CN106432720A - Method for preparing polypyrrole doped molybdate - Google Patents
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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Abstract
The invention relates to a method for preparing polypyrrole doped molybdate, which comprises the following steps: 1) using an inert electrode as an anode, an inert electrode as a cathode, mixed aqueous solution containing sodium molybdate and pyrrole as an anolyte, acid solution, alkaline solution or salt solution as the catholyte, in the double-chamber electrolyzer with cationic membrane as diaphragm, controlling the temperature from the room temperature to 90 DEG C, and using constant-current electrolysis or constant-voltage electrolysis to electrolyze; 2) after electrolysis, drying the solution obtained in the anode chamber at 80 DEG C to 120 DEG C; filtering and cleaning the resulting powder and drying at 80 DEG C to 120 DEG C and then cooling to room temperature to obtain a sample of polypyrrole doped molybdate. The prepared polypyrrole doped molybdate sample is pure, free of impurities, and evenly distributed, and the follow-up treatment is simple, the investment is small and the synthesis amount is large, which solves the problems of product heterogeneity, low stability, high cost, complex operation, and others in the process of preparing polypyrrole doped molybdate.
Description
[technical field]
The invention belongs to chemical field, specifically a kind of method preparing doped polypyrrole molybdate.
[background technology]
In inorganic material, molybdate is a critically important class salt, and molybdate has optical property and the electrochemistry of uniqueness
Can, have in fields such as sensor, scintillation material, magnetic material, fiber optic materials, microwave, catalyst and widely should
With.
In recent years, researchers to the research of conducting polymer more extensively and profoundly, because it has special optics, electricity
The physicochemical properties such as, mechanics and magnetics, are increasingly used as solaode, sensor, photoelectric material, super capacitor, memory
The important composition material of material, driver and artificial muscle.And there is the conducting polymer of nanostructured and its composite more
Have the characteristic of conducting polymer and nano material concurrently, in catalysis, sensing, medical and health, magnetic material, optical material, microelectronics
There is the potential application of giant in field.Wherein, polypyrrole have the advantages that environmental stability good, doping after electric conductivity high, because
This polypyrrole nano material by the advantage with reference to organic conductor and nanostructured, molecular wire, chemical sensor or driver,
The aspects such as gas separation membrane have potential application.
But because polypyrrole not readily dissolves under normal conditions and melts, processing characteristics is very poor, which has limited answering of it
With.
[content of the invention]
Present invention aim to solving above-mentioned deficiency and providing a kind of method preparing doped polypyrrole molybdate,
Solve traditional method preparation doped polypyrrole molybdate during product is uneven, stability is low, high cost, complex operation
Etc. technical problem.
Design a kind of method preparing doped polypyrrole molybdate for achieving the above object, comprise the following steps：
1) using inert electrode as anode, with inert electrode as negative electrode, with containing sodium molybdate and the scattered mixing water of pyrroles
Solution is anolyte, with acid solution, aqueous slkali or saline solution as catholyte, in cationic membrane in the two-compartment cell of barrier film,
Control temperature for room temperature to 90 DEG C, be electrolysed by the way of constant-current electrolysis or constant-potential electrolysis；In described anolyte, described
The scattered mixed aqueous solution of pyrroles adds, for pyrroles, the solution obtaining after ultrasonic disperse 1-4h after sodium molybdate aqueous solution；Described acid is molten
Liquid is the aqueous hydrochloric acid solution of 0.001-1mol/L for concentration or concentration is the aqueous sulfuric acid of 0.001-1mol/L, described aqueous slkali
It is the sodium hydrate aqueous solution for 0.001-1mol/L for the concentration or concentration is the potassium hydroxide aqueous solution of 0.001-1mol/L, described
Saline solution is the sodium-chloride water solution of 0.001-1mol/L for concentration or concentration is the aqueous sodium carbonate of 0.001-1mol/L；Institute
The electric current stating constant-current electrolysis is 0.08-0.8A, and electric current density is 1-100mA/cm2；Voltage range 10- of described constant-potential electrolysis
300V；
2), after being electrolysed, the solution that anode chamber is obtained is dried at 80-120 DEG C, after gained powder cleans in filtration
Dry at 80-120 DEG C, then naturally cool to room temperature, that is, obtain the sample of doped polypyrrole molybdate.
