CN1030374C - Fabrication of epoxy sealing head for fibrous membrane separator - Google Patents
Fabrication of epoxy sealing head for fibrous membrane separator Download PDFInfo
- Publication number
- CN1030374C CN1030374C CN 91106006 CN91106006A CN1030374C CN 1030374 C CN1030374 C CN 1030374C CN 91106006 CN91106006 CN 91106006 CN 91106006 A CN91106006 A CN 91106006A CN 1030374 C CN1030374 C CN 1030374C
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- China
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- epoxy
- sealing head
- epoxy resin
- agent
- temperature
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Abstract
The present invention relates to a method for preparing an epoxy sealing head of a fibrous membrane separator. An epoxy resin adhesive is prepared according to certain proportioning, and then a program temperature rising or gradient temperature rising type solidifying technology is adopted after a sealing head is cast. The sealing end or an epoxy resin tube plate of a separator, which is prepared by the present invention, has the advantages of high mechanical and compressive strength, wide range of usage temperature, etc., and the separator composed of the sealing head or the epoxy resin tube plate can fully exert the penetration of a membrane, and has the advantages of separation performance and wide practical value in industries.
Description
The present invention relates to a kind of preparation method of building block epoxy sealing head and Resins, epoxy tube sheet of hollow fiber membrane separator.Exactly provide a kind of tubular fibre N
2-H
2The preparation method of membrane separation apparatus epoxy sealing head.
Tubular fibre N
2-H
2Membrane separation apparatus is the new technology that late nineteen seventies is succeeded in developing, and this technology has separation efficiency height, low, simple to operate, the no driving arrangement of energy expenditure and overhauls advantages such as convenient.Successfully be applied to from gas and synthetic ammonia purge, reclaim H
2, CO/H
2The accent ratio, H in the petroleum chemical plant waste gas
2Recovery, CO in the oil field gas
2Recovery, and from air, produce rich N
2In commercial run.Tubular fibre N
2-H
2Membrane separation apparatus is hollow-fibre membrane to be made fibrous bundle be contained in the withstand voltage steel shell, be similar to tubular heat exchanger, fibrous bundle is made up of to tens thousand of composite hollow fiber membranes thousands of, and an end is shut, and it is one of vitals of separator that the other end forms the Resins, epoxy tube sheet.It is hollow-fibre membrane one end with no several high dispersive to be bonded and sealed at separator one end with epoxy resin binder be epoxy sealing head, and the other end sticks into the Resins, epoxy tube sheet with epoxy resin binder, as the card of interchanger.High pressure feed and low-pressure permeability air bound are opened, thus the effect that performance seals and bears pressure.Therefore, an epoxy sealing head and a Resins, epoxy tube sheet rational in infrastructure, that performance is good will play crucial effect to the performance of hollow fiber membrane separator.For achieving the above object, when the Resins, epoxy end socket of preparation separator or Resins, epoxy tube sheet, the selection and the casting process of epoxy resin binder all there is harsh requirement.The epoxy resin binder of the usefulness of promptly casting will have good flowability, the hollow-fibre membrane of polymolecularity is distributed equably, and can not produce bubble and hole, in order to avoid influence intensity and stopping property.Epoxy resin binder must be able to make the hollow-fibre membrane surface fully soak into before curing simultaneously, good cohesiveness is arranged after the curing, do not produce and peel off phenomenon, also should avoid the epoxy resin binder corrosive component to destroy the hollow-fibre membrane surface, enter the inner chamber of hollow-fibre membrane, and the obstruction hollow-fibre membrane, the result reduces the useful area of film.Though the tubular fibre N of success is abroad arranged at present
2-H
2The membrane separation apparatus operation of putting into production, but the report of relevant separator epoxy sealing head or Resins, epoxy tube sheet technology of preparing is still rarely known by the people.
Purpose of the present invention provides a kind of preparation tubular fibre N
2-H
2The method of membrane separation apparatus epoxy sealing head and Resins, epoxy tube sheet promptly provides the technology (prescription) of an assembly system epoxy resin binder and utilizes the processing method of this tackiness agent casting epoxy sealing head and Resins, epoxy tube sheet.
