CN106279049A - One class temperature induced color changing triazole ferrum (II) coordination compound and its preparation method and application - Google Patents
One class temperature induced color changing triazole ferrum (II) coordination compound and its preparation method and application Download PDFInfo
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Abstract
The invention discloses class temperature induced color changing triazole ferrum (II) coordination compound and its preparation method and application, belong to temperature induced color changing coordination compound preparing technical field.Containing 3 in this triazole ferrum (II) coordination compound, 4,5 tri-alkoxy benzene fragment and triazole unit, 3,4,5 tri-alkoxy benzene fragments have the advantages such as environment sensitive to external world, strong model ylid bloom action power, amino triazole has good coordination ability to ferrum (II), and coordination compound temperature induced color changing phenomenon is obvious.The two is constructed the introducing of primitive and is made coordination polymer have extremely abundant assembly behavior and good temperature induced color changing characteristic.Utilize this triazole ferrum (II) coordination compound can prepare temperature induced color changing nano material, and prepared nano-material surface is controlled without other Coated with Organic Matters, pattern and size.The method is significant for preparing of triazole ferrum (II) complex nano material.
Description
Technical field
The invention belongs to the preparing technical field of reversible temperature induced color changing nano material, be specifically related to class temperature induced color changing three nitrogen
Azole ferrum (II) coordination compound and its preparation method and application.
Background technology
At present, owing to temperature induced color changing Spin crossover is in sensing and the potential using value of optoelectronic memory part,
The development of its nano material synthetic technology gets most of the attention.At present, the method being most frequently with is reversed phase micelle technology, but uses and be somebody's turn to do
Nano material prepared by method is often coated with by substantial amounts of surfactant, and is difficult to remove, and causes spin crossover nanometer
The dilution of material and character weak, is difficulty with in nano-yardstick measure spin crossover character.Close compared to reversed phase micelle
One-tenth technology, polymer is easy as the homogeneous phase synthetic method of stabilizer, mild condition, and solvent polarity selects face width, and is not required to
To prepare microemulsion in advance.Additionally, spin crossover nano material prepared by the method shows abundant microscopic appearance.More important
, owing to using Homogeneous synthesis technology, heterogeneous synthetic technology such compared to reverse micelle method, it is more convenient in preparation
During introduce the functional material such as fluorescence molecule.But, the method still cannot be avoided Coated with Organic Matter to spin crossover material
The impact of nature.In sum, seek new synthetic method and obtain without Surface coating, and there is controlled dimensions and pattern
Spin crossover nano material is the vital task of research molecule bi-stable character.
Summary of the invention
It is an object of the invention to provide class temperature induced color changing triazole ferrum (II) coordination compound and preparation method thereof and answer
With, the method is easy and simple to handle, mild condition, it is possible to overcome lacking of Coated with Organic Matter that prior art faces and complex operation
Point, the nano material size of preparation and morphology controllable.
The present invention is to be achieved through the following technical solutions:
The invention discloses class temperature induced color changing triazole ferrum (II) coordination compound, the structural formula of such coordination compound is as follows:
Wherein, m is the positive integer more than or equal to 1；N is the positive integer more than or equal to 1.
The invention also discloses the preparation method of above-mentioned temperature induced color changing triazole ferrum (II) coordination compound, including following step
Rapid:
1) synthesis compound I
Being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, adds wherein
Enter Anhydrous potassium carbonate and potassium iodide, after backflow 2h, add alkyl bromide, at 100～150 DEG C, react 48h, filter, wash, heavily tie
Brilliant, dry, prepare white powdery solids；Put it in the ethanol solution containing potassium hydroxide, be heated to reflux at 80 DEG C 8～
12h, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains compound I；
2) synthesis compound II
Compound I is added in DMF, adds N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride, 4-
Dimethylamino naphthyridine and amino triazole, react mixture to 48h at 40 DEG C, be spin-dried for DMF, wash, be vacuum dried, changed
Compound II；
3) synthesis temperature induced color changing triazole ferrum (II) coordination compound
Compound II is dissolved in chloroform, adds ferrum (II) salt, fully after mixing, centrifugation, washing, very
Empty dry, obtain temperature induced color changing triazole ferrum (II) coordination compound.
Step 1) in, trihydroxybenzoate is 1:(3～20 with the mol ratio of alkyl bromide).
Step 2) in, compound I is 1:(1～10 with the mol ratio of amino triazole).
Step 3) in, described ferrum (II) salt is FeCl2、Fe(BF4)2、Fe(SO3CF3)2Or Fe (NO3)2。
Step 3) in, compound II is 3:(1～5 with the mol ratio of ferrum (II) salt).
