CN106543960A - FeCl3‑The preparation method of Schiff's base composite - Google Patents

FeCl3‑The preparation method of Schiff's base composite Download PDF

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Publication number
CN106543960A
CN106543960A CN201611012774.1A CN201611012774A CN106543960A CN 106543960 A CN106543960 A CN 106543960A CN 201611012774 A CN201611012774 A CN 201611012774A CN 106543960 A CN106543960 A CN 106543960A
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CN
China
Prior art keywords
schiff
fecl
phenylenediamine
glutaraldehyde
base
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CN201611012774.1A
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李长英
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Shaanxi Yipinda Petrochemical Co Ltd
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Shaanxi Yipinda Petrochemical Co Ltd
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Priority to CN201611012774.1A priority Critical patent/CN106543960A/en
Publication of CN106543960A publication Critical patent/CN106543960A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
    • C07C249/02—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of compounds containing imino groups
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The present invention discloses a kind of FeCl3The preparation method of Schiff's base composite, comprises the steps of：P-phenylenediamine is dissolved in into ethanol solution, add the ethanol solution of glutaraldehyde again by constant pressure burette, 4 h of isothermal reaction at 60 DEG C, add tripolycyanamide, the precipitation of generation is carried out into decompression sucking filtration, and absolute ethanol washing is used, it is finally vacuum dried to obtain contracting glutaraldehyde p-phenylenediamine Schiff's base；In FeCl3Ethanol solution in add contracting glutaraldehyde p-phenylenediamine Schiff's base, the dehydrated alcohol for obtaining, stirring reaction 4h at 80 DEG C is by the precipitation decompression sucking filtration for generating, with absolute ethanol washing, last vacuum dried to obtain FeCl3Schiff's base composite.The method is simple to operate, the FeCl of preparation3Schiff's base composite has good electric conductivity and wave-absorbing effect.

Description

FeCl3-The preparation method of Schiff's base composite
Technical field
The invention belongs to meet the preparation field of material, and in particular to a kind of FeCl3The preparation side of-Schiff's base composite Method.
Background technology
At present, electromagenetic wave radiation produced during a large amount of electronic product uses has become dirty after atmospheric pollution, water The another pollution problem of facing mankind after dye, sound pollution.To protect the physical and mental health of the mankind, countries in the world are all actively being sent out Exhibition microwave defense material.Schiff's base is a kind of imine derivative, is by containing active carbonyl compound and the compound containing amino And its derivant is generated in the basic conditions.Due to containing-C=N- keys in Schiff's base, orphan's electricity of N atoms on its hybrid orbital Son is to introducing various functions group, therefore which is had in the field such as catalysis, pharmacy, photochromic, analytical chemistry, stealth material And be widely applied.
There are good electric conductivity and absorbing property after Schiff's base is doped, and its electrical conductivity is adjustable, become new in recent years The study hotspot of type absorbing material.Schiff basess conduction is to lose its lonely electricity as electron donor by the use of the N atoms of-C=N- groups Son, supplies the material of doping, so as to reach the conductive purpose for inhaling ripple.But, existing regulation by chemical method obtains suction ripple The wave-absorbing effect of material is not good.
The content of the invention
The present invention provides a kind of FeCl3The preparation method of-Schiff's base composite, the conductivity of composite material of preparation is good, Absorbing property is good.
The present invention is achieved by the following technical solutions.
FeCl3The preparation method of-Schiff's base composite, comprises the steps of：
（1）The synthesis of contracting glutaraldehyde p-phenylenediamine Schiff's base：P-phenylenediamine is dissolved in dehydrated alcohol, p-phenylenediamine is obtained Ethanol solution, then the ethanol solution of glutaraldehyde is added by constant pressure burette, it is anti-in 60 DEG C of thermostat water bath Answer 4 h, add tripolycyanamide, the precipitation of generation is carried out into decompression sucking filtration, and with absolute ethanol washing 2-3 time, most after Jing it is true Empty drying to obtain contracting glutaraldehyde p-phenylenediamine Schiff's base, wherein, p-phenylenediamine, glutaraldehyde, the mol ratio of tripolycyanamide are 5： 5：1；
（2）FeCl3The preparation of-Schiff's base composite：Weigh FeCl3It is dissolved in dehydrated alcohol, obtains FeCl3Anhydrous second Alcoholic solution, adds step（1）The contracting glutaraldehyde p-phenylenediamine Schiff's base for obtaining, the matter that contracting glutaraldehyde p-phenylenediamine Schiff's base is added Amount and FeCl3Ethanol solution volume ratio be 1.76:20, then added by constant pressure funnel and FeCl3Dehydrated alcohol it is molten The dehydrated alcohol of liquid phase same volume, stirring reaction 4h at 80 DEG C, by the precipitation decompression sucking filtration for generating, with absolute ethanol washing 3 Time, it is finally vacuum dried to obtain FeCl3- Schiff's base composite.
Preferably, above-mentioned steps（1）In, the concentration of the ethanol solution of p-phenylenediamine is 2.19g/mL, glutaraldehyde The concentration of ethanol solution is 0.001mol/mL.
Preferably, above-mentioned steps（2）In, FeCl3Ethanol solution concentration be 0.002 mol/mL.
Preferably, in methods described, vacuum drying temperature is 80 DEG C.
Advantages of the present invention is：
The present invention provides a kind of FeCl3The preparation method of-Schiff's base composite, the FeCl of preparation3- Schiff's base composite has There are good electric conductivity and wave-absorbing effect.
Specific embodiment
Embodiment 1
1. FeCl3The preparation method of-Schiff's base composite, comprises the steps of：
（1）The synthesis of contracting glutaraldehyde p-phenylenediamine Schiff's base：P-phenylenediamine is dissolved in dehydrated alcohol, p-phenylenediamine is obtained Ethanol solution, then the ethanol solution of glutaraldehyde is added by constant pressure burette, it is anti-in 60 DEG C of thermostat water bath Answer 4 h, add tripolycyanamide, the precipitation of generation is carried out into decompression sucking filtration, and with absolute ethanol washing 2-3 time, most after Jing it is true It is empty to be dried（80℃）Obtain contracting glutaraldehyde p-phenylenediamine Schiff's base, wherein, p-phenylenediamine, glutaraldehyde, tripolycyanamide mole Than for 5：5：1；
（2）FeCl3The preparation of-Schiff's base composite：Weigh FeCl3It is dissolved in dehydrated alcohol, obtains FeCl3Anhydrous second Alcoholic solution, adds step（1）The contracting glutaraldehyde p-phenylenediamine Schiff's base for obtaining, the matter that contracting glutaraldehyde p-phenylenediamine Schiff's base is added Amount and FeCl3Ethanol solution volume ratio be 1.76:20, then added by constant pressure funnel and FeCl3Dehydrated alcohol it is molten The dehydrated alcohol of liquid phase same volume, stirring reaction 4h at 80 DEG C, by the precipitation decompression sucking filtration for generating, with absolute ethanol washing 3 Time, it is last vacuum dried（80℃）FeCl is obtained3- Schiff's base composite.
Above-mentioned steps（1）In, the concentration of the ethanol solution of p-phenylenediamine is 2.19g/mL, the dehydrated alcohol of glutaraldehyde The concentration of solution is 0.001mol/mL.
Above-mentioned steps（2）In, FeCl3Ethanol solution concentration be 0.002 mol/mL.

