CN109876667A - A kind of preparation method of porous stainless steel membrane - Google Patents
A kind of preparation method of porous stainless steel membrane Download PDFInfo
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- CN109876667A CN109876667A CN201910271899.3A CN201910271899A CN109876667A CN 109876667 A CN109876667 A CN 109876667A CN 201910271899 A CN201910271899 A CN 201910271899A CN 109876667 A CN109876667 A CN 109876667A
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Abstract
The invention discloses a kind of preparation methods of porous stainless steel membrane, it is characterized in that, including following parts by weight material: metal-to-metal adhesive 5.1-8.2 parts by weight, plasticizer 3.4-6.4 parts by weight, pore-foaming agent 5.4-8.6 parts by weight, metal-powder 8.8-9.6 parts by weight, dispersing agent 15.6-17.8 parts by weight, organic solvent 27.2-38.6 and deionized water 8.4-10.8 parts by weight, step 1: processing staff carries out sanding and polishing to porous stainless steel base using sand paper, and it is poured into supersonic wave cleaning machine with the solution of the HCL of 3mol/L in advance and porous stainless steel base is cleaned by ultrasonic, and it is washed with deionized until neutrality, drying box is put into be dried for standby；Invention stainless steel membrane preparation uses sol-gel method porous stainless steel base coating process, chemical reaction is easy to carry out, and only need lower synthesis temperature, it is convenient and practical, it is easy to operate, and several nanometers of porous metal film, the seperation film that pore-size distribution is narrow, porosity is big can be prepared, at low cost, yield rate is higher.
Description
Technical field
The invention belongs to porous stainless steel membrane preparation technology fields, and in particular to a kind of preparation side of porous stainless steel membrane
Method.
Background technique
The method for preparing asymmetric porous stainless steel membrane at present can be divided into: step sintering and two kinds of co-sintering, step sintering
Be that asymmetric coating is prepared on the macropore matrix sintered, prepares coating method mainly have hot spray process, magnetron sputtering method,
Wet-milling spray coating method, spread coating etc..And there is some shared problems for these methods: 1, gradation sintering process is complicated, and repeatedly burns
It is high to tie energy consumption；2, since substrate has been sintered, the expansion of matrix and coating sintering shrinkage are mismatched during the sintering process, easy to crack,
It peels off, yield rate is low.In order to can be well solved problem as above, researcher attempts a step and prepares asymmetric porous stainless steel membrane
Green body, by long-term experiment, researcher passes through multilayer pressing [Liu Zhongjun, a kind of preparation of asymmetric stainless steel filter
Method, number of patent application 201210024816.9] and [Huang Yan, Yu Jian, a kind of porous ceramics-metal composite membrane material
Preparation method, application number: CN201110168259], centrifugal deposition method [Xi Zhengping, Tang Huiping Liu Zhongjun, Wang Qiangbing, one
The preparation method of kind of gradual-change bore diameter stainless steel antipriming pipe, number of patent application 200810232583.5] one step of success is made non-right
Claim porous stainless steel membrane green body.It is well known that the thermal expansion coefficient of the powder of material not of the same race is different and different
The sintering temperature of the powder of the same race of partial size be it is inconsistent, due to the presence of these odjective causes, current asymmetric porous stainless
The preparation process of the steel or excess agglomeration flux of film layer is relatively low or film layer is easily peeled off, bad mechanical strength.In general, mesh
There is problems for the preceding method for preparing asymmetric porous stainless steel membrane.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of porous stainless steel membrane, by using sol-gel fado
Hole stainless steel base coating process chemically reacts and is easy to carry out, and only needs lower synthesis temperature, convenient and practical, easily grasps
Make, and several nanometers of porous metal film, the seperation film that pore-size distribution is narrow, porosity is big, at low cost, yield rate can be prepared
It is higher；Meanwhile film layer powder of the present invention and porous stainless steel base bond properties are good, moulding is high, and porous stainless steel base with
Film layer powder co-sintering, and then film layer is improved in the adhesiveness of porous stainless steel base outer surface, to solve above-mentioned background skill
The preparation process of the current asymmetric porous stainless steel proposed in art the or excess agglomeration flux of film layer is relatively low or film layer is easy
The problem of peeling, bad mechanical strength.
