CN104140641B - A kind of composite with photochromic properties and preparation method thereof - Google Patents
A kind of composite with photochromic properties and preparation method thereof Download PDFInfo
- Publication number
- CN104140641B CN104140641B CN201410384293.8A CN201410384293A CN104140641B CN 104140641 B CN104140641 B CN 104140641B CN 201410384293 A CN201410384293 A CN 201410384293A CN 104140641 B CN104140641 B CN 104140641B
- Authority
- CN
- China
- Prior art keywords
- photochromic properties
- parts
- composite
- molybdenum compound
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
A kind of composite with photochromic properties and preparation method thereof, it relates to a kind of photochromic functional composite and preparation method thereof.The invention aims to solve existing preparation and have the complex process of composite of photochromic properties, cost height, the prepared composite quality with photochromic properties is unstable, photochromic properties is insensitive and applied environment requires high problem.A kind of composite with photochromic properties is prepared from by having the molybdenum compound of photochromic properties, solvent, firming agent and resin matrix by weight.Preparation method: one, preparation has the molybdenum compound of photochromic properties；Two, weigh；Three, preparation has the molybdenum compound/solvent mixture of photochromic properties；Four, preparation has the mixture of photochromic properties；Five, firming agent is added；Six, solidification, molding, obtain the composite with photochromic properties.The present invention can obtain a kind of composite with photochromic properties.
Description
Technical field
The present invention relates to a kind of photochromic functional composite and preparation method thereof.
Background technology
Can there is the change of color in one class material, this kind of material is referred to as photochromic material after being subject to light source activation.Because having photochromic performance characteristics, photochromic material has occupied consequence in the research and application of functional material.Simple photochromic material is broadly divided into inorganic photochromic material and the big class of organic photochromic material two.Along with going deep into of research, the novel composite with photochromic properties also becomes research emphasis.Have the composite of photochromic properties generally by photochromic material as additive, polymer or ceramic material as matrix.Inorganic photochromic material is because having optical, electrical, the magnetic property of excellence, and high heat stability, the advantage such as fatigue resistance becomes a class additive important in photochromic functional composite.
Inorganic photochromic material mainly has following a few class: transition metal oxide, rare earth compounding, oxometallate, metal azide etc..Wherein, there is the transistion metal compound of photochromic properties because its good photosensitivity, environmental stability, optical contrast and reversible coloring, become the photochromic material having application potential most.Mo, as the Typical Representative in transistion metal compound, has good performance and application potential in photochromic, electrochromism, photic catalysis, electroluminescent catalysis.The compound of molybdenum has photochromic feature and is primarily due to the Mo (V) of pentavalent and can generate the molybdenum bronze of blueness.At present, preparation has the method for photochromic molybdenum compound and is concentrated mainly on and utilizes molybdenum salt chemistry reaction synthesis method or adopt physical vapour deposition (PVD) or chemical precipitation method at substrate deposit molybdenum oxide.Chemical reactive synthesis method complex process, and sometimes raw material poisonous or generate by-product；Substrate deposition molybdenum oxide equipment is complicated, cost is high, and deposition quality is also unstable.Therefore, the compound exploring the molybdenum that technique preparation simple, with low cost, free of contamination has photochromic properties becomes research emphasis.
The composite prepared by inorganic photochromic material and polymeric matrix has photochromic performance of excellence.Because the environmental suitability that polymeric matrix is excellent and stability, make the existence that the photochromic properties of such composite can be stable in complex environment.It addition, polymeric material has high light transmittance, inorganic photochromic is dispersed in and wherein can receive more energy of light source, makes the photochromic sensitivity with excellence of this composite.Polymeric matrix also has the manufacturability of excellence, it is possible to according to the different difform composites of mould molding to meet the different demands of various environment；Meanwhile, polymeric matrix is also used as coating and is coated on different base surface so that it is have photochromic performance, significantly expands application and the scope of this kind of composite.The Mo with photochromic properties has the good compatibility with polymeric material, and the composite that both compound preparations have photochromic properties will be had the performance of excellence and huge application potential.
