CN107722280A - A kind of preparation method of FePC polymer - Google Patents
A kind of preparation method of FePC polymer Download PDFInfo
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- CN107722280A CN107722280A CN201711033822.XA CN201711033822A CN107722280A CN 107722280 A CN107722280 A CN 107722280A CN 201711033822 A CN201711033822 A CN 201711033822A CN 107722280 A CN107722280 A CN 107722280A
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
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Abstract
The present invention relates to a kind of preparation method of FePC polymer, using FePC as reaction monomers, dimethoxym ethane is external crosslinker, aluminum trichloride (anhydrous) is catalyst, FePC polymer has been prepared using a pair gram alkylated reaction in double oil-based systems, the inventive method is without functional modification process, the synthesis of its polymer is directly realized using FePC as monomer, this method has simple to operate, the characteristics of route is short, it is important that while limited reaction is realized in double oil phase reactions, be advantageous to pay the progress of gram alkylated reaction, such FePC polymeric material is being catalyzed, environment, inhale ripple, there is potential using value in the fields such as the energy.
Description
Technical field
The invention belongs to polymer hybridisation Material Field, is related to a kind of preparation method of FePC polymer.
Background technology
Optical physics chemical property and higher stability of the phthalocyanine due to uniqueness, make it be obtained extensively in dye field
Beyond general application, also received significant attention in fields such as solar cell, sensitising agent, photocatalytic degradation and liquid crystal materials.Phthalocyanine
Molecule cavity is substituted by metallic atom just obtains metal phthalocyanine, because metallic atom species is various, and different valence state be present, therefore
Metal phthalocyanine kind is also very various.
In recent years, the research of phthalocyanine polymer is increasingly becoming the focus of phthalocyanine area research, and this is due to that this kind of material is same
When there is the double grading of phthalocyanine and polymer, the feature of material is enriched, while can overcome the difficult processing of pure phthalocyanine, no
Molten insoluble shortcoming.Phthalocyanine polymer is generally divided into two major classes：Phthalocyanine in the form of chemical bond combine on polymer, phthalein
Phthalocyanine molecule forms polymer in the form of Supramolecular self assembly.At present, the polymerized phthalocyanine on various structures and performance has been reported
Road is a lot, and is applied in fields such as catalysis, the energy, photoconduction, environment, electrochemistry.The preparation method master of phthalocyanine polymer
To include by double bond or can polycondensation base group modification to trigger on Phthalocyanine polymerization (CN200810160563.1,
CN201310252611.0), reacted using the functional group in the functional group and polymer on phthalocyanine derivates molecule
(CN201310516262.9, CN201310138388.7) etc., the above method requires specific reactive functionality, and path is relative
It is longer, therefore, there is simple, the quick method for preparing phthalocyanine polymer to be developed.
The content of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of preparation method of FePC polymer, it is based on
" outer braiding " method in super cross-linked polymer is prepared using pair-gram alkylated reaction, using FePC as reaction monomers, dimethoxym ethane is
External crosslinker, aluminum trichloride (anhydrous) are catalyst, and FePC polymer has been prepared in double oil-based systems.This method is grasped
Work is simple, route is short, and class spherical particles are presented in obtained FePC polymer.Such FePC polymeric material is in catalysis, ring
There is potential using value in the fields such as border, suction ripple, the energy.
Technical scheme
A kind of preparation method of FePC polymer, it is characterised in that step is as follows：
Step 1：FePC is dispersed in solvent I, then adds dimethoxym ethane thereto, obtains solution A；Wherein FePC,
The mass ratio of solvent I and dimethoxym ethane is 1: 4~6: 1~3；The solvent I is 1,2- dichloroethanes, chloroform or the chloroethenes of 1,1- bis-
Alkane；
Step 2：Solution A is added in the there-necked flask for filling silicone oil, after opening 10~30min of stirring, added thereto
Dissolved with the solvent I of aluminum trichloride (anhydrous)；Wherein the volume ratio of solution A and silicone oil is 1: 10~15；Aluminum trichloride (anhydrous) and phthalocyanine
The mass ratio of iron is 1~2: 1, and the mass fraction of catalyst is 2~3%；
Step 3：System is 80~90 DEG C in temperature and is incubated 12~18h of sustained response, after being cooled to room temperature, after suction filtration,
Solid matter after being cleaned using solvent I loads gauze bag, and surname extraction is carried out to it using absolute ethyl alcohol, and extraction 18~
It is vacuum dried to produce FePC polymer after 24h.