The epoxy resin binder that the present invention selects, it mainly comprises Resins, epoxy, solidifying agent, linking agent, toughner, thinner and weighting agent, it is characterized in that pressing weight percent and is mixed and made into: Resins, epoxy: 30～80%; Solidifying agent: 5～50%; Linking agent: 1～5%; Toughner: 5～20%; Thinner: 1-10%; Filler 0～300%(is by prescription total amount ratio); In addition, also can be added with a small amount of activator in the binder ingredients, its content (weight) is 0～1%.Resins, epoxy can be selected bisphenol-type epoxy resin for use in the above-mentioned component, and is two-2,3-epoxy group(ing) cyclopentyl ether, 4,5-epoxy cyclohexane and 1,2-dioctyl phthalate 2-glycidyl fat, titanium dioxide dicyclo the eleventh of the twelve Earthly Branches base ether or above-mentioned epoxy derivative; Solidifying agent can be selected the aliphatic amide class for use, as: quadrol, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, hexanediamine, m-xylene diamine; The modified fat amine, as: beta-hydroxy quadrol, diethyl triamine and butylglycidyl ether, β-cyanoethylation diethylenetriamine; Aromatic amine: as mphenylenediamine, 4,4 '-diaminodiphenylmethane, 4,4 '-dioxy base sulfobenzide a, amino-benzylamine; Acid anhydride type curing agent, as Tetra hydro Phthalic anhydride and radical derivative or imidazoles and derivative thereof, as: imidazoles, methylimidazole, 2-ethyl 4-methylimidazole, glyoxal ethyline and butylglycidyl ether, second first imidazoles and iso-octyl glycidyl ether; Linking agent can be selected silicone based coupling agent for use; Toughner can be selected poly-inkstone, poly-sulphur, poly-phenol, epoxy resins, polyester etc. for use; Thinner can be selected glycerine, benzene, dimethylbenzene, turps, acetone, dibutyl phthalate, dioctyl phthalate (DOP) for use; Filler can be selected the fine powder of asbestos, carbon black, graphite, silicon-dioxide, glass fibre, metal oxide or metal (copper, aluminium, iron) for use.Can select SnCl for use as adding activator in the tackiness agent
22H
2O, FeCl
36H
2O, ZnCl
215H
2O or SrCl
26H
2O etc.After the various components of above-mentioned tackiness agent take by weighing mixing in proportion, stir, add again when filled as needs and can be used as tackiness agent after the certain proportion filler is mixed and use.
Utilize the tackiness agent of above-mentioned preparation can the cast epoxy sealing head or the Resins, epoxy tube sheet of separator, should to initial solidification value, carry out in room temperature (25 ℃) in tackiness agent preparation and the casting operation, the casting operation does not have the special technique requirement, but the hot setting operation after the casting should be carried out under temperature programming or gradient increased temperature mode, and keeps certain set time.It is to be raised to continuously under 80～150 ℃ of the solidification values with 0.5～2 ℃ of/hour heat-up rate to be cured that so-called temperature programming formula is solidified, and is no less than 20 hours set time; It is to be cured to be no less than in two temperature sections that so-called gradient increased temperature mode is solidified, in the end solidification value is cured the time and is no less than 10 hours, other heats up to solidify in the section and is no less than 2 hours, optional 10～30 ℃ of temperature gradients of gradient increased temperature scope carry out intensifications at different levels and solidify, for example: 20～50 ℃ of initial temperature sections, back sections such as 70～90 ℃, 100～120 ℃, 130～150 ℃, but final solidification value should not be higher than 150 ℃, can select in 80～150 ℃ of scopes, i.e. gradient increased temperature formula curing is carried out for general optional 2～5 sections.Below by example technology of the present invention is further described.
Example 1～4 tubular fibre N
2-H
2The preparation of separator epoxy sealing head.