Further, described inert electrode is glass-carbon electrode, graphite electrode, Ti electrode or platinum electrode, step 2) gained product
Thing is the sample of polypyrrole.
Further, described molybdic acid na concn is 0.001-1mol/L, and the scattered mixed aqueous solution concentration of described pyrroles is
1-100g/L.
Further, described cationic membrane is perfluorinated sulfonic acid cation exchange membrane.
Present invention also offers a kind of method preparing doped polypyrrole molybdate, comprise the following steps：
1) using anode soluble metal as anode, with inert electrode as negative electrode, with scattered with pyrroles containing sodium molybdate
Mixed aqueous solution is anolyte, with acid solution, aqueous slkali or saline solution as catholyte, is electrolysed for the dual chamber of barrier film in cationic membrane
In groove, control temperature for room temperature to 90 DEG C, be electrolysed by the way of constant-current electrolysis or constant-potential electrolysis；In described anolyte
In, the scattered mixed aqueous solution of described pyrroles is the solution obtaining after ultrasonic disperse 1-4h after pyrroles adds sodium molybdate aqueous solution；
Described acid solution is the aqueous hydrochloric acid solution of 0.001-1mol/L for concentration or concentration is the aqueous sulfuric acid of 0.001-1mol/L, institute
State that aqueous slkali is the sodium hydrate aqueous solution of 0.001-1mol/L for concentration or concentration is the potassium hydroxide water of 0.001-1mol/L
Solution, described saline solution is the sodium-chloride water solution of 0.001-1mol/L for concentration or concentration is the sodium carbonate of 0.001-1mol/L
Aqueous solution；The electric current of described constant-current electrolysis is 0.08-0.8A, and electric current density is 1-100mA/cm2；The voltage of described constant-potential electrolysis
Scope 10-300V；
2), after being electrolysed, the solution that anode chamber is obtained is dried at 80-120 DEG C, after gained powder cleans in filtration
Dry at 80-120 DEG C, then naturally cool to room temperature, that is, obtain doped polypyrrole molybdate.
Further, described metal be Cu, Fe, Ni or Zn anode soluble metal, step 2) products therefrom be polypyrrole
Doping copper molybdate, the sample of doped polypyrrole iron molybdate, doped polypyrrole nickel molybdate or doped polypyrrole zinc molybdate.
Further, described molybdic acid na concn is 0.001-1mol/L, and the scattered mixed aqueous solution concentration of described pyrroles is
1-100g/L.
Further, described cationic membrane is perfluorinated sulfonic acid cation exchange membrane.
Further, described metal is Fe or Ni anode soluble metal, and described anolyte is the molybdenum containing depolarizing agent
Sour sodium and the scattered mixed aqueous solution of pyrroles, the concentration of described depolarizing agent is the 1/10 of sodium molybdate aqueous solution concentration.
Further, described depolarizing agent be soluble chloride, citrate, any one or two kinds of in tartrate
Above mixture, described soluble chloride is ammonium chloride or sodium chloride, and described citrate is sodium citrate, ammonium citrate
Or ammonium hydrogen citrate, described tartrate is sodium tartrate, sodium bitartrate, ammonium tartrate or L-tartaric acid monoammonium salt.
The present invention compared with the existing technology, can be prepared in the short time before polypyrrole and molybdic acid salt dopping by a step
Drive body, and the method for the present invention has that molybdate and polypyrrole ratio are controlled, reaction condition temperature, reaction temperature are low and operation is simple
Single, stability is high, and the doped polypyrrole molybdate sample preparing is pure, free from admixture, the advantages of be evenly distributed, and follow-up locate
Reason is simple, and investment is little, and synthetic quantity is big；Additionally, the catholyte scope used by the present invention is wide, acid solution, alkali liquor and saline solution are all permissible, and
And the mode of electrolytic process either constant-current electrolysis or constant-potential electrolysis, the pure doped polypyrrole molybdic acid being evenly distributed can be obtained
Salt product.
[brief description]
Fig. 1 is the SEM comparison diagram of embodiment of the present invention iron molybdate and doped polypyrrole iron molybdate；
Fig. 2 is the IR comparison diagram of embodiment of the present invention iron molybdate and doped polypyrrole iron molybdate.
