CN109731553A - A kind of TiO2The preparation method of@Mofs modified glass-fiber film - Google Patents
A kind of TiO2The preparation method of@Mofs modified glass-fiber film Download PDFInfo
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Abstract
A kind of TiO disclosed by the invention2The preparation method of@Mofs modified glass-fiber film, the following steps are included: epoxychloropropane and Strong oxdiative sodium solution is taken to be added in beaker, in the above solution by glass fibre membrane, 10-12h is reacted at 20-25 DEG C, and the impurity of repeatedly removal film surface is then rinsed with deionized water/ethyl alcohol；By TiO2@Mofs particle is dissolved in methanol solution, and film is put into TiO2In@Mofs solution, 20-24h is reacted at 70-90 DEG C, and the impurity for the glass fibre film surface that repeatedly removal is modified is then rinsed with deionized water/ethyl alcohol, the glass fibre membrane of above-mentioned modification is put into air dry oven, the dry 12-24h at 40-50 DEG C.The TiO2@Mofs modified glass-fiber film, not only remains that glass fibre is resistant to chemical etching, advantage resistant to high temperature, and can effectively remove the oil in oily waste water.
Description
Technical field
The present invention relates to the technical field of oiliness sewage treatment, in particular to a kind of TiO2@Mofs modified glass-fiber film
Preparation method.
Background technique
With the continuous development of industry, petrochemical industry, metallurgy industry, pharmaceutical industry, food service industry, sanitary sewage etc. are various
Occasion can all discharge a large amount of oily waste water daily.In addition, oily waste water mostly complicated component, includes many solid particles, profit
The noxious materials such as lubrication prescription, salt, demulsifier, defoaming agent and a variety of organic solvents.Membrane separation technique is the screening using seperation film
The affinity interaction different to water, oil with seperation film is acted on, thus the method for realizing water-oil separating.Glass fibre membrane not only remains
Many advantages, such as glass fibre is resistant to chemical etching, high temperature resistant, but it is low to the separative efficiency of oil slick, it is therefore desirable to glass fibers
Dimension film is modified, and improves the separative efficiency to oil slick.
Summary of the invention
The object of the present invention is to provide a kind of TiO2The preparation method of@Mofs modified glass-fiber film solves above-mentioned existing
One or more in technical problem.
A kind of TiO provided by the invention2The preparation method of@Mofs modified glass-fiber film, comprising the following steps:
A1, glass fibre membrane diaphragm is put into beaker, suitable washing lotion is added, 1-2h is boiled at 95-98 DEG C, removed
The impurity of film surface, and it is made to generate more Si-OH, then will treated film pure water to neutrality, it is dry with air blast
Dry case is dried for standby at 40 DEG C；
A2, epoxychloropropane and Strong oxdiative sodium solution is taken to be added in beaker, wherein epoxychloropropane and sodium hydroxide rub
Then you use than being that 1:2-1:5 in the above solution by the glass fibre membrane in step A1 reacts 10-12h at 20-25 DEG C
Deionized water/ethyl alcohol rinses the impurity of repeatedly removal film surface；
A3, by TiO2@Mofs particle is dissolved in methanol solution, and by step A2, treated that film is put into TiO2In@Mofs solution,
20-24h is reacted at 70-90 DEG C, then rinses repeatedly the miscellaneous of the glass fibre film surface of removal modification with deionized water/ethyl alcohol
Matter, finally, the glass fibre membrane of above-mentioned modification is put into air dry oven, the dry 12-24h at 40-50 DEG C.
In some embodiments, the aperture of glass fibre membrane diaphragm is 0.5-0.7 μm, diameter 40-55mm.
In some embodiments, washing lotion is the sulfuric acid that concentration is 98% and the hydrogen peroxide that concentration is 30% with volume ratio 7:
3 are mixed to prepare.
