CN106752122B - A kind of nitridation carbon complex, preparation method and application - Google Patents
A kind of nitridation carbon complex, preparation method and application Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses a kind of azotized carbon nano pieces and preparation method thereof, and the azotized carbon nano piece and polymer are compounded to form nitridation carbon complex.Nitridation carbon dust is ground, water is added to obtain the suspension of carbonitride, is centrifuged, lower sediment is collected, it is dry, obtain the nitridation carbon dust of preliminary ball milling；Solvent is added, the suspension that ultrasound obtains carbonitride is centrifuged by ultrasound, and obtained upper layer dispersion liquid A is centrifuged again, is collected upper layer dispersion liquid B and is obtained azotized carbon nano piece solution.It dissolves a polymer in solvent, is mixed with azotized carbon nano piece, ultrasound, dried to get carbonitride complex thin film is arrived.The hydroxyl in amino and polymer in carbonitride or the available stable nitridation carbon complex of hydrogen bond of acetyl group formation, improve the film forming of nitridation carbon complex, the addition of carbonitride improves the thermal stability of polymer, improves the fire protecting performance of polymer.
Description
Technical field
The present invention relates to high thermal stability material, fire proofing material field, and in particular to a kind of nitridation carbon complex, its
Preparation method and application.
Background technique
With the development of synthetic material industry and the continuous expansion of application field, fire retardant chemical building material, electronic apparatus,
It is had a vast market foreground in the clothing, food, lodging and transportion -- basic necessities of life every field such as communications and transportation, space flight and aviation, household furniture, interior decoration.This
Outside, the fields such as coalfield, oil field, forest extinguishing also promote fire-retardant, the faster development of extinguishing chemical production.
Bromine phosphorus fire-retardant agent, especially bromide fire retardant are extremely important and common fire retardant types.Although fire-retardant
Most common halogenated flame retardant has a unrivaled high efficiency of other fire retardants series in agent, but its danger to environment and people
Evil is very important.Environmental issue is therefore auxiliary agent development and application quotient's focus of attention adjusts the product knot of fire retardant
Structure increases the emphasis for being developed into flame retardant area work of Efficient environment-friendlyflame flame retardant.
Engineering plastics are just rapidly developed in the 1950s.Although nylon 66 resin early in nineteen thirty-nine just
It succeeds in developing and puts into production, but it was used mainly for the manufacture of synthetic fibers until the fifties just breaks through pure fiber tradition at that time
On the way, plastics are manufactured by processing and forming.It is in later period fifties polyformaldehyde and poly- carbonic acid that engineering plastics, which really obtain rapidly developing,
After ester is succeeded in developing, their appearance has especially great meaning.Polycarbonate is have excellent comprehensive performance transparent
Engineering plastics are widely used, and are one of engineering plastics with fastest developing speed, and in engineering plastics field, yield and consumption figure are only secondary
Second is occupied in polyamide.The 1980s mid-term to succeed in developing thermotropic liquid crystal polymer be special engineering plastics development history
Upper another major event.Liquid crystal polymer excellent heat resistance, using temperature up to 200 DEG C or more, have self-reinforcing, high intensity,
The characteristics such as high-modulus, chemical-resistant resistance, melt viscosity is low, convenient formation, has boundless application in electronics industry
Prospect.
Compared with general-purpose plastics, engineering plastics mechanical performance, durability, corrosion resistance, in terms of can reach
Higher requirement, and process more convenient and alternative metal material.Engineering plastics be widely used in electric, automobile,
The industries such as building, office equipment, machinery, aerospace, to mould Dai Gang, have become international popular trend to mould Dai Mu.Engineering plastic
Material has become the field that growth rate is most fast in world today's plastics industry, and development is not only high to national pillar industry and modern times
New technological industry plays supporting role, while also pushing the adjustment of Transform of Traditional Industrial Equipment and product structure.
