CN107746455A - Hollow-fibre membrane epoxy curing agent and preparation method thereof - Google Patents
Hollow-fibre membrane epoxy curing agent and preparation method thereof Download PDFInfo
- Publication number
- CN107746455A CN107746455A CN201710822982.6A CN201710822982A CN107746455A CN 107746455 A CN107746455 A CN 107746455A CN 201710822982 A CN201710822982 A CN 201710822982A CN 107746455 A CN107746455 A CN 107746455A
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- Prior art keywords
- curing agent
- hollow
- epoxy curing
- preparation
- fibre membrane
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
- C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
- C08G59/5073—Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5026—Amines cycloaliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
Abstract
The invention discloses hollow-fibre membrane epoxy curing agent, it is by by weight for 6 ~ 8% IPDs, 36 ~ 40% mannich bases, 30 ~ 36% amine terminated polyethers, 2 ~ 3% aminoethyl piperazines, 2 ~ 3% diamines, 12 ~ 16% phenmethylols, 2 ~ 3% salicylic acids and the ethoxy silane of 3 ~ 4% aminopropyl three have formed；It also discloses the preparation method of the curing agent.The beneficial effects of the invention are as follows：Few reaction heating concentration, good penetrability, avoid producing and burn silk, strong shock resistance.
Description
Technical field
The present invention relates to hollow-fibre membrane epoxy curing agent and preparation method thereof.
Background technology
At present, with the continuous development of human society and the continuous propulsion of process of industrialization, all kinds of sanitary sewages and industry
Waste water is largely produced, and serious influence and destruction are caused to the ecological environment that people depend on for existence.Since 19th century, the mankind
Include the miscellaneous purified treatment measures such as biology, physics, chemistry with regard to having carried out.At the beginning of 21 century, with advanced developed country
As successively employed the isolation technics based on various film exemplified by the U.S., Japan, Europe, to domestic water and trade effluent and waste water
Scientific and effective separation and purification have been carried out, has been allowed to obtain the standard of domestic water requirement and industrial wastewater discharge, so as to subtract
Less or pollution of the industrial wastewater to ecological environment is prevented.
Membrane separation technique is most practical, reliable, economical and effective processing method in current water process.It is widely used in life
With fields such as the purification of water, the processing of industrial wastewater, desalinization, medical treatment and pharmacy, food processings.Big flow sewage is general at present
Filtration treatment is carried out using hollow-fibre membrane, hollow-fibre membrane includes more film wires, is distributed with film wire and along its length
Several to be used to handling the micropores of sewage, one end of hollow-fibre membrane gluing is connected to one by blocking.During embedding, first by hollow fibre
One end of dimension film enters in the mould with die cavity, and then end-blocking glue is melted and injected in cavity, each after cooling hollow
One is adhered between tunica fibrosa, it is achieved thereby that the envelope of film wire fills.
At present, end-blocking glue includes following three types：Epoxyn, polyurethane adhesive and acrylate are gluing
Agent, 1, epoxyn the advantages of it is high for adhesion strength, shrinkage factor is low, and stability is good, and electrical insulating property is excellent, processability
It is good, but shock resistance be present and the defects of peel strength is relatively low, and fragility is bigger than normal.2nd, it is adhesion strength the advantages of polyurethane adhesive
Still, lower temperature resistance is excellent, and pliability is good, and manufacturability is excellent, but heat resistance, poor water resistance be present, to film wire adhesion strength
The defects of relatively low.3rd, it is low temperature the advantages of acrylate adhesive, normal temperature cure is fast, to strictly by bonding surface processing
Ask, but it is big quick solidifying thermal discharge to be present, working life short easy implode, causes serious burning silk phenomenon, is not suitable for the viscous of large area
Knot and embedding.In addition the glue penetration of end-blocking more than is poor, after being injected into cavity, can not flow, lead to not completely into cavity
It is interior.
The content of the invention
The shortcomings that it is an object of the invention to overcome prior art, there is provided reduce reaction heating concentration, good penetrability, avoid
Produce hollow-fibre membrane epoxy curing agent for burning silk, strong shock resistance and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions：Hollow-fibre membrane epoxy curing agent, it is by by weight
Amount is than being 6~8% IPDs, 36~40% mannich bases, 30~36% amine terminated polyethers, 2~3% aminoethyl piperazines
Diamines, 12~16% phenmethylols, 2~3% salicylic acids and the ethoxy silane of 3~4% aminopropyl three form for piperazine, 2~3%.
The preparation method of described hollow-fibre membrane epoxy curing agent, it comprises the following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by 10~15g mixed liquors that diamines and 60~80g phenmethylols form, start stirring
Device, mixeding liquid temperature is risen to 44~45 DEG C using heating water bath；
30~40g IPDs, 180~200g mannich bases, 120~180g ends ammonia are sequentially added after S3, heating
Base polyethers, 10~15g aminoethyl piperazines, 10g salicylic acids, the ethoxy silane of 15~20g aminopropyls three, after addition stir 15~
16min, then mixed liquor is slowly warming up to 70 DEG C；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that in
The preparation of empty fiber membrane epoxy curing agent, the amine value of curing agent are 310~315mgKOH/g, viscosity is 70~
100mpa.s。
Before mixed liquor is added into reaction bulb in described step S1, first by 10~15g, diamines adds in water-bath
Heat fusing, then weigh 60~80g phenmethylols and add in water-bath, finally stir until transparent uniform liquid.
