CN113731181A - Potting process for hollow fiber membrane module and preparation method of potting material - Google Patents
Potting process for hollow fiber membrane module and preparation method of potting material Download PDFInfo
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- CN113731181A CN113731181A CN202111071365.XA CN202111071365A CN113731181A CN 113731181 A CN113731181 A CN 113731181A CN 202111071365 A CN202111071365 A CN 202111071365A CN 113731181 A CN113731181 A CN 113731181A
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- hollow fiber
- fiber membrane
- polyurethane
- component
- pouring
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- 239000012528 membrane Substances 0.000 title claims abstract description 140
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000004382 potting Methods 0.000 title claims abstract description 36
- 230000008569 process Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000463 material Substances 0.000 title description 13
- 239000000565 sealant Substances 0.000 claims abstract description 56
- 229920002635 polyurethane Polymers 0.000 claims abstract description 44
- 239000004814 polyurethane Substances 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000004927 clay Substances 0.000 claims abstract description 24
- 239000011148 porous material Substances 0.000 claims abstract description 24
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 238000007711 solidification Methods 0.000 claims abstract description 8
- 230000008023 solidification Effects 0.000 claims abstract description 8
- 229920005862 polyol Polymers 0.000 claims description 43
- 150000003077 polyols Chemical class 0.000 claims description 34
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 33
- 229920000570 polyether Polymers 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 229910021485 fumed silica Inorganic materials 0.000 claims description 23
- 239000000945 filler Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
- -1 aromatic polyol Chemical class 0.000 claims description 10
- 239000006260 foam Substances 0.000 claims description 10
- 239000003112 inhibitor Substances 0.000 claims description 10
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 9
- 239000012948 isocyanate Substances 0.000 claims description 9
- 150000002513 isocyanates Chemical class 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002518 antifoaming agent Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- ALQLPWJFHRMHIU-UHFFFAOYSA-N 1,4-diisocyanatobenzene Chemical compound O=C=NC1=CC=C(N=C=O)C=C1 ALQLPWJFHRMHIU-UHFFFAOYSA-N 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 4
- 229920005906 polyester polyol Polymers 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- WUKNPIYSKBLCQI-UHFFFAOYSA-N CC(C=C1)=CC=C1C1=CC=C(C)C=C1.N=C=O.N=C=O Chemical compound CC(C=C1)=CC=C1C1=CC=C(C)C=C1.N=C=O.N=C=O WUKNPIYSKBLCQI-UHFFFAOYSA-N 0.000 claims description 3
- 229920000538 Poly[(phenyl isocyanate)-co-formaldehyde] Polymers 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- 125000000160 oxazolidinyl group Chemical group 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 15
- 230000001070 adhesive effect Effects 0.000 abstract description 15
- 238000007789 sealing Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000003292 glue Substances 0.000 description 15
- 239000002981 blocking agent Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000011049 filling Methods 0.000 description 8
- 230000010412 perfusion Effects 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000004513 sizing Methods 0.000 description 5
- 230000009194 climbing Effects 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000007605 air drying Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000010440 gypsum Substances 0.000 description 3
- 229910052602 gypsum Inorganic materials 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ICLCCFKUSALICQ-UHFFFAOYSA-N 1-isocyanato-4-(4-isocyanato-3-methylphenyl)-2-methylbenzene Chemical compound C1=C(N=C=O)C(C)=CC(C=2C=C(C)C(N=C=O)=CC=2)=C1 ICLCCFKUSALICQ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000011179 visual inspection Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001631 haemodialysis Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000000322 hemodialysis Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
- B01D63/022—Encapsulating hollow fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
- B01D63/022—Encapsulating hollow fibres
- B01D63/023—Encapsulating materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a polyurethane potting process for a hollow fiber membrane component and a preparation method of the potting adhesive, which are characterized by comprising the following steps: a. arranging a plurality of hollow fiber membrane filaments in parallel to form a membrane filament bundle with the tail end being flush, and plugging one end of the membrane filament bundle by using modeling clay as a pore plugging agent; b. placing the hollow fiber membrane tows in a shell, and pouring a polyurethane pouring sealant with moderate thixotropy into one end with the hole plugging agent by adopting a pouring mode of vibration and gradual vacuum; c. repeating the steps a-b after the solidification is finished, and encapsulating the other end of the shell; d. cutting off the polyurethane pouring sealant with the pore plugging agent parts at the two ends of the membrane filament bundle to conduct membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed; the polyurethane pouring sealant is mainly prepared by the reaction of a component A and a component B. The sealing process is safe and environment-friendly, simple to operate and good in sealing effect.