[specific embodiment]
The invention provides a kind of method preparing doped polypyrrole molybdate, comprise the steps：1) with inert electrode
Or anode soluble metal is as anode, with inert electrode as negative electrode, with containing sodium molybdate and the scattered mixed aqueous solution of pyrroles
For anolyte, with acid solution, aqueous slkali or saline solution as catholyte, in cationic membrane for, in the two-compartment cell of barrier film, controlling
Temperature, is electrolysed by the way of constant-current electrolysis or constant-potential electrolysis to 90 DEG C for room temperature；Molybdic acid na concn is 0.001-1mol/
L；The scattered concentration of aqueous solution of pyrroles is 1-100g/L；Acid solution is the aqueous hydrochloric acid solution of 0.001-1mol/L or concentration for concentration
Aqueous sulfuric acid for 0.001-1mol/L；Aqueous slkali is the sodium hydrate aqueous solution of 0.001-1mol/L for concentration or concentration is
The potassium hydroxide aqueous solution of 0.001-1mol/L；Saline solution is the sodium-chloride water solution of 0.001-1mol/L for concentration or concentration is
The aqueous sodium carbonate of 0.001-1mol/L；Cationic membrane is perfluorinated sulfonic acid cation exchange membrane；The electric current of constant-current electrolysis is
0.08-0.8A, electric current density is 1-100mA/cm2；Voltage range 10-300V of constant-potential electrolysis；When anode adopts inert electrode
When, inert electrode is glass-carbon electrode, graphite electrode, Ti electrode (as titanium net) or platinum electrode；When anode adopts anode solubility gold
During genus, metal is Cu, Fe, Ni or Zn anode soluble metal；In anolyte, the scattered aqueous solution of pyrroles adds for pyrroles
The solution obtaining after ultrasonic disperse 1-4h after entering sodium molybdate aqueous solution.2), after being electrolysed, the solution that anode chamber is obtained is in 80-
Dry at 120 DEG C, gained powder is dried after cleaning in filtration at 80-120 DEG C, then naturally cools to room temperature and is gathered
The sample of pyrroles's doping molybdate.
Wherein, cationic membrane is Nafion perfluorinated sulfonic acid 212 type cation exchange membrane.When anode is inert electrode, step
2) products therefrom is the sample of polypyrrole.When anode is Cu, Fe, Ni or Zn anode soluble metal, step 2) products therefrom is
Doped polypyrrole copper molybdate, the sample of doped polypyrrole iron molybdate, doped polypyrrole nickel molybdate or doped polypyrrole zinc molybdate.When
When anode is Fe or Ni anode soluble metal, anolyte is the sodium molybdate containing depolarizing agent and the scattered mixing of pyrroles is water-soluble
Liquid, the concentration of depolarizing agent is the 1/10 of sodium molybdate aqueous solution concentration, and depolarizing agent is soluble chloride, citrate, wine
The mixture of any one or more in stone hydrochlorate, soluble chloride is ammonium chloride or sodium chloride, and citrate is lemon
Lemon acid sodium, ammonium citrate or ammonium hydrogen citrate, tartrate is sodium tartrate, sodium bitartrate, ammonium tartrate or hydrogen tartrate
Ammonium.
The present invention has certain selective penetrated property, particularly Nafion system due to the cationic membrane adopting in preparation process
Row perfluorinated sulfonic acid cation exchange membrane can allow the Na in anode chamber+Ion permeable ionic membrane enters cathode chamber, thus eliminating
Na+The impact to final products doped polypyrrole molybdate product for the ionic impurity, and can be by dense to sodium molybdate in anolyte
Degree and the regulation of pyrrole concentrations and the replacing of anode species, obtain the metal molybdate of dissimilar different proportion and polypyrrole
Alloy.The preparation method of the therefore present invention has the doped polypyrrole molybdate product of final gained, has no dephasign, distribution
Uniformly, molybdate and polypyrrole ratio are controlled, the selectable feature of molybdate composition.
Combine accompanying drawing below by specific embodiment the present invention is expanded on further, but be not intended to limit the present invention.
Perfluorinated sulfonic acid cation exchange membrane used in embodiments of the invention is the Nafion that du pont company produces
Perfluorinated sulfonic acid 212 type cation exchange membrane.