Summary of the invention
The invention aims to solve existing preparation and there is the complex process of composite of photochromic properties, cost height, the prepared composite quality with photochromic properties is unstable, photochromic properties is insensitive and applied environment requires high problem, and provides a kind of composite with photochromic properties and preparation method thereof.
A kind of composite with photochromic properties is had the molybdenum compound of photochromic properties, 10 parts～35 parts solvents, 6 parts～20 parts firming agent and 50 parts～150 parts resin matrixes by 0.02 part～1.5 parts by weight and is prepared from.
The preparation method of a kind of composite with photochromic properties, is specifically realized by the following steps:
One, preparation has the molybdenum compound of photochromic properties: 1., ethanol or acetone is mixed with distilled water, prepares mixed solution；
Step 1. described in mixed solution in the volume fraction of ethanol or acetone be 25%～75%；
2., by the MoS of natural hexagonal structure2Powder mixes with mixed solution, obtains containing MoS2Mixed liquor；
Step 2. described in the MoS of natural hexagonal structure2The quality of powder and the volume ratio of mixed solution are (25mg～180mg): 1mL；
3., adopt high speed shear emulsification instrument to containing MoS2Mixed liquor carry out high speed shear process, obtain the mixed liquor after shear treatment；
Step 3. described in high speed shear to process be shear 45min～150min with the speed of 8000r/min～19000r/min；
4., the mixed liquor after shear treatment is carried out water bath sonicator process, the mixed liquor after being disperseed；
Step 4. described in the power of supersound process be 200W～240W, ultrasonic time is 45min～90min；
5., the mixed liquor after dispersion is stood 6h～8h, take the supernatant, obtain the molybdenum compound suspension with photochromic properties；
6., be dry 4h～10h at 60 DEG C～80 DEG C by there is the molybdenum compound suspension of photochromic properties in temperature, obtain the molybdenum compound with photochromic properties；
Two, weigh: weigh 0.02 part～1.5 parts by weight and there are the molybdenum compound of photochromic properties, 10 parts～35 parts solvents, 6 parts～20 parts firming agent and 50 parts～150 parts resin matrixes；
Three, preparation has the molybdenum compound/solvent mixture of photochromic properties: is dissolved in 10 parts～35 parts solvents by weigh 0.02 part～1.5 parts molybdenum compounds with photochromic properties, obtains the molybdenum compound/solvent mixture with photochromic properties；Being ultrasonic disperse 15min～30min under 150W～200W by there is the molybdenum compound/solvent mixture of photochromic properties at ultrasonic power, obtaining the molybdenum compound/solvent mixture with photochromic properties after ultrasonic disperse；
Four, preparation has the mixture of photochromic properties: in the molybdenum compound/solvent mixture with photochromic properties after weigh 50 parts～150 parts resin matrixes are joined the ultrasonic disperse that step 3 obtains, low whipping speed is stirring 10min～30min under 200r/min～400r/min, it is ultrasonic disperse 1h～2h under 150W～240W at ultrasonic power again, obtains the mixture with photochromic properties；
Five, firming agent is added: join in the mixture with photochromic properties that step 4 obtains by weigh 6 parts～20 parts firming agent, low whipping speed is for stirring 10min～20min under 100r/min～200r/min again, obtains the mixture with photochromic properties to be solidified；
Six, solidification, molding: the mixture cast molding with photochromic properties to be solidified that step 5 is obtained, more at room temperature place 8h～12h, obtain the composite with photochromic properties.
Advantages of the present invention:
One, the composite with photochromic properties that prepared by the present invention, the raw material of use is simple and easy to get, with low cost, and environmental pollution is little；
The technological process of the composite with photochromic properties that two, prepared by the present invention is simple, operates easy, and device therefor is this area conventional instrument, and process cycle is short, and the requirement of process environments is relatively low；
Three, the steady quality of the composite with photochromic properties, the photochromic properties that prepared by the present invention are obvious, and reversibility is better；Meanwhile, the environmental stability of this composite is good, has good photochromic properties in various environment；
The composite range of application of what four, prepared by the present invention have photochromic properties is very wide, information can be prepared either directly or as coating and store material, decoration protective material, detection radiative material etc., in information, electronics, Non-Destructive Testing, Aero-Space, the field such as military suffers from being widely applied potentiality.