Description
Technical Field
The invention belongs to the technical field of hollow fiber membrane components, and particularly relates to a potting process for a hollow fiber membrane component and a preparation method of a potting material.
Background
The hollow fiber membrane is a membrane with fibrous appearance and self-supporting function, belongs to the field of separation membranes, and is widely applied to the technologies of sewage treatment, pure water preparation, hemodialysis, seawater desalination, solvent dehydration, humidification, dehumidification and the like. In practice, hollow fiber membranes are typically used as modules, including: the hollow fiber membrane comprises a shell, hollow fiber membrane tows and pouring sealant, wherein the shell is designed according to a specific application scene, and two ends of the membrane tows are fixed in the shell through the pouring sealant. The preparation steps of the hollow fiber membrane module are generally as follows: firstly, a plurality of hollow fiber membrane yarns form a membrane tow, after the membrane tow holes are blocked by a pore blocking agent, the membrane tow is put into a shell, and then pouring sealant is poured into two ends of the membrane tow to form a sealing end. The hole blocking agent is used for preventing the pouring sealant from entering the film wire holes. And finally, cutting off the parts of the membrane silk bundle with the pore-plugging agent at the two ends to communicate the membrane silk pores, thereby forming the final hollow fiber membrane component.
Liquid resins are commonly used as the pore blocking agent, such as epoxy resins as the pore blocking agent in patent application No. 200610053745.X and uv glue as the pore blocking agent in application No. 200910186419. X. Further, the patent of application No. 201210350080.4 discloses the use of gypsum powder as a pore blocking agent, and the patent of application No. 201611131099.4 discloses the use of putty powder or gypsum powder with water in the ratio of (1.5-3): 1 to form a pore-plugging substance. The above techniques have the following disadvantages: (1) due to the wetting adsorption force and the capillary effect, the liquid resin before solidification can climb upwards along the inner wall and the outer wall of the membrane silk hole, so that the silk climbing phenomenon is caused, the plugging height is difficult to control, the cut-off part is increased, and the material is wasted; the film threads are adhered, so that the permeation of the later pouring sealant is influenced; (2) the putty powder or the gypsum powder is light powdery substance, dust is inevitably generated in the using process, and the body health is damaged.
Polyurethane pouring sealant is often used as pouring sealant for hollow fiber membrane module due to its characteristics of large hardness range, high strength, good toughness, adjustable operation time and curing time, etc. The application No. 201710341514.7 discloses a two-component polyurethane pouring sealant for a water treatment membrane, wherein the highest hardness of the polyurethane pouring sealant is 95A, and the application No. 201710728852.6 discloses a polyurethane pouring sealant for a water treatment curtain type membrane assembly, wherein the highest hardness of the polyurethane pouring sealant is 68D. The technology of the polyurethane encapsulating glue with higher hardness is less involved. And the conventional polyurethane potting process also has problems: (1) is easily influenced by moisture in the air, trace moisture in the membrane wires and the like, generates bubbles in the curing process and influences the service life of the membrane component. (2) The creeping wire is high, and the membrane wire is easy to break in the using process after the pouring sealant is solidified.
