CN110124524A - A kind of method of humic acid on cleaning ultrafiltration membrane - Google Patents
A kind of method of humic acid on cleaning ultrafiltration membrane Download PDFInfo
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- CN110124524A CN110124524A CN201910441390.9A CN201910441390A CN110124524A CN 110124524 A CN110124524 A CN 110124524A CN 201910441390 A CN201910441390 A CN 201910441390A CN 110124524 A CN110124524 A CN 110124524A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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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- 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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Abstract
The method of humic acid, is related to fouling membrane cleaning technique field on a kind of cleaning ultrafiltration membrane.The invention aims to solve the problem of that existing physical method cleaning ultrafiltration membrane cannot remove the humic acid chemical method cleaning ultrafiltration membrane in fenestra to be easy to cause the material of ultrafiltration membrane a degree of performance in turn of damaging to be affected.Method: the cleaning material of humic acid is added in the hydrogen peroxide that mass fraction is 0.3%~0.5%, obtain cleaning solution, the ultrafiltration membrane for being attached with humic acid is immersed in 5min~10min in cleaning solution, deionized water is reused after taking-up and rinses 5min~10min, completes the cleaning to humic acid on ultrafiltration membrane.The present invention can get a kind of method for cleaning humic acid on ultrafiltration membrane.
Description
Technical field
The present invention relates to fouling membrane cleaning technique fields.
Background technique
Ultrafiltration membrane can remove the impurity that filtered fluid contains, such as can remove some turbidity of filtered fluid, it can become
The optimal selection of people's Drinking Water Filtration in daily life.The chemical property of PVDF ultrafiltration membrane is good, stain resistance, oxidative resistance
It is excellent, there are good tensile strength and high water flux, therefore obtained swift and violent hair in sewage treatment field in recent years
It opens up and is widely applied.But as PVDF ultrafiltration membrane is in the application of every field, also occurs various fouling membranes in the application
Situation, affects the normal operation of engineering, and expensive film renewal cost frequently to replace membrane module unrealistic.Therefore, effectively
Control membrane fouling and cleaning method be film successful application important link.
The purpose of Membrane cleaning is that contaminated film is cleaned and regenerated by using reasonable cleaning method, destroys film table
The Adsorption of solute layer in face removes the impurity in fenestra road, film is made to be restored to original flux as far as possible.Membrane cleaning method can be divided into
Physical cleaning method and chemical cleaning method.Physical cleaning includes waterpower cleaning, gas pulses cleaning, ultrasonic cleaning etc., can be compared with
The pollutant of film surface is removed well, but cannot remove the pollutant in fenestra road, and cleaning effect is bad.Chemical cleaning is to pass through
Achieve the effect that loosening, dissolution dirt, oxidation of organic compounds, inactivation microorganism remove fouling membrane using chemical agent；It is common clear
Washing method has pickling, alkali cleaning, alcohol to wash, oxidant and fungicide (such as ozone, hypochlorous acid, potassium permanganate) are clear by oxidation reaction
Fouling membrane etc. is washed, but is easy to cause a degree of damage to the material of ultrafiltration membrane, performance is affected.
The development and application of ultrafiltration membrane are with advances in technology, also increasing to the contribution of human society.In ultrafiltration point
From in, when the humic acid solution particle of filtering passes through ultrafiltration membrane, the big particle in solution will be retained by the hole of ultrafiltration membrane
Or absorption, can thus fenestra be made to gradually become smaller, just will form cake layer for a long time, it, will since filter cake gradually thickeies
The appearance for leading to concentration polarization phenomenon will be such that membrane resistance becomes larger when concentration polarization is larger, influence the filtering of super film
Effect.It causes Pore Blocking and declines water flux；In the processing of actual river, we are not only required consideration for how ultrafiltration
Foulant removal on film is clean, also to guarantee that ultrafiltration membrane flux and material, performance are unaffected.Currently, about ultrafiltration membrane corruption
The cost control and cleaning method for growing the material clean method especially cleaning material of acid pollution are also rarely reported.
Summary of the invention
The invention aims to solve existing physical method cleaning ultrafiltration membrane to remove humic acid in fenestra, chemistry
The problem of method cleaning ultrafiltration membrane is easy to cause the material of ultrafiltration membrane a degree of damage and then performance is affected, and mention
For a kind of method of humic acid on cleaning ultrafiltration membrane.
