CN109133088A - A kind of preparation method of high separating efficiency molecular screen membrane - Google Patents
A kind of preparation method of high separating efficiency molecular screen membrane Download PDFInfo
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- CN109133088A CN109133088A CN201811078380.5A CN201811078380A CN109133088A CN 109133088 A CN109133088 A CN 109133088A CN 201811078380 A CN201811078380 A CN 201811078380A CN 109133088 A CN109133088 A CN 109133088A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0044—Inorganic membrane manufacture by chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/028—Molecular sieves
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/005—Silicates, i.e. so-called metallosilicalites or metallozeosilites
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Abstract
The present invention relates to molecular screen membrane preparation technical fields, and in particular to a kind of preparation method of high separating efficiency molecular screen membrane.The present invention is first using fresh black tea leaf as raw material, red tea fungus fermented date liquid is obtained through everfermentation, then it is acted on by sodium metasilicate and acid, nano silica is obtained by heating, aluminum nitrate is added into bacteria cellulose film and nano silica mixture, obtain molecular screen membrane supporter, by alkali source, silicon source, silicon source and deionized water mix in proportion, stirring ageing obtains molecular screen membrane crystallization liquid, finally by molecular screen membrane supporter and molecular screen membrane crystallization liquid Hybrid Heating up to high separating efficiency molecular screen membrane, nano silica is incorporated in the surface of bacteria cellulose film, reducing solution is after high temperature sintering, eliminate bacterial fibers film, as molecular screen membrane supporter, network structure with nanofiber, so that molecular screen membrane thickness reduces, improve molecular sieve membrane separation efficiency, it has broad application prospects.
Description
Technical field
The present invention relates to molecular screen membrane preparation technical fields, and in particular to a kind of preparation side of high separating efficiency molecular screen membrane
Method.
Background technique
UF membrane is a kind of isolation technics developed in recent years, is that one or more substances are utilized to compare other materials
Semipermeable obstacle (film) can be passed through more quickly to achieve the purpose that incoming mixture of the separation containing there are two types of or more.Film
Isolation technics mainly includes micro porous filtration, ultrafiltration, reverse osmosis, nanofiltration, electrodialysis, gas separation and pervaporation.
Molecular sieve is a kind of microporous inorganic crystalline material formed using oxygen-octahedron and aluminum-oxygen tetrahedron as basic framework,
It is a kind of novel inorganic membrane material that molecule screening may be implemented that developed recently gets up, since it is with unique screening
Property, the performances such as hydrophilic/hydrophobic and shape selective catalysis, the fields such as separating in organics dehydration, micro-molecular gas has wide answer
Use prospect.
Molecular sieve has the advantage that as inorganic material film
(1) molecular sieve has the neat duct of specification, and pore-size distribution is single, and the pore size size of molecular sieve and many heavy
The molecular dimension size for the raw material of industry wanted is close, and molecule can be sieved by molecule or shape-selective diffusion is separated.
Molecular sieve has good chemical stability and thermal stability.
The diversity of molecular sieve structure leads to its property qualitative diversity, such as different pore sizes, different hydrophilic and hydrophobics,
Therefore, it is possible to select suitable molecular sieve as membrane material according to different separation requirements.
The modifiability of molecular sieve pore passage and hole outer surface leads to the adjustable denaturation of molecular sieve bore diameter and absorption property, thus
The accurate control of separation may be implemented.Due to molecular screen membrane have excellent shape-selective separation and catalytic performance, and have high temperature resistant,
The features such as chemical resistance of concrete is strong, it is anti-in gas separation, steam separation, Liquid Penetrant vaporization separation, membrane catalytic reaction, Subjective and Objective
It answers, environmental protection, Life Engineering, the various fields such as electrode and sensor can all be applied.