Five, the composite with photochromic properties that prepared by the present invention is after ultra-vioket radiation 1h, at the absorbance of wavelength 710nm for will improve 50%～160%, it was shown that it has the photochromic sensitivity of excellence；After ultra-vioket radiation 16h, at the absorbance of wavelength 710nm for 200%～500% will be improved, it was shown that it has the photochromic properties of excellence.
The present invention can obtain a kind of composite with photochromic properties.
Accompanying drawing explanation
The composite with photochromic properties that Fig. 1 is test one preparation is the change curve with the irradiation under ultraviolet ray time of absorbance during 710nm at wavelength.
Detailed description of the invention
Detailed description of the invention one: present embodiment is that a kind of composite with photochromic properties is had the molybdenum compound of photochromic properties, 10 parts～35 parts solvents, 6 parts～20 parts firming agent and 50 parts～150 parts resin matrixes by 0.02 part～1.5 parts by weight and is prepared from.
The advantage of this detailed description of the invention:
One, the composite with photochromic properties that prepared by this detailed description of the invention, the raw material of use is simple and easy to get, with low cost, and environmental pollution is little；
The technological process of the composite with photochromic properties that two, prepared by this detailed description of the invention is simple, operates easy, and device therefor is this area conventional instrument, and process cycle is short, and the requirement of process environments is relatively low；
Three, the steady quality of the composite with photochromic properties, the photochromic properties that prepared by this detailed description of the invention are obvious, and reversibility is better；Meanwhile, the environmental stability of this composite is good, has good photochromic properties in various environment；
The composite range of application of what four, prepared by this detailed description of the invention have photochromic properties is very wide, information can be prepared either directly or as coating and store material, decoration protective material, detection radiative material etc., in information, electronics, Non-Destructive Testing, Aero-Space, the field such as military suffers from being widely applied potentiality.
Five, the composite with photochromic properties that prepared by this detailed description of the invention is after ultra-vioket radiation 1h, at the absorbance of wavelength 710nm for will improve 50%～160%, it was shown that it has the photochromic sensitivity of excellence；After ultra-vioket radiation 16h, at the absorbance of wavelength 710nm for 200%～500% will be improved, it was shown that it has the photochromic properties of excellence.
This detailed description of the invention can obtain a kind of composite with photochromic properties.
Detailed description of the invention two: present embodiment and detailed description of the invention one difference be: described resin matrix is epoxy resin E51, epoxy resin TDE-85 or polyester resin.Other steps are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment with one of detailed description of the invention one or two difference is: described solvent is 1-Methyl-2-Pyrrolidone or dimethylformamide.Other steps are identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment with one of detailed description of the invention one to three difference is: described firming agent is triethylene tetramine.Other steps are identical with detailed description of the invention one to three.
Detailed description of the invention five: present embodiment with one of detailed description of the invention one to four difference is: the preparation method of the described molybdenum compound with photochromic properties is specifically realized by the following steps:
One, ethanol or acetone are mixed with distilled water, prepare mixed solution；
In mixed solution described in step one, the volume fraction of ethanol or acetone is 25%～75%；
Two, by the MoS of natural hexagonal structure2Powder mixes with mixed solution, obtains containing MoS2Mixed liquor；
The MoS of the natural hexagonal structure described in step 22The quality of powder and the volume ratio of mixed solution are (25mg～180mg): 1mL；
Three, adopt high speed shear emulsification instrument to containing MoS2Mixed liquor carry out high speed shear process, obtain the mixed liquor after shear treatment；
Four, the mixed liquor after shear treatment is carried out water bath sonicator process, the mixed liquor after being disperseed；
Five, the mixed liquor after dispersion is stood 6h～8h, take the supernatant, obtain the molybdenum compound suspension with photochromic properties；
Six, being dry 4h～10h at 60 DEG C～80 DEG C by there is the molybdenum compound suspension of photochromic properties in temperature, obtaining the molybdenum compound with photochromic properties.Other steps are identical with detailed description of the invention one to four.
