CN104829860A - Melamine cyanurate and montmorillonite nano-composite and preparation method thereof - Google Patents
Melamine cyanurate and montmorillonite nano-composite and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a melamine cyanurate and montmorillonite nano-composite and a preparation method thereof and belongs to the technical field of nano materials. The preparation method includes: adding one part of montmorillonite and 20-200 parts of solvent into a reaction container, controlling temperature of the reaction container to be room temperature to 120 DEG C, and stirring for 0-10h in a heat-insulating manner; adding 0.05-20 parts of melamine in the process of reaction, adding 0.05-20 parts of a mixture of cyanuric acid and urea after a certain period of time of thermal reaction, and cooling to room temperature after a certain period of time of thermal reaction; adopting suction filtration, centrifuging or rotary evaporation to separate a material obtained by reaction, washing the product for many times by using distilled water and alcohol, and drying, grinding and sifting to obtain the melamine cyanurate and montmorillonite nano-composite. The preparation method is mild and stable in reaction condition, high in repeatability, high in yield and suitable for expanded production, and the nano-composite can improve flame retardancy, high temperature resistance, water-absorbing resistance and mechanical performance of polymer.
Description
Technical field
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.
Background technology
Melamine cyanurate (melamine cyanurate, MCA) melamine cyanurate salt is had another name called, it is a kind of fines of white crystalline, have soapy feeling, molecular formula is C6H9N9O3, density 1.5 ~ 1.6g/cm3, odorless, tasteless, be insoluble in water and other organic solvents, slightly acidic, less than 350 DEG C stable chemical natures.Melamine cyanurate is a kind of important nitrogenated flame retardant, there is the advantages such as nitrogen content is high, Halogen, low cigarette, low toxicity, low-corrosiveness, and good with resin compatible, flame retarding efficiency is high, can be used in multiple polymers material, be particularly useful for the flame-retardant modified of polymeric amide (as nylon 6, nylon66 fiber) material.
Melamine cyanurate is formed by hydrogen bonded by trimeric cyanamide and cyanuric acid molecule, concrete production technique mainly contains following three kinds by selecting the difference of initial feed: 1, cyanuric acid method, the trimeric cyanamide of certain mol proportion and cyanuric acid are placed in water and form suspension, stoichiometric number hour under certain temperature, until slip obviously become sticky thick after continue reaction for some time, again after filtration, washing, dry, fragmentation obtain finished product, and mother liquor is recyclable to be recycled.Need in this technique to add a large amount of water, to reduce the viscosity that reaction system constantly increases, therefore also can be referred to as solvent method.Solvent method complete processing is simple, and speed of response is fast, and product purity is high, but production process needs to consume large water gaging and large volume device, therefore production efficiency reduces.2, Wyler's process, normally while urea pyrolysis generates cyanuric acid, add trimeric cyanamide to react, or urea and trimeric cyanamide together added carry out heat fusing, single step reaction generates melamine cyanurate crude product, then boil through acid, wash, it is dry etc. that operation is refining obtains product.The method raw material is cheap and easy to get, production cost is low, good in economic efficiency, but products therefrom purity low (being generally 80%-85%) after frit reaction, need wash with the boiling water of times amount more than ten, or the trimeric cyanamide, cyanuric acid and the urea derivative that do not react is removed with pickling, relate to a large amount of waste water handling problem.3, high-temperature melting method, reaction process does not introduce any solvent, therefore can be called solid process.In solid process preparation technology, first raw material trimeric cyanamide and cyanuric acid are carried out superfine grinding, (more than 300 DEG C) direct frit reaction is to generate the high melamine cyanurate of productive rate then under the high temperature conditions.Owing to not needing to introduce solvent, the technical process of preparation is simplified, but during reaction, volatility of raw material is lost in about 10%, and yield reduces.