But since common molecular screen membrane at present is in order to certain mechanical strength, film thickness obtained in preparation process
It is larger, cause its separative efficiency to be not achieved perfect condition, how in the premise for reducing molecular screen membrane thickness and improving its separative efficiency
Down while there is certain mechanical strength to become one of the hot spot studied instantly.In addition the synthesis of most molecular screen membrane be all
It is directly carried out on carrier, because of the difference of thermal expansion coefficient, it is easy to so that film falls off, and crystal film essentially no orientation
Property, the effect of affecting molecular screen membrane and development.
Therefore, needing to develop a kind of molecular screen membrane for being able to solve the above problem is highly desirable.
Summary of the invention
Present invention mainly solves the technical issues of, for presently, there are molecular sieve film thickness it is larger, lead to its separation
The undesirable defect of effect provides a kind of preparation method of high separating efficiency molecular screen membrane.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of high separating efficiency molecular screen membrane, it is characterised in that specific preparation step are as follows:
It (1) is 40~50 in temperature in the beaker after fresh black tea leaf, white sugar, distilled water to be put into disinfection after mixing
20~30min of heating water bath at DEG C obtains heating water bath product, then heating water bath product is added in fermentor, to fermentor
Middle addition fermented tea bacteria suspension is sealed by fermentation 5~6 days under conditions of temperature is 40~50 DEG C, takes out fermentation liquid table with tweezers
The gel bacteria cellulose film that layer is formed, obtains bacteria cellulose film；
(2) bacteria cellulose film obtained above is put into beaker bottom, sodium silicate solution is added into beaker, then into beaker
Hydrochloric acid solution is added, adjusting pH value of solution is 4~5, obtains mixed liquor, mixed liquor is poured into heating device, and setting temperature is 50
~60 DEG C, heating 2~3h of reaction, after reaction, the bacteria cellulose film after taking out beaker bottom reaction；
(3) by after above-mentioned reaction bacteria cellulose film and aluminum nitrate solution mix after, shaking table 10~15min of concussion reaction is obtained
To reaction solution, then glucose solution is added dropwise into reaction solution, under conditions of temperature is 40~50 DEG C, it is stirred to react 30~
40min, collection obtain modified bacteria cellulose film；
(4) above-mentioned modified bacteria cellulose film is added in Muffle furnace, pyroreaction obtains molecular screen membrane supporter, spare；
(5) it is stirred to react after mixing sodium metasilicate, sodium aluminate, plant ash and deionized water, obtains stirring thing, then stirring thing is put
Enter in aging device, at 120~150 DEG C be aged 20~for 24 hours, obtain molecular screen membrane crystallization liquid；
(6) it is put into reaction kettle after mixing spare molecular screen membrane supporter with above-mentioned molecular screen membrane crystallization liquid, is in temperature
Under conditions of 80~90 DEG C, heating water bath synthesize 40~50min, obtain hydrothermal synthesis product, by hydrothermal synthesis product spend from
It is put into baking oven after sub- water washing, setting temperature is 100~110 DEG C, and dry 50~60min collects desciccate to get high score
From efficiency molecular screen membrane.
Fresh black tea leaf described in step (1), white sugar, distilled water mass ratio be 2 ︰, 1 ︰ 3, fermented tea bacteria suspension it is dense
Degree is 106cfu/mL, and the quality of fermented tea bacteria suspension is heating water bath product quality 7~10%.
The mass fraction of sodium silicate solution described in step (2) is 40%, and the mass fraction of hydrochloric acid solution is 30%.
The mass ratio of bacteria cellulose film and aluminum nitrate solution after above-mentioned reaction described in step (3) is 1:1, aluminum nitrate
The mass fraction of solution is 30%, and the mass fraction for the glucose solution being added dropwise into reaction solution is 25%, the matter of glucose solution
Amount is the 10% of reaction solution quality.
Temperature in Muffle furnace described in step (4) is 700~800 DEG C, and the reaction time is 3~4h.
Sodium metasilicate described in step (5), sodium aluminate, plant ash and deionized water mass ratio be 3 ︰, 2 ︰, 2 ︰ 3, speed of agitator
For 40~60r/min, mixing time is 30~40min.