Claims (4)

1.FeCl3The preparation method of-Schiff's base composite, it is characterised in that：Comprise the steps of：
（1）The synthesis of contracting glutaraldehyde p-phenylenediamine Schiff's base：P-phenylenediamine is dissolved in dehydrated alcohol, p-phenylenediamine is obtained Ethanol solution, then the ethanol solution of glutaraldehyde is added by constant pressure burette, it is anti-in 60 DEG C of thermostat water bath Answer 4 h, add tripolycyanamide, the precipitation of generation is carried out into decompression sucking filtration, and with absolute ethanol washing 2-3 time, most after Jing it is true Empty drying to obtain contracting glutaraldehyde p-phenylenediamine Schiff's base, wherein, p-phenylenediamine, glutaraldehyde, the mol ratio of tripolycyanamide are 5： 5：1；
（2）FeCl3The preparation of-Schiff's base composite：Weigh FeCl3It is dissolved in dehydrated alcohol, obtains FeCl3Anhydrous second Alcoholic solution, adds step（1）The contracting glutaraldehyde p-phenylenediamine Schiff's base for obtaining, the matter that contracting glutaraldehyde p-phenylenediamine Schiff's base is added Amount and FeCl3Ethanol solution volume ratio be 1.76:20, then added by constant pressure funnel and FeCl3Dehydrated alcohol it is molten The dehydrated alcohol of liquid phase same volume, stirring reaction 4h at 80 DEG C, by the precipitation decompression sucking filtration for generating, with absolute ethanol washing 3 Time, it is finally vacuum dried to obtain FeCl3- Schiff's base composite.
2. FeCl according to claim 13The preparation method of-Schiff's base composite, it is characterised in that：Step（1）In, The concentration of the ethanol solution of p-phenylenediamine is 2.19g/mL, and the concentration of the ethanol solution of glutaraldehyde is 0.001mol/ mL。
3. FeCl according to claim 13The preparation method of-Schiff's base composite, it is characterised in that：Step（2）In, FeCl3Ethanol solution concentration be 0.002 mol/mL.
4. FeCl according to claim 13The preparation method of-Schiff's base composite, it is characterised in that：It is vacuum drying Temperature is 80 DEG C.
CN201611012774.1A 2016-11-17 2016-11-17 FeCl3‑The preparation method of Schiff's base composite Pending CN106543960A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107043370A (en) * 2017-04-27 2017-08-15 桂林理工大学 The schiff bases iron complex absorbing material and preparation method of a kind of methylene aldehyde structure containing pyrroles 2
CN109369936A (en) * 2018-09-21 2019-02-22 河南工程学院 A kind of preparation method of porous wave absorbing thin film that wanting raw material based on block type Schiff alkali salt
CN111659357A (en) * 2019-03-06 2020-09-15 中南大学 Polymeric Schiff base type adsorption material, preparation and application thereof in heavy metal adsorption

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107043370A (en) * 2017-04-27 2017-08-15 桂林理工大学 The schiff bases iron complex absorbing material and preparation method of a kind of methylene aldehyde structure containing pyrroles 2
CN107043370B (en) * 2017-04-27 2019-10-11 桂林理工大学 A kind of the schiff bases iron complex absorbing material and preparation method of the methylene of -2- containing pyrroles aldehyde structure
CN109369936A (en) * 2018-09-21 2019-02-22 河南工程学院 A kind of preparation method of porous wave absorbing thin film that wanting raw material based on block type Schiff alkali salt
CN109369936B (en) * 2018-09-21 2021-06-08 河南工程学院 Preparation method of porous wave-absorbing film with block type Schiff base salt as main raw material
CN111659357A (en) * 2019-03-06 2020-09-15 中南大学 Polymeric Schiff base type adsorption material, preparation and application thereof in heavy metal adsorption
CN111659357B (en) * 2019-03-06 2021-08-24 中南大学 Polymeric Schiff base type adsorption material, preparation and application thereof in heavy metal adsorption

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