Graphite type carbon nitride (g-C3N4) it is the most stable of allotrope of carbonitride, there is the two-dimensional structure of stacking, due to
Its with quite high thermal stability, chemical stability, optically and electrically stability and cause more and more concerns.g-
C3N4There is-NH more than needed in structure2With-NH, the number of these groups is with g-C3N4The reduction of condensation degree of dissolved and increase, and this
A little groups can be used as active site and other groups such as-SH ,-OH ,-COOH act on forming hydrogen bond.g-C3N4And its derivative
Photoelectrocatalysis, decompose aquatic products hydrogen, electrooptical device, in terms of be all widely studied, in addition, researcher is to g-
C3N4Quasi polymer composite material is also studied.
Summary of the invention
Goal of the invention: in view of the deficiencies of the prior art, technical problem to be solved by the invention is to provide a kind of carbonitrides
Nanometer sheet, and it is compound with polymer material, to improve the film forming of compound, thermal stability and fire protecting performance.
Technical solution: to achieve the goals above, one aspect of the present invention provides a kind of system of azotized carbon nano piece
Preparation Method comprising following steps:
(1) nitridation carbon dust is ground, then plus water obtains the suspension of carbonitride；
(2) suspension of the carbonitride obtained to step (1) is centrifuged, and collects lower sediment, dry, obtains preliminary ball
The nitridation carbon dust of mill；
(3) solvent is added into the nitridation carbon dust of the preliminary ball milling, ultrasound is obtained the suspension of carbonitride by ultrasound
It is centrifuged, collects upper layer dispersion liquid A；
(4) the upper layer dispersion liquid A that step (3) obtains is centrifuged again and obtains upper layer dispersion liquid B, the upper layer dispersion liquid B
As azotized carbon nano piece solution.
In step (1), grinding carries out in the ball mill, in order to be fully ground to nitridation carbon dust, by ball milling
The revolving speed of machine is set as 20~2000rpm/min, and Ball-milling Time is set as 0.1~12h.
Another aspect of the present invention provides carbonitride made from a kind of preparation method as above-mentioned azotized carbon nano piece
Nanometer sheet.
Another aspect of the present invention provides a kind of nitridation carbon complex, which is azotized carbon nano piece
With the compound of polymer, azotized carbon nano piece is made by the preparation method of above-mentioned azotized carbon nano piece, and polymer contains hydroxyl
With one or both of acetyl group group, nitrogenizing mass ratio shared by carbonitride in carbon complex is 0.5%~10%.
Wherein, polymer is high molecular polymer, and high molecular polymer is cellulose acetate, polycarbonate, polypropylene, gathers
One of vinyl alcohol, polystyrene, polyamide, polyformaldehyde are a variety of.
An additional aspect of the present invention provides a kind of method for preparing nitridation carbon complex, comprising the following steps:
(1) it dissolves a polymer in solvent, obtains uniform solution, this solution is mixed with azotized carbon nano piece, ultrasound,
Obtain mixture；
(2) mixture obtained after step (1) processing is poured in horizontal container, is dried, obtain nitridation carbon complex
Film.
In order to make azotized carbon nano piece and polymer be sufficiently formed hydrogen bond, secondary distilled water, acetone, ethyl alcohol, isopropyl are selected
One of alcohol, n,N-Dimethylformamide or a variety of solvents as in step (1), 60 are set by ultrasonic power~
100W, ultrasonic time are set as 6~16 hours.
Another aspect of the invention provides a kind of nitridation carbon complex in terms of high thermal stability material, fire proofing material
Application.
The utility model has the advantages that compared with prior art, the invention has the following advantages that the present invention is prepared for azotized carbon nano piece,
It can effectively improve compound, the hydroxyl in amino and polymer especially in carbonitride of azotized carbon nano piece and polymer solution
The available stable nitridation carbon complex of hydrogen bond that base or acetyl group are formed, improves the film forming of nitridation carbon complex, nitrogen
The addition for changing carbon improves the thermal stability of polymer, this improves the fire protecting performance of polymer to a certain extent.