Detailed description of the invention six: present embodiment with one of detailed description of the invention one to five difference is: it is shear 45min～150min with the speed of 8000r/min～19000r/min that the high speed shear described in step 3 processes.Other steps are identical with detailed description of the invention one to five.
Detailed description of the invention seven: present embodiment with one of detailed description of the invention one to six difference is: the power of the supersound process described in step 4 is 200W～240W, and ultrasonic time is 45min～90min.Other steps are identical with detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment with one of detailed description of the invention one to seven difference is: the preparation method of a kind of composite with photochromic properties is specifically realized by the following steps:
One, preparation has the molybdenum compound of photochromic properties: 1., ethanol or acetone is mixed with distilled water, prepares mixed solution；
Step 1. described in mixed solution in the volume fraction of ethanol or acetone be 25%～75%；
2., by the MoS of natural hexagonal structure2Powder mixes with mixed solution, obtains containing MoS2Mixed liquor；
Step 2. described in the MoS of natural hexagonal structure2The quality of powder and the volume ratio of mixed solution are (25mg～180mg): 1mL；
3., adopt high speed shear emulsification instrument to containing MoS2Mixed liquor carry out high speed shear process, obtain the mixed liquor after shear treatment；
Step 3. described in high speed shear to process be shear 45min～150min with the speed of 8000r/min～19000r/min；
4., the mixed liquor after shear treatment is carried out water bath sonicator process, the mixed liquor after being disperseed；
Step 4. described in the power of supersound process be 200W～240W, ultrasonic time is 45min～90min；
5., the mixed liquor after dispersion is stood 6h～8h, take the supernatant, obtain the molybdenum compound suspension with photochromic properties；
6., be dry 4h～10h at 60 DEG C～80 DEG C by there is the molybdenum compound suspension of photochromic properties in temperature, obtain the molybdenum compound with photochromic properties；
Two, weigh: weigh 0.02 part～1.5 parts by weight and there are the molybdenum compound of photochromic properties, 10 parts～35 parts solvents, 6 parts～20 parts firming agent and 50 parts～150 parts resin matrixes；
Three, preparation has the molybdenum compound/solvent mixture of photochromic properties: is dissolved in 10 parts～35 parts solvents by weigh 0.02 part～1.5 parts molybdenum compounds with photochromic properties, obtains the molybdenum compound/solvent mixture with photochromic properties；Being ultrasonic disperse 15min～30min under 150W～200W by there is the molybdenum compound/solvent mixture of photochromic properties at ultrasonic power, obtaining the molybdenum compound/solvent mixture with photochromic properties after ultrasonic disperse；
Four, preparation has the mixture of photochromic properties: in the molybdenum compound/solvent mixture with photochromic properties after weigh 50 parts～150 parts resin matrixes are joined the ultrasonic disperse that step 3 obtains, low whipping speed is stirring 10min～30min under 200r/min～400r/min, it is ultrasonic disperse 1h～2h under 150W～240W at ultrasonic power again, obtains the mixture with photochromic properties；
Five, firming agent is added: join in the mixture with photochromic properties that step 4 obtains by weigh 6 parts～20 parts firming agent, low whipping speed is for stirring 10min～20min under 100r/min～200r/min again, obtains the mixture with photochromic properties to be solidified；
Six, solidification, molding: the mixture cast molding with photochromic properties to be solidified that step 5 is obtained, more at room temperature place 8h～12h, obtain the composite with photochromic properties.Other steps are identical with detailed description of the invention one to seven.
The advantage of this detailed description of the invention:
One, the composite with photochromic properties that prepared by this detailed description of the invention, the raw material of use is simple and easy to get, with low cost, and environmental pollution is little；
The technological process of the composite with photochromic properties that two, prepared by this detailed description of the invention is simple, operates easy, and device therefor is this area conventional instrument, and process cycle is short, and the requirement of process environments is relatively low；
Three, the steady quality of the composite with photochromic properties, the photochromic properties that prepared by this detailed description of the invention are obvious, and reversibility is better；Meanwhile, the environmental stability of this composite is good, has good photochromic properties in various environment；
The composite range of application of what four, prepared by this detailed description of the invention have photochromic properties is very wide, information can be prepared either directly or as coating and store material, decoration protective material, detection radiative material etc., in information, electronics, Non-Destructive Testing, Aero-Space, the field such as military suffers from being widely applied potentiality.
