CN104829860B - A kind of melamine cyanurate and montmorillonite nano complex and preparation method thereof - Google Patents
A kind of melamine cyanurate and montmorillonite nano complex and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of melamine cyanurate and montmorillonite nano complex and preparation method thereof, belong to technical field of nano material.1 part of montmorillonite and 20~200 parts of solvents are added in reaction vessel, the temperature for controlling reaction vessel is room temperature~120 DEG C, 0~10h of insulated and stirred；0.05~20 part of melamine is added in course of reaction, insulation reaction adds the mixture of 0.05~20 part of cyanuric acid and urea afterwards for a period of time, and insulation reaction is cooled to room temperature afterwards for a period of time；Reaction resulting material is separated using suction filtration, centrifugation or revolving, products therefrom is repeatedly washed with distilled water, ethanol, then drying, grinding, sieving, acquisition melamine cyanurate and montmorillonite nano complex.The reaction condition of the present invention is gently stablized, reproducible, and yield is high, is adapted to the production of expansion property；And the nano-complex can improve many performances such as the fire-retardant of polymer, high temperature resistant, water absorption resistance, mechanics.
Description
Technical field
The present invention relates to a kind of melamine cyanurate and montmorillonite nano complex and preparation method thereof, belong to nanometer
Field of material technology.
Background technology
Melamine cyanurate (melamine cyanurate, MCA) also known as melamine cyanurate salt, are a kind of white
The crystalloid attritive powder of color, there is soapy feeling, and molecular formula is C6H9N9O3,1.5~1.6g/cm3 of density, odorless, tasteless, indissoluble
In water and other organic solvents, faintly acid, less than 350 DEG C chemical property are stable.Melamine cyanurate is a kind of important
Nitrogenated flame retardant, has the advantages that nitrogen content height, Halogen, low cigarette, low toxicity, low-corrosiveness, and good, fire-retardant with resin compatible
Efficiency high, available in multiple polymers material, the polyamide that is particularly suitable for use in (such as nylon 6, nylon66 fiber) material it is flame-retardant modified.
Melamine cyanurate is formed by melamine and cyanuric acid molecule by Hydrogenbond, specific production
Technique mainly has following three kinds by the difference from initial feed：1st, cyanuric acid method, by the melamine and cyanogen of certain mol proportion
Uric acid is placed in water to form suspension, and a few hours are reacted under certain temperature, when continuing to react one section after slurry substantially becomes viscous
Between, then through filtering, washing, dry, it is broken obtain finished product, mother liquor is recyclable to be recycled.Need to add largely in this technique
Water, to reduce the viscosity that reaction system constantly increases, therefore solvent method can also be referred to as.The letter of solvent method processing technology
Single, reaction speed is fast, and product purity is high, but production process needs to consume a large amount of water and big volume device, therefore production efficiency is reduced.
2nd, urea method, is typically to add melamine while urea pyrolysis generates cyanuric acid to be reacted, or by urea and trimerization
Cyanamide together adds carry out heat fusing, and single step reaction generates melamine cyanurate crude product, then is boiled through acid, wash, dry
Process is refining to obtain product.This method raw material is cheap and easy to get, production cost is low, good in economic efficiency, but gained is produced after frit reaction
Thing purity is low (generally 80%-85%), need to be washed with more than ten times of amount boiling water, or the melamine not reacted is removed with pickling
Amine, cyanuric acid and urea derivative, are related to a large amount of waste water handling problems.3rd, high-temperature melting method, course of reaction does not introduce any molten
Agent, therefore solid process can be referred to as.In solid process preparation technology, raw material melamine and cyanuric acid are subjected to superfine powder first
It is broken, then under the high temperature conditions (more than 300 DEG C) directly frit reaction to generate the melamine cyanurate that yield is high.By
In that need not introduce solvent, the technological process of preparation is simplified, but volatility of raw material loss is in 10% or so, yield during reaction
Reduction.
In addition, it is proposed that some new melamine cyanurate preparation methods, such as a kind of hydro-thermal method synthesize nanometer
The method (patent No. ZL201210230199.8) of level melamine cyanurate, bar-shaped crystal formation trimeric-cyanamide cyanurate fire-retardant
Agent and preparation method thereof (patent No. ZL201110029371.9) and a kind of system of the wide distribution melamine cyanurate of big particle diameter
Preparation Method (patent No. ZL201210066842.8) etc., its advantage, which is concentrated on, improves product raising matrix after polymer is added
In mechanical property, but its production process still suffer from it is all such as the problem of in above-mentioned traditional processing technology.