To achieve the above object, the invention provides the following technical scheme: a kind of preparation method of porous stainless steel membrane, including
Following parts by weight material: metal-to-metal adhesive 5.1-8.2 parts by weight, plasticizer 3.4-6.4 parts by weight, pore-foaming agent 5.4-8.6 weight
Part, metal-powder 8.8-9.6 parts by weight, dispersing agent 15.6-17.8 parts by weight, organic solvent 27.2-38.6 and deionized water
8.4-10.8 parts by weight.
The preparation step of the porous stainless steel membrane is as follows:
Step 1: processing staff carries out sanding and polishing to porous stainless steel base using sand paper, and in advance with the HCL's of 3mol/L
Solution, which pours into supersonic wave cleaning machine, is cleaned by ultrasonic porous stainless steel base, and is washed with deionized to neutrality and is
Only, drying box is put into be dried for standby；
Step 2: processing staff pours into weighted metal-powder and dispersing agent in No.1 cylindrical reaction vessel, and stirring is equal
It is even to be prepared into metal alkoxide raw material；
Step 3: immediately processing staff poured into No. two cylindrical reaction vessels weighted organic solvent metal-to-metal adhesive and
Deionized water, and the metal alkoxide raw material in step 2 is poured into No. two cylindrical reaction vessels and is quickly stirred, revolving speed is
250r/min, control mixing time is 5min and controls mixeding liquid temperature to be 30-45 DEG C, and then metal alkoxide raw material is organic
After solvent dissolution and condensation reaction, stable low viscosity vitreosol solution is formed in the solution；
Step 4: weighted metal-to-metal adhesive, plasticising are added into No. two cylindrical reaction vessels of step 3 by processing staff
Agent and pore-foaming agent to be mixed with the low viscosity vitreosol solution in No. two cylindrical reaction vessels, and control stirring
Revolving speed is 150r/min, mixing time 10min, and then improves bonding, moulding and the pore of low viscosity vitreosol solution
Energy；
Step 5: processing staff's porous stainless using spray gun that vitreosol solution spraying in step 4 is spare in step 1
Steel matrix surface is put into drying box with the porous stainless steel base that will coat vitreosol solution and is dried, promotes
Bright sol solution carries out condensation cure on porous stainless steel base surface, and in the drying process, holding drying temperature is 20-30
DEG C, humidity 15%-25%, drying time 15min；
Step 6: the porous stainless steel base after drying and processing in step 5 is put into sintering furnace high temperature and is sintered by processing staff,
Control heating rate is 3-5 DEG C/min, and finally control baking temperature is 450-500 DEG C, soaking time 3.5-4.5h；
Step 7: the porous stainless steel base in step 6 obtains after natural cooling on its surface with a thickness of 5 μm~50 μm
Porous metal film, complete porous stainless steel base porous outer surface metal film preparation operation.
Further, the metal-to-metal adhesive is specially polyurethane adhesive, and the plasticizer is specially phthalic acid
Dioctyl ester, the pore-foaming agent are specially lithium chloride.
Further, the dispersing agent is specially ethylene glycol, the organic solvent be methanol, ethyl alcohol, isopropanol, acetone or
Butanone.
Further, the metal-powder is specially stainless steel powder, nickel powder or silver powder.
Further, sand paper uses 400-1000 mesh sand paper in the step 1.
Further, the aperture of porous metal film is not more than 18 μm in the step 6.
Compared with prior art, the beneficial effects of the present invention are:
The preparation method raw material of porous stainless steel membrane of the present invention is dispersed to the solution in solvent and forming low viscosity first, because
This, so that it may the uniformity for obtaining molecular level in a short period of time is likely between reactant when forming gel
It is uniformly mixed on molecular level, chemically reacts and be easy to carry out, and only need lower synthesis temperature, it is convenient and practical, easily
Operation, and several nanometers of porous metal film, the seperation film that pore-size distribution is narrow, porosity is big, at low cost, finished product can be prepared
Rate is higher；Meanwhile film layer powder of the present invention and porous stainless steel base bond properties are good, moulding is high, and porous stainless steel base
With film layer powder co-sintering, solves film layer and easily peel off this problem.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of porous stainless steel membrane, including following parts by weight material: 5.1 parts by weight of metal-to-metal adhesive, plasticizer
3.4 parts by weight, 5.4 parts by weight of pore-foaming agent, 8.8 parts by weight of metal-powder, 15.6 parts by weight of dispersing agent, organic solvent 27.2 and nothing
8.4 parts by weight of ionized water.