1, epoxy resin binder is pressed the weight percent preparation: bisphenol A type epoxy resin (commodity 616# Resins, epoxy, Wuxi resin processing plant): 75%; Acid anhydride type curing agent (commodity NF-841, Jin Dong chemical plant, Tianjin): 8%; Silicone based linking agent (commodity KH-550, chemical plant, Gai County, Yingkou): 1%; Toughner polysulfones 10%, polyester 5%; Thinner acetone: 1%.Tackiness agent casting back adopts three sections gradient increased temperature formulas to solidify: 50 ℃, and 30 hours; 75 ℃, 30 hours; Final 95 ℃, 10 hours, make end socket 1.
2, epoxy resin binder is pressed the weight percent preparation: titanium dioxide dicyclo amyl ether (commodity 400# Resins, epoxy, Jin Dong chemical plant, Tianjin): 55%; 2-ethyl 4 Methylimidazoles: 33%; Silicone based linking agent (commodity KH560, Shanghai jump magnificent glasswork) 1%; Toughner gathers sulphur 5%, polyester 5%; Thinner dimethylbenzene 1%; Activator ZnCl
215H
2O 0.70%.Tackiness agent casting back adopts two sections gradient increased temperature formulas to solidify; 40 ℃ of initial temperature sections, 48 hours; Eventually 110 ℃ of temperature sections are 20 hours, make end socket 2.
3, to press heavily be per-cent preparation to epoxy resin binder: 4, and 5-oxyethane and 1,2-dioctyl phthalate 2-glycidyl fat (commodity TDE-85, Jin Dong chemical plant, Tianjin) 50%; Acid anhydride type curing agent (commodity 308# acid anhydrides, Xinhua Resin Factory, Shanghai) 39%, silicone based linking agent (commodity KH570, Tianjin reagent one factory) 1%, toughner polysulfones 5%, polyester 5%; Thinner glycerine 1%, filler iron powder 200%.
Adopt the temperature programming formula to solidify after tackiness agent is cast and rise to 120 ℃ of curing 20 hours, get end socket 3 by 30 ℃ of initial temperature with 1 ℃/speed at one hour rating.
4, epoxy resin binder is pressed weight percent preparation: two-2, and 3-epoxy group(ing) cyclopentyl ether (commodity W-95 Resins, epoxy, Jin Dong chemical plant, Tianjin) 40%, solidifying agent second diene triamine 47%; Silicone based linking agent (commodity KH550, chemical plant, Gai County, Yingkou) 2%; Toughner polysulfones 5%, polyester 5%; Thinner glycerine 1%.
Tackiness agent casting back adopts 5 sections gradient increased temperature formulas to solidify, with 40 ℃ 4 hours, 60 ℃ 10 hours, 75 ℃ 10 hours, 85 ℃ 12 hours, 120 ℃ of terminal sections 12 hours make end socket 4.
Example 5, adhesive therefor and separator epoxy sealing head performance
Utilize the tackiness agent that example 1～4 provides and the end socket of preparation to carry out performance test, test event is undertaken by the respective country standard, its result such as table 1, table 2.
Table 1, binder performance
Tackiness agent elastic strength shearing resistance ultimate compression strength thermal change intensity
（70℃）MPa （25℃）MPa （25℃）MPa ℃
Example 1 60 18.2 96.9 92
Example 2 70 18.0 110 95
Example 3 140 12.0 158 132
Example 4 80 17.0 142 115
Table 2 separator end socket performance
Separator end socket epoxy sealing head specification heat resisting and pressure resisting
（φCm） ℃ MPa
End socket 1 2.5 55 8.0
End socket 2 10 55 8.0
End socket 3 10 70 12.0
End socket 4 2.5～20 60 11.0
By above-mentioned example, utilize the tubular fibre N of technology preparation provided by the invention
2-H
2The epoxy sealing head of membrane separation apparatus (can prepare the Resins, epoxy tube sheet equally), have machinery and compressive strength height, advantages such as use temperature wide ranges, the separator that adopts this technology to be assembled into can be given full play to infiltration, the separation performance of film, has the wide industrial actual application value.