Embodiment
(1) using anode soluble metal Fe as anode, with inert electrode as negative electrode, with the 90ml molybdenum containing depolarizing agent
Sour sodium and the scattered mixed aqueous solution of pyrroles are anolyte, in cationic membrane in the two-compartment cell of barrier film, using Constant Electric Current
The mode of solution, controls temperature range to be that room temperature carries out being electrolysed the aqueous solution 20min of sodium molybdate to 50 DEG C, described inert electrode is titanium
Net；Affiliated depolarizing agent is the sodium chloride of 0.01mol/L；The concentration of described sodium molybdate aqueous solution is 0.1mol/L；Affiliated pyrroles
Dispersion liquid concentration is 5.4g/L；Described acid solution is the aqueous hydrochloric acid solution of 0.1mol/L for concentration；Described cationic membrane is perfluor
Sulfonic acid cation exchange membrane；The electric current of described constant-current electrolysis is 0.6A, and electric current density is 85.7mA/cm2；
(2), after being electrolysed, the solution that anode chamber is obtained is dried at 100 DEG C, gained powder clean in filtration after
Dry at 100 DEG C, then naturally cool to the sample that room temperature obtains doped polypyrrole iron molybdate.
The SEM figure of contrast iron molybdate and doped polypyrrole iron molybdate, SEM result such as Fig. 1 it can be seen that pyrroles there occurs bright
Aobvious polymerization, the spherical polymer of formation is also very uniform.
The IR spectrogram of contrast iron molybdate and doped polypyrrole iron molybdate, IR result such as Fig. 2 is it can be seen that doped polypyrrole
The sample of iron molybdate has obvious polypyrrole peak.
In sum, the preparation method of a kind of doped polypyrrole molybdate of the present invention, can get pure, be evenly distributed
Doped polypyrrole molybdate material.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention and principle
Lower made change, modification, replacement, combination, simplification, all should be equivalent substitute mode, are included in the protection model of the present invention
Within enclosing.
Claims (10)
1. a kind of method preparing doped polypyrrole molybdate is it is characterised in that comprise the following steps：
1) using inert electrode as anode, with inert electrode as negative electrode, with containing sodium molybdate and the scattered mixed aqueous solution of pyrroles
For anolyte, with acid solution, aqueous slkali or saline solution as catholyte, in cationic membrane for, in the two-compartment cell of barrier film, controlling
Temperature, is electrolysed by the way of constant-current electrolysis or constant-potential electrolysis to 90 DEG C for room temperature；
In described anolyte, the scattered mixed aqueous solution of described pyrroles is that pyrroles adds ultrasonic disperse 1- after sodium molybdate aqueous solution
The solution obtaining after 4h；
Described acid solution is the aqueous hydrochloric acid solution of 0.001-1mol/L for concentration or sulphuric acid that concentration is 0.001-1mol/L is water-soluble
Liquid, described aqueous slkali is the sodium hydrate aqueous solution of 0.001-1mol/L for concentration or concentration is the hydroxide of 0.001-1mol/L
Aqueous solutions of potassium, described saline solution is the sodium-chloride water solution of 0.001-1mol/L for concentration or concentration is the carbon of 0.001-1mol/L
Acid sodium aqueous solution；
The electric current of described constant-current electrolysis is 0.08-0.8A, and electric current density is 1-100mA/cm2；The voltage range of described constant-potential electrolysis
10-300V；
2), after being electrolysed, the solution that anode chamber is obtained is dried at 80-120 DEG C, gained powder clean in filtration after in 80-
Dry at 120 DEG C, then naturally cool to room temperature, that is, obtain the sample of doped polypyrrole molybdate.
2. the method for claim 1 it is characterised in that：Described inert electrode is glass-carbon electrode, graphite electrode, Ti electrode
Or platinum electrode, step 2) products therefrom be polypyrrole sample.
3. the method for claim 1 it is characterised in that：Described molybdic acid na concn is 0.001-1mol/L, described pyrroles
Scattered mixed aqueous solution concentration is 1-100g/L.
4. the method for claim 1 it is characterised in that：Described cationic membrane is perfluorinated sulfonic acid cation exchange membrane.