The preparation step of the porous stainless steel membrane is as follows:
Step 1: processing staff carries out sanding and polishing to porous stainless steel base using sand paper, and in advance with the HCL's of 3mol/L
Solution, which pours into supersonic wave cleaning machine, is cleaned by ultrasonic porous stainless steel base, and is washed with deionized to neutrality and is
Only, drying box is put into be dried for standby；
Step 2: processing staff pours into weighted metal-powder and dispersing agent in No.1 cylindrical reaction vessel, and stirring is equal
It is even to be prepared into metal alkoxide raw material；
Step 3: immediately processing staff poured into No. two cylindrical reaction vessels weighted organic solvent metal-to-metal adhesive and
Deionized water, and the metal alkoxide raw material in step 2 is poured into No. two cylindrical reaction vessels and is quickly stirred, revolving speed is
250r/min, control mixing time is 5min and controls mixeding liquid temperature to be 30-45 DEG C, and then metal alkoxide raw material is organic
After solvent dissolution and condensation reaction, stable low viscosity vitreosol solution is formed in the solution；
Step 4: weighted metal-to-metal adhesive, plasticising are added into No. two cylindrical reaction vessels of step 3 by processing staff
Agent and pore-foaming agent to be mixed with the low viscosity vitreosol solution in No. two cylindrical reaction vessels, and control stirring
Revolving speed is 150r/min, mixing time 10min, and then improves bonding, moulding and the pore of low viscosity vitreosol solution
Energy；
Step 5: processing staff's porous stainless using spray gun that vitreosol solution spraying in step 4 is spare in step 1
Steel matrix surface is put into drying box with the porous stainless steel base that will coat vitreosol solution and is dried, promotes
Bright sol solution carries out condensation cure on porous stainless steel base surface, and in the drying process, holding drying temperature is 20-30
DEG C, humidity 15%-25%, drying time 15min；
Step 6: the porous stainless steel base after drying and processing in step 5 is put into sintering furnace high temperature and is sintered by processing staff,
Control heating rate is 3-5 DEG C/min, and finally control baking temperature is 450-500 DEG C, soaking time 3.5-4.5h；
Step 7: the porous stainless steel base in step 6 obtains after natural cooling on its surface with a thickness of 5 μm~50 μm
Porous metal film, complete porous stainless steel base porous outer surface metal film preparation operation.
Wherein, the metal-to-metal adhesive is specially polyurethane adhesive, and the plasticizer is specially that phthalic acid two is pungent
Ester, the pore-foaming agent are specially lithium chloride.
Wherein, the dispersing agent is specially ethylene glycol, and the organic solvent is methanol, ethyl alcohol, isopropanol, acetone or fourth
Ketone.
Wherein, the metal-powder is specially stainless steel powder, nickel powder or silver powder.
Wherein, sand paper uses 400-1000 mesh sand paper in the step 1.
Wherein, the aperture of porous metal film is not more than 18 μm in the step 6.
Embodiment 2
A kind of preparation method of porous stainless steel membrane, including following parts by weight material: 8.2 parts by weight of metal-to-metal adhesive, plasticizer
6.4 parts by weight, 8.6 parts by weight of pore-foaming agent, 9.6 parts by weight of metal-powder, 17.8 parts by weight of dispersing agent, organic solvent 38.6 and nothing
10.8 parts by weight of ionized water.
