting cleaning equipment to carry out circulating cleaning for 1h, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the mass ratio of the sodium dodecyl sulfate powder to the water is 1: 1000.
(4) Adding disodium citrate powder into water, then adding sodium hydroxide to adjust the pH value to 10.0 to obtain a third cleaning solution, then starting cleaning equipment to carry out circulating cleaning for 1h, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the weight ratio of the water to the disodium citrate powder is 2000: 1.
(5) Starting a cleaning device to carry out low-pressure circulating cleaning, then operating the separation device under the state that a cleaning water discharge valve is opened, measuring the conductivity of the water at a discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 15% of the conductivity of the water at the inlet.
It is worth noting that: 1. the rinse water of the system must be clean, hardness-removed, RO product water or deionized water free of metal ions and residual chlorine to prevent secondary contamination of the membrane elements. 2. The water for preparing the chemical cleaning solution must be RO product water or deionized water free of metal ions and residual chlorine for removing hardness. The temperature and pH should be adjusted to the desired values. 3. Before all cleaning fluid enters the membrane element, thorough and uniform mixing is required, the pH value is adjusted according to a target value, and the temperature is stabilized according to the target temperature value. 4. In the initial stage, the initial reflux is drained before the cleaning solution is returned to the system cleaning tank to avoid dilution of the cleaning solution by water trapped in the system. 5. The equipment is started and the cyclic cleaning is carried out for one hour. 6. The working pressure of the cleaning is lower than or equal to 4bar, and the final flushing is continued until the flushing water is clean and does not contain any foam and cleaning agent residues. 7. Confirmation of the end of the rinse: an operator can sample by using a clean sampling bottle, shake the sample evenly, monitor the residual conditions of the detergent and the foam in the flushing water at the discharge port, and simultaneously measure whether the conductivity of the flushing water at the discharge port is within 10% of that of the inlet water by using a conductivity meter to confirm the flushing end point; the pH can also be measured to compare if the pH of the discharge outlet flush water is close to the pH of the influent water.
The flux and salt rejection for each membrane element in each cleaning step are shown in table 1.
TABLE 1
The comparative states of the cleaning solutions are shown in Table 2.
TABLE 2
As can be seen from tables 1 and 2, the flux of the membrane element is not recovered after the physical cleaning, the RO cleaning water is changed from clear and transparent to the color of the PCB wastewater during the physical cleaning process, and the conductivity is increased, which indicates that the physical cleaning only washes away the PCB wastewater and the pollutants remained on the surfaces of the system and the membrane element; the flux of the membrane element is still not recovered after the membrane element is cleaned by the first cleaning solution, the first cleaning solution is changed into the color of PCB wastewater from clear and transparent, and the conductivity is increased, which indicates that the first cleaning solution cleans part of pollutants on the surface of the membrane element; and the flux of the membrane element is restored to a new membrane state through the second cleaning solution and the third cleaning solution, which indicates that the second chemical cleaning and the third chemical cleaning thoroughly clean the pollutants. It follows that membrane cleaning, as well as membrane fouling, is a progressive process. The flux of the special separation membrane polluted by the PCB wastewater is completely recovered by combining physical cleaning and chemical cleaning and selecting a specific cleaning agent, so that the use cost of the membrane component is greatly reduced, the service life of the membrane component is prolonged, and the application market of the membrane component is expanded.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (4)
1. A membrane flux recovery method after PCB wastewater is filtered by a separation membrane is characterized by comprising the following steps:
s101: introducing washing water into a washing water tank of separation equipment, starting the washing equipment to carry out low-pressure circulating washing, measuring the conductivity of water at a discharge port by using a conductivity meter, and stopping washing when the conductivity of the water at the discharge port is 10-20% of the conductivity of water inlet;
s102: adding sodium hydroxide powder into water, adjusting the pH value to 11.5-12.5 to obtain a first cleaning solution, starting cleaning equipment for circular cleaning, sampling and detecting the conductivity of the first cleaning solution at a discharge port after cleaning, then draining a cleaning tank, cleaning with water at low pressure, and filling the cleaning tank with water;
s103: adding sodium dodecyl sulfate powder into water, then adding sodium hydroxide to adjust the pH value of the solution to 10.5-11.5 to obtain a second cleaning solution, then starting cleaning equipment to carry out circulating cleaning, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the mass ratio of the sodium dodecyl sulfate powder to the water is 1:1000, parts by weight;
s104: adding disodium citrate powder into water, then adding sodium hydroxide to adjust the pH value of the disodium citrate powder to 9.0-11.0 to obtain a third cleaning solution, then starting cleaning equipment to carry out circulating cleaning, sampling and detecting the conductivity of the second cleaning solution at a discharge port after cleaning is finished, then draining a cleaning tank, carrying out low-pressure cleaning by using water, and filling water into the cleaning tank; wherein the weight ratio of the water to the disodium citrate powder is 2000: 1;
s105: starting cleaning equipment to carry out low-pressure circulating cleaning, then operating the separation equipment in a state that a cleaning water discharge valve is opened, measuring the conductivity of water at a discharge port by using a conductivity meter, and stopping flushing when the conductivity of the water at the discharge port is 10-20% of the conductivity of water inlet;
in the step S101, the low-pressure circulating flushing time is 15 min-25 min, and the water inlet pressure is 3 bar-4 bar;
in the step S101, low-pressure circulation washing is carried out for 2 to 3 times;
the water is product water or deionized water which is free of metal ions and residual chlorine and is used for removing hardness;
the cleaning temperature is 25-30 ℃.
2. The method for recovering membrane flux after PCB wastewater is filtered by the separation membrane according to claim 1, wherein in the step S102, the time for circulating cleaning is 0.8h to 1.2 h.
3. The method for recovering membrane flux after PCB wastewater is filtered by the separation membrane of claim 1, wherein in the step S103, the time for circulating cleaning is 0.8h to 1.2 h.
4. The method for recovering membrane flux after PCB wastewater is filtered by the separation membrane of claim 1, wherein in the step S104, the time for circulating cleaning is 0.8h to 1.2 h.
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