Detailed description of the invention
Fig. 1 is method of the embodiment 1 by water ultrasound, using the surface sweeping of carbonitride in the supernatant liquid being centrifugally separating to obtain
Electron microscope (SEM) image；
Fig. 2 is different content azotized carbon nano piece in experimental example 4, the nitridation that cellulose acetate (CA) is prepared as polymer
The TGA of carbon complex schemes.
Specific embodiment
The preparation of 1 azotized carbon nano piece of embodiment
Azotized carbon nano piece is prepared according to the following steps: nitridation carbon dust being placed in grinding pot, distillation is added thereto
Water closes the lid, then grinding pot is fixed on ball milling in ball mill；The revolving speed of the ball mill is 300rpm/min, when grinding
Between be 5h；Then distilled water flushing inner wall is added into grinding pot and obtains the suspension of carbonitride, by the suspension of this carbonitride
It is transferred to the lower sediment being centrifuged in centrifuge tube to collect, drying obtains the nitridation carbon dust of preliminary ball milling.At the beginning of taking 1g
The nitridation carbon dust of step ball milling is placed in bottle, and 100mL acetone is added thereto, tightens bottle cap, is sealed bottleneck and then is put in 100W
High power numerical control ultrasonic cleaner in 10~16h of ultrasound；Ultrasound terminates to obtain the suspension of carbonitride, by this carbonitride
Suspension is transferred in centrifuge tube and is centrifuged, and is centrifuged 15min at 3000rpm/min, and obtained upper layer dispersion liquid A is collected,
Upper layer dispersion liquid A is centrifuged again again, obtained upper layer dispersion liquid B is exactly azotized carbon nano piece solution, and azotized carbon nano piece is molten
The content of carbonitride is 0.12mg/mL in liquid.
The preparation of 2 azotized carbon nano piece of embodiment
Azotized carbon nano piece is prepared according to the following steps: nitridation carbon dust being placed in grinding pot, distillation is added thereto
Water closes the lid, then grinding pot is fixed on ball milling in ball mill；The revolving speed of the ball mill is 300rpm/min, and the time is
5h；Then distilled water flushing inner wall is added into grinding pot and obtains the suspension of carbonitride, the suspension of this carbonitride is shifted
The lower sediment being centrifuged into centrifuge tube collects, and drying obtains the nitridation carbon dust of preliminary ball milling.By the preliminary ball of 2g
The nitridation carbon dust of mill is placed in bottle, and 100mL acetone is added thereto, tightens bottle cap, is sealed bottleneck and then is put in the height of 100W
10~16h of ultrasound in power numerical control ultrasonic cleaner；Ultrasound terminates to obtain the suspension of carbonitride, by the suspension of this carbonitride
Liquid is transferred in centrifuge tube and is centrifuged, and is centrifuged 15min at 3000rpm/min, and obtained upper layer dispersion liquid A is collected, then
Upper layer dispersion liquid A is centrifuged again, and obtained upper layer dispersion liquid B is exactly azotized carbon nano piece solution, in azotized carbon nano piece solution
The content of carbonitride is 0.18mg/mL.
The preparation of 3 azotized carbon nano piece of embodiment
Azotized carbon nano piece is prepared according to the following steps: nitridation carbon dust being placed in grinding pot, distillation is added thereto
Water closes the lid, then grinding pot is fixed on ball milling in ball mill；The revolving speed of the ball mill is 300rpm/min, and the time is
5h；Then distilled water flushing inner wall is added into grinding pot and obtains the suspension of carbonitride, the suspension of this carbonitride is shifted
The lower sediment being centrifuged into centrifuge tube collects, and drying obtains the nitridation carbon dust of preliminary ball milling.By the preliminary ball of 3g
The nitridation carbon dust of mill is placed in bottle, and 100mL acetone is added thereto, tightens bottle cap, is sealed bottleneck and then is put in the height of 100W
10~16h of ultrasound in power numerical control ultrasonic cleaner；Ultrasound terminates to obtain the suspension of carbonitride, by the suspension of this carbonitride
Liquid is transferred in centrifuge tube and is centrifuged, and is centrifuged 15min at 3000rpm/min, and obtained upper layer dispersion liquid A is collected, then
The upper layer dispersion liquid B that upper layer dispersion liquid A is centrifuged again is exactly azotized carbon nano piece solution, nitrogen in azotized carbon nano piece solution
The content for changing carbon is 0.24mg/mL.
