CN105536560A - Method For Preparing Double-Layer Polysulfone Support Film of Different Ingredients and Structures - Google Patents

11/13/23, 9:51 AM CN105536560A - Method for preparing double-layer polysulfone support film of different ingredients and structures - Google
ingredients and structures - Google Patents
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Method for preparing double-layer polysulfone support film of different ingredients and structures
Abstract
CN105536560A
The invention relates to preparation methods for polysulfone support films and particularly relates to
China
a method for preparing a double-layer polysulfone support film which has different ingredients and
structures and is stable in compacting resistance under the condition of high-pressure operation.
According to the method, the double-layer polysulfone support film is prepared through enabling a Download PDF Find Prior Art Similar
polysulfone support film formed by a polysulfone film casting solution A of low mass percentage
concentration and a hydrophobic nano-material added polysulfone film casting solution B to Other languages: Chinese
simultaneously enter a gel bath in an interleaved coating manner, and carrying out solvent/non-
Inventor: 王铭, 潘巧明, 张宇
solvent phase conversion. The method has the advantages that the defect that the peeling strength
between a support film and non-woven fabrics is lowered due to the fact that the overall viscosity of Current Assignee : Hangzhou Water Treatment Technology
the film casting solutions are improved after a nano-material is added into the film casting solutions Development Center Co Ltd
is overcome; and the hydrophobic nano-material is added, so that flow pore walls in the film and film
surface are hydrophobic, the flowing-through rate of water molecules is increased, and the produced
Worldwide applications
water flux of the film is improved while efficient salt removing performance of the film is maintained.
2015 CN
Classifications
Application CN201510967360.3A events
B01D69/105 Support pretreatment
2015-12-19 Application filed by Hangzhou Water Treatment
View 2 more classifications Technology Development Center Co Ltd
2015-12-19 Priority to CN201510967360.3A
2016-05-04 Publication of CN105536560A
2018-01-16 Application granted
2018-01-16 Publication of CN105536560B
Status Active
2035-12-19 Anticipated expiration
Info: Patent citations (4), Cited by (8), Legal events, Similar

