CN108947936A - Graphene/piperazine pyrophosphate nano-complex and preparation method thereof - Google Patents
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- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/04—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms
- C07D295/08—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms substituted by singly bound oxygen or sulfur atoms
- C07D295/084—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms substituted by singly bound oxygen or sulfur atoms with the ring nitrogen atoms and the oxygen or sulfur atoms attached to the same carbon chain, which is not interrupted by carbocyclic rings
- C07D295/088—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms substituted by singly bound oxygen or sulfur atoms with the ring nitrogen atoms and the oxygen or sulfur atoms attached to the same carbon chain, which is not interrupted by carbocyclic rings to an acyclic saturated chain
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Abstract
The present invention discloses a kind of graphene/piperazine pyrophosphate nano-complex and preparation method thereof, preparation method are as follows: will be on piperazine and epoxy-functional reactive grafting to graphene oxide GO, it adds phosphoric acid and forms piperazine phosphate salt, the graphene/piperazine pyrophosphate nano-complex is finally prepared using high temperature dehydration.Graphene of the invention/piperazine pyrophosphate nano-complex heat, due to graphene, with good flame retarding efficiency and thermal conductivity, and preparation method is to introduce graphene oxide GO during piperazine pyrophosphate synthesis, efficiently solves the dispersion of nano material；Simultaneously, graphene oxide GO is reduced using alkalinity and strong acid (phosphoric acid) dehydration of piperazine and hot conditions, efficiently avoid the reduction step in graphene preparation process, efficiently, low cost, environmental protection it is low prepare graphene/piperazine pyrophosphate nano-complex, have good industrial application prospect.
Description
Technical field
The present invention relates to a kind of graphene/piperazine pyrophosphate nano-complexes and preparation method thereof.
Background technique
Simultaneously containing acid source needed for expansion type flame retardant (pyrophosphoric acid) and charcoal source (piperazine in piperazine pyrophosphate molecular structure
Piperazine), it is used as expansion type flame retardant flame retarding efficiency with higher, is particularly suitable for the flame-retardant modified of polyolefine material.This
Outside, piperazine pyrophosphate also has many advantages, such as thermal stability height, water-tolerant.It is swollen compared to traditional ammonium polyphosphate (APP) system
Swollen type fire retardant, piperazine pyrophosphate system has great advantages in performance, therefore is widely applied.
With the fast development of the technologies such as electronics is integrated, quick charge, the sharply diminution of electronic component volume, simultaneously
Working frequency sharply increases, the environment temperature gradually high temperature of instrument work, this, which becomes the radiating efficiency of instrument, influences device
The key factor of precision and service life.For the stability and safety for keeping device element to operate normally, good heat conductive is had both
The heat conductive flame-retarding plastics of performance and flame retardant property are ideal materials.
In general, the thermal conductivity of polymer material is realized by inorganics filled, common filler includes that metal is filled out
Material, carbon material, metal oxide, nitride and carbide etc..It is well known that the inorganic fill in polymer material can shadow
Ring expansion type flame retardant at charcoal process, so that layer of charcoal compactness is deteriorated, and then substantially reduce flame retarding efficiency, or even make its failure.
It is still to use based on bromide fire retardant in some materials for needing using a large amount of inorganics filled polymer.Therefore, swollen
The application of swollen type fire retardant has certain limitation.
Carbon material be it is thermally conductive come phenomenon by electronics thermal conduction mechanism, common carbon material include carbon nanotube, carbon black,
Carbon fiber, graphene etc., their not only thermal conductivities with higher, but also have sheet, tubulose or fibrous morphology, make it
Be easier to be overlapped to form network in a polymer matrix, the thermal coefficient of material can be effectively promoted under lower content, still
Grapheme material is applied limited as high-performance nano Heat Conduction Material because of hardly possible dispersion.
Summary of the invention
Aiming at the problem that flame retarding efficiency of above-mentioned expansion type flame retardant is affected by inorganic filler, of the invention
One purpose is to provide a kind of graphene and expansion type flame retardant, compound with good flame retarding efficiency and thermal conductivity of integrating
Object.
The second object of the present invention is to provide the preparation method of above-mentioned compound, and reaction process is continuous and the time is short, very
It is suitble to industrialized production, there is fabulous application prospect.