The invention also discloses above-mentioned temperature induced color changing triazole ferrum (II) coordination compound of employing and prepare temperature induced color changing nanometer
The method of material, comprises the following steps:
1) synthetic molecules gel
Temperature induced color changing triazole ferrum (II) coordination compound is dissolved in organic solvent, is configured to storing solution, ultrasonic, heating,
Cooling stands after processing, and obtains uniform and stable molecular gel；
2) nano materials
By molecular gel dried, after desolvation, prepare temperature induced color changing nano material.
Described organic solvent is normal hexane, hexamethylene, oxirane, chloroform or dichloromethane.
The concentration of described storing solution is 1 × 10-6～1 × 10-3mol/L；Time of repose is 1～168h.
The invention also discloses the temperature induced color changing nano material using said method to prepare at preparation mutagens color sensing or light
Application in electrical storage device.
Compared with prior art, the present invention has a following useful technique effect:
The invention discloses one and there is temperature induced color changing triazole ferrum (II) coordination compound, this coordination compound introduces amino
Triazole and 3,4,5-tri--alkoxy benzene fragments, 3,4,5-tri--alkoxy benzene fragments have environment sensitive to external world, Qiang Fande
The advantages such as China's active force, amino triazole has good coordination ability to ferrum (II), and coordination compound temperature induced color changing phenomenon is obvious.
The two is constructed the introducing of primitive and is made coordination polymer have extremely abundant assembly behavior and good temperature induced color changing spy
Property.Therefore, this triazole ferrum (II) coordination compound is utilized can to prepare temperature induced color changing nano material, and prepared nano material
Surface is controlled without other Coated with Organic Matters, pattern and size.Therefore, the present invention has researching and developing such temperature induced color changing nano material
Important meaning.
The invention also discloses the synthetic method of above-mentioned temperature induced color changing triazole ferrum (II) coordination compound, the method operation letter
Single, raw material is easy to get, low for equipment requirements, is suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is that the environmental scanning electronic microscope of triazole ferrum (II) coordination compound temperature induced color changing nano material prepared by the present invention shines
Sheet；Wherein, (a) be mass volume ratio be that the coordination compound of 2% is at normal hexane system xerogel photo；B () is the high multiple of a system
Stereoscan photograph (c) be mass volume ratio be that the coordination compound of 2% is at hexamethylene system xerogel photo；D () is the height of b system
Multiple stereoscan photograph.
Fig. 2 is the transmission electron microscope photo of triazole ferrum (II) coordination compound temperature induced color changing nano material prepared by the present invention；
Wherein, (a) be mass volume ratio be 0.1% coordination compound normal hexane system assemble pattern photo；B () is the high power of a system
Number transmission electron microscope photo；(c) be mass volume ratio be 0.1% coordination compound hexamethylene system assemble pattern photo；D () is b
The high multiple transmission electron microscope photo of system.
Fig. 3 is the temperature induced color changing photo of triazole ferrum (II) coordination compound temperature induced color changing nano material prepared by the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, described in be explanation of the invention and
It not to limit.
Present invention temperature induced color changing nano material based on triazole ferrum (II) coordination compound can be prepared by following steps:
1) synthetic compound of formula i
Being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, adds wherein
Enter Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add alkyl bromide, react 48 hours at 100～150 DEG C, mistake
Filter, washing, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the ethanol solution containing potassium hydroxide
In, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtain formula
I.
Wherein trihydroxybenzoate is 1: 3～20 with the mol ratio of alkyl bromide, and its reaction equation is as follows:
2) synthesis Formula II compound
Compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.
Its compounds of formula I is 1: 1～10 with the mol ratio of amino triazole, and its reaction equation is as follows:
3) synthesis formula III coordination compound
Take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in mixed
In even device after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.
Wherein ferrum (II) salt can be: FeCl2、Fe(BF4)2、Fe(SO3CF3)2、Fe(NO3)2Deng, Formula II compound and ferrum
(II) mol ratio of salt is 3: 1～5, and its reaction equation is as follows:
4) molecular gel based on formula III coordination compound is synthesized
Being dissolved in organic solvent by formula III coordination compound, be configured to storing solution, ultrasonic, heating/cooling stands after processing.Put
After putting a period of time, obtain uniform and stable molecular gel.
Wherein Stock concentrations is 1 × 10-6～1 × 10-3Mol/L, standing time is 1 hour～7 days.
5) nano material based on formula III coordination compound is synthesized
The molecular gel dried of the formula III coordination compound that different solvents and variable concentrations are prepared, desolvation
After prepare nano material.
Embodiment 1
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add dodecyl bromide, at 100～150 DEG C, react 48
Hour, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the second containing potassium hydroxide
In alcoholic solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying,
Obtain compound of formula I.Wherein, trihydroxybenzoate is 1: 3 with the mol ratio of alkyl bromide.Wherein, the value of m is 12.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 2 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein ferrum (II) salt is Fe (BF4)2,
Formula II compound is 3: 2 with the mol ratio of ferrum (II) salt.