documents, Priority and Related Applications
External links: Espacenet, Global Dossier, Discuss
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11/13/23, 9:51 AM CN105536560A - Method for preparing double-layer polysulfone support film of different ingredients and structures - Google Patents
1. the double-deck polysulfones support membrane preparation method of a different component and structure, it is characterized in that, double-deck polysulfones support
membrane is the polysulfones support membrane that formed by the polysulfones casting solution A of low quality percent concentration and with the addition of the
polysulfones casting solution B of hydrophobic nano material by coating method of staggering the time, and enters simultaneously and carries out the preparation of
solvent/non-solvent inversion of phases in coagulation bath and obtain;
Wherein, the mass percent concentration of polysulfones casting solution B is equal to or greater than polysulfones casting solution A;
In described polysulfones casting solution A, shared by polysulfones raw material, mass percent concentration is 10-16wt%; In polysulfones casting solution B, shared by
polysulfones raw material, mass percent concentration is 16-22wt%;
The solvent of described dissolving polysulfones raw material is the combination of one or more in dimethyl formamide, dimethylacetylamide, N-methyl pyrrole network alkane
ketone;
Described hydrophobic nano material is one or both the combination in hydrophobic nano-silica, hydrophobic nano zeolite.
2. a kind of preparation method according to claim 1, is characterized in that, the quality of hydrophobic nano material in casting solution of interpolation is the 0.1-10wt%
of polysulfones material quality; The particle diameter of hydrophobic nano material is 0.1-150nm.
3. a kind of preparation method according to claim 1, it is characterized in that, in above-mentioned polysulfones casting solution B, polysulfones material quality percent
concentration is 17-19wt%, and wherein the quality of hydrophobic nano material in polysulfones casting solution B is the 3-5wt% of polysulfones material quality;
Wherein the particle diameter of hydrophobic nano material is 10-30nm.
4. a kind of preparation method according to claim 1, is characterized in that, described method comprises the following steps:
(A) add quantitative polysulfones raw material and solvents, 120 DEG C add thermal agitation 12h, after deaeration process 2h, are configured to the polysulfones casting
solution A of low quality percent concentration;
(B) by with the addition of hydrophobic nano material polysulfones casting solution ultrasonic wave process 5-10min after, add quantitative polysulfones raw material,
120 DEG C add thermal agitation 12h after, carry out deaeration process, be configured to the polysulfones casting solution B containing hydrophobic nano material;
(C) step (A) being configured the polysulfones casting solution A obtained is coated with first in nonwoven cloth material surface coating one deck feed liquid by
scheduled volume;
(D) step B is configured the polysulfones casting solution obtained and in the middle ground floor feed liquid formed of step (A), be coated with second layer feed liquid
by scheduled volume dispense tip two;
(E) surface is coated with step (C), the non-woven fabrics of double-deck feed liquid layer that (D) coating is formed, be delivered in coagulation bath and carry out
solvent/non-solvent inversion of phases film forming;
(F) diaphragm having carried out inversion of phases enters post rinse tank after walking out from gel bath, uses deionized water to carry out rinsing to diaphragm; After
40-60 DEG C of rinsed with deionized water, make internal residual solvent thoroughly exchange precipitation, support membrane overall structure is more fine and close.
5. a kind of preparation method according to claim 3, is characterized in that, the thickness of the ground floor polysulfone supporting layer that polysulfones casting
solution A is formed is 15-20 μm, and wherein the polysulfone supporting layer degree of depth embedded in non-woven fabrics hole is 40-50 μm.
6. a kind of preparation method according to claim 3, is characterized in that, the thickness of the second layer polysulfone supporting layer that polysulfones casting
solution B is formed is 15-20 μm, and wherein the polysulfone supporting layer degree of depth embedded in non-woven fabrics hole is 40-50 μm.
7. a kind of preparation method according to claim 3, is characterized in that, the ground floor polysulfone supporting layer that polysulfones casting solution A is formed
is made up of single polysulfones component.
8. a kind of preparation method according to claim 3, is characterized in that, the second layer polysulfone supporting layer that polysulfones casting solution B is formed
is made up of hydrophobic nano material and polysulfones hydridization component.