In some embodiments, TiO2The preparation method of@Mofs the following steps are included:
B1, by TiO2Particle is scattered in methanol solution with polyvinylpyrrolidone, and the concentration of obtained solution is after dispersion
15-20mg/mL；
B2, in vial be added the DMF solution containing 15-20mol/L zirconium chloride and containing 15-20mol/L to benzene
The methanol solution of dioctyl phthalate, wherein the volume ratio of DMF solution and methanol solution is 1:1-1:2, and ultrasound is uniformly mixed solution；
B3, the TiO dispersed in advance in step B1 is added into vial with the volume ratio of 1:200-1:502Particle methanol is molten
Liquid, it is ultrasonic again, it is uniformly mixed the solution in vial；
B4, mixed solution being placed at 100-120 DEG C and reacts 12-24h, obtained product removes supernatant by centrifugation,
It is precipitated, and the precipitating being collected into is washed with methanol, placed and dry 10-12h in a vacuum drying oven, obtain TiO2@
Mofs particle.
TiO obtained by the above method2The advantages of@Mofs particle has both Mofs and TiO2 has bigger serface and excellent
Adsorption desorption performance, can effectively adsorb the oil molecule in oily waste water.
In some embodiments, TiO2The preparation method of particle the following steps are included:
C1, by TiO2·nH2Both O and inorganic base molar ratio are 0.4-0.6, and suitable water is added, is ground, then
2h is kept the temperature after being warming up to 880-900 DEG C in Muffle furnace, slow cooling to room temperature obtains interphase K6Ti2O7；
C2, then by scattered intermediate product K6Ti2O7It puts into a small amount of water, places 1-2 days, it then will be resulting
It is stirred in hydrated product investment suitable quantity of water, the diluted acid of 0.5mol/L is constantly added dropwise, the pH value with acidometer control solution is
2.0-3.0；
C3, intermediate product is filtered out after stable system reaches balance, is washed with water to neutral and drying to constant weight and is produced
Then object metatitanic acid sinters to 1000-1200 DEG C in Muffle furnace with the speed of 10 DEG C of min-1, keep the temperature 2h, slow cooling to room temperature,
Obtain TiO2Particle.
TiO obtained by the above method2Particle is with bigger serface and has meso-hole structure, can effectively adsorb oil-containing
Oil molecule in waste water.
In some embodiments, inorganic base is one of potassium hydroxide, sodium hydroxide or calcium hydroxide or a variety of.
In some embodiments, diluted acid is one of dilute sulfuric acid, dust technology or dilute hydrochloric acid or a variety of.
In some embodiments, TiO2The solid-to-liquid ratio that@Mofs particle is dissolved in methanol solution is 1:20-1:50.
The utility model has the advantages that
The TiO of the embodiment of the present application2@Mofs modified glass-fiber film, it is resistant to chemical etching, resistance to not only to remain glass fibre
The advantages of high temperature, and can effectively remove the oil in oily waste water.
Specific embodiment
Below with reference to embodiment, the present invention is described in more detail.
Case study on implementation 1:
α 1, by TiO2·nH2Both O and inorganic base molar ratio are 0.4, and suitable water is added, is ground, then in horse
2h is kept the temperature after being not warming up to 880 DEG C in furnace, slow cooling to room temperature obtains interphase K6Ti2O7；
α 2, then by scattered intermediate product K6Ti2O7It puts into a small amount of water, places 1 day, then by resulting water
It closes and is stirred in product investment suitable quantity of water, the diluted acid of 0.5mol/L is constantly added dropwise, the pH value with acidometer control solution is
2.0；
α 3, intermediate product is filtered out after stable system reaches balance, is washed with water to neutral and drying to constant weight and is produced
Then object metatitanic acid sinters to 1000 DEG C in Muffle furnace with the speed of 10 DEG C of min-1, keep the temperature 2h, and slow cooling to room temperature obtains
TiO2Particle；
α 4, by TiO2Particle is scattered in methanol solution with polyvinylpyrrolidone, and the concentration of obtained solution is after dispersion
15mg/mL；
α 5, the DMF solution containing 15mol/L zirconium chloride and the terephthalic acid (TPA) containing 15mol/L are added in vial
Methanol solution, wherein the volume ratio of DMF solution and methanol solution be 1:1, ultrasound make solution be uniformly mixed；
α 6, the TiO dispersed in advance in step α 5 is added into vial with the volume ratio of 1:2002Particle methanol solution, then
Secondary ultrasound is uniformly mixed the solution in vial；
α 7, mixed solution is placed at 100 DEG C to the product for reacting and for 24 hours, obtaining by centrifugation, removes supernatant, is sunk
It forms sediment, and the precipitating being collected into is washed with methanol, place and dry 10h in a vacuum drying oven, obtain TiO2@Mofs particle；
α 8, glass fibre membrane diaphragm is put into beaker, suitable washing lotion is added, boil 2h at 95 DEG C, remove striping table
The impurity in face, and it is made to generate more Si-OH, then will treated film pure water to neutrality, use air dry oven
It is dried for standby at 40 DEG C；
α 9, epoxychloropropane and Strong oxdiative sodium solution is taken to be added in beaker, wherein epoxychloropropane and sodium hydroxide rub
You than be 1:2 12h in the above solution by the glass fibre membrane in step α 8 is reacted at 20 DEG C, then with deionized water/
Ethyl alcohol rinses the impurity of repeatedly removal film surface；
α 10, by TiO2@Mofs particle is dissolved in methanol solution, and by step α 9, treated that film is put into TiO2In@Mofs solution,
It is reacted at 70 DEG C for 24 hours, the impurity for the glass fibre film surface that repeatedly removal is modified is then rinsed with deionized water/ethyl alcohol, most
Afterwards, the glass fibre membrane by above-mentioned modification is put into air dry oven, is dried for 24 hours at 40 DEG C.