In addition, someone proposes some new melamine cyanurate preparation methods, as a kind of method (patent No. ZL201210230199.8) of water heat transfer nano level melamine cyanurate, the preparation method (patent No. ZL201210066842.8) etc. of bar-shaped crystal formation melamine cyanurate flame retardant and preparation method thereof (patent No. ZL201110029371.9) and the wide distribution melamine cyanurate of a kind of Large stone, its advantage concentrates on raising product and improves after adding polymkeric substance in the mechanical property of matrix, but still there is the problem in such as above-mentioned traditional processing technology in its production process.
Polynite (MMT) is the hydrosilicate clay that a class has laminate structure, its frame sheet is nanoscale, each thickness about 1 nanometer, the silicate lamella with negative charge be made up of with the silicon-oxy tetrahedron being positioned at both sides the alumina octahedral being positioned at centre, through the counter cation balancing charge of interlayer (as H+, Na+, K+, Ca2+, Mg2+ etc.), a kind of natural multilayered structure clay of formation.Silicon in silicon-oxy tetrahedron can be replaced by aluminium, and the aluminium in alumina octahedral can be replaced by magnesium, iron, zinc, lithium, chromium plasma.Due to water and the effect of interlayer cation, polynite can stable dispersion in water, its interlayer cation can carry out ion-exchange with outside organic and inorganic cation.The spacing of polynite silicate plate interlayer is different because cationic kind is different, at 1 to 2 ran.
Polynite is a large amount of inorganic cation and show as hydrophilic oleophobic property because interlayer has, and is unfavorable for its dispersion in organic phase and the absorption to organic substance.Better consistency is had in order to make polynite and organic phase, polynite (referring generally to sodium-based montmorillonite) interstitial inorganic cations is replaced with organic cation, to change the cationic form of polynite crystal layer, make it surface-hydrophobicized, and there is good expansion character, form organic modification montmonrillonite.By organically-modified, improve interface polarity and the chemical micro-environment of inorganics, add two alternate affinities, define the mixture of the large interlamellar spacing can receiving larger organic molecule and group.Organic modification montmonrillonite and polymkeric substance by suitable blended after, polymkeric substance enters between cheating engaging layer, and interlamellar spacing is expanded, the nano composite polymer-montmorillonoid material of formation intercal type; When polymkeric substance makes the silicate lamella of polynite expand further, reach the degree of stripping, form exfoliated nano composite polymer-montmorillonoid material; If polynite and polymkeric substance can not be compatible, then form the micro-composites of polymer-montmorillonoid.In recent years, polymer/laminated silicate clay nanocomposites rises rapidly as a kind of novel high-performance fire retardant material, polynite add flame retardant properties, mechanical property and some other Practical Performance that can improve polymkeric substance, and during the burning of this kind of fire retardant material, there is the advantages such as low cigarette, nontoxic, environmental protection.
Summary of the invention
The object of the invention is to propose a kind of melamine cyanurate and montmorillonite nano complex and preparation method thereof to solve prior art Problems existing.
Melamine cyanurate of the present invention and montmorillonite nano complex, due to adding of melamine cyanurate, its intercalation is made to enter between the lamella of polynite, the interlamellar spacing of polynite expands, the polynite added reaches the state of stripping, completely dispersed is the laminated structure of nanoscale, thus obtains the nano-complex of the two.
The object of the invention is to be achieved through the following technical solutions.
A kind of melamine cyanurate of the present invention and montmorillonite nano complex, be reacted by melamine cyanurate and polynite to be prepared from, its mass percent is: melamine cyanurate 5%-95%, polynite 95%-5%.
