CN102690661A - Hybrid fire retardant and preparing method thereof - Google Patents
Hybrid fire retardant and preparing method thereof Download PDFInfo
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- CN102690661A CN102690661A CN2012101867857A CN201210186785A CN102690661A CN 102690661 A CN102690661 A CN 102690661A CN 2012101867857 A CN2012101867857 A CN 2012101867857A CN 201210186785 A CN201210186785 A CN 201210186785A CN 102690661 A CN102690661 A CN 102690661A
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Abstract
The invention relates to the technical field of a hybrid fire retardant and relates to the hybrid fire retardant and a preparing method thereof. The hybrid fire retardant, which is mainly used as an adding type fire retardant, can be added to a polymer material. A nano-scale melamine formaldehyde polycondensate is synthesized in an acid bittern solution, and the melamine formaldehyde polycondensate is used as a nucleating agent used in the synthesis process of magnesium hydroxide so as to prepare a magnesium hydroxide/nano-scale melamine formaldehyde polycondensate hybrid fire retardant. According to the invention, a magnesium hydroxide fire retardant is provided, and at the same time a fire retardant element N is added, thus the hybrid fire retardant synthesized by using the method is high in fire retardant efficiency, simple in synthesis method and better in market prospect.
Description
Technical field
The present invention relates to hydridization fire retardant technical field, relates to a kind of hydridization fire retardant and preparation method thereof.
Background technology
Marinco H is a kind of Halogen, environmental friendliness additive flame retardant, is applied to fire-retardant superpolymer by increasing.It mainly absorbs the heat of combustion zone through (a), (b) decomposes discharges water vapor, (c) generates the generation that the charcoal layer reduces cigarette simultaneously, and the modes such as the isolated macromolecular material of MOX and contacting of oxygen that (d) generate show excellent fire retardant and smoke suppressing.But its flame retarding efficiency is lower, and addition need reach 50% above competence exertion effect of matrix, and so high addition can produce influence greatly to the mechanical property of superpolymer, influence the application of superpolymer then.
Trimeric cyanamide is a kind of triazines nitrogen heterocyclic ring organic cpds, and nitrogen content is up to 67% (massfraction), and its melting temperature is up to 345 ℃, and distillation possesses significant thermostability, flame retardant resistance about 350 ℃.Trimeric cyanamide can be in suitable temperature and potential of hydrogen scope; Successively methylolation takes place with formaldehyde and polycondensation obtains terpolycyantoamino-formaldehyde resin, it is widely used in fields such as sizing agent, porous plastics, synthon, photovaltaic material, leather tanning agent, water repellent agent, coating linking agent.
Summary of the invention
The invention provides a kind of hydridization fire retardant and preparation method thereof.
A kind of hydridization fire retardant of the present invention is to be formed by Marinco H and nano melamine formaldehyde condensation products hydridization, is nuclear with the nano melamine formaldehyde condensation products, and flake magnesium hydroxide is the nucleocapsid structure of shell.
Wherein said nano melamine formaldehyde condensation products is by the methylol (CH in the melamine methylol with structure in tart bittern liquid
2-OH) with other melamine methylol molecule in amino (NH
2), imino-(NH-) or hydroxyl (OH) condensation reaction takes place and forms the nano level melamino-formaldehyde polycondensate with line style or branched chain type structure.
Wherein said Marinco H is that the nano melamine formaldehyde condensation polymer composition granule with above-mentioned generation is a nucleator in bittern liquid, forms in its surface growth, has sheet structure.
The preparation method of above-mentioned hydridization fire retardant, carry out according to following step:
The massfraction of (1) measuring certain volume is 37% formaldehyde solution; Use the water dilution back adjustment pH value of 20 times of volumes to be 8-9; Add the trimeric cyanamide of certain mole, under 70 ℃, be stirred well to clarification, obtain melamino-formaldehyde performed polymer (melamine methylol).
(2) take by weighing a certain amount of bittern, it is dissolved in the deionized water, be added with a little H
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, the Mg in the constant volume filtrating
2+Concentration is 0.5mol/L, transfers its pH for acid, and the pH value is 1-7, obtains tart bittern solution.