A kind of method of humic acid on cleaning ultrafiltration membrane, is completed according to the following steps:
One, the cleaning material of humic acid is prepared:
1., paraffin and manganese dioxide is placed in conical flask, under the conditions of 75 DEG C~80 DEG C of temperature, with 200r/min~
Revolving speed agitating and heating 1h~1.5h of 300r/min, obtains paraffin manganese dioxide lotion, after paraffin manganese dioxide lotion is cooling
It pours into beaker；
Step 1 1. described in paraffin and manganese dioxide mass ratio be 4~5:1；
2., deionized water is added into beaker 3min~5min is cleaned with the frequency ultrasound of 30kHz~40kHz；
3., repeat step 1 2. 3 times~8 times, then outwell deionized water and paraffin manganese dioxide lotion upper layer be not anti-
The paraffin chip solid and residual manganese dioxide answered, obtain graininess paraffin/manganese dioxide composites, by graininess paraffin/bis-
Manganese oxide compound is dried under the conditions of 30 DEG C~40 DEG C of temperature, and graininess paraffin/manganese dioxide after being dried is compound
Object；
4., dehydrated alcohol, triethylamine and stearoyl are added into graininess paraffin/manganese dioxide composites after drying
Chlorine is stirred to react 3h~4h with the revolving speed of 180r/min~230r/min, pours out supernatant liquid, obtains mixture a；Again to mixing
Carbon tetrachloride is added in object a, 8h~10h is stirred to react with the revolving speed of 100r/min~150r/min, it is complete to graininess paraffin
After dissolution, after being centrifuged 8min~10min with the revolving speed of 4000r/min~5000r/min, remove upper layer centrifugate, 50 DEG C~
It is dried under the conditions of 60 DEG C of temperature, obtains the cleaning material of humic acid；
Step 1 3. described in drying after graininess paraffin/quality of manganese dioxide composites and the body of dehydrated alcohol
Long-pending ratio is 25g~50g:1mL, and the mass ratio of graininess paraffin/manganese dioxide composites and triethylamine after drying is 1:0.5
~1, the ratio of the volume of graininess paraffin/manganese dioxide composites quality and stearyl chloride after drying be 2g~5g:3mL~
The ratio of 5mL, the volume of carbon tetrachloride and graininess paraffin/manganese dioxide composites quality after drying is 0.6mL~1mL:
1g；
Two, the configuration of hydrogen peroxide: deionized water is added in the hydrogen peroxide for being 30% to mass fraction, obtaining mass fraction is
0.3%~0.5% hydrogen peroxide；
Three, on ultrafiltration membrane humic acid cleaning method: the cleaning material of 4. humic acid that step 1 obtains is added to step
In the hydrogen peroxide that rapid two obtained mass fractions are 0.3%~0.5%, cleaning solution is obtained, the ultrafiltration membrane of humic acid will be attached with
It is immersed in 5min~10min in cleaning solution, deionized water is reused after taking-up and rinses 5min~10min, is completed on ultrafiltration membrane
The cleaning of humic acid；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.3%~0.5%
For 20mg~30mg:90mL~105mL.
Beneficial effects of the present invention:
One, the present invention is a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane, using paraffin and two
Manganese oxide adds stearyl chloride to add hydrogen peroxide as cleaning material, and the free radical that cleaning material reaction generates is to Kynoar ultrafiltration
The humic acid of film is cleaned, and is detected to the water flux of polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaning, and testing result is shown:
It is rinsed by the polyvinylidene fluoride (PVDF) ultrafiltration membrane that hydrogen peroxide soaking and washing is crossed using deionized water, on polyvinylidene fluoride (PVDF) ultrafiltration membrane
Humic acid remove substantially, and water flux has significant recovery and increase, has basically reached the original performance of new film, further
It demonstrates cleaning material and cleaning method is effective.
Two, the present invention is a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane, can not only eliminate
Most hydrophobicity humic acid pollutants, the water flux of polyvinylidene fluoride (PVDF) ultrafiltration membrane also restore on polyvinylidene fluoride (PVDF) ultrafiltration membrane
To normal perfect condition, and it is operating method economical and effective, easy to operate, there is biggish application prospect.
Three, the present invention is a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane, main material dioxy
Change manganese, paraffin, stearyl chloride and hydrogen peroxide, cheap, the nontoxic and of the invention cleaning material that has the characteristics that be easy to get is attached to
The surface of polyvinylidene fluoride (PVDF) ultrafiltration membrane, cleaning way can not only reduce the dosage of cleaning solution, reduce scavenging period, Er Qieqing
The one side for washing material hydrophobic is contacted with humic acid, and other end hydrogen peroxide interface starts to degrade, and a small amount of hydrogen peroxide is just
It can be reacted with other cleaning materials, the free radical of generation carries out targeting contact with humic acid first, without humic acid
Local polyvinylidene fluoride (PVDF) ultrafiltration membrane only contacted with hydrogen peroxide, damage of the free radical to polyvinylidene fluoride (PVDF) ultrafiltration membrane be reduced to most
It is small.