The preparation method of a kind of melamine cyanurate of the present invention and montmorillonite nano complex, its concrete preparation process is as follows:
1) join in reaction vessel by polynite and solvent, stir, heating is reacted, and the temperature controlling reaction vessel is room temperature ~ 120 DEG C, and heat-up time is 0 ~ 10h, obtains reaction solution;
2) directly add trimeric cyanamide or trimeric cyanamide be dissolved in solvent in advance, then joining step 1) in the reaction solution that obtains, stir, control temperature of reaction is room temperature ~ 120 DEG C, and insulation reaction 0-10h, obtains reaction solution;
3) mixture of cyanuric acid and urea is directly added in step 2) in the reaction solution that obtains, or the mixture of cyanuric acid and urea is dissolved in solvent in advance, then step 2 is joined) in the reaction solution that obtains, stir, control temperature of reaction is room temperature ~ 120 DEG C, insulation reaction 0-10h;
4) adopt suction filtration, centrifugal or revolve steam step 3) solvent of product that obtains after terminating of reaction removes, products therefrom distilled water, ethanol repeatedly wash, then dry, grind, sieve, bake out temperature is: 40 ~ 120 DEG C, finally obtains melamine cyanurate and montmorillonite nano complex;
Above-mentioned steps 1) in polynite used can be the polynite of original soil or organically-modified mistake, or the clay containing polynite structure; The mass ratio of polynite and solvent is 1g:20 ~ 200ml;
Above-mentioned steps 2) in trimeric cyanamide be dissolved in solvent be in advance specially, join in reaction vessel by trimeric cyanamide and solvent, heating makes melamine goes, and Heating temperature is 40 ~ 200 DEG C, and the mass ratio of trimeric cyanamide and solvent is 1g:20 ~ 200ml;
Above-mentioned steps 3) in the mixture of cyanuric acid and urea, its mass percent is 100:0 ~ 0:100;
Above-mentioned steps 3) in the mixture of cyanuric acid and urea be dissolved in solvent be in advance specially, the mixture of cyanuric acid and urea and solvent are joined in reaction vessel, heating makes the mixture of cyanuric acid and urea dissolve, Heating temperature is 40 ~ 200 DEG C, and the mixture of cyanuric acid and urea and the mass ratio of solvent are 1g:20 ~ 200ml;
Above-mentioned steps 1) in solvent be one in the alcohol of C1 ~ C3, formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile or its mixture;
Above-mentioned steps 2) in solvent be one in the alcohol of C1 ~ C3, formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile or its mixture;
Above-mentioned steps 3) in solvent be one in the alcohol of C1 ~ C3, formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile or its mixture.
The advantage that the present invention has and positively effect are: owing to adopting technique scheme, melamine cyanurate is made to be intercalation between the lamella of polynite, cheating engaging layer spacing is expanded, the polynite added reaches the state of stripping, completely dispersed is the laminated structure of nanoscale, obtain the nano-complex of melamine cyanurate and polynite, its X-ray diffraction curve as shown in Figure 1.Present method technique is simple, and raw material is easy to get, and cost is low.The melamine cyanurate of preparation and the nano-complex of polynite with traditional melamine cyanurate, polynite or melamine cyanurate compared with the micron mixture of polynite, flame retardance of polymer performance and mechanical property can be significantly improved in polymer materials is fire-retardant, and reduces water absorbing properties.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of melamine cyanurate, sodium-based montmorillonite, and the XRD spectra of the melamine cyanurate montmorillonite nano complex of embodiment 1 preparation.
Embodiment
Below by embodiment, the present invention will be further described, but embodiment does not limit the scope of the invention.
Embodiment 1
The polynite of 1 part of quality is joined in reaction vessel, and the distilled water adding 40 parts of quality is as solvent, stirs and is warming up to 60 DEG C, insulated and stirred 30 minutes; Add the trimeric cyanamide of 0.05 part of quality and insulated and stirred 1 hour, then add the cyanuric acid of 0.05 part of quality, continue insulated and stirred and be cooled to room temperature after 1 hour; Employing is revolved to steam and is carried out solid-liquid separation to suspension liquid, adopts distilled water, ethanolic soln repeatedly to wash filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
From the XRD spectra of melamine cyanurate montmorillonite nano complex, 2 θ=6.91 ° are the diffraction peak of polynite, calculate learn that the sheet interlayer spacing of polynite is 1.28 nanometers according to Bragg equation; From the XRD spectra of sodium-based montmorillonite, 2 θ=8.98 ° are the diffraction peak of polynite, calculate learn that the sheet interlayer spacing of polynite is 0.98 nanometer according to Bragg equation.The sheet interlayer spacing of polynite increases to 1.28 nanometers by 0.98 nanometer, and prove that melamine cyanurate has been intercalation among the laminated structure of polynite, polynite reaches the state of stripping, and completely dispersed is the laminated structure of nanoscale.