Montmorillonite (MMT) is the hydrosilicate clay that a class has layer structure, and its frame sheet is nanoscale,
Each about 1 nanometer of piece thickness, negative electricity is carried by what the silicon-oxy tetrahedron positioned at middle alumina octahedral and positioned at both sides was constituted
The silicate lamella of lotus, the counter cation balancing charge (such as H+, Na+, K+, Ca2+, Mg2+ etc.) through interlayer, one kind of formation
Natural sandwich construction clay.Silicon in silicon-oxy tetrahedron can be replaced by aluminium, the aluminium in alumina octahedral can by magnesium, iron,
Zinc, lithium, the displacement of chromium plasma.Water and effect due to interlayer cation, montmorillonite can be stably dispersed in water, its interlayer sun
Ion can carry out ion exchange with outside organic and inorganic cation.The spacing of montmorillonite silicate plate interlayer is because of cation
Species it is different and different, in 1 to 2 ran.
Montmorillonite is unfavorable for its point in organic phase because showing as hydrophilic and oleophobic property interlayer has a large amount of inorganic cations
Dissipate and the absorption to organic substance.In order that montmorillonite has more preferable compatibility with organic phase, replaced and covered with organic cation
De- soil (referring generally to sodium-based montmorillonite) interstitial inorganic cations, to change the cationic form of montmorillonite crystal layer, dredge its surface
Aquation, and with preferable expansion character, form organic modification montmonrillonite.By organically-modified, the interface of inorganic matter is improved
Polarity and chemical micro-environment, add two alternate compatibilities, and the big layer of larger organic molecule and group can be received by foring
The compound of spacing.After organic modification montmonrillonite and polymer are by appropriate blending, polymer enters between cheating engaging layer, makes layer
Spacing expands, and forms the nano composite polymer-montmorillonoid material of intercal type；When polymer enters the silicate lamella of montmorillonite
When one step expands, the degree of stripping is reached, exfoliated nano composite polymer-montmorillonoid material is formed；If montmorillonite with
Polymer can not be compatible, then form the micro-composites of polymer-montmorillonoid.In recent years, polymer/laminated silicate clay
Nano composite material is rapidly growing as a kind of novel high-performance fire proofing, and the addition of montmorillonite can improve the fire-retardant of polymer
Performance, mechanical property and some other practical performance, and have low cigarette, nontoxic, environmentally friendly etc. excellent during the burning of this kind of fire proofing
Point.
The content of the invention
A kind of melamine cyanurate is proposed the invention aims to solve the problem of prior art is present
With montmorillonite nano complex and preparation method thereof.
The melamine cyanurate and montmorillonite nano complex of the present invention, due to adding for melamine cyanurate
Enter, its intercalation is entered between the lamella of montmorillonite, the interlamellar spacing of montmorillonite expands, and the montmorillonite of addition reaches the shape of stripping
State, substantially uniformity is separated into the lamellar structure of nanoscale, so as to obtain the nano-complex of the two.
The purpose of the present invention is achieved through the following technical solutions.
The present invention a kind of melamine cyanurate and montmorillonite nano complex, be by melamine cyanurate with
Montmorillonite reaction is prepared from, and its mass percent is：Melamine cyanurate 5%-95%, montmorillonite 95%-5%.