The preparation step of the porous stainless steel membrane is as follows:
Step 1: processing staff carries out sanding and polishing to porous stainless steel base using sand paper, and in advance with the HCL's of 3mol/L
Solution, which pours into supersonic wave cleaning machine, is cleaned by ultrasonic porous stainless steel base, and is washed with deionized to neutrality and is
Only, drying box is put into be dried for standby；
Step 2: processing staff pours into weighted metal-powder and dispersing agent in No.1 cylindrical reaction vessel, and stirring is equal
It is even to be prepared into metal alkoxide raw material；
Step 3: immediately processing staff poured into No. two cylindrical reaction vessels weighted organic solvent metal-to-metal adhesive and
Deionized water, and the metal alkoxide raw material in step 2 is poured into No. two cylindrical reaction vessels and is quickly stirred, revolving speed is
250r/min, control mixing time is 5min and controls mixeding liquid temperature to be 30-45 DEG C, and then metal alkoxide raw material is organic
After solvent dissolution and condensation reaction, stable low viscosity vitreosol solution is formed in the solution；
Step 4: weighted metal-to-metal adhesive, plasticising are added into No. two cylindrical reaction vessels of step 3 by processing staff
Agent and pore-foaming agent to be mixed with the low viscosity vitreosol solution in No. two cylindrical reaction vessels, and control stirring
Revolving speed is 150r/min, mixing time 10min, and then improves bonding, moulding and the pore of low viscosity vitreosol solution
Energy；
Step 5: processing staff's porous stainless using spray gun that vitreosol solution spraying in step 4 is spare in step 1
Steel matrix surface is put into drying box with the porous stainless steel base that will coat vitreosol solution and is dried, promotes
Bright sol solution carries out condensation cure on porous stainless steel base surface, and in the drying process, holding drying temperature is 20-30
DEG C, humidity 15%-25%, drying time 15min；
Step 6: the porous stainless steel base after drying and processing in step 5 is put into sintering furnace high temperature and is sintered by processing staff,
Control heating rate is 3-5 DEG C/min, and finally control baking temperature is 450-500 DEG C, soaking time 3.5-4.5h；
Step 7: the porous stainless steel base in step 6 obtains after natural cooling on its surface with a thickness of 5 μm~50 μm
Porous metal film, complete porous stainless steel base porous outer surface metal film preparation operation.
Wherein, the metal-to-metal adhesive is specially polyurethane adhesive, and the plasticizer is specially that phthalic acid two is pungent
Ester, the pore-foaming agent are specially lithium chloride.
Wherein, the dispersing agent is specially ethylene glycol, and the organic solvent is methanol, ethyl alcohol, isopropanol, acetone or fourth
Ketone.
Wherein, the metal-powder is specially stainless steel powder, nickel powder or silver powder.
Wherein, sand paper uses 400-1000 mesh sand paper in the step 1.
Wherein, the aperture of porous metal film is not more than 18 μm in the step 6.
Embodiment 3
A kind of preparation method of porous stainless steel membrane, including following parts by weight material: 6.65 parts by weight of metal-to-metal adhesive, plasticizer
4.9 parts by weight, 7 parts by weight of pore-foaming agent, 9.2 parts by weight of metal-powder, 16.7 parts by weight of dispersing agent, organic solvent 32.9 and without from
Sub- 9.6 parts by weight of water.
The preparation step of the porous stainless steel membrane is as follows:
Step 1: processing staff carries out sanding and polishing to porous stainless steel base using sand paper, and in advance with the HCL's of 3mol/L
Solution, which pours into supersonic wave cleaning machine, is cleaned by ultrasonic porous stainless steel base, and is washed with deionized to neutrality and is
Only, drying box is put into be dried for standby；
Step 2: processing staff pours into weighted metal-powder and dispersing agent in No.1 cylindrical reaction vessel, and stirring is equal
It is even to be prepared into metal alkoxide raw material；
Step 3: immediately processing staff poured into No. two cylindrical reaction vessels weighted organic solvent metal-to-metal adhesive and
Deionized water, and the metal alkoxide raw material in step 2 is poured into No. two cylindrical reaction vessels and is quickly stirred, revolving speed is
250r/min, control mixing time is 5min and controls mixeding liquid temperature to be 30-45 DEG C, and then metal alkoxide raw material is organic
After solvent dissolution and condensation reaction, stable low viscosity vitreosol solution is formed in the solution；
Step 4: weighted metal-to-metal adhesive, plasticising are added into No. two cylindrical reaction vessels of step 3 by processing staff
Agent and pore-foaming agent to be mixed with the low viscosity vitreosol solution in No. two cylindrical reaction vessels, and control stirring
Revolving speed is 150r/min, mixing time 10min, and then improves bonding, moulding and the pore of low viscosity vitreosol solution
Energy；
Step 5: processing staff's porous stainless using spray gun that vitreosol solution spraying in step 4 is spare in step 1
Steel matrix surface is put into drying box with the porous stainless steel base that will coat vitreosol solution and is dried, promotes
Bright sol solution carries out condensation cure on porous stainless steel base surface, and in the drying process, holding drying temperature is 20-30
DEG C, humidity 15%-25%, drying time 15min；
Step 6: the porous stainless steel base after drying and processing in step 5 is put into sintering furnace high temperature and is sintered by processing staff,
Control heating rate is 3-5 DEG C/min, and finally control baking temperature is 450-500 DEG C, soaking time 3.5-4.5h；
Step 7: the porous stainless steel base in step 6 obtains after natural cooling on its surface with a thickness of 5 μm~50 μm
Porous metal film, complete porous stainless steel base porous outer surface metal film preparation operation.