Embodiment 2
The polynite of 1 part of quality is joined in reaction vessel, and the distilled water adding 200 parts of quality is as solvent, stirs and is warming up to 120 DEG C, insulated and stirred 2 hours; Add the trimeric cyanamide of 20 parts of quality and insulated and stirred 3 hours, then add the cyanuric acid of 20 parts of quality, continue insulated and stirred and be cooled to room temperature after 3 hours; Adopt and centrifugal solid-liquid separation carried out to suspension liquid, adopt distilled water, ethanolic soln repeatedly washs filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Embodiment 3
The polynite of 1 part of quality is joined in reaction vessel, and the distilled water adding 100 parts of quality is as solvent, stirs and is warming up to 100 DEG C, insulated and stirred 1 hour; Add the trimeric cyanamide of 1 part of quality and insulated and stirred 2 hours, then add the urea of 3 parts of quality, continue insulated and stirred and be cooled to room temperature after 2 hours; Adopt suction filtration to carry out solid-liquid separation to suspension liquid, adopt distilled water, ethanolic soln repeatedly to wash filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Embodiment 4
The polynite of 1 part of quality is joined in reaction vessel, and the distilled water adding 150 parts of quality is as solvent, stirs and is warming up to 90 DEG C, insulated and stirred 1.5 hours; Add the trimeric cyanamide of 10 parts of quality and insulated and stirred 2 hours, then add the cyanuric acid of 10 parts of quality, continue insulated and stirred and be cooled to room temperature after 2 hours; Employing is revolved to steam and is carried out solid-liquid separation to suspension liquid, adopts distilled water, ethanolic soln repeatedly to wash filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Embodiment 5
The polynite of 1 part of quality is joined in reaction vessel, and the distilled water adding 200 parts of quality is as solvent, stirs and is warming up to 100 DEG C, insulated and stirred 2 hours; Add the trimeric cyanamide of 15 parts of quality and the cyanuric acid of 15 parts of quality simultaneously, continue insulated and stirred and be cooled to room temperature after 2.5 hours; Adopt and centrifugal solid-liquid separation carried out to suspension liquid, adopt distilled water, ethanolic soln repeatedly washs filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Embodiment 6
The polynite of 1 part of quality is joined in reaction vessel, and the distilled water adding 80 parts of quality is as solvent, stirs and is warming up to 85 DEG C, insulated and stirred 1 hour; First add the cyanuric acid of 0.05 part of quality and insulated and stirred 1.5 hours, then add the trimeric cyanamide of 0.05 part of quality, continue insulated and stirred and be cooled to room temperature after 1.5 hours; Employing is revolved to steam and is carried out solid-liquid separation to suspension liquid, adopts distilled water, ethanolic soln repeatedly to wash filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Embodiment 7
The trimeric cyanamide of 8 parts of quality is joined in reaction vessel, and the distilled water adding 150 parts of quality is as solvent, stirs and is warming up to 90 DEG C, insulated and stirred 1.5 hours; Add the cyanuric acid of 8 parts of quality and insulated and stirred 1.5 hours; Add the polynite of 1 part of quality again, continue insulated and stirred and be cooled to room temperature after 2 hours; Adopt suction filtration to carry out solid-liquid separation to suspension liquid, adopt distilled water, ethanolic soln repeatedly to wash filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Embodiment 8
The trimeric cyanamide of 4 parts of quality is joined in reaction vessel, and the distilled water adding 120 parts of quality is as solvent, stirs and is warming up to 90 DEG C, insulated and stirred 2 hours; Add the cyanuric acid of 12 parts of quality and insulated and stirred 2 hours; Add the polynite of 1 part of quality again, continue insulated and stirred and be cooled to room temperature after 1 hour; Adopt and centrifugal solid-liquid separation carried out to suspension liquid, adopt distilled water, ethanolic soln repeatedly washs filter cake, after dries, grind, sieve, acquisition melamine cyanurate and montmorillonite nano complex.