Patent application numbers 201110143337.4, 201611131099.4 pass through one or more glue injection points, and glue automatically flows into the shell to be encapsulated under the action of gravity. Because the gaps between the hollow fiber membrane filaments are small, the method has the following problems: (1) the sizing material is difficult to uniformly penetrate between the membrane filaments; (2) air bubbles generated in the perfusion process are not easy to be discharged; (3) the potting adhesive has larger filament climbing height to the fiber membrane in the curing process. Currently, two perfusion modes, i.e. vibration perfusion and centrifugal perfusion, are disclosed to solve the above problems, for example, patent application No. 201210571562.2 discloses a perfusion method in which a vibration motor is used to vibrate a shell in a vertical direction during perfusion so as to promote the uniform distribution of glue among membrane filaments. For example, patent application No. 200610053745.X, 201210350080.4, the potting compound is poured into one or both ends of the housing by centrifugal force, but the above method still has disadvantages: (1) the shell is vibrated when the membrane module is poured, the loose degree of membrane filaments in the membrane module is uneven, and the glue among the membrane filaments with small gaps cannot be completely filled in a permeating mode. And the single vibration mode is difficult to achieve the effect of complete defoaming; (2) after the encapsulating glue is led into the shell by the soft rubber tube, the glue extrudes the hollow fiber membrane yarns under the action of centrifugal force, so that the permeation of the glue is influenced, and the performance and the appearance of the product are influenced due to uneven distribution of the membrane yarns.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a polyurethane pouring sealant filling and sealing process for a hollow fiber membrane component, which is safe and environment-friendly, simple to operate and good in filling and sealing effect.
The invention also aims to provide a preparation method of the polyurethane pouring sealant for the hollow fiber membrane component, and the pouring sealant has high hardness, high temperature resistance and excellent humidity resistance.
The invention adopts the following technical scheme to realize the purpose: the encapsulating process of the polyurethane encapsulating adhesive for the hollow fiber membrane component is characterized by comprising the following steps.
a. A plurality of hollow fiber membrane filaments are arranged in parallel to form a membrane filament bundle with the tail end being parallel and level, and one end of the membrane filament bundle is blocked by a pore blocking agent.
b. And placing the hollow fiber membrane silk bundle in a shell, and pouring a polyurethane pouring sealant into one end with the pore blocking agent.
c. And (c) repeating the steps a-b after the solidification is finished, and filling and sealing the other end of the shell.
d. And cutting off the part of the pouring sealant with the pore plugging agent at the two ends of the membrane filament bundle to conduct the membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed.
The polyurethane pouring sealant is prepared by reacting a component A and a component B.
Wherein the component A is polymethylene polyphenyl isocyanate (PAPI).
The component B comprises the following raw materials in parts by weight:
50 parts of modified polyether polyol,
30 parts of aromatic polyol,
5-10 parts of porous filler,
5-10 parts of lamellar filler,
5-10 parts of heat-conducting filler,
1.6-2.8 parts of fumed silica,
1-3 parts of foam inhibitor,
0.02 portion of catalyst,
0.01 part of defoaming agent.
As a further illustration of the above scheme, the pore-plugging agent in step a is modeling clay, and one of ultralight clay and resin clay is adopted; the clay of the types can be rolled into slices, is easy to shape and strong in viscosity, can effectively block membrane filaments, and does not have any filament creeping phenomenon on the inner wall and the outer wall; the method comprises the following steps: grinding clay into 0.5-1.0mm uniform sheets, cutting into film tows with the same size, pressing the film tows onto the clay sheets, removing clay attached to the outer walls of the film tows, and air drying for 3-6h in a ventilated and dry environment.
The perfusion process in the step b is as follows: placing the shell on a vibrating table, keeping the end with the pore-plugging agent facing downwards, keeping vibrating at the frequency of 10Hz for 3-5min, pouring the pouring sealant into the shell, continuously keeping vibrating the shell and vacuumizing the shell in the pouring process, controlling the vacuum degree to be-0.05 MPa, increasing the vacuum degree to be-0.1 MPa after pouring, closing the vacuum after 3-5min, closing the vibrating after 5-8min, and curing at room temperature for 2-4h to obtain the anti-blocking sealant.
Further, the modified polyether polyol is obtained by reacting polyether polyol and isocyanate under certain conditions, and the hydroxyl value is 200-400 mgKOH/g; wherein the polyether polyol is any one or a mixture of two of high-functionality polyether polyol with the functionality of 4-8 and the hydroxyl value of 300-600 mKOH/g; the isocyanate is any one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), p-phenylene diisocyanate (PPDI) and dimethylbiphenyl diisocyanate (TODI).
The aromatic polyol comprises either one or a mixture of two of aromatic polyether polyol and aromatic polyester polyol, and the hydroxyl value is preferably 250-350 mgKOH/g.
The porous filler can absorb trace gas in the sizing material and comprises one of a molecular sieve, activated alumina and hollow activated carbon microspheres.