9. a kind of preparation method according to claim 3, is characterized in that, the second layer polysulfone supporting layer that polysulfones casting solution B is formed
has hydrophobicity runner hole wall, hydrophobic film surface texture.
10. a kind of preparation method according to claim 1, is characterized in that, described is Flat Membrane, hollow-fibre membrane.
Description
The double-deck polysulfones support membrane preparation method of a kind of different component and structure
Technical field
The present invention relates to a kind of preparation method of polysulfones support membrane, more specifically relate to a kind of double-deck polysulfones support
membrane preparation method that there is pressure tightness under different component and structure, high pressure operating conditions can be stable.
Background technology
Reverse osmosis composite membrane diffusion barrier or NF membrane is formed at present by aqueous phase/organic phase interfacial polycondensation reaction,
be one of comparatively ripe preparation technology of the extensive preparative separation membrane component of industrialization, the respective support film
formed by solvent/non-solvent phase inversion is the main carriers material of load bearing interface polymerisation.The material of fine-porous support membrane
roughly can divide into polysulfones, polyether sulfone, cellulose acetate or its modification body etc.Because polysulfone material has higher chemistry, machinery,
thermal stability in these materials, therefore it is widely adopted in industrialization is prepared on a large scale.
Along with increase and the economic development of world population, the requirement of water is also in quick increase, in addition the factor such as greenhouse
effects of the earth also produces larger impact to water circulation, global water resources is not enough, and this problem annoyings countries in the world just day by
day, seawater desalination reverse osmosis membrane technology can for the most effective of the freshwater resources of the mankind and one of environmentally
friendly technological means as can directly obtain from high concentration salt solution now, and application is in the world just increasingly extensive.China's reverse
osmosis membrane seawater treatment technologies and low-temperature multiple-effect distillation Seawater Treatment method are jointly by as two large
desalinization mainstream technologys according to statistics, and reach advanced world standards.
In fact, along with constantly carrying out of seawater desalination desalination process, seawater stoste is constantly concentrated, its concentration can constantly
rise, for continuing uninterrupted and high efficiency can obtain the target product that salinity meets fresh water standards, need in seawater UF membrane film both
sides to apply 800psi-900psi, even higher driving pressure, guarantee film feed side has enough driving net pressures to exit side direction.Due to the polysulfones
support membrane in the seawater diaphragm basic structure of non-woven fabrics, polysulfones support membrane, polyamide composite film composition and aramid
layer, under higher net pressure drives operation continuously, fenestra easily breaks and collapses, produce larger densification decay, in addition polyamide reverse
osmose membrane further by densification, have a strong impact on the stability of seawater diaphragm and element thereof, cause the significant problem such as the
sharp-decay of flux and the sharply increase of salt rejection rate index.To this, numerous researcher both domestic and external has done large quantifier elimination
and Science Explorations by aspects such as blended, the raw-material modifications of nano inorganic particle in membrane surface modification, composite film.
The people such as Zheng Sheng spoon uses and comprises the surface that the solution having a mixed solvent of the solvent of different solubilities parameter value
containing two or more is applied to porous support layer, forms polysulfones layer, described polysulfones layer forms polyamide active layer.Its 25 DEG C, the flow
velocity of 800psi, 4.5L/min, under 32000ppmNaCl aqueous solution water inlet test condition, film properties reaches sodium chloride removal efficiency, permeant flux
reaches 97.1-98.4%, 30.5-47.3gfd respectively.And the pore size on polysulfone supporting layer surface, hole number are tested, result show hole total quantity is 12500-
12907/1.054um 2, the hole number that diameter is greater than more than 40nm is 26-58/1.054um 2, shared by the hole that diameter is greater than more than 40nm,
the ratio of all well is 0.20-0.45%/1.054um 2(publication CN103648622A)
The people such as Ma Jun use and are added in organic solvent by nano materials such as the nano silicon after hydrophilic organic process, nano titanium oxide,