Claims (7)
1. melamine cyanurate and a montmorillonite nano complex, is characterized in that: reacted by melamine cyanurate and polynite and be prepared from, its mass percent is,
Melamine cyanurate 5%-95%
Polynite 95%-5%.
2. a preparation method for melamine cyanurate and montmorillonite nano complex, is characterized in that concrete preparation process is as follows:
1) join in reaction vessel by polynite and solvent, stir, heating is reacted, and the temperature controlling reaction vessel is room temperature ~ 120 DEG C, and heat-up time is 0 ~ 10h, obtains reaction solution
2) directly add trimeric cyanamide or trimeric cyanamide be dissolved in solvent in advance, then joining step 1) in the reaction solution that obtains, stir, control temperature of reaction is room temperature ~ 120 DEG C, and insulation reaction 0-10h, obtains reaction solution
3) mixture of cyanuric acid and urea is directly added in step 2) in the reaction solution that obtains, or the mixture of cyanuric acid and urea is dissolved in solvent in advance, then joins step 2) in the reaction solution that obtains, stir, control temperature of reaction is room temperature ~ 120 DEG C, insulation reaction 0-10h
4) adopt suction filtration, centrifugal or revolve steam step 3) solvent of product that obtains after terminating of reaction removes, products therefrom distilled water, ethanol repeatedly wash, then dry, grind, sieve, bake out temperature is: 40 ~ 120 DEG C, finally obtains melamine cyanurate and montmorillonite nano complex
Above-mentioned steps 1) in polynite used can be the polynite of original soil or organically-modified mistake, or the clay containing polynite structure; The mass ratio of polynite and solvent is 1g:20 ~ 200ml
Above-mentioned steps 1) in solvent be one in the alcohol of C1 ~ C3, formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile or its mixture
Above-mentioned steps 2) in solvent be one in the alcohol of C1 ~ C3, formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile or its mixture
Above-mentioned steps 3) in solvent be one in the alcohol of C1 ~ C3, formaldehyde, acetic acid, glycerine, deionized water, pyridine, acetonitrile or its mixture.
3. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, is characterized in that: reaction vessel is with condensation reflux unit, temperature regulating device and whipping appts.
4. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, it is characterized in that: step 2) in trimeric cyanamide be dissolved in solvent be in advance specially, trimeric cyanamide and solvent are joined in reaction vessel, heating makes melamine goes, Heating temperature is 40 ~ 200 DEG C, and the mass ratio of trimeric cyanamide and solvent is 1g:20 ~ 200ml.
5. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, is characterized in that: step 3) in the mixture of cyanuric acid and urea, its mass percent is 100:0 ~ 0:100.
6. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, it is characterized in that: step 3) in the mixture of cyanuric acid and urea be dissolved in solvent be in advance specially, the mixture of cyanuric acid and urea and solvent are joined in reaction vessel, heating makes the mixture of cyanuric acid and urea dissolve, Heating temperature is 40 ~ 200 DEG C, and the mixture of cyanuric acid and urea and the mass ratio of solvent are 1g:0 ~ 200ml.
7. the preparation method of a kind of melamine cyanurate according to claim 2 and montmorillonite nano complex, is characterized in that: step 1) order constant, step 2) and step 3) order can exchange, remaining step is constant; Or first carry out step 2, then carry out step 3), then carry out step 1), remaining step is constant; Or first carry out step 3), then carry out step 2), then carry out step 1), remaining step is constant.
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| CN115160646A (en) * | 2022-06-27 | 2022-10-11 | 北京理工大学 | Modified kaolinite and preparation method thereof |
| CN115160646B (en) * | 2022-06-27 | 2024-01-26 | 北京理工大学 | Modified kaolinite and preparation method thereof |
| CN115229913A (en) * | 2022-08-11 | 2022-10-25 | 小森新材料科技有限公司 | Method for manufacturing formaldehyde-free flame-retardant plywood |
| CN115232388A (en) * | 2022-09-21 | 2022-10-25 | 江苏恒尚节能科技股份有限公司 | Heat-insulating refractory material for building curtain wall and preparation method thereof |
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