The lamellar filler can improve the barrier property of the pouring sealant and comprises one of nano montmorillonite, nano kaolin and nano mica powder.
The heat-conducting filler can form a heat-conducting path in the potting adhesive sizing material, so that the accumulation of reaction heat is reduced, and the shrinkage of the potting adhesive sizing material is reduced, wherein the heat-conducting filler comprises one of boron nitride, magnesium oxide, silicon carbide or silicon micropowder.
The gas isThe fumed silica is hydrophobic fumed silica with a specific surface area of 200m2(ii)/g; the using amount of the fumed silica accounts for 2.0-3.5% of the total amount of the polyhydric alcohol, the using amount of the fumed silica is excessive, the thixotropy of the encapsulating glue material is too strong, the permeability is poor, and the encapsulating qualification rate is low; the dosage of the fumed silica is too small, the thixotropic effect of the encapsulating rubber is weak, and the creeping height of the rubber after the curing of the rubber is larger.
The foam inhibitor is an oxazolidine latent curing agent, the latent curing agent reacts with water faster than NCO groups of the component A, and reactants do not contain gas, so that air holes in the pouring sealant can be avoided.
The catalyst is selected from one of tertiary amine catalysts or organic metal catalysts; the defoaming agent is an organic silicon defoaming agent.
A preparation method of polyurethane pouring sealant for hollow fiber membrane components is characterized by comprising the following steps.
a. Heating the dried polyether polyol to 50-60 ℃, adding metered isocyanate, reacting for 2-3h at 70-80 ℃, and cooling to room temperature to obtain the modified polyether polyol.
b. And c, uniformly stirring and mixing the aromatic polyol and the modified polyether polyol obtained in the step a, adding fumed silica to uniformly disperse at a high speed, heating to 110-130 ℃, adding other fillers, stirring and dehydrating for 2-3h in vacuum, cooling to 70-90 ℃, adding the foam inhibitor, the catalyst and the defoamer to uniformly stir, and cooling to room temperature to obtain the component B.
c. And (3) mixing and stirring the component A and the component B uniformly at room temperature according to the mass ratio, and defoaming in vacuum for 2-3min to obtain the polyurethane pouring sealant for the hollow fiber membrane module.
Preferably, in step b, the high-speed dispersion is performed for 30min at a rotation speed of 4000r/min by using a high-speed disperser, wherein the conventional method is to add all the fillers into the polyol for dispersion, but the molecular van der Waals force of the fumed silica is large, the fumed silica is difficult to disperse uniformly in the polyol, and the dispersion of other fillers is influenced. The invention pre-disperses the fumed silica in the polyol to obtain a uniform dispersion system.
Preferably, in step c, the mass ratio of the component A to the component B is 100: 100.
The invention adopts the technical scheme to achieve the beneficial effects.
The pouring sealant for the hollow fiber membrane component adopted by the invention comprises the following components: (1) after the polyether in the component B is modified by isocyanate, the length and rigidity of a molecular chain are increased, and a long and hard crosslinking structure is generated after the polyether reacts with PAPI, so that the pouring sealant can keep high hardness at normal temperature and high temperature; (2) the benzene ring structure in the aromatic polyol provides high hardness and excellent moisture and heat resistance for the pouring sealant; (3) the use of the latent curing agent inhibits the generation of bubbles of the material due to moisture; (4) the synergistic use of various fillers further improves the encapsulation and blocking effects of the pouring sealant; (5) the fumed silica makes the pouring sealant have moderate thixotropy. The pouring sealant has the following performance advantages: the hardness is high, and the Shore D hardness at 25 ℃ is not less than 85; the high temperature resistance is good, and the Shore D hardness at 150 ℃ is not less than 80; the moisture and heat resistance is good, and the Shore D hardness is not less than 80 after the membrane is soaked in hot water at 100 ℃ for 200 hours.