The mass ratio of spare molecular screen membrane supporter described in step (6) and above-mentioned molecular screen membrane crystallization liquid is 2 ︰ 1.
The beneficial effects of the present invention are:
(1) present invention obtains red tea fungus fermented date liquid through everfermentation, in red tea fungus fermented date liquid first using fresh black tea leaf as raw material
Acetic acid bacteria energy metabolism formed bacteria cellulose film, then by sodium metasilicate and acid act on, obtain nanometer titanium dioxide by heating
Silicon is added aluminum nitrate into bacteria cellulose film and nano silica mixture, aluminum nitrate is reduced to list using glucose
Matter aluminium removes bacteria cellulose film by high temperature sintering, molecular screen membrane supporter is obtained, by alkali source, silicon source, silicon source and deionization
Water mixes in proportion, and stirring ageing obtains molecular screen membrane crystallization liquid, finally by molecular screen membrane supporter and molecular screen membrane crystallization liquid
Re-dry is after mixing heating in water bath for reaction up to high separating efficiency molecular screen membrane, and the present invention is using fresh black tea leaf as raw material, warp
Everfermentation obtains red tea fungus fermented date liquid, and the acetic acid bacteria energy metabolism in red tea fungus fermented date liquid forms bacteria cellulose film, bacterial fibers
Plain film is a kind of natural biopolymer, it has hyperfine Nanofiber Network, and this layer of bacteria cellulose film is in height
It can disappear in temperature sintering, sodium metasilicate reacts in acid condition can be made orthosilicic acid precipitating, and orthosilicic acid solution obtained is added
Thermal response generates nano silica, so that nano silica is incorporated in the surface of bacteria cellulose film, silica is in wadding
Shape and netted quasi- grain structure, the bacterial fibers film for combining nano silica can be used as the template of molecular screen membrane, Portugal
Grape sugar juice has reproducibility, and aluminum nitrate is reduced to aluminium simple substance under the action of reducing substances, and the modification collected is thin
Containing the bacterial fibers film for combining nano silica and pure aluminum in fungin film, modified bacteria cellulose film is through high temperature
After sintering, bacterial fibers film is eliminated, generates pore structure, as molecular screen membrane supporter, the network knot with nanofiber
Structure improves molecular sieve membrane separation efficiency, has broad application prospects so that molecular screen membrane thickness reduces.
Specific embodiment
It is that the fresh black tea leaf, white sugar, distilled water of 2 ︰, 1 ︰ 3 are put into the beaker after disinfection after mixing by mass ratio
In, 20~30min of heating water bath at being 40~50 DEG C in temperature obtains heating water bath product, then heating water bath product is added
In fermentor, the concentration that heating water bath product quality 7~10% is added into fermentor is 106The fermented tea bacteria suspension of cfu/mL,
It under conditions of temperature is 40~50 DEG C, is sealed by fermentation 5~6 days, takes out the gel bacterium that fermentation liquid surface layer is formed with tweezers
Cellulose membrane obtains bacteria cellulose film；Bacteria cellulose film obtained above is put into beaker bottom, matter is added into beaker
Measure score be 40% sodium silicate solution, then into beaker be added mass fraction be 30% hydrochloric acid solution, adjust pH value of solution be 4~
5, mixed liquor is obtained, mixed liquor is poured into heating device, setting temperature is 50~60 DEG C, and heating 2~3h of reaction, reaction terminates
Afterwards, the bacteria cellulose film after taking out beaker bottom reaction；By mass ratio be 1:1 above-mentioned reaction after bacteria cellulose film and
After the aluminum nitrate solution mixing that mass fraction is 30%, shaking table 10~15min of concussion reaction obtains reaction solution, then into reaction solution
The glucose solution that the mass fraction of dropwise reaction liquid quality 10% is 25%, under conditions of temperature is 40~50 DEG C, stirring is anti-
30~40min is answered, collection obtains modified bacteria cellulose film；Above-mentioned modified bacteria cellulose film is added in Muffle furnace, in temperature
Degree reacts 3~4h under conditions of being 700~800 DEG C, obtains molecular screen membrane supporter, spare；The silicon for being 3 ︰, 2 ︰, 2 ︰ 3 by mass ratio
30~40min is stirred with the speed of agitator of 40~60r/min after sour sodium, sodium aluminate, plant ash and deionized water mixing, is stirred
Mix object, then stirring thing be put into aging device, at 120~150 DEG C be aged 20~for 24 hours, obtain molecular screen membrane crystallization liquid；It will
Spare molecular screen membrane supporter and above-mentioned molecular screen membrane crystallization liquid are that 2 ︰ 1 are put into reaction kettle in mass ratio, are 80 in temperature
Under conditions of~90 DEG C, heating water bath synthesizes 40~50min, hydrothermal synthesis product is obtained, by hydrothermal synthesis product deionization
Be put into baking oven after water washing, setting temperature is 100~110 DEG C, dry 50~60min, collect desciccate to get high score from
Efficiency molecular screen membrane.