The present invention has advantages below：(1) present invention use addition different proportion aminoethyl piperazine and diamines with must
To the purpose of control reaction heating, heat release during envelope filling is avoided to concentrate, it is difficult to from controlling temperature.(2) present invention is using addition phenmethylol
Method make product viscosity less than normal, reduce infiltration, avoid being difficult to flow.(3) present invention using addition different proportion Manny this
Alkali and IPD to react gently in solidification process, and caloric value is low, avoids and burns silk phenomenon.(4) present invention uses
The method for adding amine terminated polyether solves the problem of product solidification brittleness is big, and poor toughness is easy to crack, shock resistance difference.
Embodiment
The present invention will be further described below, and protection scope of the present invention is not limited to as described below：
Embodiment one：Hollow-fibre membrane epoxy curing agent, it is by being 6~8% IPDs, 36 by weight
~40% mannich base, 30~36% amine terminated polyethers, 2~3% aminoethyl piperazines, 2~3% diamines, 12~16% benzene first
Alcohol, 2~3% salicylic acids and the ethoxy silane of 3~4% aminopropyl three composition.
The preparation method of described hollow-fibre membrane epoxy curing agent, it comprises the following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by the 15g mixed liquors that diamines and 60g phenmethylols form, start agitator, using water
Mixeding liquid temperature is risen to 45 DEG C by bath heating；
30g IPDs, 200g mannich bases, 160g amine terminated polyethers, 10g ammonia second are sequentially added after S3, heating
Base piperazine, 10g salicylic acids, the ethoxy silane of 15g aminopropyls three, stirs 15min, then mixed liquor slowly is warming up into 70 after addition
℃；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that in
The preparation of empty fiber membrane epoxy curing agent, the amine value of curing agent is 310mgKOH/g, viscosity 80mpa.s.
Before mixed liquor is added into reaction bulb in described step S1, first by 10~15g, diamines adds in water-bath
Heat fusing, then weigh 60~80g phenmethylols and add in water-bath, finally stir until transparent uniform liquid.
The present invention uses the aminoethyl piperazine of addition different proportion and diamines to obtain the purpose of control reaction heating, is kept away
Exempt from heat release when envelope fills to concentrate, it is difficult to control temperature.The present invention makes product viscosity less than normal using the method for addition phenmethylol, and reduction is oozed
Thoroughly, avoid being difficult to flow.The present invention is caused in solidification process using the mannich base and IPD of addition different proportion
Reaction is gentle, and caloric value is low, avoids and burns silk phenomenon.The present invention is crisp using the method solution product solidification of addition amine terminated polyether
Big, the poor toughness of property, it is easy to crack, the problem of shock resistance difference.
Embodiment two：The preparation method of described hollow-fibre membrane epoxy curing agent, it comprises the following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by the 10g mixed liquors that diamines and 60g phenmethylols form, start agitator, using water
Mixeding liquid temperature is risen to 44~45 DEG C by bath heating；
40g IPDs, 200g mannich bases, 150g amine terminated polyethers, 15g ammonia second are sequentially added after S3, heating
Base piperazine, 10g salicylic acids, the ethoxy silane of 15g aminopropyls three, 15~16min is stirred after addition, then be slowly warming up to mixed liquor
70℃；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that in
The preparation of empty fiber membrane epoxy curing agent, the amine value of curing agent is 311mgKOH/g, viscosity 100mpa.s.
Embodiment three：The preparation method of described hollow-fibre membrane epoxy curing agent, it comprises the following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by the 10g mixed liquors that diamines and 60g phenmethylols form, start agitator, using water
Mixeding liquid temperature is risen to 44~45 DEG C by bath heating；
30g IPDs, 180g mannich bases, 180g amine terminated polyethers, 15g ammonia second are sequentially added after S3, heating
Base piperazine, 10g salicylic acids, the ethoxy silane of 15g aminopropyls three, stirs 16min, then mixed liquor slowly is warming up into 70 after addition
℃；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that in
The preparation of empty fiber membrane epoxy curing agent, the amine value of curing agent is 315mgKOH/g, viscosity 70mpa.s.
Example IV：The preparation method of described hollow-fibre membrane epoxy curing agent, it comprises the following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by the 10g mixed liquors that diamines and 60g phenmethylols form, start agitator, using water
Mixeding liquid temperature is risen to 45 DEG C by bath heating；
30g IPDs, 180g mannich bases, 180g amine terminated polyethers, 15g ammonia second are sequentially added after S3, heating
Base piperazine, 10g salicylic acids, the ethoxy silane of 15g aminopropyls three, 15~16min is stirred after addition, then be slowly warming up to mixed liquor
70℃；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that in
The preparation of empty fiber membrane epoxy curing agent, the amine value of curing agent is 315mgKOH/g, viscosity 70mpa.s.