The hollow fiber membrane module potting process comprises the following steps: 1. using moldable clay as a pore plugging agent: (1) the operation is simple, safe and environment-friendly; (2) the plugging height is controllable, and the membrane silk adhesion cannot be caused; 2. perfusion principle and effect: (1) the fumed silica enables the encapsulating glue to have moderate thixotropy, the glue is thinned by shearing force generated by stirring and vibration, and the glue is promoted to permeate by combining a vibration mode, so that a cavity is avoided; after the vibration stops, the thixotropy thickens the sizing material, and the creeping height of the pouring sealant to the fiber membrane can be effectively reduced; (2) before filling, the shell is vibrated to ensure that the hollow fiber membrane yarn bundle is in a loose state, which is beneficial to glue penetration; (3) the mode of vibration and gradual vacuum ensures that the working surface of the pouring sealant is smooth, and simultaneously effectively eliminates bubbles generated in the pouring process, thereby improving the product quality.
Detailed Description
The invention relates to a potting process for a hollow fiber membrane component and a preparation method of a potting material, wherein the polyurethane potting adhesive for the hollow fiber membrane component is prepared by reacting a component A and a component B, wherein the component A is polymethylene polyphenyl isocyanate (PAPI).
The component B comprises the following raw materials in parts by weight:
50 parts of modified polyether polyol,
30 parts of aromatic polyol,
5-10 parts of porous filler,
5-10 parts of lamellar filler,
5-10 parts of heat-conducting filler,
1.6-2.8 parts of fumed silica,
2 parts of foam inhibitor,
0.02 portion of catalyst,
0.01 part of defoaming agent.
The modified polyether polyol is obtained by reacting polyether polyol and isocyanate under certain conditions, and has a hydroxyl value of 200-400 mgKOH/g; the polyether polyol is one or two of high-functionality polyether polyol with the functionality of 4-8 and the hydroxyl value of 300-600mKOH/g, and the mixture of the high-functionality polyether polyol and the high-hydroxyl value polyether polyol is more preferably polyether polyol ZS-4110I, the functionality of 8 and the hydroxyl value of 450mgKOH/g, Jiangsu clock mountain chemical industry Co.
The isocyanate is any one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), p-phenylene diisocyanate (PPDI) and dimethylbiphenyl diisocyanate (TODI), and is preferably diphenylmethane diisocyanate (MDI).
The aromatic polyol comprises any one or a mixture of two of aromatic polyether polyol and aromatic polyester polyol, and the hydroxyl value is 250-350 mgKOH/g; phthalic anhydride polyester polyol PS-3152, hydroxyl value of 315 mgKOH/g, Qingdao Ruinor chemical Co.
The foam inhibitor is an oxazolidine latent curing agent, preferably CH-3, ash and Hao industries (Shanghai) Co.
By adopting the preferable formula design of the technical scheme, the polyurethane pouring sealant for the hollow fiber membrane component has the characteristics of high hardness, high temperature resistance and excellent humidity resistance.
Example 1.
In this embodiment, a preparation process of the polyurethane potting adhesive for the hollow fiber membrane module and a potting process of the membrane module are provided.
1. Arranging a plurality of hollow fiber membrane yarns in parallel to form a membrane yarn bundle with the flush tail end, rolling ultralight clay into a uniform sheet with the size of 0.5mm, cutting the uniform sheet into a sheet with the same size as the membrane yarn bundle, pressing one end of the membrane yarn bundle on the ultralight clay sheet with force, removing clay attached to the outer wall of the membrane yarn, and air-drying for 3 hours in a ventilated and dry environment to obtain the hollow fiber membrane yarn bundle with one end of a membrane yarn hole blocked.
2. Heating 375g of ZS-4110I to 50 ℃, adding 125g of pure MDI, reacting for 2.5h at 80 ℃, and cooling to room temperature to obtain the modified polyether polyol.
Uniformly stirring the modified polyether polyol and 300g of PS-3152, adding 16g of fumed silica, uniformly dispersing at a high speed, heating to 120 ℃, adding 80g of hollow activated carbon microspheres, 60g of nano kaolin and 60g of magnesium oxide, stirring in vacuum, dehydrating for 2.5h, cooling to 80 ℃, adding 20g of foam inhibitor CH-3, 0.2g of catalyst organic bismuth and 0.1g of defoamer BYK066N, uniformly stirring, and cooling to room temperature to obtain a component B.
And (3) mixing and stirring the PAPI and the component B uniformly at room temperature according to the mass ratio of 100:100, and defoaming in vacuum for 2min to obtain the polyurethane pouring sealant for the hollow fiber membrane module.