The present invention can get a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane.
Detailed description of the invention
Fig. 1 is to be cleaned using a kind of cleaning material for cleaning humic acid on ultrafiltration membrane to humic acid on ultrafiltration membrane
Method flow diagram.
Specific embodiment
Specific embodiment 1: a kind of method for cleaning humic acid on ultrafiltration membrane of present embodiment, is completed according to the following steps:
One, the cleaning material of humic acid is prepared:
1., paraffin and manganese dioxide is placed in conical flask, under the conditions of 75 DEG C~80 DEG C of temperature, with 200r/min~
Revolving speed agitating and heating 1h~1.5h of 300r/min, obtains paraffin manganese dioxide lotion, after paraffin manganese dioxide lotion is cooling
It pours into beaker；
Step 1 1. described in paraffin and manganese dioxide mass ratio be 4~5:1；
2., deionized water is added into beaker 3min~5min is cleaned with the frequency ultrasound of 30kHz~40kHz；
3., repeat step 1 2. 3 times~8 times, then outwell deionized water and paraffin manganese dioxide lotion upper layer be not anti-
The paraffin chip solid and residual manganese dioxide answered, obtain graininess paraffin/manganese dioxide composites, by graininess paraffin/bis-
Manganese oxide compound is dried under the conditions of 30 DEG C~40 DEG C of temperature, and graininess paraffin/manganese dioxide after being dried is compound
Object；
4., dehydrated alcohol, triethylamine and stearoyl are added into graininess paraffin/manganese dioxide composites after drying
Chlorine is stirred to react 3h~4h with the revolving speed of 180r/min~230r/min, pours out supernatant liquid, obtains mixture a；Again to mixing
Carbon tetrachloride is added in object a, 8h~10h is stirred to react with the revolving speed of 100r/min~150r/min, it is complete to graininess paraffin
After dissolution, after being centrifuged 8min~10min with the revolving speed of 4000r/min~5000r/min, remove upper layer centrifugate, 50 DEG C~
It is dried under the conditions of 60 DEG C of temperature, obtains the cleaning material of humic acid；
Step 1 3. described in drying after graininess paraffin/quality of manganese dioxide composites and the body of dehydrated alcohol
Long-pending ratio is 25g~50g:1mL, and the mass ratio of graininess paraffin/manganese dioxide composites and triethylamine after drying is 1:0.5
~1, the ratio of the volume of graininess paraffin/manganese dioxide composites quality and stearyl chloride after drying be 2g~5g:3mL~
The ratio of 5mL, the volume of carbon tetrachloride and graininess paraffin/manganese dioxide composites quality after drying is 0.6mL~1mL:
1g；
Two, the configuration of hydrogen peroxide: deionized water is added in the hydrogen peroxide for being 30% to mass fraction, obtaining mass fraction is
0.3%~0.5% hydrogen peroxide；
Three, on ultrafiltration membrane humic acid cleaning method: the cleaning material of 4. humic acid that step 1 obtains is added to step
In the hydrogen peroxide that rapid two obtained mass fractions are 0.3%~0.5%, cleaning solution is obtained, the ultrafiltration membrane of humic acid will be attached with
It is immersed in 5min~10min in cleaning solution, deionized water is reused after taking-up and rinses 5min~10min, is completed on ultrafiltration membrane
The cleaning of humic acid；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.3%~0.5%
For 20mg~30mg:90mL~105mL.
Present embodiment the utility model has the advantages that
One, present embodiment is a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane, using paraffin
Add hydrogen peroxide as cleaning material with manganese dioxide plus stearyl chloride, the free radical that cleaning material reaction generates is to Kynoar
The humic acid of ultrafiltration membrane is cleaned, and is detected to the water flux of polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaning, testing result
Display: rinsing by the polyvinylidene fluoride (PVDF) ultrafiltration membrane that hydrogen peroxide soaking and washing is crossed using deionized water, and Kynoar is super
Humic acid on filter membrane removes substantially, and water flux has significant recovery and increase, has basically reached the original performance of new film,
It further demonstrates cleaning material and cleaning method is effective.
Two, present embodiment is a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane, can not only go
In addition to hydrophobicity humic acid pollutant most on polyvinylidene fluoride (PVDF) ultrafiltration membrane, the water flux of polyvinylidene fluoride (PVDF) ultrafiltration membrane
It is restored to normal perfect condition, and operating method economical and effective, easy to operate, there is biggish application prospect.