It is that the fresh black tea leaf, white sugar, distilled water of 2 ︰, 1 ︰ 3 are put into the beaker after disinfection after mixing by mass ratio
In, heating water bath 20min at being 40 DEG C in temperature obtains heating water bath product, then heating water bath product is added in fermentor,
The concentration that heating water bath product quality 7% is added into fermentor is the fermented tea bacteria suspension of 106cfu/mL, is 40 DEG C in temperature
Under conditions of, it is sealed by fermentation 5 days, takes out the gel bacteria cellulose film that fermentation liquid surface layer is formed with tweezers, obtain bacterium fibre
Tie up plain film；Bacteria cellulose film obtained above is put into beaker bottom, the sodium metasilicate that mass fraction is 40% is added into beaker
Solution, then the hydrochloric acid solution that mass fraction is 30% is added into beaker, adjusting pH value of solution is 4, mixed liquor is obtained, by mixed liquor
It pours into heating device, setting temperature is 50 DEG C, heating reaction 2h, after reaction, the bacterium after taking out beaker bottom reaction
Cellulose membrane；The aluminum nitrate solution that the bacteria cellulose film after above-mentioned reaction for being 1:1 by mass ratio and mass fraction are 30% mixes
After conjunction, shaking table concussion reaction 10min obtains reaction solution, then the mass fraction of dropwise reaction liquid quality 10% is into reaction solution
25% glucose solution is stirred to react 30min under conditions of temperature is 40 DEG C, and collection obtains modified bacteria cellulose film；
Above-mentioned modified bacteria cellulose film is added in Muffle furnace, 3h is reacted under conditions of temperature is 700 DEG C, obtains molecular screen membrane branch
Support body, it is spare；With 40r/min's after sodium metasilicate, sodium aluminate, plant ash and deionized water that mass ratio is 3 ︰, 2 ︰, 2 ︰ 3 are mixed
Speed of agitator stirs 30min, obtains stirring thing, then stirring thing is put into aging device, is aged 20h at 120 DEG C, is divided
Sub- sieve membrane crystallization liquid；It is in mass ratio that 2 ︰ 1 are put into and react by spare molecular screen membrane supporter and above-mentioned molecular screen membrane crystallization liquid
In kettle, under conditions of temperature is 80 DEG C, heating water bath synthesizes 40min, obtains hydrothermal synthesis product, hydrothermal synthesis product is used
It is put into baking oven after deionized water washing, setting temperature is 100 DEG C, and dry 50min collects desciccate to get high score from effect
Rate molecular screen membrane.