(3) measure the above-mentioned bittern liquid of certain volume, place the there-necked flask that is added with condensing reflux and stirring, keep certain temperature and stirring velocity; Taking by weighing the melamino-formaldehyde performed polymer that the step (1) of certain volume makes is added dropwise in the bittern liquid; Treat after being added dropwise to complete that liquid level is just become when light blue or white by transparent, reduce rapidly below the temperature to 30 ℃, improve rotating speed simultaneously; Treat to begin dropping ammonia behind the temperature-stable 10min; Abundant suction filtration behind the reaction 3h, with deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Wherein the mol ratio of trimeric cyanamide described in the step (1) and formaldehyde is 1: (1-6).
Wherein the melamino-formaldehyde performed polymer described in the step (1) is a melamine methylol formaldehyde prepolymer; Dihydroxymethyl melamino-formaldehyde performed polymer; Trihydroxy-melamino-formaldehyde performed polymer; Tetra methylol melamino-formaldehyde performed polymer, pentamethylol melamine formaldehyde prepolymer, the mixture of one or several in the hexamethylolmelamine formaldehyde prepolymer.
The bittern described in the step (2) wherein, its staple is a magnesium chloride hexahydrate.
Wherein the pH value preferable range of the filtrating of the bittern described in the step (2) is 2-4.
Wherein in the dropping melamino-formaldehyde performed polymer process described in the step (3), the temperature maintenance of bittern liquid is at 50-90 ℃.
Wherein the melamino-formaldehyde performed polymer volume of the adding described in the step (3) is 10% of a bittern volume.
Mg in ammoniacal liquor described in the step (3) and the bittern liquid wherein
2+Mol ratio is 2:1.
Advantage of the present invention is to use comparatively cheap raw material; Synthesize nano level melamino-formaldehyde polycondensate through simple technology; And with this as the nucleator in the Marinco H building-up process, prepare the Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant that has than high flame retardant.
Description of drawings
Accompanying drawing 2 is the XRD diffraction curve of hydridization fire retardant among the embodiment 2.
Accompanying drawing 3 is the TG and the DTG curve of hydridization fire retardant among the embodiment 2.
Accompanying drawing 4 is the SEM image of hydridization fire retardant among the embodiment 2.
Embodiment
Provide embodiment so that the present invention is described further below in conjunction with technical scheme, but embodiment does not limit protection scope of the present invention.
Embodiment 1:
(1) measures 37% formaldehyde solution (0.005mol) of 0.37ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 2:
(1) measures 37% formaldehyde solution (0.0125mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 3:
(1) measures 37% formaldehyde solution (0.03mol) of 2.21ml, use the water dilution back adjustment pH value of 40ml to be 8-9, add 2.52g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, measures the melamino-formaldehyde performed polymer that obtains in the 20ml step (1) to be added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 4:
(1) measures 37% formaldehyde solution (0.0125mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 1 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 5:
(1) measures 37% formaldehyde solution (0.0125mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 6:
(1) measures 37% formaldehyde solution (0.0125mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 6 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 7:
(1) measures 37% formaldehyde solution (0.005mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 50 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 8:
(1) measures 37% formaldehyde solution (0.005mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 70 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Embodiment 9:
(1) measures 37% formaldehyde solution (0.005mol) of 0.92ml, use the water dilution back adjustment pH value of 20ml to be 8-9, add 0.63g (0.005mol) trimeric cyanamide, under 70 ℃, be stirred well to liquid level and clarify, obtain the melamino-formaldehyde performed polymer.
(2) take by weighing the bittern of 20.3g, it is dissolved in the deionized water, add 1-2mlH
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, and behind the constant volume, transferring pH is 2.5 in the 200ml volumetric flask.