Based on above-mentioned first purpose, the present invention provides a kind of graphene/piperazine pyrophosphate nano-complex, structures
Shown in general formula such as formula (I):
Wherein,R is the bilvalent radical of the piperazine pyrophosphate as shown in formula (II),
R1 is the pyrophosphate ion as shown in formula (III),
Based on above-mentioned second purpose, the present invention provides above-mentioned graphene/piperazine pyrophosphate nano-complex preparation sides
Method includes the following steps:
Step (1): graphene oxide GO being added into polar solvent, and ultrasonic agitation makes graphene oxide GO in the pole
Property solvent in it is fully dispersed, piperazine is then added, and at 60~120 DEG C react 12~36h obtain reaction solution, wherein it is described
The mass ratio of piperazine and the graphene oxide GO are (0.1~0.5): 1；
Step (2): being added phosphoric acid in the reaction solution obtained to the step (1), stirs 1~5h, at room temperature to obtain phosphorus
Mcpp acid salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried, wherein institute
The molar ratio for stating piperazine in phosphoric acid and the step (1) is (1~1.5): 1；
Step (3): graphene/piperazine phosphate salt that the step (2) obtains is subjected to dehydration condensation and prepares graphite
Alkene/piperazine pyrophosphate nano-complex, wherein the process conditions of the dehydration condensation are in inert atmosphere or vacuum item
Under part, 1~12h is heated at a temperature of 200~280 DEG C of dehydrating condensation.
In above-mentioned technical proposal, it is preferable that polar solvent described in the step (1) is n,N-Dimethylformamide
Or water.
In above-mentioned technical proposal, it is preferable that the temperature of reaction described in the step (1) is 80~100 DEG C, reaction
Time is 20~25h.
In above-mentioned technical proposal, it is preferable that the quality of piperazine and the graphene oxide GO described in the step (1)
Than for (0.2~0.3): 1.
In above-mentioned technical proposal, it is further preferred that piperazine described in the step (1) and the graphene oxide GO
Mass ratio be 0.25:1.
In above-mentioned technical proposal, it is preferable that piperazine in the phosphoric acid being added in the step (2) and the step (1)
Molar ratio is 1.2:1.
In above-mentioned technical proposal, it is preferable that inert atmosphere described in the step (3) is nitrogen, argon gas, helium, two
One of carbonoxide, the vacuum condition are 0.02~0.03MPa of vacuum degree.
In above-mentioned technical proposal, it is further preferred that the inert gas is the High Purity Nitrogen of 99.99% or more purity
Gas or argon gas, the vacuum condition are 0.02~0.025MPa of vacuum degree.
In above-mentioned technical proposal, it is preferable that dehydrating condensation temperature described in the step (3) is 220~260 DEG C, is added
The time of heat is 2~10h.
The present invention obtains compared with prior art following the utility model has the advantages that graphene/piperazine pyrophosphate nanometer of the invention is multiple
Object is closed, by introducing graphene oxide GO in the synthesis process of piperazine pyrophosphate, to have good flame retarding efficiency and lead
It is hot；In addition in graphene/piperazine pyrophosphate nano-complex preparation method, draw during piperazine pyrophosphate synthesis
Enter graphene oxide GO, efficiently solves the dispersion of nano material；Meanwhile utilizing the alkalinity and strong acid (phosphorus of piperazine
Acid) dehydration and hot conditions be reduced graphene oxide GO, efficiently avoid the recovery step in graphene preparation process
Suddenly, efficiently, low cost, environmental protection it is low prepare graphene/piperazine pyrophosphate nano-complex, have good industrial application before
Scape.
Specific embodiment
By the technology contents of invention are described in detail, construction feature, are reached purpose and efficacy, below in conjunction with embodiment
It is described in detail.
Graphene of the present invention/piperazine pyrophosphate nano-complex is by piperazine and epoxy-functional reactive grafting to oxidation
On graphene GO, adds phosphoric acid and forms piperazine phosphate salt, be finally prepared using high temperature dehydration, reaction principle is as follows:
Wherein,R is the bilvalent radical of the piperazine pyrophosphate as shown in formula (II),
R1 is the pyrophosphate ion as shown in formula (III),
Piperazine, phosphoric acid are obtained by commercially available, and graphene oxide GO makes by oneself to obtain by known Hummers oxidizing process, i.e., logical
It is graphene oxide GO that the concentrated sulfuric acid, potassium permanganate and sodium nitrate etc., which are crossed, by graphite oxidation.