Claims (2)
1, a kind of tubular fibre N
2-H
2The preparation method of membrane separation apparatus epoxy sealing head, it is to adopt epoxy resin binder, tackiness agent casting back to adopt high temperature curing process, it is formulated to it is characterized in that tackiness agent is pressed column weight amount per-cent:
Resins, epoxy: 30～80%; Solidifying agent: 5～50%; Linking agent: 1～5%; Toughner: 5～20%; Thinner: 1～10%; Filler 0～300% (by prescription total amount ratio); Curing process adopts temperature programming or gradient increased temperature mode to carry out, and it is to be raised to continuously under 80～150 ℃ of the solidification values with 0.5～2 ℃ of/hour heat-up rate to be cured that so-called temperature programming formula is solidified; And the curing of gradient increased temperature formula is to be cured in two temperature sections to be no less than, and final solidification value should not be higher than 150 ℃, can be 80～150 ℃ of selections.
2, according to the described preparation method of claim 1, it is characterized in that also can being added with a small amount of promoting agent in the epoxy resin binder, its content is≤1%, promoting agent can be selected SnCl for use
22H
2O, FeCl
26H
2O, ZnCl
215H
2O or SrCl
26H
2O.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106006 CN1030374C (en) | 1991-01-09 | 1991-01-09 | Fabrication of epoxy sealing head for fibrous membrane separator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106006 CN1030374C (en) | 1991-01-09 | 1991-01-09 | Fabrication of epoxy sealing head for fibrous membrane separator |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1063054A CN1063054A (en) | 1992-07-29 |
| CN1030374C true CN1030374C (en) | 1995-11-29 |
Family
ID=4907445
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91106006 Expired - Lifetime CN1030374C (en) | 1991-01-09 | 1991-01-09 | Fabrication of epoxy sealing head for fibrous membrane separator |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1030374C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327941C (en) * | 2005-06-28 | 2007-07-25 | 谷宗岳 | Capsulation pouring method of hollow fibrous membrane element and pouring arrangement thereof |
| CN102352212B (en) * | 2011-09-06 | 2013-08-21 | 蚌埠市立群电子有限公司 | High-strength metal adhesive and preparation method thereof |
| CN102329591A (en) * | 2011-09-06 | 2012-01-25 | 蚌埠市立群电子有限公司 | Metal binder and preparation method thereof |
| CN102500238A (en) * | 2011-12-19 | 2012-06-20 | 天邦膜技术国家工程研究中心有限责任公司 | Device and method for casting end socket of hollow fiber membrane assembly |
| CN104476486B (en) * | 2014-11-14 | 2016-03-09 | 天邦膜技术国家工程研究中心有限责任公司 | Certain films assembly epoxy sealing head assembling technique |
| US11478753B2 (en) | 2016-06-29 | 2022-10-25 | Dic Corporation | Hollow fiber membrane module and production method therefor, and epoxy resin used in hollow fiber membrane and production method |
-
1991
- 1991-01-09 CN CN 91106006 patent/CN1030374C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1063054A (en) | 1992-07-29 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
| OR01 | Other related matters | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20090220 Address after: Liaoning province Dalian City High-tech Park Qixianling Torch Road No. 28 Patentee after: Tianbang National Engineering Research Center of Membrane Technology, Co., Ltd. Address before: No. 161, Zhongshan Road, Liaoning, Dalian Patentee before: Dalian Institute of Chemical Physics, Chinese Academy of Sciences |
|
| ASS | Succession or assignment of patent right |
Owner name: TIANBANG MEMBRANE TECHNOLOGY COUNTRY ENGINEERING R Free format text: FORMER OWNER: DALIAN INST OF CHEMICOPHYSICS, CHINESE ACADEMY OF SCIENCES Effective date: 20090220 |
|
| C17 | Cessation of patent right | ||
| CX01 | Expiry of patent term |
Expiration termination date: 20110109 Granted publication date: 19951129 |