The preparation of the compound different amounts of nitridation carbon complex of embodiment 4
6 parts of cellulose acetates (CA) are taken, every part of cellulose acetate weight is 0.48g.6 parts of cellulose acetates are being stirred
In the lower 18.72mL acetone being dissolved under room temperature respectively, mixing time 2h, obtaining 6 parts of mass percents containing cellulose acetate is
2.5% cellulose acetate homogeneous phase solution.The content prepared in Example 1 is the azotized carbon nano piece solution of 0.12mg/mL,
The weight for making azotized carbon nano piece in azotized carbon nano piece solution is respectively 0,2.5mg, 5mg, 10mg, 20mg, 28mg, will be above-mentioned
Azotized carbon nano piece solution is mixed with cellulose acetate homogeneous phase solution respectively under ultrasound, ultrasonic 6h, obtains nitridation carbon complex
Solution, it is 60cm that carbonitride complex solution, which is poured on horizontal area,2Sheet glass on, degassing after be placed in again in baking oven do
It is dry to finally obtain nitridation carbon complex for 24 hours, wherein in each sample the mass percentage content of carbonitride be respectively 0,0.5%,
1%, 2%, 4%, 6%.Sample is denoted as CA-0, CA-0.5, CA-1, CA-2, CA-4, CA-6 respectively.
It can effectively avoid material during the formation of complexes with azotized carbon nano piece prepared by the method for acetone ultrasound
The problem of interface interaction unevenness between carbonitride and cellulose acetate.Simultaneously in acetone system azotized carbon nano piece surface-
NH2,-NH and surface of cellulose acetate hydroxyl, acetyl group can form strong hydrogen bond action well, to mention acetate fiber
The thermal stability of element.
By nitridation carbon complex obtained above, the sample of 5mg is taken to carry out heat to its thermal stability with thermal analyzer respectively
Weight analysis test, temperature test range is 50~700 DEG C, and heating rate is 10 DEG C/min, and carrier gas is air, and air velocity is
100mL/min has obtained the TGA figure of sample, as shown in Figure 2.It is compounded with the cellulose acetate thermostabilization of carbonitride as shown in Figure 2
Property than being significantly improved without the cellulose acetate of carbonitride, wherein at 50~200 DEG C of the initial period, the initial heat point of sample
Solution temperature increases 28.7 DEG C；Within 200~700 DEG C of this stages, the thermal decomposition temperature of the loss 60wt% of sample CA-1 is
559 DEG C, 258 DEG C of thermal decomposition temperature of the loss 60wt% than blank sample CA-0 improve 117%；The phase III 580~
700 DEG C, the carbon yield of sample is all higher than the carbon yield of CA-0.This shows that the compound of appropriate carbonitride can effectively improve acetic acid fibre
The thermal stability of element is tieed up, i.e. the cellulose acetate compound of carbonitride can be used as fire proofing material.
The preparation of the compound different amounts of nitridation carbon complex of embodiment 5
6 parts of polycarbonate are taken, every part of polycarbonate weight is 0.48g.6 parts of polycarbonate are dissolved in respectively under stiring
In 18.72mL chloroform under room temperature, jitter time 2h obtains the polycarbonate that mass percent containing polycarbonate is 2.5%
Homogeneous phase solution.The content prepared in Example 1 is the azotized carbon nano piece solution of 0.12mg/mL, keeps azotized carbon nano piece molten
The weight of azotized carbon nano piece is respectively 0,2.5mg, 5mg, 10mg, 20mg, 28mg in liquid.By above-mentioned azotized carbon nano piece solution
It is mixed under ultrasound with polycarbonate homogeneous phase solution, 6h is stirred by ultrasonic, obtains carbonitride complex solution, carbon complex will be nitrogenized
Solution is poured on horizontal 60cm2On sheet glass, drying in baking oven is placed in after degassing again and for 24 hours, finally obtains nitridation carbon complex,
Wherein the mass percentage content of carbonitride is respectively 0,0.5%, 1%, 2%, 4%, 6% in each sample.Thermogravimetric analysis table
The compound thermal stability that can effectively improve polycarbonate of bright appropriate carbonitride, the i.e. polycarbonate compound of carbonitride can be with
As fire proofing material.
