CN109019616A - A kind of preparation and application of silica/molybdenum disulfide three-dimensional hybrid material - Google Patents
A kind of preparation and application of silica/molybdenum disulfide three-dimensional hybrid material Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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Abstract
The invention discloses a kind of molybdenum disulfide nanos to spend the preparation and application in situ for loading extra small functionalized SiO 2 nano particle hybridization material, belongs to inorganic nano hybrid material preparation field.The method of the present invention is prepared for three layers of atom of one kind and forms the molybdenum disulfide similar to the layer structure of sandwich as carrier, the method in situ for loading extra small functionalized SiO 2 nanoparticle, construct a kind of hybrid material fire retardant of silica/molybdenum disulfide three-dimensional structure, the fire retardant is made of nano SiO 2 particle uniform load to molybdenum disulfide nano flower, preparation process is simple, green high-efficient, wherein the molybdenum disulfide similar to sandwich layer structure is a kind of nanometer flower structure, instead of traditional nanometer chip architecture, stereochemical structure, space is big, the load capacity of nanometer titanium dioxide silicon nano can be effectively increased, and improve the flame retarding efficiency of Hybrid fire retardant, the compatibility and mechanics enhancement effect of matrix.
Description
Technical field
The present invention relates to a kind of silica/molybdenum disulfide three-dimensional hybrid material preparations and application, belong to inorganic nano
Hybrid material preparation field.
Background technique
In recent years, all kinds of civilian, decoration use and industrial yarn and non-woven cloth application field rapid expansions, become day
Often life and the indispensable part of industrial production.However, these materials itself have flammable properties, easily drawn by external heat source
Combustion, and discharge a large amount of heat, flue gas in combustion and have poison gas, serious threat to life property safety, according to statistics, China
Size fire every year on average can all cause 500,000,000 yuan or more of loss to society, and be caused tight by the inflammable of fibre
Weight fire just accounts for more than half.The fire retardant for developing high-performance, low dosage is the added value and safety for improving fibre
Property, so that it is not easy ignition or a kind of effective ways of burning velocity can be slowed down.
Fire retardant can be divided into organic fire-retardant and inorganic fire retardants by chemical structure.Organic based flame retardant include machine phosphorus,
Nitrogen, boron flame retardant, when being added in material matrix, the based flame retardant is there are dosage big (> 20%), compatibility is poor, no
Environmental protection, the problems such as thermal stability is poor；When reacting with fibrous material, the drop of its mechanical property, wash durability etc. is easily caused
It is low.Inorganic based flame retardant mainly has metal hydrate, red phosphorus, boron compound, antimony class compound etc., and especially silica is received
Rice corpuscles has the characteristics that thermal stability is good, non-volatile, effect is lasting, cheap compared to organic fire-retardant, however
Metal hydroxides is since polarity is big, and high molecular material poor compatibility, and additive amount is big in use, can greatly
Deteriorate the physical property of material.
Inorganic nano material due to it with excellent gas barrier property, excellent heat stability, additive amount be few, green ring
It protects, and the negative effect of the mechanical property and thermal stability to matrix is smaller, or even can also play enhancement effect, it has also become
The new lover of flame retardant area.Molybdenum disulfide has relatively low thermal conductivity and high-melting-point as a kind of emerging fire proofing
(1185 DEG C), can effectively inhibit the infiltration of outside heat and oxygen and the release of noxious material, and molybdenum atom can also catalysis matrix shape
At a large amount of carbon-coatings to reduce heat exchange.But the flame retarding efficiency for depending merely on molybdenum disulfide is limited, it is often in polymeric matrix
In show serious aggregation, weaken the interfacial interaction of molybdenum disulfide and matrix.