acidifying CNT or clays, and then the casting solution of preparation containing this kind of nano material.The support membrane of the materials such as nano
hybridization polysulfones/polyvinylidene fluoride/polyethersulfone sulfone is prepared by solvent/non-solvent phase inversion.Nano material is after hydrophilic organic
process, high dispersion in support membrane matrix is greatly improved, solve the caducous problem of nano material, and add the surface hydrophilicity of support
membrane because adding hydrophilic nano material, the antifouling property of its milipore filter gets a promotion.(authorizing, publication CN201210044045)
High-ranking military officer's people benzenediol analog derivatives such as Hu Yunxia join in the casting film blend solution of nano material and polymer, promote the
bonding between the good polymer of nano material, and in inversion of phases film forming procedure, by oxidation neck diphenol compounds Cheng Juling diphenol
compounds, thus the dispersion of the various nano material of crosslinking curing in polymeric matrix.(authorizing, publication CN103464013A)
Also rarely has the nano hybridization support membrane material that can be applicable to the higher driving pressure condition of sea water desalination membrane at
present.Its reason mainly contain following some: 1) in polysulfones or derivatives thereof, add hydrophilic nano material, though its surface hydrophilic performance can
be improved, reduce film surface contamination, but there is the problems such as easy deliquescence water suction in hydrophilic nano material in preservation, cause
when adding in corresponding casting solution, need the vacuum drying process through the long period, with prevent adsorbed water be mixed into casting solution
impact prepared by polysulfones support membrane membrane structure.2) nano material, the interpolation in casting solution such as crosslinking and curing agent,
though the pressure tightness of polysulfones support membrane material can be increased considerably, but the viscosity of casting solution can be increased
considerably simultaneously, in the preparation process of counter-infiltration Flat Membrane, increasing considerably of casting solution viscosity means that the degree
of depth that its infiltration embeds in nonwoven layer in same time can significantly reduce, significantly reduce the peel strength between non-woven fabrics and
polysulfones support membrane, the partial exfoliation between polysulfones support membrane and nonwoven layer is very easily caused under high-voltage
applications environment, foaming phenomena, film properties is caused to produce defect.3) the industrialization preparation method that sea-water reverse osmose
composite membrane is comparatively conventional is at present: the non-woven fabrics being coated with polysulfone supporting layer infiltrates in aqueous phase
solution entirely, then blow down film surface excess aqueous phase solution with nitrogen air knife, and then coating organic phase solution forms polyamide function
separating layer by interface polymerization reaction.Blended in such as polysulfones support membrane of hydrophilic nano material, the film surface hydrophilicity of
raising, can increase the difficulty that the superfluous aqueous phase solution of face makes a clean sweep of on the contrary, cause the polyamide functional layer
formed to occur flaw and bad point.4) in casting solution, hydrophilic nano material is added, strong hydrogen bond action is produced between the hydroxyl that its rich
surface contains and polysulfones sulfuryl group, the polysulfones feed liquid solvent/non-solvent speed that is separated is caused significantly to decline, easy
generation finger-like macroporous structure, as needing to bear the highest seawater support membrane material of net pressure in diffusion barrier, the defect of this
kind of structure is fairly obvious.5) development trend of seawater separation membrane has 2 points: low energy consumption and high separating efficiency.Be
embodied in a) under lower driving pressure, can stablize and obtain high-quality fresh water; B), under equal driving pressure, while ensureing that high-quality produces
water, its permeant flux is increased.The interpolation of hydrophilic nano material in polysulfones support membrane, its hydrophily effect, not only at film upper surface,
also can change the hydrophily of its fenestra wall simultaneously, makes its more hydrophiling.Numerous result of study shows, have hydrophilic-structure at port,
runner inner wall has in the aquaporin of hydrophobic structure, the through-rate of hydrone is the highest, and namely its permeant flux is maximum.The more
hydrophilic then hydrone of counter current inwall is larger by resistance, and its permeant flux is less on the contrary, and product water efficiency is lower.
Therefore, need to study to have compared with high-peeling strength between a kind of and non-woven fabrics, have that hydrophobicity runner hole wall is surperficial