The preparation of the compound different amounts of nitridation carbon complex of embodiment 6
6 parts of polypropylene are taken, every part of polypropylene weight is 0.48g.6 parts of polypropylene are dissolved under room temperature respectively under stiring
18.72mL benzene in, jitter time 2h, obtain mass percent containing polypropylene be 2.5% polypropylene homogeneous phase solution.Take reality
The azotized carbon nano piece solution that the content prepared in example 1 is 0.12mg/mL is applied, azotized carbon nano in azotized carbon nano piece solution is made
The weight of piece is respectively 0,2.5mg, 5mg, 10mg, 20mg, 28mg.By above-mentioned azotized carbon nano piece solution with poly- third under ultrasound
The mixing of alkene homogeneous phase solution, ultrasonic 6h obtain carbonitride complex solution, carbonitride complex solution are poured on to horizontal 60cm2
On sheet glass, drying in baking oven is placed in after degassing again and for 24 hours, nitridation carbon complex is finally obtained, wherein nitrogenizing in each sample
The mass percentage content of carbon is respectively 0,0.5%, 1%, 2%, 4%, 6%.Thermogravimetric analysis shows the compound of appropriate carbonitride
It can effectively improve polyacrylic thermal stability, i.e. the polypropylene composite of carbonitride can be used as fire proofing material.
Claims (5)
1. a kind of nitridation carbon complex, which is characterized in that the nitridation carbon complex is answering for azotized carbon nano piece and polymer
Object is closed, mass ratio shared by carbonitride is 0.5%~10% in the nitridation carbon complex；
The preparation method of the azotized carbon nano piece the following steps are included:
(1) nitridation carbon dust is ground, then plus water obtains the suspension of carbonitride；
(2) suspension of the carbonitride obtained to step (1) is centrifuged, and collects lower sediment, dry, obtains preliminary ball milling
Nitrogenize carbon dust；
(3) acetone is added into the nitridation carbon dust of the preliminary ball milling, ultrasound carries out the suspension that ultrasound obtains carbonitride
Upper layer dispersion liquid A is collected in centrifugation；
(4) the upper layer dispersion liquid A that step (3) obtains is centrifuged again and obtains upper layer dispersion liquid B, the upper layer dispersion liquid B is
Azotized carbon nano piece solution；
The polymer is one of cellulose acetate, polyvinyl alcohol, polyamide or a variety of；
The preparation method of the described nitridation carbon complex the following steps are included:
(1) it dissolves a polymer in solvent, obtains uniform solution, this solution is mixed with azotized carbon nano piece, ultrasound obtains
Mixture；The solvent is acetone；
(2) mixture that step (1) obtains is poured in horizontal container, dries, obtains carbonitride complex thin film.
2. nitridation carbon complex according to claim 1, which is characterized in that in step (1), grinding be in the ball mill into
Capable, the revolving speed of ball mill is 20~2000rpm/min, and Ball-milling Time is 0.1~12h.
3. it is a kind of prepare it is described in claim 1 nitridation carbon complex method, which is characterized in that the preparation method include with
Lower step:
(1) it dissolves a polymer in solvent, obtains uniform solution, this solution is mixed with azotized carbon nano piece, ultrasound obtains
Mixture；The solvent is acetone；
(2) mixture that step (1) obtains is poured in horizontal container, dries, obtains carbonitride complex thin film.
4. according to the method described in claim 3, it is characterized in that, the ultrasonic power be 60~100W, ultrasonic time be 6~
16 hours.
5. application of the nitridation carbon complex described in claim 1 in terms of high thermal stability material, fire proofing material.
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