In order to improve the flame retarding efficiency and interfacial interaction of molybdenum disulfide, domestic and foreign scholars are to molybdenum disulfide inorganic hybridization
Cooperative flame retardant is studied, such as: XiamingFeng in 2014 is in " Journal of Materials Chemistry A "
It delivers for 13299-13308 pages of volume 2 and molybdenum disulfide/hydroxy cobalt oxide (MoS2/CoOOH) hydridization material is prepared by in-situ synthesis
Material, can significantly improve the thermal stability of epoxy resin and reduce the release of CO.Dong Wang in 2016 etc. is in " ACS Applied
Materials&Interfaces " 34735-34743 pages of volume 8 deliver molybdenum disulfide nano sheet/graphene hybrid material and be used for
Unsaturated polyester (UP) it is fire-retardant, reached preferable cooperative flame retardant effect.H é lioRibeiro in 2017 etc. is in " ACS Applied
Materials &Interfaces " deliver molybdenum disulfide/hexagonal nanometer boron nitride hybrid for ethoxyline resin antiflaming, effectively
Improve its thermal stability.Silica has the advantages that environmental protection, nontoxic, can improve material as a kind of inorganic nano fire retardant
The thermal stability of material and the stability of carbon-coating.Currently, Keqing Zhou is at " Journal of Hazardous Materials "
Molybdenum disulfide nano sheet/silicon dioxide hybrid materials are reported for 1078-1089 pages of volume 344 (2018) for flame retardant epoxy tree
The research of rouge, but active site contained by molybdenum disulfide nano sheet is less in the hybrid material, and silica partial size is big and uneven
(150nm), so that silicon dioxide carried amount is low, pattern is difficult to control, and flame retardant effect is not significant.
Above-mentioned document is all to prepare nano-hybrid material by substrate of molybdenum disulfide nano sheet, and sheet layer material is easy to stack,
Poor dispersion, active reaction sites (sulphur defect, vacancy, edge site) are less, specific surface area and can load area it is smaller,
It is difficult to reach effective preparation of more defects, high load amount and morphology controllable molybdenum disulfide Hybrid fire retardant, flame retarding efficiency is difficult to reach
To maximization.
Summary of the invention
It to solve the above-mentioned problems, is that flame retarding efficiency realizes maximization, the present invention devises a kind of three layers of atom formation classes
Like sandwich layer structure molybdenum disulfide as carrier, the side in situ for loading extra small functionalized SiO 2 nanoparticle
Method, constructs a kind of silica/molybdenum disulfide three-dimensional hybrid material fire retardant, and the fire retardant is equal by nano SiO 2 particle
The even molybdenum disulfide nano flower that loads to is constituted, and preparation process is simple, green high-efficient, wherein similar to two sulphur of sandwich layer structure
Changing molybdenum is a kind of nanometer flower structure, and instead of traditional nanometer chip architecture, stereochemical structure, space is big, can effectively increase nanometer two
The load capacity of silicon oxide nanoparticle, and improve the flame retarding efficiency of Hybrid fire retardant, the compatibility of matrix and mechanics enhancement effect.
The first purpose of the invention is to provide a kind of silica/molybdenum disulfide three-dimensional hybrid material preparation method,
The described method includes: molybdenum source and sulphur source are utilized hydrothermal synthesis of carbon/molybdenum disulfide nano flower, then by obtained molybdenum disulfide
Nano flower as substrate, with silicon source, the silane coupling agent containing sulfydryl by chemical bond it is bonded, the extra small silica of fabricated in situ is received
Rice corpuscles simultaneously take to molybdenum disulfide nano by uniform load, obtains silica/molybdenum disulfide three-dimensional hybrid material.
In one embodiment of the present invention, the molybdenum source includes Ammonium Molybdate Tetrahydrate, sodium molybdate, one in molybdenum oxide
Kind.
In one embodiment of the present invention, the sulphur source includes one of thiocarbamide, thioacetamide, sodium sulfocyanate.
In one embodiment of the present invention, the additive amount mass fraction ratio of the molybdenum source and sulphur source is (1~1.5):
(2~3).
In one embodiment of the present invention, the silicon source includes one of tetraethyl orthosilicate, sodium metasilicate.
In one embodiment of the present invention, the silane coupling agent containing sulfydryl includes γ-mercapto propyl-triethoxysilicane
Alkane (KH580), one of (3- mercaptopropyi) trimethoxy silane (KH590).
In one embodiment of the present invention, the silicon source, the additive amount volume ratio of silane coupling agent containing sulfydryl are (2
~4): (0.5~1.5).
In one embodiment of the present invention, the colored mass volume ratio with silicon source of the molybdenum disulfide nano be (0.1~
0.2): (2~4).
In one embodiment of the present invention, the partial size of the molybdenum disulfide nano flower is 100-200nm.
In one embodiment of the present invention, the partial size of the extra small Nano particles of silicon dioxide is 10-15nm.