A kind of melamine cyanurate of the present invention and the preparation method of montmorillonite nano complex, its specific prepares walk
It is rapid as follows：
1) montmorillonite and solvent are added in reaction vessel, stirred, heating is reacted, control the temperature of reaction vessel
For room temperature~120 DEG C, the heat time is 0~10h, obtains reaction solution；
2) be directly added into melamine or melamine be previously dissolved in solvent, be then added to step 1) obtain it is anti-
Answer in liquid, stir, controlling reaction temperature is room temperature~120 DEG C, insulation reaction 0-10h obtains reaction solution；
3) mixture of cyanuric acid and urea is directly added into step 2) in obtained reaction solution, or by cyanuric acid and urine
The mixture of element is previously dissolved in solvent, is then added to step 2) in obtained reaction solution, stirring, controlling reaction temperature is room temperature
~120 DEG C, insulation reaction 0-10h；
4) using suction filtration, centrifugation or rotate step 3) solvent of product that is obtained after terminating of reaction removes, gained production
Thing is repeatedly washed with distilled water, ethanol, is then dried, grinds, is sieved, drying temperature is：40~120 DEG C, finally obtain trimerization
Cyanamide cyanurate and montmorillonite nano complex；
Above-mentioned steps 1) in montmorillonite used can be original soil or organically-modified mistake montmorillonite, it is or de- containing covering
The clay of soil structure；The mass ratio of montmorillonite and solvent is 1g：20~200ml；
Above-mentioned steps 2) in melamine be previously dissolved in solvent hold specifically, melamine and solvent are added into reaction
In device, heating dissolves melamine, and heating-up temperature is 40~200 DEG C, and the mass ratio of melamine and solvent is 1g：20~
200ml；
Above-mentioned steps 3) in cyanuric acid and urea mixture, its mass percent be 100:0~0:100；
Above-mentioned steps 3) in the mixture of cyanuric acid and urea is previously dissolved in solvent specifically, by cyanuric acid and urea
Mixture is added in reaction vessel with solvent, and heating dissolves the mixture of cyanuric acid and urea, and heating-up temperature is 40~200
DEG C, the mass ratio of the mixture and solvent of cyanuric acid and urea is 1g：20~200ml；
Above-mentioned steps 1) in solvent be C1~C3 alcohol, one in formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile
Plant or its mixture；
Above-mentioned steps 2) in solvent be C1~C3 alcohol, one in formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile
Plant or its mixture；
Above-mentioned steps 3) in solvent be C1~C3 alcohol, one in formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile
Plant or its mixture.
The present invention has the advantages and positive effects of：Due to using above-mentioned technical proposal, make melamine cyanurate
It is intercalation between the lamella of montmorillonite, expands cheating engaging layer spacing, the montmorillonite of addition reaches the state of stripping, substantially uniformity
The lamellar structure of nanoscale is separated into, melamine cyanurate and the nano-complex of montmorillonite is obtained, its X-ray diffraction
Curve is as shown in Figure 1.This method technique is simple, and raw material is easy to get, and cost is low.The melamine cyanurate of preparation and montmorillonite
Nano-complex is combined with traditional melamine cyanurate, montmorillonite or melamine cyanurate and the micron of montmorillonite
Thing is compared, and flame retardance of polymer performance and mechanical property can be significantly improved in polymeric material is fire-retardant, and reduce water absorbing properties.
Brief description of the drawings
Fig. 1 be melamine cyanurate, the XRD spectra of sodium-based montmorillonite, and embodiment 1 prepare melamine cyanogen
The XRD spectra of lithate montmorillonite nano complex.
Embodiment
Below by embodiment, the present invention will be further described, but embodiment is not intended to limit protection scope of the present invention.
Embodiment 1
The montmorillonite of 1 part of quality is added in reaction vessel, and adds the distilled water of 40 parts of quality as solvent, stirring
It is uniformly heating to 60 DEG C, insulated and stirred 30 minutes；The melamine and insulated and stirred 1 hour of 0.05 part of quality are added, is added
The cyanuric acid of 0.05 part of quality, continues insulated and stirred and is cooled to room temperature after 1 hour；Solid-liquid point is carried out to suspension liquid using revolving
From, filter cake is repeatedly washed using distilled water, ethanol solution, dries, grind, sieve after finishing, acquisition melamine cyanogen
Lithate and montmorillonite nano complex.
It was found from the XRD spectra of melamine cyanurate montmorillonite nano complex, 2 θ=6.91 ° are spread out for montmorillonite
Peak is penetrated, is calculated according to Bragg equation and learns the piece interlamellar spacing of montmorillonite for 1.28 nanometers；Can from the XRD spectra of sodium-based montmorillonite
Know, 2 θ=8.98 ° are the diffraction maximum of montmorillonite, calculated according to Bragg equation and learn that the piece interlamellar spacing of montmorillonite is received for 0.98
Rice.The piece interlamellar spacing of montmorillonite increases to 1.28 nanometers by 0.98 nanometer, it was demonstrated that it is de- that melamine cyanurate has been intercalation into illiteracy
Among the lamellar structure of soil, montmorillonite reaches the state of stripping, and substantially uniformity is separated into the lamellar structure of nanoscale.