with film, under high pressure operating conditions permeant flux densification attenuation rate low, easily realize the polysulfones support membrane preparation
method that industrialization prepared continuously fast.
Summary of the invention
The object of present disclosure there are provided a kind of double-deck polysulfones support membrane preparation method with different component and structure,
and by the polyamide seawater reverse osmosis membrane of this double layer support film preparation.Described double-deck polysulfones support membrane, it
possesses features: 1) between double-deck polysulfones support membrane entirety and non-woven fabrics, peel strength is greater than more than 45CN.2) possess
hydrophobicity runner hole wall and film surface, film surface contact angle be greater than or substantially equal former film.3) upper strata of double-deck polysulfones
support membrane is the hydridization PS membrane being added with hydrophobic nano material.4) lower floor of double-deck polysulfones support membrane is
single PS membrane.
The present invention is realized by following technical proposals, be the polysulfones support membrane that formed by the polysulfones casting solution A of low
quality percent concentration and with the addition of the polysulfones casting solution B of hydrophobic nano material by coating method of staggering the time by
double-deck polysulfones support membrane, enter simultaneously and carry out the preparation of solvent/non-solvent inversion of phases in coagulation bath and
obtain; Under using this optimized double-deck polysulfones support membrane, same compound film formulation condition, prepared sea-water reverse osmose
diaphragm salt rejection rate, permeant flux performance can reach 99.8% respectively under simulated seawater test condition (sodium chloride concentration:
32000ppm, 25 DEG C, 800psi), more than 29.41GFD, and permeant flux does not add the single polysulfones layer of hydrophobic nano material compared with upper
strata and promotes more than 40%.Use this seawater reverse osmosis membrane prepared by optimized double-deck polysulfones support membrane to run 24h
continuously after 800psi pressure is issued to stable state, its permeant flux attenuation rate is less than 2%.
Wherein, the mass percent concentration of polysulfones casting solution B is equal to or greater than polysulfones casting solution A;
In described polysulfones casting solution A, shared by polysulfones raw material, mass percent concentration is 10-16wt%; In polysulfones casting solution B, shared by
polysulfones raw material, mass percent concentration is 16-22wt%;
The solvent of described dissolving polysulfones raw material is the combination of one or more in dimethyl formamide, dimethylacetylamide, N-methyl pyrrole network
alkane ketone; In above-mentioned polysulfones casting solution A, polysulfones material quality percent concentration is 12-14wt%, and the solvent wherein dissolving
this polysulfones raw material is that dimethyl formamide is best;
In above-mentioned polysulfones casting solution B, polysulfones material quality percent concentration is 17-19wt%, and wherein the quality of hydrophobic nano
material in polysulfones casting solution B is the 3-5wt% of polysulfones material quality; Wherein the particle diameter of hydrophobic nano material is 10-30nm.
Described hydrophobic nano material is one or both the combination in hydrophobic nano-silica, hydrophobic nano zeolite.
The mass percent of hydrophobic nano material in casting solution is the 0.1-10wt% of polysulfones material quality percentage; The particle diameter of hydrophobic
nano material is between 0.1nm-300nm;
Wherein the solvent of dissolving polysulfones raw material is one or more the above combinations in the organic solvents such as dimethyl formamide,
dimethylacetylamide, N-methyl pyrrole network alkane ketone;
Wherein coagulation bath component is one or more the above combinations in deionized water, 0-10wt% dimethylformamide in water, 0-10wt% dimethylacetamide
amine aqueous solution, 0-10wt%N-methyl pyrrole network alkane ketone;
As preferably, in above-mentioned preparation method, described method comprises the following steps:
(A) add quantitative polysulfones raw material and solvents, 120 DEG C add thermal agitation 12h, after deaeration process 2h, are configured to the polysulfones casting
solution A of low quality percent concentration;
(B) by with the addition of hydrophobic nano material polysulfones casting solution ultrasonic wave process 5-10min after, add quantitative polysulfones raw material,
120 DEG C add thermal agitation 12h after, carry out deaeration process, be configured to the polysulfones casting solution B containing hydrophobic nano material;
(C) step (A) being configured the polysulfones casting solution A obtained is coated with first in nonwoven cloth material surface coating one deck feed liquid by