Embodiment 1
The graphene of the present embodiment/piperazine pyrophosphate nano-complex preparation method includes the following steps:
Step (1): into 250ml water be added 250mg GO, ultrasonic agitation GO keep it fully dispersed in water, then plus
Enter 62.5mg piperazine, and reacted for 24 hours at 80 DEG C, obtains reaction solution；
Step (2): 97% concentrated phosphoric acid of 73.5mg is added into reaction solution, stirs 3h, at room temperature to obtain piperazine phosphate
Salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried；
Step (3): graphene/piperazine phosphate salt obtained by step (2) being placed in revolving burner, 230 DEG C of set temperature, and
And graphene/piperazine pyrophosphate nano-complex is made in logical nitrogen protection, heated at constant temperature 12h.
To graphene/piperazine pyrophosphate nano-complex obtained by the present embodiment, thermal stability is good, passes through thermogravimetric analysis sample
1% weightless temperature is 265 DEG C to product in a nitrogen atmosphere.
Embodiment 2
The graphene of the present embodiment/piperazine pyrophosphate nano-complex preparation method includes the following steps:
Step (1): into 250ml water be added 250mg GO, ultrasonic agitation GO keep it fully dispersed in water, then plus
Enter 62.5mg piperazine, and reacted for 24 hours at 80 DEG C, obtains reaction solution；
Step (2): 97% concentrated phosphoric acid of 85.75mg is added into reaction solution, stirs 3h, at room temperature to obtain phosphoric acid piperazine
Piperazine salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried；
Step (3): graphene/piperazine phosphate salt obtained by step (2) being placed in revolving burner, 230 DEG C of set temperature, and
And graphene/piperazine pyrophosphate nano-complex is made in logical nitrogen protection, heated at constant temperature 12h.
To graphene/piperazine pyrophosphate nano-complex obtained by the present embodiment, thermal stability is good, passes through thermogravimetric analysis sample
1% weightless temperature is 265 DEG C to product in a nitrogen atmosphere.
Embodiment 3
The graphene of the present embodiment/piperazine pyrophosphate nano-complex preparation method includes the following steps:
Step (1): into 250ml water be added 250mg GO, ultrasonic agitation GO keep it fully dispersed in water, then plus
Enter 75mg piperazine, and reacted for 24 hours at 80 DEG C, obtains reaction solution；
Step (2): 97% concentrated phosphoric acid of 105mg is added into reaction solution, stirs 3h, at room temperature to obtain piperazine phosphate
Salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried；
Step (3): graphene/piperazine phosphate salt obtained by step (2) being placed in revolving burner, 230 DEG C of set temperature, and
And graphene/piperazine pyrophosphate nano-complex is made in logical nitrogen protection, heated at constant temperature 12h.
To graphene/piperazine pyrophosphate nano-complex obtained by the present embodiment, thermal stability is good, passes through thermogravimetric analysis sample
1% weightless temperature is 265 DEG C to product in a nitrogen atmosphere.
Embodiment 4
The graphene of the present embodiment/piperazine pyrophosphate nano-complex preparation method includes the following steps:
Step (1): into 250ml water be added 250mg GO, ultrasonic agitation GO keep it fully dispersed in water, then plus
Enter 62.5mg piperazine, and reacted for 24 hours at 80 DEG C, obtains reaction solution；
Step (2): 97% concentrated phosphoric acid of 85.75mg is added into reaction solution, stirs 3h, at room temperature to obtain phosphoric acid piperazine
Piperazine salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried；
Step (3): graphene/piperazine phosphate salt obtained by step (2) being placed in revolving burner, 240 DEG C of set temperature, and
And graphene/piperazine pyrophosphate nano-complex is made in logical nitrogen protection, heated at constant temperature 12h.
To graphene/piperazine pyrophosphate nano-complex obtained by the present embodiment, thermal stability is good, passes through thermogravimetric analysis sample
1% weightless temperature is 275 DEG C to product in a nitrogen atmosphere.
Embodiment 5
The graphene of the present embodiment/piperazine pyrophosphate nano-complex preparation method includes the following steps:
Step (1): into 250ml water be added 250mg GO, ultrasonic agitation GO keep it fully dispersed in water, then plus
Enter 62.5mg piperazine, and reacted for 24 hours at 80 DEG C, obtains reaction solution；
Step (2): 97% concentrated phosphoric acid of 85.75mg is added into reaction solution, stirs 3h, at room temperature to obtain phosphoric acid piperazine
Piperazine salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried；
Step (3): graphene/piperazine phosphate salt obtained by step (2) being placed in revolving burner, 250 DEG C of set temperature, and
And graphene/piperazine pyrophosphate nano-complex is made in logical nitrogen protection, heated at constant temperature 6h.