Wherein, the metal-to-metal adhesive is specially polyurethane adhesive, and the plasticizer is specially that phthalic acid two is pungent
Ester, the pore-foaming agent are specially lithium chloride.
Wherein, the dispersing agent is specially ethylene glycol, and the organic solvent is methanol, ethyl alcohol, isopropanol, acetone or fourth
Ketone.
Wherein, the metal-powder is specially stainless steel powder, nickel powder or silver powder.
Wherein, sand paper uses 400-1000 mesh sand paper in the step 1.
The working principle of the invention and process for using: colloidal sol -- gel method (S0l--Gel method, abbreviation SG method) are exactly with nothing
Machine object or metal alkoxide make presoma, uniformly mix these raw materials in liquid phase, and are hydrolyzed, are condensed chemical reaction, molten
Stable vitreosol system is formed in liquid, colloidal sol is aged, slowly polymerize between micelle, forms the solidifying of three-dimensional space network structure
Glue is filled with the solvent to lose flowability between gel network, forms gel, and gel prepares molecule by dry, sintering curing
Or even the material of nanometer substructure, and then improve plating piece mechanical strength.Processing process, step 1: processing staff uses sand
Paper carries out sanding and polishing to porous stainless steel base, and poured into advance with the solution of the HCL of 3mol/L it is right in supersonic wave cleaning machine
Porous stainless steel base is cleaned by ultrasonic, and is washed with deionized until neutrality, is put into drying box and is dried for standby；Step
Two: processing staff pours into weighted metal-powder and dispersing agent in No.1 cylindrical reaction vessel, stirs evenly and is prepared into
Metal alkoxide raw material；Step 3: processing staff pours into weighted organic solvent gold into No. two cylindrical reaction vessels immediately
Belong to adhesive and deionized water, and the metal alkoxide raw material in step 2 is poured into No. two cylindrical reaction vessels and is quickly stirred
It mixes, revolving speed 250r/min, control mixing time is 5min and controls mixeding liquid temperature to be 30-45 DEG C, and then metal alkoxide is former
Material is dissolved by an organic solvent and after condensation reaction, forms stable low viscosity vitreosol solution in the solution；Step 4: processing
Weighted metal-to-metal adhesive, plasticizer and pore-foaming agent is added into No. two cylindrical reaction vessels of step 3 in personnel, thus
It is mixed with the low viscosity vitreosol solution in No. two cylindrical reaction vessels, and controlling speed of agitator is 150r/min,
Mixing time is 10min, and then improves bonding, moulding and the pore performance of low viscosity vitreosol solution；Step 5: processing people
Member is using spray gun porous stainless steel base surface that vitreosol solution spraying in step 4 is spare in step 1, with will
The porous stainless steel base of coating vitreosol solution is put into drying box and is dried, promote vitreosol solution it is porous not
Rust steel matrix surface carries out condensation cure, and in the drying process, keeping drying temperature is 20-30 DEG C, humidity 15%-25%, does
Dry time 15min；Step 6: the porous stainless steel base after drying and processing in step 5 is put into sintering furnace high by processing staff
Temperature sintering, control heating rate are 3-5 DEG C/min, and finally control baking temperature is 450-500 DEG C, soaking time 3.5-
4.5h；Step 7: the porous stainless steel base in step 6 obtains after natural cooling on its surface with a thickness of 5 μm~50 μ
The porous metal film of m completes the preparation operation of porous stainless steel base porous outer surface metal film.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of preparation method of porous stainless steel membrane, which is characterized in that including following parts by weight material: metal-to-metal adhesive 5.1-