3. Placing the hollow fiber membrane silk bundle obtained in the step (1) in a shell, placing the shell on a vibration table, keeping the end with the pore blocking agent facing downwards, keeping vibrating at the frequency of 10Hz for 4min, then pouring the pouring sealant obtained in the step (2) into the shell, continuously keeping vibrating the shell and vacuumizing the shell in the pouring process, wherein the vacuum degree is-0.05 MPa, increasing the vacuum degree to-0.1 MPa after pouring is finished, closing the vacuum after 4min, and closing the vibration after 7 min; curing at room temperature for 2h to obtain the final product.
4. And (5) repeating the steps 1-3 after the solidification is finished, and filling and sealing the other end of the shell.
5. And cutting off the part of the pouring sealant with the pore plugging agent at the two ends of the membrane filament bundle to conduct the membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed.
Example 2.
In this embodiment, a preparation process of the polyurethane potting adhesive for the hollow fiber membrane module and a potting process of the membrane module are provided.
1. Arranging a plurality of hollow fiber membrane yarns in parallel to form a membrane yarn bundle with the flush tail end, rolling resin clay into a uniform sheet with the size of 0.8mm, cutting the uniform sheet into a sheet with the same size as the membrane yarn bundle, pressing one end of the membrane yarn bundle on the ultralight clay sheet with force, removing clay attached to the outer wall of the membrane yarn, and air-drying for 4 hours in a ventilated and dry environment to obtain the hollow fiber membrane yarn bundle with one end of a membrane yarn hole blocked.
2. Heating 375g of ZS-4110I to 50 ℃, adding 125g of pure MDI, reacting for 2.5h at 80 ℃, and cooling to room temperature to obtain the modified polyether polyol.
Uniformly stirring the modified polyether polyol and 300g of PS-3152, adding 28g of fumed silica, uniformly dispersing at a high speed, heating to 130 ℃, adding 70g of activated alumina, 65g of nano-montmorillonite and 65g of silicon carbide, stirring and dehydrating in vacuum for 2.0h, cooling to 75 ℃, adding 20g of foam inhibitor CH-3, 0.2g of catalyst organic bismuth and 0.1g of defoamer BYK06 066N, uniformly stirring, and cooling to room temperature to obtain a component B.
And (3) mixing and stirring the PAPI and the component B uniformly at room temperature according to the mass ratio of 100:100, and defoaming in vacuum for 2min to obtain the polyurethane pouring sealant for the hollow fiber membrane module.
3. Placing the hollow fiber membrane silk bundle obtained in the step (1) in a shell, placing the shell on a vibration table, keeping the end with the pore blocking agent facing downwards, keeping vibrating at the frequency of 10Hz for 5min, then pouring the pouring sealant obtained in the step (2) into the shell, continuously keeping vibrating the shell and vacuumizing the shell in the pouring process, wherein the vacuum degree is-0.05 MPa, increasing the vacuum degree to-0.1 MPa after pouring is finished, closing the vacuum after 5min, and closing the vibration after 8 min; curing at room temperature for 3h to obtain the final product.
4. And (5) repeating the steps 1-3 after the solidification is finished, and filling and sealing the other end of the shell.
5. And cutting off the part of the pouring sealant with the pore plugging agent at the two ends of the membrane filament bundle to conduct the membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed.
Comparative example 1.
This comparative example is substantially the same as example 1 except that 35g of fumed silica was used in step 2.
Comparative example 2.
This comparative example is substantially the same as example 1 except that 10g of fumed silica was used in step 2.
Comparative example 3.
1. A commercially available polyurethane potting adhesive was used.
2. And (2) arranging a plurality of hollow fiber membrane yarns in parallel to form a membrane yarn bundle with the tail ends being flush, coating a polyurethane adhesive sold in the step (1) on one end of the membrane yarn bundle to block a membrane yarn hole, curing at room temperature for 8 hours, and scattering the fiber membrane yarns subjected to hole sealing treatment to obtain the hollow fiber membrane yarn bundle with one end of the membrane yarn hole being blocked.