Five, the composite with photochromic properties that prepared by this detailed description of the invention is after ultra-vioket radiation 1h, at the absorbance of wavelength 710nm for will improve 50%～160%, it was shown that it has the photochromic sensitivity of excellence；After ultra-vioket radiation 16h, at the absorbance of wavelength 710nm for 200%～500% will be improved, it was shown that it has the photochromic properties of excellence.
This detailed description of the invention can obtain a kind of composite with photochromic properties.
Detailed description of the invention nine: present embodiment with one of detailed description of the invention one to eight difference is: the solvent described in step 2 is 1-Methyl-2-Pyrrolidone or dimethylformamide；Described firming agent is triethylene tetramine.Other steps are identical with detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment with one of detailed description of the invention one to nine difference is: the resin matrix described in step 3 is epoxy resin E51, epoxy resin TDE-85 or polyester resin.Other steps are identical with detailed description of the invention one to nine.
Adopt tests below checking beneficial effects of the present invention:
Test one: the preparation method of a kind of composite with photochromic properties, is specifically realized by the following steps:
One, preparation has the molybdenum compound of photochromic properties: 1., is mixed with distilled water by ethanol, prepares mixed solution；
Step 1. described in mixed solution in the volume fraction of ethanol be 40%；
2., by the MoS of natural hexagonal structure2Powder mixes with mixed solution, obtains containing MoS2Mixed liquor；
Step 2. described in the MoS of natural hexagonal structure2The quality of powder and the volume ratio of mixed solution are 100mg:1mL；
3., adopt high speed shear emulsification instrument to containing MoS2Mixed liquor carry out high speed shear process, obtain the mixed liquor after shear treatment；
Step 3. described in high speed shear to process be shear 120min with the speed of 16000r/min；
4., the mixed liquor after shear treatment is carried out water bath sonicator process, the mixed liquor after being disperseed；
Step 4. described in the power of supersound process be 200W, ultrasonic time is 30min；
5., the mixed liquor after dispersion is stood 8h, take the supernatant, obtain the molybdenum compound suspension with photochromic properties；
6., be dry 6h at 80 DEG C by there is the molybdenum compound suspension of photochromic properties in temperature, obtain the molybdenum compound with photochromic properties；
Two, weigh: weigh 0.25 part by weight and there are the molybdenum compound of photochromic properties, 20 parts of solvents, 13 parts of firming agent and 100 parts of resin matrixes；
Solvent described in step 2 is 1-Methyl-2-Pyrrolidone；
Firming agent described in step 2 is triethylene tetramine；
Resin matrix described in step 2 is epoxy resin E51；
Three, preparation has the molybdenum compound/solvent mixture of photochromic properties: is dissolved in 20 parts of solvents by the molybdenum compound that weigh 0.25 part has photochromic properties, obtains the molybdenum compound/solvent mixture with photochromic properties；Being ultrasonic disperse 30min under 150W by there is the molybdenum compound/solvent mixture of photochromic properties at ultrasonic power, obtaining the molybdenum compound/solvent mixture with photochromic properties after ultrasonic disperse；
Four, preparation has the mixture of photochromic properties: in the molybdenum compound/solvent mixture with photochromic properties after weigh 100 parts of resin matrixes are joined the ultrasonic disperse that step 3 obtains, low whipping speed is stirring 10min under 200r/min, it is ultrasonic disperse 1h under 200W at ultrasonic power again, obtains the mixture with photochromic properties；
Five, add firming agent: joined in the mixture with photochromic properties that step 4 obtains by 13 firming agent weighed, then low whipping speed is for stirring 10min under 100r/min, obtain the mixture with photochromic properties to be solidified；
Six, solidification, molding: the mixture cast molding with photochromic properties to be solidified that step 5 is obtained, more at room temperature place 8h, obtain the composite with photochromic properties.