Three, present embodiment is a kind of for cleaning the cleaning material and cleaning method of humic acid on ultrafiltration membrane, main material
Manganese dioxide, paraffin, stearyl chloride and hydrogen peroxide have the characteristics that be easy to get cheap, nontoxic, and the cleaning material of present embodiment
Material is attached to the surface of polyvinylidene fluoride (PVDF) ultrafiltration membrane, and cleaning way can not only reduce the dosage of cleaning solution, subtract scavenging period
It is few, and the hydrophobic one side of cleaning material is contacted with humic acid, and other end hydrogen peroxide interface starts to degrade, a small amount of mistake
Hydrogen oxide can be reacted with other cleaning materials, and the free radical of generation carries out targeting contact with humic acid first, and does not have
There is the local polyvinylidene fluoride (PVDF) ultrafiltration membrane of humic acid only and hydrogen peroxide contact, damage of the free radical to polyvinylidene fluoride (PVDF) ultrafiltration membrane
It is reduced to minimum.
Specific embodiment 2: the differences between this implementation mode and the specific implementation mode are that: step 1. in paraffin and dioxy
The mass ratio for changing manganese is 4~4.5:1.
Other steps are same as the specific embodiment one.
Specific embodiment 3: present embodiment is with specific embodiment one or two differences: step 2. in every time to
The deionized water with paraffin manganese dioxide lotion equivalent is added in beaker.
Other steps are the same as one or two specific embodiments.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: 4. by step 1
The cleaning material of obtained humic acid is added in the hydrogen peroxide that the mass fraction that step 2 obtains is 0.4%~0.5%.
Other steps are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: 4. by step 1
The cleaning material of obtained humic acid is added in the hydrogen peroxide that the mass fraction that step 2 obtains is 0.3%~0.5%, is obtained
The ultrafiltration membrane for being attached with humic acid is immersed in 5min~6min in cleaning solution by cleaning solution, and deionized water punching is reused after taking-up
5min~10min is washed, the cleaning to humic acid on ultrafiltration membrane is completed.
Other steps are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: institute in step 3
The ultrafiltration membrane stated is polyvinylidene fluoride (PVDF) ultrafiltration membrane.
Other steps are identical as specific embodiment one to five.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: institute in step 3
It states the quality of the cleaning material of humic acid and the ratio of the volume of hydrogen peroxide that mass fraction is 0.3%~0.5% is 20mg:
91.5mL。
Other steps are identical as specific embodiment one to six.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one: the configuration of the cleaning material and hydrogen peroxide of humic acid is prepared:
1., the paraffin for being pounded fritter and manganese dioxide particle is placed in conical flask, under the conditions of 80 DEG C of bath temperature,
With the revolving speed agitating and heating 1.5h of 300r/min, paraffin manganese dioxide lotion is obtained, is fallen after paraffin manganese dioxide lotion is cooling
Enter in beaker；
Step 1 1. described in paraffin and manganese dioxide mass ratio be 4:1；
2., deionized water is added into beaker 5min is cleaned with the frequency ultrasound of 40kHz；
3., repeat step 1 2. 5 times, then outwell the unreacted stone of deionized water and paraffin manganese dioxide lotion upper layer
Wax chip solid and residual manganese dioxide, obtain graininess paraffin/manganese dioxide composites, by graininess paraffin/manganese dioxide
Compound is dried under the conditions of 40 DEG C of temperature, graininess paraffin/manganese dioxide composites after being dried；
4., dehydrated alcohol, triethylamine and stearoyl are added into graininess paraffin/manganese dioxide composites after drying
Chlorine is stirred to react 4h with the revolving speed of 200r/min, pours out supernatant liquid, obtains mixture a；Tetrachloro is added into mixture a again
Change carbon, 9h is stirred to react with the revolving speed of 120r/min, after graininess paraffin is completely dissolved, is centrifuged with the revolving speed of 4500r/min
After 10min, upper layer centrifugate is removed, is dried under the conditions of 55 DEG C of temperature, obtains the cleaning material of humic acid；
4. middle centrifugation centrifuge used is flying pigeon board centrifuge to step, and Anting Scientific Instrument Factory, Shanghai manufactures, model:
TDL-5-A, voltage: 220V, maximum capacity 1000mL, frequency: 50Hz, maximum speed: 5000rpm, output power: 300W；
Step 4. in the ratio of volume of graininess paraffin/manganese dioxide composites quality and dehydrated alcohol after drying be
40g:1mL, the mass ratio of graininess paraffin/manganese dioxide composites and triethylamine after drying are 1:0.8, the particle after drying
The ratio of shape paraffin/manganese dioxide composites quality and the volume of stearyl chloride is 2g:5mL, the volume and drying of carbon tetrachloride
The ratio of graininess paraffin/manganese dioxide composites quality afterwards is 0.6mL~1mL:1g.