scheduled volume;
(D) step B is configured the polysulfones casting solution obtained and in the middle ground floor feed liquid formed of step (A), be coated with second layer feed liquid
by scheduled volume dispense tip two;
(E) surface is coated with step (C), the non-woven fabrics of double-deck feed liquid layer that (D) coating is formed, be delivered in coagulation bath and carry out
solvent/non-solvent inversion of phases film forming;
(F) diaphragm having carried out inversion of phases enters post rinse tank after walking out from gel bath, uses deionized water to carry out rinsing to diaphragm; After
40-60 DEG C of rinsed with deionized water, make internal residual solvent thoroughly exchange precipitation, support membrane overall structure is more fine and close,
avoids the solvent in film to assemble and makes membrane structure produce defect.
As preferably, in above-mentioned a kind of preparation method, the thickness of the ground floor polysulfone supporting layer that polysulfones casting solution A is
formed is 15-20 μm, and wherein the polysulfone supporting layer degree of depth embedded in non-woven fabrics hole is 40-50 μm.
As preferably, in above-mentioned a kind of preparation method, the thickness of the second layer polysulfone supporting layer that polysulfones casting solution B is
formed is 15-20 μm, and wherein the polysulfone supporting layer degree of depth embedded in non-woven fabrics hole is 40-50 μm.
As preferably, the ground floor polysulfone supporting layer that in above-mentioned a kind of preparation method, polysulfones casting solution A is formed is made up
of single polysulfones component.
As preferably, the second layer polysulfone supporting layer that in above-mentioned a kind of preparation method, polysulfones casting solution B is formed is made up
of hydrophobic nano material and polysulfones hydridization component.
As preferably, the second layer polysulfone supporting layer that in above-mentioned a kind of preparation method, polysulfones casting solution B is formed has
hydrophobicity runner hole wall, hydrophobic film surface texture.
As preferably, described in above-mentioned a kind of preparation method is Flat Membrane, hollow-fibre membrane.
As preferably, the form of the double-deck polysulfone supporting layer described in above-mentioned preparation method is Flat Membrane, hollow-fibre membrane.
In the present invention, preparing too small or between excessive double-deck polysulfones support membrane and bottom nonwoven cloth the peel strength of
polysulfones material quality percentage in the polysulfones casting solution of ground floor polysulfone supporting layer affects larger, polysulfones mass percent
concentration is too small, viscosity is too low is unfavorable for that Large-Area-Uniform is coated with, and easily causes casting solution excessive permeation to the
non-woven fabrics back side; Polysulfones mass percent concentration is excessive, then cause the peel strength between double-deck polysulfone supporting layer and
non-woven fabrics significantly to reduce.
The polysulfones casting solution concentration preparing the double-deck polysulfone supporting layer second layer is larger, the too high meeting of viscosity causes
casting solution illiquidity, be unfavorable for large area all with coating, and the aperture, hole that film surface is formed is too small, hinder the adsorbance of later
stage interfacial polymerization process aqueous phase reactions monomer, considerable influence is produced to formed composite membrane performance.In second
layer polysulfones casting solution, the particle footpath of nano material is unsuitable excessive, particle diameter crosses the sharply increase that conference causes
film surface roughness, considerable influence is produced to formed composite membrane density, causes composite film to occur defect, be unfavorable for the
preparation of high performance membrane.
Beneficial effect
Double-deck polysulfones support membrane of the present invention introduces the ground floor polysulfone supporting layer that low quality percent concentration
casting solution is formed, solve after adding nano material in casting solution, casting solution overall viscosity promotes the defect that between support membrane
and non-woven fabrics, peel strength declines caused.Hydrophobic nano material is with the addition of in the polysulfones casting solution used when forming the
second layer, make flowing hole wall, film surface presentation hydrophobicity in film, particularly by the hydrophobicity improving film inner flow passage hole wall,
define surface hydrophilicity polyamide composite film and the double-deck polysulfone supporting layer special construction of inner hydrophobic, add the speed that
hydrone passes through in flowing, the colleague keeping the efficient salt of film to remove performance, improves the permeant flux of diaphragm.