In one embodiment of the present invention, the method specifically comprises the following steps:
(1) molybdenum source, sulphur source are added in deionized water and are dissolved, stirred wiring solution-forming, be transferred to hydro-thermal after ultrasonic mixing is uniform
In kettle, 160~240 DEG C of reactions 8~for 24 hours, deionized water eccentric cleaning, 60 DEG C of drying obtain molybdenum disulfide nano flower.
(2) flower of molybdenum disulfide nano obtained in a small amount of step (1) is taken, in deionized water, silicon source is added in ultrasonic disperse,
Adjust pH=8-10.5,40~65 DEG C, 400~600rpm, reaction 12~for 24 hours, add the silane coupling agent containing sulfydryl, continue
React 8~12h.Ethyl alcohol and deionized water alternating centrifugal clean, and 60 DEG C of vacuum drying obtain molybdenum disulfide nano and spend load in situ
The molybdenum disulfide three-dimensional hybrid material of extra small functionalized SiO 2.
A second object of the present invention is to provide a kind of silica/molybdenum disulfide three being prepared using the above method
Tie up hybrid material.
Third object of the present invention is to provide a kind of flame-resistant polyacrylonitrile fiber, the flame-resistant polyacrylonitrile fiber be by
Above-mentioned silica/molybdenum disulfide three-dimensional hybrid material is added in polyacryl-nitrile spinning fluid, and wet spinning can be obtained.
Fourth object of the present invention is that above-mentioned silica/molybdenum disulfide three-dimensional hybrid material is applied to flame retardant area
In.
The invention has the advantages that:
The present invention utilizes raw material cheap and easy to get, prepares molybdenum disulfide nano flower by reaction in-situ and loads extra small titanium dioxide
Silicon nano, low in cost, reaction process is simple, morphology controllable is strong, and molybdenum disulfide nano flower reactivity site is more, compares
Surface area is big, and the silica partial size of load is small and uniform, load capacity is more, surface is without other groups.The material structure is uniform, shape
Looks are excellent, have excellent performance, and have good cooperative flame retardant effect for flame retardant area, flame retarding efficiency is high；Nanometer is improved simultaneously
Fire retardant compatibility makes the compatibility of matrix and mechanics enhancement effect be greatly improved.
Detailed description of the invention
Fig. 1 is the SEM figure of molybdenum disulfide nano flower；
Fig. 2 is that the TEM of Nano particles of silicon dioxide schemes；
Fig. 3 is silica/molybdenum disulfide three-dimensional hybrid material TEM figure；
Fig. 4 is silica/molybdenum disulfide three-dimensional hybrid material SEM figure；
Fig. 5 is silica/molybdenum disulfide three-dimensional hybrid material XRD diagram；
Fig. 6 is silica/molybdenum disulfide three-dimensional hybrid material XPS figure；
Fig. 7 is that the SEM of flame-resistant polyacrylonitrile fiber schemes；
Fig. 8 is that the TGA of flame-resistant polyacrylonitrile fiber schemes；
Fig. 9 is the heat release rate figure of flame-resistant polyacrylonitrile fiber；
Figure 10 is the heat release rate figure of flame-resistant polyacrylonitrile fiber.
Specific embodiment
Particular content of the invention is described as follows combined with specific embodiments below:
Embodiment 1
The preparation of silica/molybdenum disulfide three-dimensional hybrid material: 1.28g Ammonium Molybdate Tetrahydrate, 2.3g thiocyanic acid are weighed
Sodium is dissolved in 40mL deionized water, is then transferred in 100mL water heating kettle, 220 DEG C of reaction 10h in Muffle furnace.Use deionized water
Three times, 60 DEG C of drying obtain molybdenum disulfide nano flower to eccentric cleaning.0.2g molybdenum disulfide nano flower is weighed, ultrasonic disperse exists
In 100mL deionized water, 4mL tetraethyl orthosilicate is then added, adjusts pH=9.7 with ammonium hydroxide, 60 DEG C, 550rpm reacts for 24 hours,
1.5mL (3- mercaptopropyi) trimethoxy silane is added, the reaction was continued 12h.Solution ethyl alcohol and deionized water after reaction
Alternately three times, 60 DEG C of vacuum drying obtain molybdenum disulfide nano and spend the extra small functionalized SiO 2 nanoparticle of load in situ for cleaning
Sub- hybrid material.