Two, the configuration of hydrogen peroxide: 90mL deionized water is added in the hydrogen peroxide for being 30% to 1.5mL mass fraction, obtains
The hydrogen peroxide that mass fraction is 0.5%；
Embodiment two: the polyvinylidene fluoride (PVDF) ultrafiltration membrane for being attached with humic acid is prepared according to the following steps:
One, 1g humic acid is added in 1.2L deionized water, after stirring 30min with the revolving speed of 120r/min, through 0.45 μ
The membrane filtration of m obtains humic acid solution a, then the sodium hydroxide that 2mL concentration is 0.02mol/L is added into humic acid solution a
Solution stirs 4d with the revolving speed of 550r/min, obtains the humic acid solution b that pH is 9, concentration is 6mg/L；
Two, the humic acid solution b for obtaining step 1 filters 6h, Kynoar ultrafiltration by polyvinylidene fluoride (PVDF) ultrafiltration membrane
The transmembrane pressure (TMP) of film increases sharply in the short time, the fenestra and humic acid to humic acid blocking polyvinylidene fluoride (PVDF) ultrafiltration membrane
Pie is formed, the polyvinylidene fluoride (PVDF) ultrafiltration membrane for being attached with humic acid is obtained.
Repeat above step three times, respectively obtain the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane for being attached with humic acid, No. two it is poly- inclined
Fluoride ultrafiltration membrane and No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes；Respectively with deionized water to No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane, No. two
Polyvinylidene fluoride (PVDF) ultrafiltration membrane and No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes carry out water flux test, and the water flux obtained is respectively 35L/
m2*h、30L/m2*h、33L/m2* h, and total organic carbon (TOC) is done to the filtered deionized water of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane
Content measuring, test result 0.7466mg/L.
Humic acid purchase described in step 1 recovers fine chemistry industry research institute from Tianjin, net content: 500g, chemistry
Pure, impurity highest content: ash content 10%, moisture 8%, iron-content 0.3% authenticate number of registration: CNAB035-Q；
Polyvinylidene fluoride (PVDF) ultrafiltration membrane described in step 2 is Kynoar (PVDF) plate membrane, having a size of 10cm, film
Average pore size is 100Kda.
Embodiment three: the cleaning method of humic acid on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane for being attached with humic acid prepared by embodiment two is immersed in
5min in cleaning solution reuses deionized water and rinses 5min, completes to humic acid on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after taking-up
Cleaning.And it estimates the humic acid that dark-brown sticks shape on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane and removes substantially；Then deionized water is used
Water flux test is carried out to the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaning, the water flux obtained is 58L/m2* h, and to No.1
The filtered deionized water of polyvinylidene fluoride (PVDF) ultrafiltration membrane is total organic carbon (TOC) content measuring, test result 0.7358mg/L；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
Example IV: the cleaning method of humic acid on No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes for being attached with humic acid prepared by embodiment two are immersed in
5min in cleaning solution reuses deionized water and rinses 5min, completes to humic acid on No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after taking-up
Cleaning.And it estimates the humic acid that dark-brown sticks shape on No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes and removes substantially；Then deionized water is used
Water flux test is carried out to No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after cleaning, the water flux obtained is 61L/m2*h；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
The cleaning method of humic acid on five: No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes of embodiment:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes for being attached with humic acid prepared by embodiment two are immersed in
5min in cleaning solution reuses deionized water and rinses 5min, completes to humic acid on No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after taking-up
Cleaning.And it estimates the humic acid that dark-brown sticks shape on No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes and removes substantially；Then deionized water is used
Water flux test is carried out to No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after cleaning, the water flux obtained is 56L/m2*h；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
Comparative example one: the cleaning method of humic acid on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane for being attached with humic acid prepared by embodiment two is immersed in
5min in cleaning solution reuses deionized water and rinses 5min, then the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after flushing is soaked after taking-up
Enter into cleaning solution 5min, deionized water reused after taking-up and rinses 5min, it completes to rotten on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane
Grow the cleaning of acid.And it estimates the humic acid that dark-brown sticks shape on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane and removes substantially；Then spend from
Sub- water carries out water flux test to the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaning, and the water flux obtained is 59L/m2*h；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
Comparative example two: the cleaning method of humic acid on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane for being attached with humic acid prepared by embodiment two is immersed in
5min in cleaning solution reuses deionized water and rinses 5min, completes to humic acid on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after taking-up
Cleaning.And it estimates the humic acid that dark-brown sticks shape on No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane and removes substantially；Then deionized water is used
Water flux test is carried out to the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaning, the water flux obtained is 66L/m2* h, and to No.1
The filtered deionized water of polyvinylidene fluoride (PVDF) ultrafiltration membrane is total organic carbon (TOC) content measuring, test result 0.7849mg/L；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
The cleaning method of humic acid on three: No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes of comparative example:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes for being attached with humic acid prepared by embodiment two are immersed in