3. And (3) placing the hollow fiber membrane silk bundle obtained in the step (2) in a shell, placing the shell on a centrifuge, introducing the polyurethane adhesive into one end with the pore blocking agent through a hose, centrifuging for 40min, taking out the shell, and curing at room temperature for 8h to obtain the hollow fiber membrane silk bundle.
4. And (5) repeating the step 2-3 after the solidification is finished, and centrifugally filling and sealing the other end of the shell.
5. And cutting off the part of the pouring sealant with the pore plugging agent at the two ends of the membrane filament bundle to conduct the membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed.
Comparative example 4.
1. A commercially available polyurethane potting adhesive was used.
2. And (2) arranging a plurality of hollow fiber membrane yarns in parallel to form a membrane yarn bundle with the tail ends being flush, coating a polyurethane adhesive sold in the step (1) on one end of the membrane yarn bundle to block a membrane yarn hole, curing at room temperature for 8 hours, and scattering the fiber membrane yarns subjected to hole sealing treatment to obtain the hollow fiber membrane yarn bundle with one end of the membrane yarn hole being blocked.
3. Placing the hollow fiber membrane silk bundle obtained in the step (2) in a shell, placing the shell on a vibration table, pouring the pouring sealant obtained in the step (1) into the shell with one end with the pore blocking agent facing downwards, keeping the shell vibrating at the frequency of 10Hz in the pouring process, and keeping vibrating for 5min after pouring, and then closing the vibration; curing at room temperature for 8h to obtain the final product.
4. And (5) repeating the step 2-3 after the solidification is finished, and filling and sealing the other end of the shell.
5. And cutting off the part of the pouring sealant with the pore plugging agent at the two ends of the membrane filament bundle to conduct the membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed.
And (5) testing the performance.
1. Hardness: the test was carried out according to GB/T531.1-2008.
2. Water absorption: the test was performed according to GB/T1690-.
3. The hole sealing rate is as follows: visual inspection was carried out.
4. Plugging length: after the pore-plugging agent is solidified, the length of the pore-plugging agent is adhered in the pores of the hollow fiber membrane.
5. The wire climbing height is as follows: after the potting adhesive is solidified, the height of the potting adhesive higher than the part of the potting working surface is adhered to the outer wall of the hollow fiber membrane wire.
6. Encapsulation qualification rate: and testing the sample by using 1 atmosphere, and keeping the sample for 5min without attenuation, thus the sample is qualified.
7. Appearance: visual inspection was carried out.
Table 1: testing of pouring sealant performance and pouring effect
The test results in table 1 show that the amount of fumed silica has a greater influence on the potting effect in examples 1 and 2 than in comparative examples 1 and 2, which indicates that the amount of fumed silica plays a crucial role in the potting effect in the present invention.
Compared with comparative examples 3 and 4 in the prior art, examples 1 and 2 of the invention have the advantages that (1) the pouring sealant has high hardness, excellent high temperature resistance and excellent damp-heat resistance; (2) the modeling clay is used as a pore plugging agent, so that the plugging effect is good; (3) moderate thixotropy of the encapsulating glue material is combined with the vibration filling process, so that the wire climbing height is reduced; (4) the encapsulation qualification rate is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (10)
1. A polyurethane encapsulating process for a hollow fiber membrane component is characterized by comprising the following steps:
a. arranging a plurality of hollow fiber membrane filaments in parallel to form a membrane filament bundle with the tail end being flush, and plugging one end of the membrane filament bundle by using modeling clay as a pore plugging agent;
b. placing the hollow fiber membrane tows in a shell, and pouring a polyurethane pouring sealant with moderate thixotropy into one end with the hole plugging agent by adopting a pouring mode of vibration and gradual vacuum;
c. repeating the steps a-b after the solidification is finished, and encapsulating the other end of the shell;
d. cutting off the polyurethane pouring sealant with the pore plugging agent parts at the two ends of the membrane filament bundle to conduct membrane filament holes to obtain a finished product of the hollow fiber membrane component which is poured and sealed;
in the step a, the clay for modeling is rolled into a uniform sheet with the thickness of 0.5-1.0mm, the uniform sheet is cut into membrane tows with the same size, the membrane tows are pressed on the clay sheet with force, the clay attached to the outer wall of the membrane tows is removed, and the clay is dried for 3-6 hours in a ventilated and dry environment to obtain the composite material;
the polyurethane pouring sealant is prepared by reacting a component A and a component B;
wherein the component A is polymethylene polyphenyl isocyanate;
the component B comprises the following raw materials in parts by weight:
50 parts of modified polyether polyol,
30 parts of aromatic polyol,
5-10 parts of porous filler,
5-10 parts of lamellar filler,
5-10 parts of heat-conducting filler,
1.6-2.8 parts of fumed silica,
1-3 parts of foam inhibitor,
0.02 portion of catalyst,
0.01 part of defoaming agent.