The pattern of obtained molybdenum disulfide nano flower is as shown in Figure 1, its diameter is 100-200nm；Silica
Nanosphere is as shown in Fig. 2, the diameter of silicon dioxide nanosphere is 10~15nm, and uniform in size, nothing is obvious to reunite；Two
A large amount of silica are successfully supported on molybdenum disulfide nano flower piece layer to silica/molybdenum disulfide three-dimensional hybrid material as can be seen from Figure 3
Centre increases its interlamellar spacing；The silica that size is 10-15nm or so is uniformly modified to be taken in molybdenum disulfide nano,
Three-dimensional hierarchical structure is presented, shows excellent structural stability (Fig. 4), as can be seen from Figure 5, in addition to molybdenum disulfide nano flower
Characteristic diffraction peak, hybrid material occur the strong characteristic peak of a new silica at 23 °, show that the success of silica is negative
It carries；Compared to pure molybdenum disulfide nano flower, sulphur (14.27%), molybdenum element (6.74%) content are lower in hybrid material, silicon
(25.24%), high level (constituent content is shown in Table 1) is presented in oxygen element (53.75%), shows a large amount of loads of silica
(Fig. 6).Specific constituent content is as shown in table 1 in molybdenum disulfide nano flower and hybrid material:
The constituent content of 1 molybdenum disulfide nano of table flower and hybrid material
The preparation of flame-resistant polyacrylonitrile fiber: it weighs 0.06g molybdenum disulfide nano and spends the extra small functionalization dioxy of load in situ
SiClx nano particle hybridization material, ultrasonic disperse add 3g polyacrylonitrile powder in 15g n,N-Dimethylformamide (DMF)
End, 80 DEG C of dissolution 8h, obtained spinning solution are placed in 2h in 60 DEG C of vacuum drying ovens, carry out deaeration processing.With TYD01 spinning syringe pump
Carry out spinning, spinning parameter are as follows: 10 μ L min of speed-1, aqueous solution (the DMF content of syringe needle internal diameter 0.3mm, coagulating bath DMF
60%).The 60 DEG C of dryings of obtained polyacrylonitrile fibre for 24 hours, obtain flame-resistant polyacrylonitrile fiber.
As seen from Figure 7, the fibre section hole of obtained flame-resistant polyacrylonitrile fiber is less, gully shape crackle compared with
Short, hybrid material is evenly distributed in fibrous matrix, schemes (Fig. 8) it is found that polypropylene flame redardant according to the TGA of flame-resistant polyacrylonitrile fiber
The temperature (311.8 DEG C) and remaining carbon (58.7%) of nitrile fiber quality loss 10% are (respectively compared to virgin pp nitrile fiber
It 300.5 DEG C and 50.5%) is greatly improved；Flame-resistant polyacrylonitrile fiber maximum heat release rate (98.27W/g) is poly- compared to pure
Dralon (182.4W/g) reduces 46.1% (Fig. 9)；Flame-resistant polyacrylonitrile fiber total heat release (19.9kJ/g) phase
Than reducing 25.2% (Figure 10) in virgin pp nitrile fiber (26.6kJ/g).
Embodiment 2
1.28g Ammonium Molybdate Tetrahydrate is weighed, 2.3g sodium sulfocyanate is dissolved in 40mL deionized water, is then transferred to 100mL
In water heating kettle, 220 DEG C of reaction 10h in Muffle furnace.Three times with deionized water eccentric cleaning, 60 DEG C of drying obtain molybdenum disulfide nano
Flower.0.8g molybdenum disulfide nano flower is weighed, then 2mL tetraethyl orthosilicate is added in 100mL deionized water in ultrasonic disperse,
PH=9.7 is adjusted with ammonium hydroxide, 60 DEG C, 550rpm reacts for 24 hours, adds 0.5mL (3- mercaptopropyi) trimethoxy silane, continues anti-
Answer 12h.Alternately three times, 60 DEG C of vacuum drying obtain molybdenum disulfide nano for cleaning for solution ethyl alcohol and deionized water after reaction
Spend the extra small functionalized SiO 2 nano particle hybridization material of load in situ.
Sulfur-bearing (35.3%), molybdenum element (16.7.7%) in obtained silica/molybdenum disulfide three-dimensional hybrid material,
And silicon (16.1%), oxygen element (31.9%), load capacity are preferable, but compared to slightly worse in embodiment 1, show silicon source and coupling agent
Dosage have a certain impact to silicon dioxide carried amount.