It is that the fresh black tea leaf, white sugar, distilled water of 2 ︰, 1 ︰ 3 are put into the beaker after disinfection after mixing by mass ratio
In, heating water bath 25min at being 45 DEG C in temperature obtains heating water bath product, then heating water bath product is added in fermentor,
The concentration that heating water bath product quality 8% is added into fermentor is the fermented tea bacteria suspension of 106cfu/mL, is 45 DEG C in temperature
Under conditions of, it is sealed by fermentation 5 days, takes out the gel bacteria cellulose film that fermentation liquid surface layer is formed with tweezers, obtain bacterium fibre
Tie up plain film；Bacteria cellulose film obtained above is put into beaker bottom, the sodium metasilicate that mass fraction is 40% is added into beaker
Solution, then the hydrochloric acid solution that mass fraction is 30% is added into beaker, adjusting pH value of solution is 4, mixed liquor is obtained, by mixed liquor
It pours into heating device, setting temperature is 55 DEG C, heating reaction 2h, after reaction, the bacterium after taking out beaker bottom reaction
Cellulose membrane；The aluminum nitrate solution that the bacteria cellulose film after above-mentioned reaction for being 1:1 by mass ratio and mass fraction are 30% mixes
After conjunction, shaking table concussion reaction 13min obtains reaction solution, then the mass fraction of dropwise reaction liquid quality 10% is into reaction solution
25% glucose solution is stirred to react 35min under conditions of temperature is 45 DEG C, and collection obtains modified bacteria cellulose film；
Above-mentioned modified bacteria cellulose film is added in Muffle furnace, 3h is reacted under conditions of temperature is 750 DEG C, obtains molecular screen membrane branch
Support body, it is spare；With 50r/min's after sodium metasilicate, sodium aluminate, plant ash and deionized water that mass ratio is 3 ︰, 2 ︰, 2 ︰ 3 are mixed
Speed of agitator stirs 35min, obtains stirring thing, then stirring thing is put into aging device, is aged 22h at 135 DEG C, is divided
Sub- sieve membrane crystallization liquid；It is in mass ratio that 2 ︰ 1 are put into and react by spare molecular screen membrane supporter and above-mentioned molecular screen membrane crystallization liquid
In kettle, under conditions of temperature is 85 DEG C, heating water bath synthesizes 45min, obtains hydrothermal synthesis product, hydrothermal synthesis product is used
It is put into baking oven after deionized water washing, setting temperature is 105 DEG C, and dry 55min collects desciccate to get high score from effect
Rate molecular screen membrane.
It is that the fresh black tea leaf, white sugar, distilled water of 2 ︰, 1 ︰ 3 are put into the beaker after disinfection after mixing by mass ratio
In, heating water bath 30min at being 50 DEG C in temperature obtains heating water bath product, then heating water bath product is added in fermentor,
The concentration that heating water bath product quality 10% is added into fermentor is the fermented tea bacteria suspension of 106cfu/mL, is 50 DEG C in temperature
Under conditions of, it is sealed by fermentation 6 days, takes out the gel bacteria cellulose film that fermentation liquid surface layer is formed with tweezers, obtain bacterium fibre
Tie up plain film；Bacteria cellulose film obtained above is put into beaker bottom, the sodium metasilicate that mass fraction is 40% is added into beaker
Solution, then the hydrochloric acid solution that mass fraction is 30% is added into beaker, adjusting pH value of solution is 5, mixed liquor is obtained, by mixed liquor
It pours into heating device, setting temperature is 60 DEG C, heating reaction 3h, after reaction, the bacterium after taking out beaker bottom reaction
Cellulose membrane；The aluminum nitrate solution that the bacteria cellulose film after above-mentioned reaction for being 1:1 by mass ratio and mass fraction are 30% mixes
After conjunction, shaking table concussion reaction 15min obtains reaction solution, then the mass fraction of dropwise reaction liquid quality 10% is into reaction solution
25% glucose solution is stirred to react 40min under conditions of temperature is 50 DEG C, and collection obtains modified bacteria cellulose film；
Above-mentioned modified bacteria cellulose film is added in Muffle furnace, 4h is reacted under conditions of temperature is 800 DEG C, obtains molecular screen membrane branch
Support body, it is spare；With 60r/min's after sodium metasilicate, sodium aluminate, plant ash and deionized water that mass ratio is 3 ︰, 2 ︰, 2 ︰ 3 are mixed
Speed of agitator stirs 40min, obtains stirring thing, then stirring thing is put into aging device, is aged for 24 hours, is divided at 150 DEG C
Sub- sieve membrane crystallization liquid；It is in mass ratio that 2 ︰ 1 are put into and react by spare molecular screen membrane supporter and above-mentioned molecular screen membrane crystallization liquid
In kettle, under the conditions of at a temperature of 90 °C, heating water bath synthesizes 50min, obtains hydrothermal synthesis product, hydrothermal synthesis product is used
It is put into baking oven after deionized water washing, setting temperature is 110 DEG C, and dry 60min collects desciccate to get high score from effect
Rate molecular screen membrane.