The composite with photochromic properties of test one preparation is placed under ultraviolet light and irradiates, the composite with photochromic properties of the test different time test one preparation absorbance at wavelength 710nm place, as it is shown in figure 1, the composite with photochromic properties that Fig. 1 is test one preparation is the change curve with the irradiation under ultraviolet ray time of absorbance during 710nm at wavelength.From fig. 1, it can be seen that when the irradiation under ultraviolet ray time is 0, the absorbance of the composite with photochromic properties of test one preparation is 0.31cm-1；When the irradiation under ultraviolet ray time is 2h, the composite with photochromic properties of test one preparation is 0.59cm at the absorbance of wavelength 710nm-1；When the irradiation under ultraviolet ray time is 16h, the composite with photochromic properties of test one preparation is 0.95cm at the absorbance of wavelength 710nm-1；The composite with photochromic properties of test one preparation when the irradiation under ultraviolet ray time is 2h when the absorbance of wavelength 710nm is 0 with the irradiation under ultraviolet ray time compared with the absorbance of wavelength 710nm, improve 90%；The composite with photochromic properties of test one preparation when the irradiation under ultraviolet ray time is 16h when the absorbance of wavelength 710nm is 0 with the irradiation under ultraviolet ray time compared with the absorbance of wavelength 710nm, improve 306%；It is indicated above that the composite with photochromic properties of test one preparation has photochromic performance of excellence.
Claims (9)
1. a composite with photochromic properties, it is characterised in that a kind of composite with photochromic properties is had the molybdenum compound of photochromic properties, 10 parts～35 parts solvents, 6 parts～20 parts firming agent and 50 parts～150 parts resin matrixes by 0.02 part～1.5 parts by weight and is prepared from；
The preparation method of the described molybdenum compound with photochromic properties is specifically realized by the following steps:
One, ethanol or acetone are mixed with distilled water, prepare mixed solution；
In mixed solution described in step one, the volume fraction of ethanol or acetone is 25%～75%；
Two, by the MoS of natural hexagonal structure2Powder mixes with mixed solution, obtains containing MoS2Mixed liquor；
The MoS of the natural hexagonal structure described in step 22The quality of powder and the volume ratio of mixed solution are (25mg～180mg): 1mL；
Three, adopt high speed shear emulsification instrument to containing MoS2Mixed liquor carry out high speed shear process, obtain the mixed liquor after shear treatment；
Four, the mixed liquor after shear treatment is carried out water bath sonicator process, the mixed liquor after being disperseed；
Five, the mixed liquor after dispersion is stood 6h～8h, take the supernatant, obtain the molybdenum compound suspension with photochromic properties；
Six, being dry 4h～10h at 60 DEG C～80 DEG C by there is the molybdenum compound suspension of photochromic properties in temperature, obtaining the molybdenum compound with photochromic properties.
2. a kind of composite with photochromic properties according to claim 1, it is characterised in that described resin matrix is epoxy resin E51, epoxy resin TDE-85 or polyester resin.
3. a kind of composite with photochromic properties according to claim 1, it is characterised in that described solvent is 1-Methyl-2-Pyrrolidone or dimethylformamide.
4. a kind of composite with photochromic properties according to claim 1, it is characterised in that described firming agent is triethylene tetramine.
5. a kind of composite with photochromic properties according to claim 1, it is characterised in that it is shear 45min～150min with the speed of 8000r/min～19000r/min that the high speed shear described in step 3 processes.
6. a kind of composite with photochromic properties according to claim 1, it is characterised in that the power of the supersound process described in step 4 is 200W～240W, and ultrasonic time is 45min～90min.