The flame-resistant polyacrylonitrile fiber being prepared using the method in embodiment 1: remaining carbon 58.8%, maximum heat release
Rate 102.3W/g, total heat release 20.2kJ/g, flame retardant effect are met the requirements, but more slightly worse than in embodiment 1, illustrate titanium dioxide
Silicon load capacity has certain influence to the flame retardant property of fiber.
Embodiment 3
1.28g Ammonium Molybdate Tetrahydrate is weighed, 2.3g sodium sulfocyanate is dissolved in 40mL deionized water, is then transferred to 100mL
In water heating kettle, 220 DEG C of reaction 10h in Muffle furnace.Three times with deionized water eccentric cleaning, 60 DEG C of drying obtain molybdenum disulfide nano
Flower.0.8g molybdenum disulfide nano flower is weighed, then 4mL tetraethyl orthosilicate is added in 100mL deionized water in ultrasonic disperse,
PH=9.7 is adjusted with ammonium hydroxide, 40 DEG C, 550rpm reacts for 24 hours, adds 1.5mL (3- mercaptopropyi) trimethoxy silane, continues anti-
Answer 12h.Alternately three times, 60 DEG C of vacuum drying obtain molybdenum disulfide nano for cleaning for solution ethyl alcohol and deionized water after reaction
Spend the extra small functionalized SiO 2 nano particle hybridization material of load in situ.
Sulfur-bearing (28.2%), molybdenum element (14.3%) in obtained silica/molybdenum disulfide three-dimensional hybrid material, and
Silicon (18.7%), oxygen element (38.8%), illustrate that temperature has a certain impact to the formation of silica and load capacity.
The flame-resistant polyacrylonitrile fiber being prepared using the method in embodiment 1: remaining carbon 59.1%, maximum heat release
Rate 100.1W/g, total heat release 20.7kJ/g.
Material element content in hybrid material obtained by 2 embodiment 1-3 of table
Flame retardant property in 3 embodiment 1-3 obtained flame-retardant material of table
By table 2-3 it is found that the silicon source in loading process, coupling agent dosage and temperature all have larger shadow to the performance of material
It rings.
Comparative example 1
Silica nanometer flower preparation flame-resistant polyacrylonitrile fiber:
It weighs the molybdenum disulfide nano that 0.06g is implemented in 1 to spend, ultrasonic disperse is at 15g n,N-Dimethylformamide (DMF)
In, 3g polyacrylonitrile powder, 80 DEG C of dissolution 8h are added, obtained spinning solution is placed in 2h in 60 DEG C of vacuum drying ovens, carries out deaeration
Processing.Spinning, spinning parameter are carried out with TYD01 spinning syringe pump are as follows: 10 μ L min of speed-1, syringe needle internal diameter 0.3mm, coagulating bath
The aqueous solution (DMF content 60%) of DMF.The 60 DEG C of dryings of obtained polyacrylonitrile fibre for 24 hours, obtain flame-resistant polyacrylonitrile fiber.
Obtained flame-resistant polyacrylonitrile fiber correlation performance parameters are as shown in table 4,5: remaining carbon 54.4%, maximum heat is released
Rate 126.4W/g is put, total heat release 21.8kJ/g is inferior to hydridization fire resistance fibre.
Comparative example 2
Silicon dioxide nanosphere prepares flame-resistant polyacrylonitrile fiber:
Weigh 0.06g silicon dioxide nanosphere, ultrasonic disperse in 15g n,N-Dimethylformamide (DMF), then plus
Enter 3g polyacrylonitrile powder, 80 DEG C of dissolution 8h, obtained spinning solution is placed in 2h in 60 DEG C of vacuum drying ovens, carries out deaeration processing.With
TYD01 spinning syringe pump carries out spinning, spinning parameter are as follows: 10 μ L min of speed-1, syringe needle internal diameter 0.3mm, the water of coagulating bath DMF
Solution (DMF content 60%).The 60 DEG C of dryings of obtained polyacrylonitrile fibre for 24 hours, obtain flame-resistant polyacrylonitrile fiber.
Using the obtained flame-resistant polyacrylonitrile fiber correlation performance parameters of method in embodiment 1 as shown in table 4,5: residual
Carbon amounts 51.3%, maximum heat release rate 171.1W/g, total heat release 22.5kJ/g are slightly better than virgin pp nitrile fiber, bad
In hydridization fire resistance fibre.