Case study on implementation 2:
β 1, by TiO2·nH2Both O and inorganic base molar ratio are 0.6, and suitable water is added, is ground, then in horse
2h is kept the temperature after being not warming up to 900 DEG C in furnace, slow cooling to room temperature obtains interphase K6Ti2O7；
β 2, then by scattered intermediate product K6Ti2O7It puts into a small amount of water, places 2 days, then by resulting water
It closes and is stirred in product investment suitable quantity of water, the diluted acid of 0.5mol/L is constantly added dropwise, the pH value with acidometer control solution is
3.0；
β 3, intermediate product is filtered out after stable system reaches balance, is washed with water to neutral and drying to constant weight and is produced
Then object metatitanic acid sinters to 1200 DEG C in Muffle furnace with the speed of 10 DEG C of min-1, keep the temperature 2h, and slow cooling to room temperature obtains
TiO2Particle；
β 4, by TiO2Particle is scattered in methanol solution with polyvinylpyrrolidone, and the concentration of obtained solution is after dispersion
20mg/mL；
β 5, the DMF solution containing 20mol/L zirconium chloride and the terephthalic acid (TPA) containing 20mol/L are added in vial
Methanol solution, wherein the volume ratio of DMF solution and methanol solution be 1:2, ultrasound make solution be uniformly mixed；
β 6, the TiO dispersed in advance in step β 5 is added into vial with the volume ratio of 1:502Particle methanol solution, then
Secondary ultrasound is uniformly mixed the solution in vial；
β 7, mixed solution is placed at 120 DEG C and reacts 12h, obtained product is removed supernatant, sunk by centrifugation
It forms sediment, and the precipitating being collected into is washed with methanol, place and dry 12h in a vacuum drying oven, obtain TiO2@Mofs particle；
β 8, glass fibre membrane diaphragm is put into beaker, suitable washing lotion is added, boil 2h at 98 DEG C, remove striping table
The impurity in face, and it is made to generate more Si-OH, then will treated film pure water to neutrality, use air dry oven
It is dried for standby at 40 DEG C；
β 9, epoxychloropropane and Strong oxdiative sodium solution is taken to be added in beaker, wherein epoxychloropropane and sodium hydroxide rub
You than be 1:5 10h in the above solution by the glass fibre membrane in step β 8 is reacted at 25 DEG C, then with deionized water/
Ethyl alcohol rinses the impurity of repeatedly removal film surface；
β 10, by TiO2@Mofs particle is dissolved in methanol solution, and by step β 9, treated that film is put into TiO2In@Mofs solution,
20h is reacted at 90 DEG C, the impurity for the glass fibre film surface that repeatedly removal is modified is then rinsed with deionized water/ethyl alcohol, most
Afterwards, the glass fibre membrane by above-mentioned modification is put into air dry oven, the dry 12h at 50 DEG C.