7. the preparation method of a kind of composite with photochromic properties as claimed in claim 1, it is characterised in that the preparation method of a kind of composite with photochromic properties is specifically realized by the following steps:
One, preparation has the molybdenum compound of photochromic properties: 1., ethanol or acetone is mixed with distilled water, prepares mixed solution；
Step 1. described in mixed solution in the volume fraction of ethanol or acetone be 25%～75%；
2., by the MoS of natural hexagonal structure2Powder mixes with mixed solution, obtains containing MoS2Mixed liquor；
Step 2. described in the MoS of natural hexagonal structure2The quality of powder and the volume ratio of mixed solution are (25mg～180mg): 1mL；
3., adopt high speed shear emulsification instrument to containing MoS2Mixed liquor carry out high speed shear process, obtain the mixed liquor after shear treatment；
Step 3. described in high speed shear to process be shear 45min～150min with the speed of 8000r/min～19000r/min；
4., the mixed liquor after shear treatment is carried out water bath sonicator process, the mixed liquor after being disperseed；
Step 4. described in the power of supersound process be 200W～240W, ultrasonic time is 45min～90min；
5., the mixed liquor after dispersion is stood 6h～8h, take the supernatant, obtain the molybdenum compound suspension with photochromic properties；
6., be dry 4h～10h at 60 DEG C～80 DEG C by there is the molybdenum compound suspension of photochromic properties in temperature, obtain the molybdenum compound with photochromic properties；
Two, weigh: weigh 0.02 part～1.5 parts by weight and there are the molybdenum compound of photochromic properties, 10 parts～35 parts solvents, 6 parts～20 parts firming agent and 50 parts～150 parts resin matrixes；
Three, preparation has the molybdenum compound/solvent mixture of photochromic properties: is dissolved in 10 parts～35 parts solvents by weigh 0.02 part～1.5 parts molybdenum compounds with photochromic properties, obtains the molybdenum compound/solvent mixture with photochromic properties；Being ultrasonic disperse 15min～30min under 150W～200W by there is the molybdenum compound/solvent mixture of photochromic properties at ultrasonic power, obtaining the molybdenum compound/solvent mixture with photochromic properties after ultrasonic disperse；
Four, preparation has the mixture of photochromic properties: in the molybdenum compound/solvent mixture with photochromic properties after weigh 50 parts～150 parts resin matrixes are joined the ultrasonic disperse that step 3 obtains, low whipping speed is stirring 10min～30min under 200r/min～400r/min, it is ultrasonic disperse 1h～2h under 150W～240W at ultrasonic power again, obtains the mixture with photochromic properties；
Five, firming agent is added: join in the mixture with photochromic properties that step 4 obtains by weigh 6 parts～20 parts firming agent, low whipping speed is for stirring 10min～20min under 100r/min～200r/min again, obtains the mixture with photochromic properties to be solidified；
Six, solidification, molding: the mixture cast molding with photochromic properties to be solidified that step 5 is obtained, more at room temperature place 8h～12h, obtain the composite with photochromic properties.
8. the preparation method of a kind of composite with photochromic properties according to claim 7, it is characterised in that the solvent described in step 2 is 1-Methyl-2-Pyrrolidone or dimethylformamide；Described firming agent is triethylene tetramine.
9. the preparation method of a kind of composite with photochromic properties according to claim 7, it is characterised in that the resin matrix described in step 2 is epoxy resin E51, epoxy resin TDE-85 or polyester resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410384293.8A CN104140641B (en) | 2014-08-06 | 2014-08-06 | A kind of composite with photochromic properties and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410384293.8A CN104140641B (en) | 2014-08-06 | 2014-08-06 | A kind of composite with photochromic properties and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104140641A CN104140641A (en) | 2014-11-12 |
| CN104140641B true CN104140641B (en) | 2016-06-29 |
Family
ID=51849988
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410384293.8A Expired - Fee Related CN104140641B (en) | 2014-08-06 | 2014-08-06 | A kind of composite with photochromic properties and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104140641B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1942612A (en) * | 2004-03-16 | 2007-04-04 | 特拉华大学 | Active and adaptive photochromic fibers, textiles and membranes |