4) formula III coordination compound is dissolved in normal hexane and hexamethylene respectively, is configured to storing solution, at ultrasonic, heating/cooling
Stand after reason.After placing a period of time, obtain uniform and stable molecular gel.Wherein Stock concentrations is 1 × 10-4Mol/L, puts
The time of putting is 1 day.
5) will be 1 × 10-4The molecular gel of the formula III coordination compound prepared in mol/L normal hexane and hexamethylene system
Dried, prepares nano material after desolvation.
See Fig. 1, sweeping of the temperature induced color changing nano material prepared at normal hexane and hexamethylene system for the present embodiment
Retouch electromicroscopic photograph.Wherein, (a) be mass volume ratio be that the coordination compound of 2% is at normal hexane system xerogel photo；B () is a system
High multiple stereoscan photograph (c) be mass volume ratio be that the coordination compound of 2% is at hexamethylene system xerogel photo；D () is b
The high multiple stereoscan photograph of system.
See Fig. 2, the temperature induced color changing nano material prepared at normal hexane and hexamethylene system for the present embodiment saturating
Penetrate electromicroscopic photograph.Wherein, (a) be mass volume ratio be 0.1% coordination compound normal hexane system assemble pattern photo；B () is a
The high multiple transmission electron microscope photo of system；(c) be mass volume ratio be 0.1% coordination compound hexamethylene system assemble pattern shine
Sheet；D () is the high multiple transmission electron microscope photo of b system.
In conjunction with Fig. 1 and Fig. 2, it can be seen that the method can effectively control the warm mutagens of triazole ferrum (II) coordination compound
The pattern of color nano material and size.
See Fig. 3, for triazole ferrum (II) complex nano material photo at different temperatures in the present embodiment.Can
To find out, along with the change of temperature, the color of sample there occurs that significantly change purple is sample photo at low temperatures, greyish white
Color is sample photo at high temperature.
Embodiment 2
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add methane bromide, at 100～150 DEG C, react 48 little
Time, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the ethanol containing potassium hydroxide
In solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains
To compound of formula I.Wherein, trihydroxybenzoate is 1: 3 with the mol ratio of alkyl bromide.Wherein, the value of m is 1.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 3 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe (BF4)2,
Formula II compound is 3: 1 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Embodiment 3
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add ethane bromide, at 100～150 DEG C, react 48 little
Time, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the ethanol containing potassium hydroxide
In solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains
To compound of formula I.Wherein, trihydroxybenzoate is 1: 4 with the mol ratio of alkyl bromide.Wherein, the value of m is 2.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 4 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe (BF4)2,
Formula II compound is 3: 4 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Embodiment 4
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add propane bromide, at 100～150 DEG C, react 48 little
Time, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the ethanol containing potassium hydroxide
In solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains
To compound of formula I.Wherein, trihydroxybenzoate is 1: 4 with the mol ratio of alkyl bromide.Wherein, the value of m is 3.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 6 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe (BF4)2,
Formula II compound is 3: 1 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Embodiment 5
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add octane bromide, at 100～150 DEG C, react 48 little
Time, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the ethanol containing potassium hydroxide
In solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains
To compound of formula I.Wherein, trihydroxybenzoate is 1: 3 with the mol ratio of alkyl bromide.Wherein, the value of m is 8.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 5 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe (BF4)2,
Formula II compound is 3: 2 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Embodiment 6
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add octane bromide, at 100～150 DEG C, react 48 little
Time, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the ethanol containing potassium hydroxide
In solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains
To compound of formula I.Wherein, trihydroxybenzoate is 1: 3 with the mol ratio of alkyl bromide.Wherein, the value of m is 8.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 4 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe
(CF3SO3)2, Formula II compound is 3: 2 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Embodiment 7
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add dodecyl bromide, at 100～150 DEG C, react 48
Hour, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the second containing potassium hydroxide
In alcoholic solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, is vacuum dried,
Obtain compound of formula I.Wherein, trihydroxybenzoate is 1: 3 with the mol ratio of alkyl bromide.Wherein, the value of m is 12.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 5 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe
(CF3SO3)2, Formula II compound is 3: 1 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Embodiment 8
1) being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, wherein
Add Anhydrous potassium carbonate and a small amount of potassium iodide.After refluxing 2 hours, add dodecyl bromide, at 100～150 DEG C, react 48
Hour, filter, wash, recrystallization, be dried, be prepared as obtaining white powdery solids.Put it into the second containing potassium hydroxide
In alcoholic solution, it is heated to reflux at 80 DEG C 8～12 hours, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, is vacuum dried,
Obtain compound of formula I.Wherein, trihydroxybenzoate is 1: 3 with the mol ratio of alkyl bromide.Wherein, the value of m is 12.