5min in cleaning solution reuses deionized water and rinses 5min, completes to humic acid on No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after taking-up
Cleaning.And it estimates the humic acid that dark-brown sticks shape on No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes and removes substantially；Then deionized water is used
Water flux test is carried out to No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after cleaning, the water flux obtained is 65L/m2*h；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
The cleaning method of humic acid on four: No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes of comparative example:
It is 0.5% that the cleaning material of humic acid prepared by embodiment one, which is added to the mass fraction that embodiment one is prepared,
In hydrogen peroxide, cleaning solution is obtained, No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes for being attached with humic acid prepared by embodiment two are immersed in
5min in cleaning solution reuses deionized water and rinses 5min, completes to humic acid on No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after taking-up
Cleaning.And it estimates the humic acid that dark-brown sticks shape on No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes and removes substantially；Then deionized water is used
Water flux test is carried out to No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after cleaning, the water flux obtained is 59L/m2*h；
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of the humic acid are 0.5% is 20mg:
91.5mL。
It is deionized water that the medium of water flux is tested in above embodiments and comparative example, the method for testing water flux
It is that deionized water is poured on above polyvinylidene fluoride (PVDF) ultrafiltration membrane, makes aperture of the deionized water through polyvinylidene fluoride (PVDF) ultrafiltration membrane voluntarily
Filtering, and not against the effect of external force.
By embodiment three and comparative example two as can be seen that putting No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane in embodiment three
5min is rinsed with deionized water again after impregnating 5min in cleaning material, the water of the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after flushing is logical
Amount is 58L/m2* h, very close to the initial water flux 62L/m of completely new polyvinylidene fluoride (PVDF) ultrafiltration membrane2* h shows cleaned material
The water flux recovery situation of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane is good after material cleaning；And No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane is filtered
Deionized water afterwards is total organic carbon (TOC) content measuring, test result 0.7358mg/L, lower than the total organic carbon before cleaning
(TOC) content 0.7466mg/L shows that cleaning material does not damage the result of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane；
In comparative example two by No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane be placed in cleaning material impregnate 10min after spend again from
Sub- water rinses 5min, and the water flux of the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after flushing is 66L/m2* h is alreadyd exceed completely new poly- inclined
The initial water flux 62L/m of fluoride ultrafiltration membrane2* h shows the water of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaned material clean
Flux recovery is all right and suspects that cleaning material damages the result of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane, in order to verify this
Kind conjecture, does total organic carbon (TOC) content measuring, test result to the filtered deionized water of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane
Illustrate No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane more than total organic carbon (TOC) content 0.7466mg/L before cleaning for 0.7849mg/L
Filtering situation goes wrong, and No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane filters the total organic carbon in deionized water without completion well,
Show that cleaning material does not damage the result of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane.
By example IV and comparative example three as can be seen that putting No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes in example IV
5min is rinsed with deionized water again after impregnating 5min in cleaning material, the water of No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after flushing is logical
Amount is 61L/m2* h, very close to the initial water flux 62L/m of completely new polyvinylidene fluoride (PVDF) ultrafiltration membrane2* h shows cleaned material
The water flux recovery situation of No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes is good after material cleaning；
In comparative example three by No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes be placed in cleaning material impregnate 10min after spend again from
Sub- water rinses 5min, and the water flux of No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after flushing is 65L/m2* h is alreadyd exceed completely new poly- inclined
The initial water flux 62L/m of fluoride ultrafiltration membrane2* h shows the water of No. two polyvinylidene fluoride (PVDF) ultrafiltration membranes after cleaned material clean
Flux recovery is all right and judges cleaning material to No. two according to the total organic carbon of comparative example two (TOC) content measuring
The structure of polyvinylidene fluoride (PVDF) ultrafiltration membrane damages.
By embodiment five and comparative example four as can be seen that putting No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes in embodiment five
5min is rinsed with deionized water again after impregnating 5min in cleaning material, the water of No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after flushing is logical
Amount is 56L/m2* h, the relatively initial water flux 62L/m of completely new polyvinylidene fluoride (PVDF) ultrafiltration membrane2* h shows cleaned material
The water flux recovery situation of No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes is good after material cleaning；
In comparative example four by No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes be placed in cleaning material impregnate 10min after spend again from
Sub- water rinses 5min, and the water flux of No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after flushing is 59L/m2* h is very close completely new
The initial water flux 62L/m of polyvinylidene fluoride (PVDF) ultrafiltration membrane2* h shows No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes after cleaned material clean
Water flux recovery situation it is good.