Embodiment five：The preparation method of described hollow-fibre membrane epoxy curing agent, it comprises the following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by the 15g mixed liquors that diamines and 60g phenmethylols form, start agitator, using water
Mixeding liquid temperature is risen to 45 DEG C by bath heating；
30g IPDs, 180g mannich bases, 170g amine terminated polyethers, 10g ammonia second are sequentially added after S3, heating
Base piperazine, 10g salicylic acids, the ethoxy silane of 15g aminopropyls three, stirs 15min, then mixed liquor slowly is warming up into 70 after addition
℃；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that in
The preparation of empty fiber membrane epoxy curing agent, the amine value of curing agent is 314mgKOH/g, viscosity 80mpa.s.
Take 100 parts and 35 parts this curing agent of epoxy resin and carry out envelope filling, experimental data such as following table：
Described above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form, the exclusion to other embodiment is not to be taken as, and can be used for various other combinations, modification and environment, and can be at this
In the text contemplated scope, it is modified by the technology or knowledge of above-mentioned teaching or association area.And those skilled in the art are entered
Capable change and change does not depart from the spirit and scope of the present invention, then all should be in the protection domain of appended claims of the present invention
It is interior.
Claims (3)
1. hollow-fibre membrane epoxy curing agent, it is characterised in that：It by by weight for 6 ~ 8% IPDs, 36 ~
40% mannich base, 30 ~ 36% amine terminated polyethers, 2 ~ 3% aminoethyl piperazines, 2 ~ 3% diamines, 12 ~ 16% phenmethylols, 2 ~ 3% bigcatkin willows
Acid and the ethoxy silane of 3 ~ 4% aminopropyl three composition.
2. the preparation method of hollow-fibre membrane epoxy curing agent according to claim 1, it is characterised in that：It includes
Following steps：
S1, tetra- mouthfuls of reaction bulbs of 1000ml are taken, agitator, condenser and thermometer are installed in four mouthfuls of reaction bulbs；
S2, added into reaction bulb by 10 ~ 15g mixed liquors that diamines and 60 ~ 80g phenmethylols form, start agitator, used
Mixeding liquid temperature is risen to 44 ~ 45 DEG C by heating water bath；
S3, heating after sequentially add 30 ~ 40g IPDs, 180 ~ 200g mannich bases, 120 ~ 180g amine terminated polyethers,
10 ~ 15g aminoethyl piperazines, 10g salicylic acids, the ethoxy silane of 15 ~ 20g aminopropyls three, 15 ~ 16min is stirred after addition, then slowly
Mixed liquor is warming up to 70 DEG C；
S4,70 DEG C of lasting 1h are kept, be then cooled to 40 DEG C of dischargings, obtain rufous translucent liquid, it is achieved thereby that hollow fibre
The preparation of film epoxy curing agent is tieed up, the amine value of curing agent is 310 ~ 315mgKOH/g, and viscosity is 70 ~ 100mpa.s.
3. the preparation method of hollow-fibre membrane epoxy curing agent according to claim 1, it is characterised in that：Described
Before mixed liquor is added into reaction bulb in step S1, first by 10 ~ 15g, diamines heats fusing in water-bath, then weighs
60 ~ 80g phenmethylols are simultaneously added in water-bath, are finally stirred until transparent uniform liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710822982.6A CN107746455A (en) | 2017-09-13 | 2017-09-13 | Hollow-fibre membrane epoxy curing agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710822982.6A CN107746455A (en) | 2017-09-13 | 2017-09-13 | Hollow-fibre membrane epoxy curing agent and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107746455A true CN107746455A (en) | 2018-03-02 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710822982.6A Pending CN107746455A (en) | 2017-09-13 | 2017-09-13 | Hollow-fibre membrane epoxy curing agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864966A (en) * | 2018-06-21 | 2018-11-23 | 四川中建华兴科技有限公司 | A kind of novel reinforced type carbon cloth glue and its preparation process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1764692A (en) * | 2003-05-05 | 2006-04-26 | Sika技术股份公司 | Epoxy resin compositions containing mannich bases, suitable for high-temperature applications |
-
2017
- 2017-09-13 CN CN201710822982.6A patent/CN107746455A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1764692A (en) * | 2003-05-05 | 2006-04-26 | Sika技术股份公司 | Epoxy resin compositions containing mannich bases, suitable for high-temperature applications |
Non-Patent Citations (1)
| Title |
|---|
| 王静: "中空纤维膜分离器封头胶粘剂的研制", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864966A (en) * | 2018-06-21 | 2018-11-23 | 四川中建华兴科技有限公司 | A kind of novel reinforced type carbon cloth glue and its preparation process |
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Application publication date: 20180302 |