2) compound of formula I is added in DMF, add N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride
(EDA), DMAP (DMAP), amino triazole.Mixture reacts 48 hours at 40 DEG C, is spin-dried for DMF, wash,
Vacuum drying, obtains Formula II compound.Wherein, compound of formula I is 1: 5 with the mol ratio of amino triazole.
3) take a small amount of Formula II compound to be placed in centrifuge tube, add in chloroform and dissolve, add ferrum (II) salt, be placed in
In vortex mixer after mixing, centrifugation, washing, vacuum drying, obtain formula III coordination compound.Wherein, ferrum (II) salt is Fe (NO3)2,
Formula II compound is 3: 1 with the mol ratio of ferrum (II) salt.
Other step is similar to Example 1, prepares triazole ferrum (II) coordination compound temperature induced color changing nano material.
Triazole ferrum (II) coordination compound of 3,4,5-tri--dodecyloxy benzene fragment of synthesis in embodiment 1 is used to enter
Go a large amount of explorative experiment, find its nanometer aggregated structure in different solvents and size adjustable, and prepared nanometer
Material has good temperature induced color changing characteristic.Therefore, the present invention has important meaning to researching and developing such temperature induced color changing nano material
Justice.
Claims (10)
1. class temperature induced color changing triazole ferrum (II) coordination compound, it is characterised in that the structural formula of such coordination compound is as follows:
Wherein, m is the positive integer more than or equal to 1；N is the positive integer more than or equal to 1.
2. the preparation method of temperature induced color changing triazole ferrum (II) coordination compound described in claim 1, it is characterised in that include with
Lower step:
1) synthesis compound I
Being dissolved in DMF by trihydroxybenzoate, temperature is set to 120～160 DEG C, is added thereto to nothing
Aqueous carbonate potassium and potassium iodide, after backflow 2h, add alkyl bromide, reacts 48h at 100～150 DEG C, filter, wash, recrystallization,
It is dried, prepares white powdery solids；Put it in the ethanol solution containing potassium hydroxide, be heated to reflux at 80 DEG C 8～
12h, is cooled to room temperature, sucking filtration, washing, hot ethanol recrystallization, vacuum drying, obtains compound I；
2) synthesis compound II
Compound I is added in DMF, adds N-(3-dimethylamino-propyl)-N '-ethyl-carbodiimide hydrochloride, 4-diformazan
Aminopyridine and amino triazole, react mixture to 48h at 40 DEG C, be spin-dried for DMF, wash, be vacuum dried, obtain compound
II；
3) synthesis temperature induced color changing triazole ferrum (II) coordination compound
Being dissolved in chloroform by compound II, add ferrum (II) salt, fully after mixing, centrifugation, washing, vacuum is done
Dry, obtain temperature induced color changing triazole ferrum (II) coordination compound.
The preparation method of temperature induced color changing triazole ferrum (II) coordination compound the most according to claim 2, it is characterised in that step
Rapid 1) in, trihydroxybenzoate is 1:(3～20 with the mol ratio of alkyl bromide).
The preparation method of temperature induced color changing triazole ferrum (II) coordination compound the most according to claim 2, it is characterised in that step
Rapid 2) in, compound I is 1:(1～10 with the mol ratio of amino triazole).
The preparation method of temperature induced color changing triazole ferrum (II) coordination compound the most according to claim 2, it is characterised in that step
Rapid 3), in, described ferrum (II) salt is FeCl2、Fe(BF4)2、Fe(SO3CF3)2Or Fe (NO3)2。
The preparation method of temperature induced color changing triazole ferrum (II) coordination compound the most according to claim 2, it is characterised in that step
Rapid 3) in, compound II is 3:(1～5 with the mol ratio of ferrum (II) salt).
7. use temperature induced color changing triazole ferrum (II) coordination compound described in claim 1 to prepare the side of temperature induced color changing nano material
Method, it is characterised in that comprise the following steps:
1) synthetic molecules gel
Temperature induced color changing triazole ferrum (II) coordination compound is dissolved in organic solvent, is configured to storing solution, ultrasonic, heat, cool down
Stand after process, obtain uniform and stable molecular gel；
2) nano materials
By molecular gel dried, after desolvation, prepare temperature induced color changing nano material.
The method preparing temperature induced color changing nano material the most according to claim 7, it is characterised in that described organic solvent is
Normal hexane, hexamethylene, oxirane, chloroform or dichloromethane.
The method preparing temperature induced color changing nano material the most according to claim 7, it is characterised in that described storing solution dense
Degree is 1 × 10-6～1 × 10-3mol/L；Time of repose is 1～168h.
10. the temperature induced color changing nano material that in claim 7～9, method described in any one prepares is in preparation mutagens color sensing
Or the application in optical memory.
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