Embodiment 2
The montmorillonite of 1 part of quality is added in reaction vessel, and the distilled water for adding 200 parts of quality is stirred as solvent
Mix and be uniformly heating to 120 DEG C, insulated and stirred 2 hours；The melamine and insulated and stirred 3 hours of 20 parts of quality are added, is added
The cyanuric acid of 20 parts of quality, continues insulated and stirred and is cooled to room temperature after 3 hours；Solid-liquid point is carried out to suspension liquid using centrifugation
From, filter cake is repeatedly washed using distilled water, ethanol solution, dries, grind, sieve after finishing, acquisition melamine cyanogen
Lithate and montmorillonite nano complex.
Embodiment 3
The montmorillonite of 1 part of quality is added in reaction vessel, and the distilled water for adding 100 parts of quality is stirred as solvent
Mix and be uniformly heating to 100 DEG C, insulated and stirred 1 hour；The melamine and insulated and stirred 2 hours of 1 part of quality are added, 3 are added
The urea of part quality, continues insulated and stirred and is cooled to room temperature after 2 hours；Separation of solid and liquid is carried out to suspension liquid using suction filtration, adopted
Filter cake is repeatedly washed with distilled water, ethanol solution, dries, grind, sieve after finishing, obtain melamine cyanurate
With montmorillonite nano complex.
Embodiment 4
The montmorillonite of 1 part of quality is added in reaction vessel, and the distilled water for adding 150 parts of quality is stirred as solvent
Mix and be uniformly heating to 90 DEG C, insulated and stirred 1.5 hours；The melamine and insulated and stirred 2 hours of 10 parts of quality are added, is added
The cyanuric acid of 10 parts of quality, continues insulated and stirred and is cooled to room temperature after 2 hours；Solid-liquid point is carried out to suspension liquid using revolving
From, filter cake is repeatedly washed using distilled water, ethanol solution, dries, grind, sieve after finishing, acquisition melamine cyanogen
Lithate and montmorillonite nano complex.
Embodiment 5
The montmorillonite of 1 part of quality is added in reaction vessel, and the distilled water for adding 200 parts of quality is stirred as solvent
Mix and be uniformly heating to 100 DEG C, insulated and stirred 2 hours；While the melamine and the cyanuric acid of 15 parts of quality of 15 parts of quality of addition,
Continue insulated and stirred and be cooled to room temperature after 2.5 hours；Separation of solid and liquid is carried out to suspension liquid using centrifugation, using distilled water, second
Alcoholic solution is repeatedly washed to filter cake, is dried, grinds, is sieved after finishing, and is obtained melamine cyanurate and is received with montmorillonite
Rice compound.
Embodiment 6
The montmorillonite of 1 part of quality is added in reaction vessel, and adds the distilled water of 80 parts of quality as solvent, stirring
It is uniformly heating to 85 DEG C, insulated and stirred 1 hour；The cyanuric acid and insulated and stirred 1.5 hours of 0.05 part of quality are first added, is added
The melamine of 0.05 part of quality, continues insulated and stirred and is cooled to room temperature after 1.5 hours；Suspension liquid is consolidated using revolving
Liquid is separated, and filter cake is repeatedly washed using distilled water, ethanol solution, is dried, grinds, is sieved after finishing, obtains melamine
Amine cyanurate and montmorillonite nano complex.
Embodiment 7
The melamine of 8 parts of quality is added in reaction vessel, and add 150 parts of quality distilled water as solvent,
Stir and be warming up to 90 DEG C, insulated and stirred 1.5 hours；Add the cyanuric acid and insulated and stirred 1.5 hours of 8 parts of quality；Again plus
Enter the montmorillonite of 1 part of quality, continue insulated and stirred and be cooled to room temperature after 2 hours；Solid-liquid point is carried out to suspension liquid using suction filtration
From, filter cake is repeatedly washed using distilled water, ethanol solution, dries, grind, sieve after finishing, acquisition melamine cyanogen
Lithate and montmorillonite nano complex.
Embodiment 8
The melamine of 4 parts of quality is added in reaction vessel, and add 120 parts of quality distilled water as solvent,
Stir and be warming up to 90 DEG C, insulated and stirred 2 hours；Add the cyanuric acid and insulated and stirred 2 hours of 12 parts of quality；Add 1
The montmorillonite of part quality, continues insulated and stirred and is cooled to room temperature after 1 hour；Separation of solid and liquid is carried out to suspension liquid using centrifugation,
Filter cake is repeatedly washed using distilled water, ethanol solution, dries, grind, sieve after finishing, obtain melamine cyanurate
Salt and montmorillonite nano complex.