(3) with the bittern liquid of above-mentioned 200ml, place the there-necked flask that is added with condensing reflux and stirring, 90 ℃; 300r/min stirs down fully, and the melamino-formaldehyde performed polymer that obtains in the step (1) is added dropwise in the bittern liquid, treats after being added dropwise to complete that liquid level is just become when light blue or white by transparent; Reduce rapidly temperature to 25 ℃; Improve rotating speed simultaneously to 500r/min, treat to begin dropping ammonia behind the temperature-stable 10min, fully react suction filtration behind the 3h; With deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
Claims (9)
1. a hydridization fire retardant is characterized in that being formed by Marinco H and nano melamine formaldehyde condensation products hydridization, is nuclear with the nano melamine formaldehyde condensation products, and flake magnesium hydroxide is the nucleocapsid structure of shell;
Wherein said nano melamine formaldehyde condensation products is by the methylol (CH in the melamine methylol with structure in tart bittern liquid
2-OH) with other melamine methylol molecule in amino (NH
2), imino-(NH-) or hydroxyl (OH) condensation reaction takes place and forms the nano level melamino-formaldehyde polycondensate with line style or branched chain type structure;
Wherein said Marinco H is that the nano melamine formaldehyde condensation polymer composition granule with above-mentioned generation is a nucleator in bittern liquid, forms in its surface growth, has sheet structure.
2. the preparation method of the described hydridization fire retardant of claim 1 is characterized in that carrying out according to following step:
The massfraction of (1) measuring certain volume is 37% formaldehyde solution, uses the water dilution back adjustment pH value of 20 times of volumes to be 8-9, adds certain mole trimeric cyanamide, under 70 ℃, is stirred well to clarification, obtains the melamino-formaldehyde performed polymer;
(2) take by weighing a certain amount of bittern, it is dissolved in the deionized water, be added with a little H
2O
2, leaving standstill after fully stirring, the 4-5h after-filtration must be filtrated, the Mg in the constant volume filtrating
2+Concentration is 0.5mol/L, transfers its pH for acid, and the pH value is 1-7, obtains tart bittern solution;
(3) measure the above-mentioned bittern liquid of certain volume, place the there-necked flask that is added with condensing reflux and stirring, keep certain temperature and stirring velocity; Taking by weighing the melamino-formaldehyde performed polymer that the step (1) of certain volume makes is added dropwise in the bittern liquid; Treat after being added dropwise to complete that liquid level is just become when light blue or white by transparent, reduce rapidly below the temperature to 30 ℃, improve rotating speed simultaneously; Treat to begin dropping ammonia behind the temperature-stable 10min; Abundant suction filtration behind the reaction 3h, with deionized water and washing with alcohol 2 times, 80 ℃ of following vacuum-dryings promptly get Marinco H/nano melamine formaldehyde condensation products hydridization fire retardant.
3. the preparation method of hydridization fire retardant according to claim 2 is characterized in that wherein the mol ratio of the trimeric cyanamide described in the step (1) and formaldehyde is 1:1-6.
4. the preparation method of hydridization fire retardant according to claim 2; It is characterized in that wherein the melamino-formaldehyde performed polymer described in the step (1) is a melamine methylol formaldehyde prepolymer; Dihydroxymethyl melamino-formaldehyde performed polymer, trihydroxy-melamino-formaldehyde performed polymer, tetra methylol melamino-formaldehyde performed polymer; The pentamethylol melamine formaldehyde prepolymer, the mixture of one or several in the hexamethylolmelamine formaldehyde prepolymer.
5. the preparation method of hydridization fire retardant according to claim 2 is characterized in that the wherein bittern described in the step (2), and its staple is a magnesium chloride hexahydrate.
6. the preparation method of hydridization fire retardant according to claim 2 is characterized in that wherein the pH value of the filtrating of the bittern described in the step (2) is 2-4.
7. the preparation method of hydridization fire retardant according to claim 2 is characterized in that wherein the temperature maintenance of bittern liquid is at 50-90 ℃ in the dropping melamino-formaldehyde performed polymer process described in the step (3).
8. the preparation method of hydridization fire retardant according to claim 2 is characterized in that the melamino-formaldehyde performed polymer volume of the wherein adding described in the step (3) is 10% of a bittern volume.
9. the preparation method of hydridization fire retardant according to claim 2 is characterized in that wherein Mg in the ammoniacal liquor described in the step (3) and bittern liquid
2+Mol ratio is 2:1.
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