By embodiment three and comparative example one as can be seen that putting No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane in embodiment three
5min is rinsed with deionized water again after impregnating 5min in cleaning material, the water of the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after flushing is logical
Amount is 58L/m2* h, very close to the initial water flux 62L/m of completely new polyvinylidene fluoride (PVDF) ultrafiltration membrane2* h shows cleaned material
The water flux recovery situation of No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes is good after material cleaning；
In comparative example one by No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane be placed in cleaning material impregnate 5min after spend again from
Sub- water rinses 5min, and repeats to rinse No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane twice, the No.1 Kynoar after rinsing twice
The water flux of ultrafiltration membrane is 59L/m2* h, very close to the initial water flux 62L/m of completely new polyvinylidene fluoride (PVDF) ultrafiltration membrane2* h,
Show that the water flux recovery situation of No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane after cleaned material clean is good.
Table 1:
Table 1 is embodiment one to five, the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane of comparative example one to four, No. two polyvinylidene fluorides
The test result of the water flux of alkene ultrafiltration membrane and No. three polyvinylidene fluoride (PVDF) ultrafiltration membranes.
Table 2:
Table 2 is that the total organic carbon (TOC) of the No.1 polyvinylidene fluoride (PVDF) ultrafiltration membrane of embodiment two, three and comparative example two contains
The test result of amount.
By above embodiments and comparative example it can be concluded that polyvinylidene fluoride (PVDF) ultrafiltration membrane is placed on cleaning material
After middle immersion 5min, the water flux recovery situation of polyvinylidene fluoride (PVDF) ultrafiltration membrane is good；Polyvinylidene fluoride (PVDF) ultrafiltration membrane is placed on cleaning
5min and repeated washing are impregnated twice in material, and the water flux recovery situation and cleaning first difference of polyvinylidene fluoride (PVDF) ultrafiltration membrane are not
It is more, therefore repeated washing is unnecessary twice；Although polyvinylidene fluoride (PVDF) ultrafiltration membrane is placed on after impregnating 10min in cleaning material
The water flux recovery situation of polyvinylidene fluoride (PVDF) ultrafiltration membrane is more preferable, but polyvinylidene fluoride (PVDF) ultrafiltration membrane is placed in cleaning material and is impregnated
It is free to be easy the product after reacting by the cleaning material of humic acid with hydrogen peroxide for the structure of polyvinylidene fluoride (PVDF) ultrafiltration membrane after 10min
The destruction of base, therefore the effect that polyvinylidene fluoride (PVDF) ultrafiltration membrane is placed on immersion 5min in cleaning material is best.
Claims (7)
1. a kind of method of humic acid on cleaning ultrafiltration membrane, it is characterised in that this method is completed according to the following steps:
One, the cleaning material of humic acid is prepared:
1., paraffin and manganese dioxide is placed in conical flask, under the conditions of 75 DEG C~80 DEG C of temperature, with 200r/min~
Revolving speed agitating and heating 1h~1.5h of 300r/min, obtains paraffin manganese dioxide lotion, after paraffin manganese dioxide lotion is cooling
It pours into beaker；
Step 1 1. described in paraffin and manganese dioxide mass ratio be 4~5:1；
2., deionized water is added into beaker 3min~5min is cleaned with the frequency ultrasound of 30kHz~40kHz；
3., repeat step 1 2. 3 times~8 times, then outwell deionized water and paraffin manganese dioxide lotion upper layer be unreacted
Paraffin chip solid and residual manganese dioxide, obtain graininess paraffin/manganese dioxide composites, by graininess paraffin/titanium dioxide
Manganese compound is dried under the conditions of 30 DEG C~40 DEG C of temperature, graininess paraffin/manganese dioxide composites after being dried；
4., dehydrated alcohol, triethylamine and stearyl chloride are added into graininess paraffin/manganese dioxide composites after drying, with
The revolving speed of 180r/min~230r/min is stirred to react 3h~4h, pours out supernatant liquid, obtains mixture a；Again into mixture a
Carbon tetrachloride is added, 8h~10h is stirred to react with the revolving speed of 100r/min~150r/min, is completely dissolved to graininess paraffin
Afterwards, after being centrifuged 8min~10min with the revolving speed of 4000r/min~5000r/min, upper layer centrifugate is removed, at 50 DEG C~60 DEG C