The molecular screen membrane that comparative example is produced with Shanghai City company is as a comparison case
Molecular screen membrane in high separating efficiency molecular screen membrane produced by the present invention and comparative example is detected, testing result such as table
Shown in 1:
Toughness test
It is tested using electronic universal tester.It retest 5 times, is averaged.
Pure water flux refers under certain temperature and operating pressure that the film of unit area is penetrated pure within the unit time
Water.Pure water flux is directly proportional to filter efficiency.
Before test, the both ends of the molecular screen membrane of present invention preparation Examples 1 to 3 and comparative example are sealed respectively, are made point
Sub- sieve membrane component is then passed through pure water to one end of membrane module (water inlet) respectively under conditions of meter pressure is 0.1MPa, surveys
Determine the volume V(L of the pure water of the 30min inner membrane member other end (water outlet) transmission), calculate the pure water flux of molecular screen membrane
(PWF).
Pure water flux=through pure water volume/(molecular screen membrane tube outer surface product × penetrate molecular screen membrane required time × operation
Pressure)
CO2/CH4Gas separates test condition: temperature is 20 DEG C, atmospheric pressure 102.4kPa, and gas feed rate is
4000mL/min, mole group become 50/50vol%(, that is, CO2︰ CH4Molar ratio be 1 ︰ 1).Per-meate side is measured with soap film flowmeter
Gas flow；With the gas composition of chromatographic per-meate side.
The calculation formula of gas permeability: p=V/(S × P).Wherein, V is infiltration gas (CO2Or CH4) flow, unit
Mol/s, S are membrane area, unit m2；P is the pressure difference of membrane tube feed side and per-meate side, unit Pa.
Separation selectivity calculation formula: f=pCO2/pCH4, i.e. CO2With CH4The ratio between permeability.
1 performance measurement result of table
From the data in table 1, it can be seen that high separating efficiency molecular screen membrane produced by the present invention, has fine and close, continuous, separating property is good etc.
Feature, and excellent in mechanical performance, filter efficiency is good, with good economic efficiency and social benefit.