Case study on implementation 3:
γ 1, by TiO2·nH2Both O and inorganic base molar ratio are 0.5, and suitable water is added, is ground, then in horse
2h is kept the temperature after being not warming up to 890 DEG C in furnace, slow cooling to room temperature obtains interphase K6Ti2O7；
γ 2, then by scattered intermediate product K6Ti2O7It puts into a small amount of water, places 1.5 days, it then will be resulting
It is stirred in hydrated product investment suitable quantity of water, the diluted acid of 0.5mol/L is constantly added dropwise, the pH value with acidometer control solution is
2.5；
γ 3, intermediate product is filtered out after stable system reaches balance, is washed with water to neutral and drying to constant weight and is produced
Then object metatitanic acid sinters to 1100 DEG C in Muffle furnace with the speed of 10 DEG C of min-1, keep the temperature 2h, and slow cooling to room temperature obtains
TiO2Particle；
γ 4, by TiO2Particle is scattered in methanol solution with polyvinylpyrrolidone, and the concentration of obtained solution is after dispersion
18mg/mL；
γ 5, the DMF solution containing 18mol/L zirconium chloride and the terephthalic acid (TPA) containing 18mol/L are added in vial
Methanol solution, wherein the volume ratio of DMF solution and methanol solution be 1:1.5, ultrasound make solution be uniformly mixed；
γ 6, the TiO dispersed in advance in step γ 5 is added into vial with the volume ratio of 1:1002Particle methanol solution,
It is ultrasonic again, it is uniformly mixed the solution in vial；
γ 7, mixed solution is placed at 110 DEG C and reacts 20h, obtained product is removed supernatant, sunk by centrifugation
It forms sediment, and the precipitating being collected into is washed with methanol, place and dry 11h in a vacuum drying oven, obtain TiO2@Mofs particle；
γ 8, glass fibre membrane diaphragm is put into beaker, suitable washing lotion is added, boil 1.5 at 96 DEG C, remove striping
The impurity on surface, and it is made to generate more Si-OH, then will treated film pure water to neutrality, use forced air drying
Case is dried for standby at 40 DEG C；
γ 9, epoxychloropropane and Strong oxdiative sodium solution is taken to be added in beaker, wherein epoxychloropropane and sodium hydroxide
Molar ratio is 1:4, in the above solution by the glass fibre membrane in step γ 8,11h is reacted at 22 DEG C, then uses deionization
Water/ethyl alcohol rinses the impurity of repeatedly removal film surface；
γ 10, by TiO2@Mofs particle is dissolved in methanol solution, and by step γ 9, treated that film is put into TiO2@Mofs solution
In, 22h is reacted at 80 DEG C, and the impurity for the glass fibre film surface that repeatedly removal is modified is then rinsed with deionized water/ethyl alcohol,
Finally, the glass fibre membrane of above-mentioned modification is put into air dry oven, the dry 20h at 45 DEG C.
Film tests oily waste water separating property:
The preparation of oil emulsion: the hexadecane or n-dodecane or soybean oil of 10mL, 0.1mg neopelex are taken
(or Tween 80) is added in 1L pure water, and 2000rpm stirs 5h and ultrasonic dissolution 30min is stand-by.
The separating property of film is evaluated with the retention of water flux and oil water mixture.Test condition: self-control pure water (1.2 μ g/
L TOC), room temperature test, for gravity drive liquid level apart from film surface 10cm height, it is 1.6cm that glass fibre diaphragm, which is cut into diameter,
The disk of size, membrane sample are required to sufficiently be soaked with pure water before testing, start to test after liquid energy steady and continuous drippage.
The concentration of stoste and permeate is tested with TOC in test, is then calculated according to formula, obtains film to oil
The performance rejection of aqueous emulsion.Formula is as follows:
R=(1-Cf/C0) * 100%, wherein R is rejection (%) of the film to oil water mixture, CfIt is dense for grease after filtering
It spends (mg/L), C0For the concentration (mg/L) for filtering preceding grease.
The glass fibre membrane of the modification of embodiment 1 to 3 is carried out separating property test as can be known from the results to cut grease
Stay rate between 98.2-99.6, and the organic carbon content of permeability is respectively less than 20mg/L.
One of embodiment provided by the invention TiO2What the preparation method of@Mofs modified glass-fiber film obtained changes
Property glass fibre membrane can effectively remove the oil in oily waste water.