Temperature under the conditions of dry, obtain the cleaning material of humic acid；
Step 1 3. described in drying after graininess paraffin/manganese dioxide composites quality and dehydrated alcohol volume
Than for 25g~50g:1mL, the mass ratio of graininess paraffin/manganese dioxide composites and triethylamine after drying is 1:0.5~1,
The ratio of the volume of graininess paraffin/manganese dioxide composites quality and stearyl chloride after drying is 2g~5g:3mL~5mL,
The ratio of the volume of carbon tetrachloride and graininess paraffin/manganese dioxide composites quality after drying is 0.6mL~1mL:1g；
Two, the configuration of hydrogen peroxide: deionized water is added in the hydrogen peroxide for being 30% to mass fraction, obtaining mass fraction is
0.3%~0.5% hydrogen peroxide；
Three, on ultrafiltration membrane humic acid cleaning method: the cleaning material of 4. humic acid that step 1 obtains is added to step 2
In the hydrogen peroxide that obtained mass fraction is 0.3%~0.5%, cleaning solution is obtained, the ultrafiltration membrane for being attached with humic acid is immersed
5min~10min into cleaning solution reuses deionized water and rinses 5min~10min, completes to humic on ultrafiltration membrane after taking-up
The cleaning of acid；
The ratio of the volume for the hydrogen peroxide that the quality of the cleaning material of the humic acid is 0.3%~0.5% with mass fraction is
20mg~30mg:90mL~105mL.
2. it is according to claim 1 it is a kind of cleaning ultrafiltration membrane on humic acid method, it is characterised in that step 1. in paraffin
Mass ratio with manganese dioxide is 4~4.5:1.
3. it is according to claim 1 it is a kind of cleaning ultrafiltration membrane on humic acid method, it is characterised in that step 2. in every time
The deionized water with paraffin manganese dioxide lotion equivalent is added into beaker.
4. the method for humic acid on a kind of cleaning ultrafiltration membrane according to claim 1, it is characterised in that 4. by step 1
To the cleaning material of humic acid be added in the hydrogen peroxide that mass fraction that step 2 obtains is 0.4%~0.5%.
5. the method for humic acid on a kind of cleaning ultrafiltration membrane according to claim 1, it is characterised in that 4. by step 1
To the cleaning material of humic acid be added in the hydrogen peroxide that mass fraction that step 2 obtains is 0.3%~0.5%, obtain clear
The ultrafiltration membrane for being attached with humic acid is immersed in 5min~6min in cleaning solution by washing lotion, and deionized water flushing is reused after taking-up
5min~10min completes the cleaning to humic acid on ultrafiltration membrane.
6. the method for humic acid on a kind of cleaning ultrafiltration membrane according to claim 1, it is characterised in that described in step 3
Ultrafiltration membrane be polyvinylidene fluoride (PVDF) ultrafiltration membrane.
7. the method for humic acid on a kind of cleaning ultrafiltration membrane according to claim 1, it is characterised in that described in step 3
The ratio of the volume for the hydrogen peroxide that the quality and mass fraction of the cleaning material of humic acid are 0.3%~0.5% is 20mg:
91.5mL。
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| CN201910702109.2A CN110270227B (en) | 2019-05-24 | 2019-07-31 | Method for cleaning humic acid on ultrafiltration membrane |
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| CN112624502A (en) * | 2020-12-15 | 2021-04-09 | 长春工程学院 | System and method for ultrasonic-assisted recovery of carbon, nitrogen and phosphorus resources in urban sewage |
| CN115041021A (en) * | 2022-05-10 | 2022-09-13 | 天津城建大学 | Molybdenum disulfide composite membrane, and preparation method, cleaning method and application thereof |
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| JP3380114B2 (en) * | 1996-04-25 | 2003-02-24 | 株式会社クボタ | Backwashing method for membrane separation equipment |
| CN102716682B (en) * | 2012-06-29 | 2014-05-14 | 中国科学院上海高等研究院 | Application of hollow fiber nano-filtration membrane in removal of As in water body |
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2019
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| CN112624502A (en) * | 2020-12-15 | 2021-04-09 | 长春工程学院 | System and method for ultrasonic-assisted recovery of carbon, nitrogen and phosphorus resources in urban sewage |
| CN112624502B (en) * | 2020-12-15 | 2021-11-05 | 长春工程学院 | System and method for ultrasonic-assisted recovery of carbon, nitrogen and phosphorus resources in urban sewage |
| CN115041021A (en) * | 2022-05-10 | 2022-09-13 | 天津城建大学 | Molybdenum disulfide composite membrane, and preparation method, cleaning method and application thereof |
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