Comparative example 3
Silica nanometer piece prepares flame-resistant polyacrylonitrile fiber:
0.1g molybdenum disulfide nano sheet is weighed, then the positive silicic acid of 3.8mL is added in 100mL deionized water in ultrasonic disperse
Tetra-ethyl ester adjusts pH=9.7 with ammonium hydroxide, and 60 DEG C, 550rpm reacts for 24 hours, adds 1.5mL (3- mercaptopropyi) trimethoxy silicon
Alkane, the reaction was continued 12h.Alternately three times, 60 DEG C of vacuum drying obtain two sulphur for cleaning for solution ethyl alcohol and deionized water after reaction
Change molybdenum nanometer sheet nonloaded silica nano particle hybridization material.
Obtained silica/molybdenum disulfide hybrid material: sulfur-bearing (54.3%), molybdenum element (25.7%), and silicon
(6.1%), oxygen element (13.9%) content is lower, shows that the silica loaded on molybdenum disulfide nano sheet is few.
The flame-resistant polyacrylonitrile fiber correlation performance parameters being prepared using the method in embodiment 1 are as shown in table 4,5:
Remaining carbon 53.1%, maximum heat release rate 134.8W/g, total heat release 23.5kJ/g are inferior to three-dimensional manometer flower/titanium dioxide
Silicon hybridization fire resistance fibre.
The constituent content of 4 comparative example 1-3 resulting materials of table
Flame retardant property in 5 comparative example 1-3 obtained flame-retardant material of table
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclosing subject to the definition of the claims.
Claims (10)
1. a kind of silica/molybdenum disulfide three-dimensional hybrid material preparation method, which is characterized in that the method is by molybdenum source
Hydrothermal synthesis of carbon/molybdenum disulfide nano flower is utilized with sulphur source, then obtained molybdenum disulfide nano flower is regard as substrate, with silicon
Source, the silane coupling agent containing sulfydryl are bonded by chemical bond, and the extra small Nano particles of silicon dioxide of fabricated in situ simultaneously loads to two sulphur
Change on molybdenum nano flower, obtains silica/molybdenum disulfide three-dimensional hybrid material.
2. method according to claim 1, which is characterized in that the additive amount mass fraction ratio of the molybdenum source and sulphur source is (1
~1.5): (2~3).
3. method according to claim 1, which is characterized in that the additive amount body of the silicon source, silane coupling agent containing sulfydryl
Product is than being (2~4): (0.5~1.5).
4. method according to claim 1, which is characterized in that the molybdenum disulfide nano flower and the mass volume ratio of silicon source are
(0.1~0.2): (2~4).
5. method according to claim 1, which is characterized in that the Nano particles of silicon dioxide loads to molybdenum disulfide nano
Reaction temperature when flower is 40~65 DEG C.
6. method according to claim 1, which is characterized in that the molybdenum source includes Ammonium Molybdate Tetrahydrate, sodium molybdate, molybdenum oxide
One of；The sulphur source includes one of thiocarbamide, thioacetamide, sodium sulfocyanate.
7. method according to claim 1, which is characterized in that the silane coupling agent containing sulfydryl includes 3- mercapto propyl front three
Oxysilane, gamma-mercaptopropyltriethoxysilane, one of γ-mercaptopropyl trimethoxysilane.
8. the silica being prepared using any the method for claim 1~7/molybdenum disulfide three-dimensional hybrid material.
9. a kind of flame-resistant polyacrylonitrile fiber, which is characterized in that the flame-resistant polyacrylonitrile fiber is using described in claim 8
Silica/molybdenum disulfide three-dimensional hybrid material be prepared.
10. silica according to any one of claims 8/application of the molybdenum disulfide three-dimensional hybrid material in flame retardant area.
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| CN115181407A (en) * | 2022-08-15 | 2022-10-14 | 万华化学（宁波）有限公司 | Halogen-free flame-retardant low-smoke-density polycarbonate material and preparation method and application thereof |
| CN115181407B (en) * | 2022-08-15 | 2023-12-19 | 万华化学（宁波）有限公司 | Halogen-free flame-retardant low-smoke-density polycarbonate material and preparation method and application thereof |
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Application publication date: 20181218 |