The above statement is only preferred embodiment of the invention, it is noted that those skilled in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these also should be regarded as protection of the invention
Within the scope of.
Claims (8)
1. a kind of TiO2The preparation method of@Mofs modified glass-fiber film, which comprises the following steps:
A1, glass fibre membrane diaphragm is put into beaker, suitable washing lotion is added, boil 1-2h at 95-98 DEG C, remove striping table
The impurity in face, and it is made to generate more Si-OH, then will treated film pure water to neutrality, use air dry oven
It is dried for standby at 40 DEG C；
A2, epoxychloropropane and Strong oxdiative sodium solution is taken to be added in beaker, wherein the molar ratio of epoxychloropropane and sodium hydroxide
10-12h in the above solution by the glass fibre membrane in step A1 is reacted at 20-25 DEG C for 1:2-1:5, then spend from
Sub- water/ethyl alcohol rinses the impurity of repeatedly removal film surface；
A3, by TiO2@Mofs particle is dissolved in methanol solution, and by step A2, treated that film is put into TiO2In@Mofs solution, in 70-
20-24h is reacted at 90 DEG C, the impurity for the glass fibre film surface that repeatedly removal is modified is then rinsed with deionized water/ethyl alcohol, most
Afterwards, the glass fibre membrane by above-mentioned modification is put into air dry oven, the dry 12-24h at 40-50 DEG C.
2. a kind of TiO according to claim 12The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
The aperture of glass fibre membrane diaphragm is 0.5-0.7 μm, diameter 40-55mm.
3. a kind of TiO according to claim 12The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
The hydrogen peroxide that washing lotion is the sulfuric acid that concentration is 98% and concentration is 30% is mixed to prepare with volume ratio 7:3.
4. a kind of TiO according to claim 12The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
TiO2The preparation method of@Mofs the following steps are included:
B1, by TiO2Particle is scattered in methanol solution with polyvinylpyrrolidone, and the concentration of obtained solution is 15- after dispersion
20mg/mL；
B2, the DMF solution containing 15-20mol/L zirconium chloride and the terephthaldehyde containing 15-20mol/L are added in vial
The methanol solution of acid, wherein the volume ratio of DMF solution and methanol solution is 1:1-1:2, and ultrasound is uniformly mixed solution；
B3, the TiO dispersed in advance in step B1 is added into vial with the volume ratio of 1:200-1:502Particle methanol solution, then
Secondary ultrasound is uniformly mixed the solution in vial；
B4, mixed solution is placed at 100-120 DEG C and reacts 12-24h, obtained product is removed supernatant, obtained by centrifugation
Precipitating, and the precipitating being collected into is washed with methanol, it places and dries 10-12h in a vacuum drying oven, obtain TiO2@Mofs
Grain.
5. a kind of TiO according to claim 42The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
TiO2The preparation method of particle the following steps are included:
C1, by TiO2·nH2Both O and inorganic base molar ratio are 0.4-0.6, and suitable water is added, is ground, then in horse
2h is kept the temperature after being not warming up to 880-900 DEG C in furnace, slow cooling to room temperature obtains interphase K6Ti2O7；
C2, then by scattered intermediate product K6Ti2O7It puts into a small amount of water, places 1-2 days, then by resulting hydration
It is stirred in product investment suitable quantity of water, the diluted acid of 0.5mol/L is constantly added dropwise, the pH value with acidometer control solution is 2.0-
3.0；
C3, intermediate product is filtered out after stable system reaches balance, is washed with water to neutral and drying to constant weight and obtains product titanium
Then acid sinters to 1000-1200 DEG C in Muffle furnace with the speed of 10 DEG C of min-1, keep the temperature 2h, and slow cooling to room temperature obtains
TiO2Particle.
6. a kind of TiO according to claim 52The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
Inorganic base is one of potassium hydroxide, sodium hydroxide or calcium hydroxide or a variety of.
7. a kind of TiO according to claim 52The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
Diluted acid is one of dilute sulfuric acid, dust technology or dilute hydrochloric acid or a variety of.
8. a kind of TiO according to claim 12The preparation method of@Mofs modified glass-fiber film, which is characterized in that described
TiO2The solid-to-liquid ratio that@Mofs particle is dissolved in methanol solution is 1:20-1:50.
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Application publication date: 20190510 |