Accompanying drawing explanation
Fig. 1 double-deck polysulfones support membrane preparation technology schematic flow sheet
Fig. 2 embeds the schematic diagram of the degree of depth in non-woven fabrics hole
Fig. 3 contains the cross-sectional configuration of the double-deck polysulfones support membrane of hydrophobic nano material by the second layer prepared by
electron-microscopic analysis embodiment 2
Fig. 4 contains the surface structure of the double-deck polysulfones support membrane of hydrophobic nano material by the second layer prepared by electron-
microscopic analysis embodiment 2
Fig. 5 is by the surface structure of the seawater composite membrane prepared by electron-microscopic analysis embodiment 2
Fig. 6 carries out the variation tendency of diaphragm salt rejection rate value running time for comparative example 1-4 and embodiment 1-3 institute
Fig. 7 carries out the variation tendency of diaphragm permeant flux value running time for comparative example 1-4 and embodiment 1-3 institute
Concrete truth mode
Comparative example 1
Walking cloth speed is 10m/min,, ambient temperature and humidity is 25 DEG C, 55%, uses the polysulfones casting solution that polysulfones material quality percent
concentration is 18wt%, solvents is dimethyl formamide, is the individual layer polysulfone supporting layer of 50 μm at nonwoven cloth material striking thickness
(D2+D1).
Except the polysulfones casting solution that use with the addition of 1wt%, the particle diameter 16nm of polysulfones mass percent concentration, the polysulfones
material quality percent concentration of hydrophobic nano-silica material is 18wt%, all the other steps are identical with comparative example 1.
Except the polysulfones casting solution that use polysulfones material quality percent concentration is 13wt%, all the other steps are identical with comparative example
1.
Except using the polysulfones casting solution coating thickness D2 that polysulfones material quality percent concentration is 13wt% to be 25 μm, the polysulfones
casting solution striking thickness D1 that use with the addition of 1wt%, the particle diameter 16nm of polysulfones mass percent concentration, the polysulfones
material quality percent concentration of hydrophilic nano earth silicon material is 18wt% is outside 25 μm, and all the other steps are identical with comparative example
1
Embodiment 1
Except using the polysulfones casting solution coating thickness D2 that polysulfones material quality percent concentration is 13wt% to be 25 μm, use the polysulfones
casting solution striking thickness D1 that polysulfones material quality percent concentration is 18wt% to be outside 25 μm, all the other steps are identical with
comparative example 1
Embodiment 2
material quality percent concentration of hydrophobic nano-silica material is 18wt% is outside 25 μm, and all the other steps are identical with comparative example 1
Embodiment 3
material quality percent concentration of hydrophobic nano-silica material is 18wt% is outside 25 μm, and all the other steps are identical with comparative example 1
Test the mensuration of 1 peel strength
Use peel strength tester (BLJ-100), test comparison example 1-4 and embodiment 1-4 prepares the peel strength value between polysulfones support membrane and
non-woven fabrics.Peel strength test wherein in comparative example and embodiment: adopt 90 degree of peel strength test methods to test peel strength between
diaphragm and non-woven fabrics.Adopt the peel strength value of arithmetic mean of instantaneous value as this sample of 50 peel strength value.
Wherein embed the polysulfone supporting layer degree of depth in non-woven fabrics hole, calculated by following formula:
Thickness (the D1+D2+D3)-polysulfones thickness (D1+D2) of rear polysulfones entirety peeled off completely by the polysulfone supporting layer degree of depth (the
D3)=non-woven fabrics embedded in non-woven fabrics hole
Wherein Film thickness values D1, D2, D3 is measured by digital display film thickness instrument, gets 10 dot thickness mean values as thickness sample angle value.
Test result is as table 1
Classification Peel strength (CN) Embed degree of depth D3 (μm) in non-woven fabrics hole Embodiment 1 50.71 46.83
Embodiment 2 52.21 48.05 Embodiment 3 51.98 47.53
Comparative example 1 19.13 17.53 Comparative example 2 15.37 14.98
Comparative example 3 51.21 49.01 Comparative example 4 50.79 46.85
Test the mensuration of 2 seawater composite membrane performances
Use comparative example 1-4 and embodiment 1-4 to prepare polysulfones support membrane, under same compound film formulation condition, prepare corresponding
seawater composite membrane, assess its salt rejection rate and permeant flux.The wherein preparation of composite membrane: aqueous phase, organic phase adopt