The step 3 carries out cleaning 3~5 times using solvent I.
Beneficial effect
A kind of preparation method of FePC polymer proposed by the present invention, using FePC as reaction monomers, dimethoxym ethane is outer
Portion's crosslinking agent, aluminum trichloride (anhydrous) are catalyst, in double oil-based systems using pay-phthalocyanine has been prepared in a gram alkylated reaction
Iron polymer, the inventive method directly realize the synthesis of its polymer without functional modification process using FePC as monomer,
This method has the characteristics of simple to operate, route is short, it is important that while limited reaction is realized in double oil phase reactions, is advantageous to
Pay-the progress of gram alkylated reaction, such FePC polymeric material in catalysis, environment, inhale the fields such as ripple, the energy and have potential answer
With value.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of FePC polymer
Fig. 2 is the SEM photograph of FePC polymer
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1：The preparation of FePC polymer
2g FePCs are weighed, are dispersed in 8g 1, in 2- dichloroethanes, then 4g dimethoxym ethanes is added thereto, obtains molten
Liquid A；Solution A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：10；Stir
After mixing 30min, 1, the 2- dichloroethanes dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is 2g,
1,2- dichloroethanes quality is 98g；System temperature is set as 80 DEG C, is incubated sustained response 18h, after being cooled to room temperature, is filtered
Obtain black-and-blue solid；Obtained black-and-blue solid is subjected to cleaning 3 times with 1,2- dichloroethanes, solid matter is obtained and loads yarn
Cloth bag, surname extraction is carried out to it using absolute ethyl alcohol, it is vacuum dried to produce FePC polymer after extracting 24h.
Embodiment 2：The preparation of FePC polymer
3g FePCs are weighed, are dispersed in 15g chloroforms, then add 6g dimethoxym ethanes thereto, obtain solution A；Will be molten
Liquid A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：15；Stir 10min
Afterwards, the chloroform dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is 5g, and chloroform quality is 162g；
System temperature is set as 90 DEG C, is incubated sustained response 12h, after being cooled to room temperature, suction filtration obtains black-and-blue solid；By what is obtained
Black-and-blue solid carries out cleaning 5 times with chloroform, obtains solid matter and loads gauze bag, carries out Soxhlet to it using absolute ethyl alcohol and carry
Take, it is vacuum dried to produce FePC polymer after extracting 18h.
Embodiment 3：The preparation of FePC polymer
2g FePCs are weighed, are dispersed in 10g 1, in 1- dichloroethanes, then 4g dimethoxym ethanes is added thereto, obtains molten
Liquid A；Solution A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：12；Stir
After mixing 20min, 1, the 1- dichloroethanes dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is 3g,
1,1- dichloroethanes quality is 97g；System temperature is set as 85 DEG C, is incubated sustained response 16h, after being cooled to room temperature, is filtered
Obtain black-and-blue solid；Obtained black-and-blue solid is subjected to cleaning 4 times with 1,1- dichloroethanes, solid matter is obtained and loads yarn
Cloth bag, surname extraction is carried out to it using absolute ethyl alcohol, it is vacuum dried to produce FePC polymer after extracting 20h.
Embodiment 4：The preparation of FePC polymer
4g FePCs are weighed, are dispersed in 16g 1, in 2- dichloroethanes, then 12g dimethoxym ethanes is added thereto, obtains
Solution A；Solution A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：13；
After stirring 15min, 1, the 2- dichloroethanes dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is
6g, 1,2- dichloroethanes quality are 194g；System temperature is set as 80 DEG C, is incubated sustained response 18h, after being cooled to room temperature,
Suction filtration obtains black-and-blue solid；Obtained black-and-blue solid is subjected to cleaning 3 times with 1,2- dichloroethanes, obtains solid matter dress
Enter gauze bag, surname extraction is carried out to it using absolute ethyl alcohol, it is vacuum dried to produce FePC polymer after extracting 24h.
Embodiment 5：The preparation of FePC polymer
2g FePCs are weighed, are dispersed in 12g chloroforms, then add 6g dimethoxym ethanes thereto, obtain solution A；Will be molten
Liquid A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：15；Stir 25min
Afterwards, the chloroform dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is 3g, and chloroform quality is 147g；
System temperature is set as 90 DEG C, is incubated sustained response 12h, after being cooled to room temperature, suction filtration obtains black-and-blue solid；By what is obtained
Black-and-blue solid carries out cleaning 5 times with chloroform, obtains solid matter and loads gauze bag, carries out Soxhlet to it using absolute ethyl alcohol and carry
Take, it is vacuum dried to produce FePC polymer after extracting 18h.