2. The polyurethane potting process for a hollow fiber membrane module as claimed in claim 1, wherein the molding clay in the step a is ultra-light clay or resin clay.
3. The polyurethane potting process for hollow fiber membrane modules as claimed in claim 1, wherein the potting process in step b is: placing the shell on a vibrating table, keeping the end with the pore-plugging agent facing downwards, keeping vibrating at the frequency of 10Hz for 3-5min, pouring the pouring sealant into the shell, continuously keeping the shell vibrating and vacuumizing the shell in the pouring process, controlling the vacuum degree to be-0.05 MPa, increasing the vacuum degree to be-0.1 MPa after pouring, closing the vacuum after 3-5min, closing the vibrating after 5-8min, and curing at room temperature for 2-4h to obtain the anti-blocking sealant.
4. The polyurethane potting process for the hollow fiber membrane module as claimed in claim 1, wherein the modified polyether polyol is obtained by reacting polyether polyol and isocyanate, and has a hydroxyl value of 200-400 mgKOH/g;
the polyether polyol is any one or a mixture of two of polyether polyol with functionality of 4-8, hydroxyl value of 300-600mgKOH/g and high functionality and high hydroxyl value;
the isocyanate is any one of toluene diisocyanate, diphenylmethane diisocyanate, p-phenylene diisocyanate and dimethyl biphenyl diisocyanate.
5. The polyurethane potting process for a hollow fiber membrane module as claimed in claim 1, wherein the aromatic polyol comprises one or a mixture of two of aromatic polyether polyol and aromatic polyester polyol, and the hydroxyl value is 250-350 mgKOH/g.
6. The polyurethane potting process for the hollow fiber membrane module as claimed in claim 1, wherein the porous filler comprises one of a molecular sieve, activated alumina, hollow activated carbon microspheres; the lamellar filler comprises one of nano montmorillonite, nano kaolin and nano mica powder; the heat-conducting filler is one of boron nitride, magnesium oxide, silicon carbide or silicon micropowder.
7. The polyurethane potting process for a hollow fiber membrane module according to claim 1, wherein the fumed silica is hydrophobic fumed silica having a specific surface area of 200m2/g。
8. The polyurethane potting process for a hollow fiber membrane module according to claim 1, wherein the foam inhibitor is an oxazolidine latent curing agent; the catalyst is selected from one of tertiary amine catalysts or organic metal catalysts; the defoaming agent is an organic silicon defoaming agent.
9. A method for preparing polyurethane pouring sealant used in the polyurethane pouring sealant process for the hollow fiber membrane module according to any one of claims 1 to 8, which is characterized by comprising the following steps:
a. heating the dried polyether polyol to 50-60 ℃, adding metered isocyanate, reacting for 2-3h at 70-80 ℃, and cooling to room temperature to obtain modified polyether polyol;
b. b, uniformly stirring and mixing the aromatic polyol and the modified polyether polyol obtained in the step a, adding fumed silica to disperse uniformly at a high speed, heating to 110-130 ℃, adding other fillers, stirring and dehydrating for 2-3h in vacuum, cooling to 70-90 ℃, adding the foam inhibitor, the catalyst and the defoamer to stir uniformly, and cooling to room temperature to obtain a component B;
c. and (3) mixing and stirring the component A and the component B uniformly at room temperature according to the mass ratio, and defoaming in vacuum for 2-3min to obtain the polyurethane pouring sealant for the hollow fiber membrane module.
10. The method for preparing polyurethane pouring sealant according to claim 9, wherein in the step b, the high-speed dispersion is performed for 30min by using a high-speed dispersion machine at a rotation speed of 4000 r/min; in step c, the mass ratio of the component A to the component B is 1: 1.
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