respectively: containing 5wt% m-phenylene diamine (MPD), 3wt% triethylamine hydrochloride, use NaOH, pH value of water solution is adjusted to the aqueous phase
solution of 9.0; IsoparG organic phase solution containing 1.4wt% pyromellitic trimethylsilyl chloride; Heat treatment temperature is 90 DEG C; Heat treatment time is
6min.The seawater composite membrane prepared 25 DEG C, the flow velocity of 800psi, 1GPM, 32000ppm NaCl aqueous solution water inlet test condition under
precompressed after 1 hour, the salt rejection rate of film and permeant flux are measured.Device for assessment of reverse osmosis membrane is HWTT-six pond high
pressure diaphragm testboard (Hangzhou Water Treatment Technology Research and Development Center Co.ltd's self-control), comprising test pool, high-pressure
pump, former water pot, pressure sensor, heat exchanger, effective film area is 26.5cm 2.Seawater composite membrane prepared by comparative example 1-4 and
embodiment 1-3 is arranged on after on test pool, the NaCl aqueous solution of 32000ppm is used to carry out precompressed in 1 hour, then measure the product water
water yield of 20 minutes, calculate salt rejection rate by the salinity of the former water of use conductivity meter analysis to measure, product water.Test result is as
table 2
Table 2
The test of experiment-3 seawater film pressure tightness
Use comparative example 1-4 and embodiment 1-4 to prepare polysulfones support membrane, under same compound film formulation condition, prepare corresponding
seawater composite membrane, assess its diaphragm pressure tightness energy.The wherein preparation of composite membrane: aqueous phase, organic phase adopt
respectively: containing 5wt% m-phenylene diamine (MPD), 3wt% triethylamine hydrochloride, use NaOH, pH value of water solution is adjusted to the aqueous phase
solution of 9.0; IsoparG organic phase solution containing 1.4wt% pyromellitic trimethylsilyl chloride; Heat treatment temperature is 90 DEG C; Heat treatment time is
6min.The seawater composite membrane prepared 25 DEG C, the flow velocity of 800psi, 1GPM, 32000ppm NaCl aqueous solution water inlet test condition under
precompressed every 3h, one-shot measurement is carried out to the salt rejection rate of film and permeant flux after 1 hour, test total duration 15h, this point is as zero
point.Device for assessment of reverse osmosis membrane is HWTT-six pond high pressure diaphragm testboard (Hangzhou Water Treatment Technology Research and
Development Center Co.ltd's self-control), comprising test pool, high-pressure pump, former water pot, pressure sensor, heat exchanger, effective film area is 26.5cm
2.Test result is as Fig. 6 and Fig. 7.
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CN112191114A * 2020-09-27 2021-01-08 泰州禾益新材料科技有 Polymer ultrafiltration membrane applied to polyamide composite membrane
限公司 support and preparation method thereof
CN112191112A * 2020-09-27 2021-01-08 泰州禾益新材料科技有 Polyamide reverse osmosis membrane with acid resistance and preparation
限公司 method thereof
CN113041854A * 2019-12-27 2021-06-29 时代沃顿科技有限公司 Preparation method of MBR flat membrane and MBR flat membrane prepared by
same
CN113694743A * 2021-08-17 2021-11-26 安徽智泓净化科技股份 Reverse osmosis membrane for treating high-salinity wastewater and preparation
有限公司 method thereof
CN115770490A * 2022-12-16 2023-03-10 杭州科百特过滤器材有 Asymmetric cellulose virus-removing filter membrane and preparation process
限公司 thereof
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11/13/23, 9:51 AM CN105536560A - Method for preparing double-layer polysulfone support film of different ingredients and structures - Google

ingredients and structures - Google Patents

Patents assignee:(Hangzhou Water Treatment Technology Development Center Co Ltd) 26 of 261

2015-12-19 Priority to CN201510967360.3A

2016-05-04 Publication of CN105536560A

2018-01-16 Application granted

2018-01-16 Publication of CN105536560B

2035-12-19 Anticipated expiration

Info: Patent citations (4), Cited by (8), Legal events, Similar

External links: Espacenet, Global Dossier, Discuss

Claims (10) Hide Dependent

Summary of the invention

Accompanying drawing explanation

Concrete truth mode

Test the mensuration of 1 peel strength

Test result is as table 1

Test the mensuration of 2 seawater composite membrane performances

The test of experiment-3 seawater film pressure tightness

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Publication number Priority date Publication date Assignee Title

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* Cited by examiner, † Cited by third party, ‡ Family to family citation

Publication Publication Date Title

CN104474926A 2015-04-01 Preparation method of polyamide reverse osmosis membrane

CN108722207A 2018-11-02 A kind of preparation method of Janus composite membranes

Priority And Related Applications

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2018-01-16 GR01 Patent grant

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