Embodiment 6：The preparation of FePC polymer
3g FePCs are weighed, are dispersed in 15g 1, in 1- dichloroethanes, then 8g dimethoxym ethanes is added thereto, obtains molten
Liquid A；Solution A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：14；Stir
After mixing 12min, 1, the 1- dichloroethanes dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is 5g,
1,1- dichloroethanes quality is 245g；System temperature is set as 85 DEG C, is incubated sustained response 16h, after being cooled to room temperature, is filtered
Obtain black-and-blue solid；Obtained black-and-blue solid is subjected to cleaning 5 times with 1,1- dichloroethanes, solid matter is obtained and loads yarn
Cloth bag, surname extraction is carried out to it using absolute ethyl alcohol, it is vacuum dried to produce FePC polymer after extracting 24h.
Embodiment 7：The preparation of FePC polymer
1g FePCs are weighed, are dispersed in 5g chloroforms, then add 2g dimethoxym ethanes thereto, obtain solution A；By solution
A is added in the there-necked flask for filling silicone oil, opens stirring.Wherein the volume ratio of solution A and silicone oil is 1：15；After stirring 10min,
The chloroform dissolved with aluminum trichloride (anhydrous) is added thereto.Wherein aluminum trichloride (anhydrous) quality is 2g, and chloroform quality is 98g；By body
It is that temperature is set as 88 DEG C, is incubated sustained response 14h, after being cooled to room temperature, suction filtration obtains black-and-blue solid；The blue-black that will be obtained
Color solid carries out cleaning 5 times with chloroform, obtains solid matter and loads gauze bag, surname extraction is carried out to it using absolute ethyl alcohol,
It is vacuum dried to produce FePC polymer after extracting 18h.
Claims (2)
1. a kind of preparation method of FePC polymer, it is characterised in that step is as follows：
Step 1：FePC is dispersed in solvent I, then adds dimethoxym ethane thereto, obtains solution A；Wherein FePC, solvent I
Mass ratio with dimethoxym ethane is 1: 4~6: 1~3；The solvent I is 1,2- dichloroethanes, chloroform or 1,1- dichloroethanes；
Step 2：Solution A is added in the there-necked flask for filling silicone oil, open stirring 10~30min after, add thereto dissolved with
The solvent I of aluminum trichloride (anhydrous)；Wherein the volume ratio of solution A and silicone oil is 1: 10~15；Aluminum trichloride (anhydrous) and FePC
Mass ratio is 1~2: 1, and the mass fraction of catalyst is 2~3%；
Step 3：System is 80~90 DEG C in temperature and is incubated 12~18h of sustained response, after being cooled to room temperature, after suction filtration, is used
Solid matter after solvent I is cleaned loads gauze bag, and surname extraction is carried out to it using absolute ethyl alcohol, extracts 18~24h
Afterwards, it is vacuum dried to produce FePC polymer.
2. the preparation method of FePC polymer according to claim 1, it is characterised in that：The step 3 uses solvent I
Carry out cleaning 3~5 times.
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| CN201711033822.XA CN107722280B (en) | 2017-10-30 | 2017-10-30 | Preparation method of iron phthalocyanine polymer |
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| CN201711033822.XA CN107722280B (en) | 2017-10-30 | 2017-10-30 | Preparation method of iron phthalocyanine polymer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105251535A (en) * | 2015-11-18 | 2016-01-20 | 吉林大学 | Porous organic polymer material and preparation method thereof |
| CN105435754A (en) * | 2015-11-17 | 2016-03-30 | 西北工业大学 | Preparation method for micropore high specific surface magnetic macromolecule composite microsphere |
| WO2017098229A1 (en) * | 2015-12-08 | 2017-06-15 | The University Of Liverpool | Novel porous materials |
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- 2017-10-30 CN CN201711033822.XA patent/CN107722280B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105435754A (en) * | 2015-11-17 | 2016-03-30 | 西北工业大学 | Preparation method for micropore high specific surface magnetic macromolecule composite microsphere |
| CN105251535A (en) * | 2015-11-18 | 2016-01-20 | 吉林大学 | Porous organic polymer material and preparation method thereof |
| WO2017098229A1 (en) * | 2015-12-08 | 2017-06-15 | The University Of Liverpool | Novel porous materials |
Non-Patent Citations (1)
| Title |
|---|
| 陈碧芬: "《应用有机化学》", 30 May 2012, 宁波出版社 * |
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