Claims (6)
1. a kind of melamine cyanurate and montmorillonite nano complex, it is characterised in that：By melamine cyanurate with
Montmorillonite reaction is prepared from, and its mass percent is,
Melamine cyanurate 5%-95%；
Montmorillonite 95%-5%；
A kind of described melamine cyanurate and the preparation process of montmorillonite nano complex are as follows：
1) montmorillonite and solvent are added in reaction vessel, stirred, heating is reacted, the temperature for controlling reaction vessel is 60
~120 DEG C, the heat time is 30min~10h, obtains reaction solution；
2) it is directly added into melamine or melamine is previously dissolved in solvent, is then added to step 1) obtained reaction solution
In, stirring, controlling reaction temperature is 60~120 DEG C, and 1~10h of insulation reaction obtains reaction solution；
3) mixture of cyanuric acid and urea is directly added into step 2) in obtained reaction solution, or by cyanuric acid and urea
Mixture is previously dissolved in solvent, is then added to step 2) in obtained reaction solution, stirring, controlling reaction temperature is 60~120
DEG C, 1~10h of insulation reaction；
4) using suction filtration, centrifugation or rotate step 3) solvent of product that is obtained after terminating of reaction removes, products therefrom is used
Distilled water, ethanol are repeatedly washed, and then dried, grind, are sieved, drying temperature is：40~120 DEG C, finally obtain melamine
Cyanurate and montmorillonite nano complex.
2. the preparation method of a kind of melamine cyanurate as claimed in claim 1 and montmorillonite nano complex, it is special
Levy and be that specific preparation process is as follows：
1) montmorillonite and solvent are added in reaction vessel, stirred, heating is reacted, the temperature for controlling reaction vessel is 60
~120 DEG C, the heat time is 30min~10h, obtains reaction solution；
2) it is directly added into melamine or melamine is previously dissolved in solvent, is then added to step 1) obtained reaction solution
In, stirring, controlling reaction temperature is 60~120 DEG C, and 1~10h of insulation reaction obtains reaction solution；
3) mixture of cyanuric acid and urea is directly added into step 2) in obtained reaction solution, or by cyanuric acid and urea
Mixture is previously dissolved in solvent, is then added to step 2) in obtained reaction solution, stirring, controlling reaction temperature is 60~120
DEG C, 1~10h of insulation reaction；
4) using suction filtration, centrifugation or rotate step 3) solvent of product that is obtained after terminating of reaction removes, products therefrom is used
Distilled water, ethanol are repeatedly washed, and then dried, grind, are sieved, drying temperature is：40~120 DEG C, finally obtain melamine
Cyanurate and montmorillonite nano complex；
Above-mentioned steps 1) in montmorillonite used can be the montmorillonite of original soil or organically-modified mistake, or contain montmorillonite knot
The clay of structure；The mass ratio of montmorillonite and solvent is 1g：20~200ml；
Above-mentioned steps 1) in solvent be C1~C3 alcohol, formaldehyde, acetic acid, glycerine, deionized water, pyridine, one kind in acetonitrile or
Its mixture；
Above-mentioned steps 2) in solvent be C1~C3 alcohol, formaldehyde, acetic acid, glycerine, deionized water, pyridine, one kind in acetonitrile or
Its mixture；
Above-mentioned steps 3) in solvent be C1~C3 alcohol, formaldehyde, acetic acid, glycerine, deionized water, pyridine, one kind in acetonitrile or
Its mixture.
3. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, its
It is characterised by：Reaction vessel carries condensation reflux unit, temperature regulating device and agitating device.
4. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, its
It is characterised by：Step 2) in melamine is previously dissolved in solvent specifically, melamine and solvent are added into reaction vessel
In, heating dissolves melamine, and heating-up temperature is 40~200 DEG C, and the mass ratio of melamine and solvent is 1g：20~
200ml。
5. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, its
It is characterised by：Step 3) in cyanuric acid and urea mixture, its mass percent be 100:0~0:100.
6. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, its
It is characterised by：Step 3) in the mixture of cyanuric acid and urea is previously dissolved in solvent specifically, by the mixed of cyanuric acid and urea
Compound is added in reaction vessel with solvent, and heating dissolves the mixture of cyanuric acid and urea, and heating-up temperature is 40~200
DEG C, the mass ratio of the mixture and solvent of cyanuric acid and urea is 1g：0~200ml.
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