Claims (7)
1. a kind of preparation method of high separating efficiency molecular screen membrane, it is characterised in that specific preparation step are as follows:
It (1) is 40~50 in temperature in the beaker after fresh black tea leaf, white sugar, distilled water to be put into disinfection after mixing
20~30min of heating water bath at DEG C obtains heating water bath product, then heating water bath product is added in fermentor, to fermentor
Middle addition fermented tea bacteria suspension is sealed by fermentation 5~6 days under conditions of temperature is 40~50 DEG C, takes out fermentation liquid table with tweezers
The gel bacteria cellulose film that layer is formed, obtains bacteria cellulose film；
(2) bacteria cellulose film obtained above is put into beaker bottom, is added sodium silicate solution into beaker, then to beaker
Middle addition hydrochloric acid solution, adjusting pH value of solution is 4~5, obtains mixed liquor, mixed liquor is poured into heating device, and setting temperature is
50~60 DEG C, heating 2~3h of reaction, after reaction, the bacteria cellulose film after taking out beaker bottom reaction；
(3) by after above-mentioned reaction bacteria cellulose film and aluminum nitrate solution mix after, shaking table 10~15min of concussion reaction is obtained
To reaction solution, then glucose solution is added dropwise into reaction solution, under conditions of temperature is 40~50 DEG C, it is stirred to react 30~
40min, collection obtain modified bacteria cellulose film；
(4) above-mentioned modified bacteria cellulose film is added in Muffle furnace, pyroreaction obtains molecular screen membrane supporter, spare；
(5) will sodium metasilicate, sodium aluminate, plant ash and deionized water mix after be stirred to react, obtain stirring thing, then by stirring thing
Be put into aging device, at 120~150 DEG C be aged 20~for 24 hours, obtain molecular screen membrane crystallization liquid；
(6) it is put into reaction kettle after mixing spare molecular screen membrane supporter with above-mentioned molecular screen membrane crystallization liquid, is in temperature
Under conditions of 80~90 DEG C, heating water bath synthesize 40~50min, obtain hydrothermal synthesis product, by hydrothermal synthesis product spend from
It is put into baking oven after sub- water washing, setting temperature is 100~110 DEG C, and dry 50~60min collects desciccate to get high score
From efficiency molecular screen membrane.
2. a kind of preparation method of high separating efficiency molecular screen membrane according to claim 1, it is characterised in that: step (1)
The fresh black tea leaf, white sugar, distilled water mass ratio be 2 ︰, 1 ︰ 3, the concentration of fermented tea bacteria suspension is 106Cfu/mL,
The quality of fermented tea bacteria suspension is heating water bath product quality 7~10%.
3. a kind of preparation method of high separating efficiency molecular screen membrane according to claim 1, it is characterised in that: step (2)
The mass fraction of the sodium silicate solution is 40%, and the mass fraction of hydrochloric acid solution is 30%.
4. a kind of preparation method of high separating efficiency molecular screen membrane according to claim 1, it is characterised in that: step (3)
The mass ratio of bacteria cellulose film and aluminum nitrate solution after the above-mentioned reaction is 1:1, the mass fraction of aluminum nitrate solution
It is 30%, the mass fraction for the glucose solution being added dropwise into reaction solution is 25%, and the quality of glucose solution is reaction solution quality
10%.
5. a kind of preparation method of high separating efficiency molecular screen membrane according to claim 1, it is characterised in that: step (4)
Temperature in the Muffle furnace is 700~800 DEG C, and the reaction time is 3~4h.
6. a kind of preparation method of high separating efficiency molecular screen membrane according to claim 1, it is characterised in that: step (5)
The sodium metasilicate, sodium aluminate, plant ash and deionized water mass ratio be 3 ︰, 2 ︰, 2 ︰ 3, speed of agitator is 40~60r/min,
Mixing time is 30~40min.
7. a kind of preparation method of high separating efficiency molecular screen membrane according to claim 1, it is characterised in that: step (6)
The mass ratio of the spare molecular screen membrane supporter and above-mentioned molecular screen membrane crystallization liquid is 2 ︰ 1.
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| US6447856B1 (en) * | 2000-11-22 | 2002-09-10 | The Board Of Regents Of The University Of Nebraska | Hydrothermal gel process for preparation of silicalite particles and process for preparation of composite membrane |
| JP2002335911A (en) * | 2001-05-21 | 2002-11-26 | Japan Organo Co Ltd | Method for concentrating and refining polyphenol |
| CN105032359A (en) * | 2010-03-30 | 2015-11-11 | 索尼公司 | Fungicide, photo catalytic composite material, adsorbent, and depurative |
| CN104874300A (en) * | 2015-04-30 | 2015-09-02 | 天津大学 | Chitosan-sulfonated carbon molecular sieve hybrid composite membrane and preparation and application |
| CN108479417A (en) * | 2018-04-28 | 2018-09-04 | 邹峰 | It is a kind of using glass hollow fiber as the preparation method of carrier molecule sieve membrane |
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