| CN103771517A (en) * | 2014-01-17 | 2014-05-07 | 哈尔滨工业大学 | Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets |
-
2014
- 2014-08-06 CN CN201410384293.8A patent/CN104140641B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1942612A (en) * | 2004-03-16 | 2007-04-04 | 特拉华大学 | Active and adaptive photochromic fibers, textiles and membranes |
| CN103771517A (en) * | 2014-01-17 | 2014-05-07 | 哈尔滨工业大学 | Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets |
Non-Patent Citations (4)
| Title |
|---|
| A Mixed-Solvent Strategy for Efficient Exfoliation of Inorganic Graphene Analogues;Kai-Ge Zhou et al.;《Angew. Chem. Int. Ed.》;20110927;第50卷;第10839-10842页 * |
| Evaluation of microstructure and photochromic behavior of polyvinyl alcohol nanocomposite films containing polyoxometalates;Li-Mei Ai et al;《Materials Chemistry and Physics》;20081231;第109卷;第131–136页 * |
| Polyoxometalate cured epoxy resins with photochromic properties;xinhui zhong et al;《Colloid and Polymer Science》;20120621;第290卷(第16期);第1683-1693页 * |
| Two-Dimensional Nanosheets Produced by Liquid Exfoliation of Layered Materials;Jonathan N. Coleman et al;《science》;20110204;第331卷;第568-571页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104140641A (en) | 2014-11-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | A facile strategy to prepare smart coatings with autonomous self-healing and self-reporting functions | |
| Liu et al. | Luminescent transparent wood based on lignin-derived carbon dots as a building material for dual-channel, real-time, and visual detection of formaldehyde gas | |
| Pu et al. | Multiaddressing fluorescence switch based on a new photochromic diarylethene with a triazole-linked rhodamine B unit | |
| Wei et al. | Creating Coordination‐Based Cavities in a Multiresponsive Supramolecular Gel | |
| Pu et al. | Artificial Light‐Harvesting Material Based on Self‐Assembly of Coordination Polymer Nanoparticles | |
| Chan et al. | Controlling self-assembly mechanisms through rational molecular design in oligo (p-phenyleneethynylene)-containing alkynylplatinum (II) 2, 6-bis (N-alkylbenzimidazol-2′-yl) pyridine amphiphiles | |
| CN104212087B (en) | Preparation method of monodisperse fluorescent microspheres | |
| Chen et al. | The first europium (III) β‐diketonate complex functionalized polyhedral oligomeric silsesquioxane | |
| Zhao et al. | Preparation of carbon quantum dots based high photostability luminescent membranes | |
| CN106566542A (en) | Preparation of carbon quantum dots based on coal tar asphalt and detection method for HCHO | |
| Yuan et al. | Preparation and characterization of microencapsulated ethylenediamine with epoxy resin for self-healing composites | |
| Hassan et al. | Charge carriers modulate the bonding of semiconductor nanoparticle dopants as revealed by time-resolved X-ray spectroscopy | |
| Zhang et al. | Flexible and transparent ceramic nanocomposite for laboratory X-ray imaging of micrometer resolution | |
| Yu et al. | A novel diazoresin/poly (N‐vinyl aminobutyric acid) covalent capillary coating for the analysis of proteins by capillary electrophoresis | |
| Wan et al. | A Two‐Photon Luminescent Dye‐Loaded Metal–Organic Framework for Physiological Temperature Sensing within Biological Windows | |
| CN104140641B (en) | A kind of composite with photochromic properties and preparation method thereof | |
| Pan et al. | Control the Single‐, Two‐, and Three‐Photon Excited Fluorescence of Atomically Precise Metal Nanoclusters | |
| Ševčík et al. | The photostability of novel boron hydride blue emitters in solution and polystyrene matrix | |
| Jilani et al. | DGEBA epoxy polymer composite panels (MB: DGEBA-EPCPs): structural, optical, and dielectric properties-leanings and appliances in optical electronics | |
| Zhou et al. | Design, synthesis and performance of novel fluorescent polymer microspheres tracers based on aggregation induced emission | |
| Guo et al. | Temperature sensitive properties and preparation of europium complexes with double ligands | |
| Li et al. | Synergetic Effect of Perfluorooctanoic Acid on the Preparation of Poly (3, 4‐ethylenedioxythiophene): Lignosulfonate Aqueous Dispersions with High Film Conductivity | |
| Zhang et al. | Preparation of Smart Poly (SPAA‐co‐MMA) Film Materials for Regulating Wettability and Humidity by Electrospinning | |
| CN104625088A (en) | Environment-friendly synthesis method of 1D chain structure nano particles | |
| Yang et al. | Triphenylamine, carbazole or tetraphenylethylene-functionalized benzothiadiazole derivatives: aggregation-induced emission (AIE), solvatochromic and different mechanoresponsive fluorescence characteristics |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160629 Termination date: 20160806 |