To graphene/piperazine pyrophosphate nano-complex obtained by the present embodiment, thermal stability is good, passes through thermogravimetric analysis sample
1% weightless temperature is 275 DEG C to product in a nitrogen atmosphere.
Gained graphene/piperazine pyrophosphate nano-complex of the invention, thermal stability is good, and graphene has nano-dispersed
Scale while use as fire retardant, can play the role of thermal conducting agent, avoid or reduce the use of heat-conducting filler.And
Preparation method of the invention is simple, and reaction process is continuous and the time is short, is very suitable to industrialized production, has fabulous application
Prospect.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, this hair
Bright claimed range is delineated by the appended claims, the specification and equivalents thereof from the appended claims.
Claims (10)
1. a kind of graphene/piperazine pyrophosphate nano-complex, which is characterized in that shown in its general structure such as formula (I):
Wherein,R is the bilvalent radical of the piperazine pyrophosphate as shown in formula (II),
R1 is the pyrophosphate ion as shown in formula (III),
2. a kind of preparation method of graphene described in claim 1/piperazine pyrophosphate nano-complex, which is characterized in that packet
Include following steps:
Step (1): graphene oxide GO being added into polar solvent, and ultrasonic agitation makes graphene oxide GO in the polar solvent
In it is fully dispersed, piperazine is then added, and at 60~120 DEG C react 12~36h obtain reaction solution, wherein the piperazine with
The mass ratio of the graphene oxide GO is (0.1~0.5): 1；
Step (2): being added phosphoric acid in the reaction solution obtained to the step (1), stirs 1~5h, at room temperature to obtain phosphoric acid piperazine
Piperazine salt is separated by solid-liquid separation and obtains graphene/piperazine phosphate salt after obtained solid is repeatedly washed and dried, wherein the phosphorus
The sour molar ratio with piperazine in the step (1) is (1~1.5): 1；
Step (3): graphene/piperazine phosphate salt that the step (2) obtains is subjected to dehydration condensation and prepares graphene/coke
Piperazine phosphate nano-complex, wherein the process conditions of the dehydration condensation be under inert atmosphere or vacuum condition,
1~12h is heated at a temperature of 200~280 DEG C of dehydrating condensation.
3. graphene according to claim 2/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
Stating polar solvent described in step (1) is n,N-Dimethylformamide or water.
4. graphene according to claim 2/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
The temperature for stating reaction described in step (1) is 80~100 DEG C, and the time of reaction is 20~25h.
5. graphene according to claim 2/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
The mass ratio for stating piperazine described in step (1) and the graphene oxide GO is (0.2~0.3): 1.
6. graphene according to claim 5/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
The mass ratio for stating piperazine described in step (1) and the graphene oxide GO is 0.25:1.
7. graphene according to claim 2/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
The molar ratio for stating piperazine in the phosphoric acid being added in step (2) and the step (1) is 1.2:1.
8. graphene according to claim 2/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
Stating inert atmosphere described in step (3) is one of nitrogen, argon gas, helium, carbon dioxide, and the vacuum condition is true
0.02~0.03MPa of reciprocal of duty cycle.
9. graphene according to claim 8/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
The inert gas stated be 99.99% or more purity high pure nitrogen or argon gas, the vacuum condition be vacuum degree 0.02~
0.025MPa。
10. graphene according to claim 2/piperazine pyrophosphate nano-complex preparation method, which is characterized in that institute
Stating dehydrating condensation temperature described in step (3) is 220~260 DEG C, and the time of heating is 2~10h.
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Cited By (2)
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| CN110643068A (en) * | 2019-09-02 | 2020-01-03 | 厦门大学 | Metal phenylphosphonate flame-retardant material with adjustable morphology, preparation method and application thereof |
| CN115010996A (en) * | 2022-06-24 | 2022-09-06 | 云南锡业集团（控股）有限责任公司研发中心 | Preparation method of microencapsulated core-shell structure coated piperazine pyrophosphate composite flame retardant |
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| CN115010996A (en) * | 2022-06-24 | 2022-09-06 | 云南锡业集团（控股）有限责任公司研发中心 | Preparation method of microencapsulated core-shell structure coated piperazine pyrophosphate composite flame retardant |
| CN115010996B (en) * | 2022-06-24 | 2024-02-13 | 云南锡业集团（控股）有限责任公司研发中心 | Preparation method of microcapsule core-shell structure coated piperazine pyrophosphate composite flame retardant |
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