5. a kind of method preparing doped polypyrrole molybdate is it is characterised in that comprise the following steps：
1) using anode soluble metal as anode, with inert electrode as negative electrode, to mix containing sodium molybdate is scattered with pyrroles
Aqueous solution be anolyte, with acid solution, aqueous slkali or saline solution as catholyte, cationic membrane for barrier film two-compartment cell
In, control temperature for room temperature to 90 DEG C, be electrolysed by the way of constant-current electrolysis or constant-potential electrolysis；
In described anolyte, the scattered mixed aqueous solution of described pyrroles is that pyrroles adds ultrasonic disperse 1- after sodium molybdate aqueous solution
The solution obtaining after 4h；
Described acid solution is the aqueous hydrochloric acid solution of 0.001-1mol/L for concentration or sulphuric acid that concentration is 0.001-1mol/L is water-soluble
Liquid, described aqueous slkali is the sodium hydrate aqueous solution of 0.001-1mol/L for concentration or concentration is the hydroxide of 0.001-1mol/L
Aqueous solutions of potassium, described saline solution is the sodium-chloride water solution of 0.001-1mol/L for concentration or concentration is the carbon of 0.001-1mol/L
Acid sodium aqueous solution；
The electric current of described constant-current electrolysis is 0.08-0.8A, and electric current density is 1-100mA/cm2；The voltage range of described constant-potential electrolysis
10-300V；
2), after being electrolysed, the solution that anode chamber is obtained is dried at 80-120 DEG C, gained powder clean in filtration after in 80-
Dry at 120 DEG C, then naturally cool to room temperature, that is, obtain doped polypyrrole molybdate.
6. method as claimed in claim 5 it is characterised in that：Described metal is Cu, Fe, Ni or Zn anode soluble metal,
Step 2) products therefrom is doped polypyrrole copper molybdate, doped polypyrrole iron molybdate, doped polypyrrole nickel molybdate or polypyrrole are mixed
The sample of miscellaneous zinc molybdate.
7. method as claimed in claim 5 it is characterised in that：Described molybdic acid na concn is 0.001-1mol/L, described pyrroles
Scattered mixed aqueous solution concentration is 1-100g/L.
8. method as claimed in claim 5 it is characterised in that：Described cationic membrane is perfluorinated sulfonic acid cation exchange membrane.
9. method as claimed in claim 5 it is characterised in that：Described metal is Fe or Ni anode soluble metal, described sun
Pole liquid is the sodium molybdate containing depolarizing agent and the scattered mixed aqueous solution of pyrroles, and the concentration of described depolarizing agent is sodium molybdate water
The 1/10 of solution concentration.
10. method as claimed in claim 9 it is characterised in that：Described depolarizing agent be soluble chloride, citrate,
The mixture of any one or more in tartrate, described soluble chloride is ammonium chloride or sodium chloride, described lemon
Lemon hydrochlorate is sodium citrate, ammonium citrate or ammonium hydrogen citrate, and described tartrate is sodium tartrate, sodium bitartrate, winestone
Sour ammonium or L-tartaric acid monoammonium salt.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106928434A (en) * | 2017-03-07 | 2017-07-07 | 常州大学 | A kind of method and its application by the tartrate ion synthesis of chiral conducting polymer that adulterates |
| CN107189429A (en) * | 2017-07-20 | 2017-09-22 | 北京化工大学 | A kind of molybdenum base polyacid/polyaniline/graphene oxide trielement composite material and its production and use |
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| CN104357875A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing iron molybdate by using cationic membrane electrolysis process |
| CN105001759A (en) * | 2015-07-21 | 2015-10-28 | 中国科学院金属研究所 | Molybdate doped polypyrrole/epoxy resin self-healing coating, preparation method thereof and application thereof |
| CN105331981A (en) * | 2015-09-29 | 2016-02-17 | 安徽工业大学 | Composite metal surface treatment agent based on conducting polymer |
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| CN104357875A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing iron molybdate by using cationic membrane electrolysis process |
| CN105001759A (en) * | 2015-07-21 | 2015-10-28 | 中国科学院金属研究所 | Molybdate doped polypyrrole/epoxy resin self-healing coating, preparation method thereof and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928434A (en) * | 2017-03-07 | 2017-07-07 | 常州大学 | A kind of method and its application by the tartrate ion synthesis of chiral conducting polymer that adulterates |
| CN107189429A (en) * | 2017-07-20 | 2017-09-22 | 北京化工大学 | A kind of molybdenum base polyacid/polyaniline/graphene oxide trielement composite material and its production and use |
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