8.2 parts by weight, plasticizer 3.4-6.4 parts by weight, pore-foaming agent 5.4-8.6 parts by weight, metal-powder 8.8-9.6 parts by weight, dispersion
Agent 15.6-17.8 parts by weight, organic solvent 27.2-38.6 and deionized water 8.4-10.8 parts by weight；
The preparation step of the porous stainless steel membrane is as follows:
Step 1: processing staff carries out sanding and polishing to porous stainless steel base using sand paper, and in advance with the HCL's of 3mol/L
Solution, which pours into supersonic wave cleaning machine, is cleaned by ultrasonic porous stainless steel base, and is washed with deionized to neutrality and is
Only, drying box is put into be dried for standby；
Step 2: processing staff pours into weighted metal-powder and dispersing agent in No.1 cylindrical reaction vessel, and stirring is equal
It is even to be prepared into metal alkoxide raw material；
Step 3: immediately processing staff poured into No. two cylindrical reaction vessels weighted organic solvent metal-to-metal adhesive and
Deionized water, and the metal alkoxide raw material in step 2 is poured into No. two cylindrical reaction vessels and is quickly stirred, revolving speed is
250r/min, control mixing time is 5min and controls mixeding liquid temperature to be 30-45 DEG C, and then metal alkoxide raw material is organic
After solvent dissolution and condensation reaction, stable low viscosity vitreosol solution is formed in the solution；
Step 4: weighted metal-to-metal adhesive, plasticising are added into No. two cylindrical reaction vessels of step 3 by processing staff
Agent and pore-foaming agent to be mixed with the low viscosity vitreosol solution in No. two cylindrical reaction vessels, and control stirring
Revolving speed is 150r/min, mixing time 10min, and then improves bonding, moulding and the pore of low viscosity vitreosol solution
Energy；
Step 5: processing staff's porous stainless using spray gun that vitreosol solution spraying in step 4 is spare in step 1
Steel matrix surface is put into drying box with the porous stainless steel base that will coat vitreosol solution and is dried, promotes
Bright sol solution carries out condensation cure on porous stainless steel base surface, and in the drying process, holding drying temperature is 20-30
DEG C, humidity 15%-25%, drying time 15min；
Step 6: the porous stainless steel base after drying and processing in step 5 is put into sintering furnace high temperature and is sintered by processing staff,
Control heating rate is 3-5 DEG C/min, and finally control baking temperature is 450-500 DEG C, soaking time 3.5-4.5h；
Step 7: the porous stainless steel base in step 6 obtains after natural cooling on its surface with a thickness of 5 μm~50 μm
Porous metal film, complete porous stainless steel base porous outer surface metal film preparation operation.
2. a kind of preparation method of porous stainless steel membrane according to claim 1, it is characterised in that: the metal-to-metal adhesive
Specially polyurethane adhesive, the plasticizer are specially dioctyl phthalate, and the pore-foaming agent is specially lithium chloride.
3. a kind of preparation method of porous stainless steel membrane according to claim 1, it is characterised in that: the dispersing agent is specific
For ethylene glycol, the organic solvent is methanol, ethyl alcohol, isopropanol, acetone or butanone.
4. a kind of preparation method of porous stainless steel membrane according to claim 1, it is characterised in that: the metal-powder tool
Body is stainless steel powder, nickel powder or silver powder.
5. a kind of preparation method of porous stainless steel membrane according to claim 1, it is characterised in that: sand in the step 1
Paper uses 400-1000 mesh sand paper.
6. a kind of preparation method of porous stainless steel membrane according to claim 1, it is characterised in that: more in the step 6
The aperture of mesoporous metal film is not more than 18 μm.
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