CN105585855A - Organized montmorillonite flame-retarding asphalt and preparation method thereof - Google Patents
Organized montmorillonite flame-retarding asphalt and preparation method thereof Download PDFInfo
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Abstract
The invention provides organized montmorillonite flame-retarding asphalt, which comprises, by weight, 100 parts of basic asphalt, and 2-15 parts of an organic/inorganic composite flame retardant which is an organic/inorganic composite flame retarding material having a core-shell structure and formed by coating surface of montmorillonite granules with amine polyphosphate. The organic/inorganic composite flame retarding material having the core-shell structure increases dispersibility and uniformity of the montmorillonite inorganic powder particles in asphalt, thereby reducing filling use amount of a flame retardant and achieving advantage complement between organic and inorganic flame retardants.
Description
Technical field
The invention belongs to flame-retardant pitch technical field, be specifically related to a kind of organic montmorillonite flame-retardant pitch and preparation method thereof.
Background technology
Pitch is the organic high molecular compound that essential element forms by carbon, hydrogen, has inflammable feature. The process of pitch burning, first melting, drippage, trickling, be then bead burning,, trickling unrestrained by the bead burning again, causes fire spreading to expand. The burning of pitch is the chemical process of a heat release, decomposition, in burning, decomposite hydrogen, methane, benzene and alkanes inflammable gas, these burning of gas further can be accelerated again the thermal decomposition of pitch, especially in tunnel, once breaking out of fire, intensity of a fire expansion is fast, scope is wide, loss is large. Continuing to bring out and the increase of tunnel traffic amount of vcehicular tunnel, the frequency that tunnel fire hazard occurs also can increase gradually. Due to the closure in tunnel, once breaking out of fire accident, its consequence is hardly imaginable. The built tunnel safety measure of coming into operation of China at present causes anxiety, and potential safety hazard is very large. The massive losses of tunnel fire hazard accident, has caused the security of people to tunnel and the very big concern of fire problem. These road surfaces need to have good fire resistance, to ensure safety. Many countries classify the research of tunnel fire hazard control as important problem as. China recent years has also started to pay attention to the research to tunnel fire hazard, tries hard to the danger of tunnel fire hazard and loss to drop to minimum point. And the anti-flammability of raising pitch, making flame-retardant pitch concrete road surface is one of important measures that reduce at present medium pitch road surface, tunnel fire casualties and material damage.
Conventional fire retardant has halogen system, phosphorus system, nitrogen system, antimonial class, boron compound class, magnesium compound class, aluminium compound class etc. As Chinese patent, CN101817936A discloses a kind of composite fire retardant used for asphalt mixture and preparation method thereof, wherein contains organic bromine flame retardant. This type of organic fire-retardant (as halogen contained compound) flame retardant effect is better, but it can discharge poisonous irritative gas in the time of high temperature, this has not only all proposed very high requirement for the production of hot-mix asphalt mixture and construction, and to workmen and in the future in running personnel health also very unfavorable. At present, fire retardant is just towards the future development of Halogen, low toxicity, low cigarette. Wherein, metal hydroxides is as environment friendly flame retardant, have fire-retardant, press down cigarette, reduce the features such as secondary pollution, be widely used. But metal hydroxides also exists certain shortcoming while application as fire retardant, for example, need that addition is higher just can demonstrate obvious flame retardant effect.
Imvite, as a kind of conventional fire proofing, is used for the fire-retardant of the material such as textile, nylon. As Chinese patent CN201110427336 discloses a kind of nano flame retardant nylon, CN201310211318 discloses the flame-retardant finishing method of a kind of Intumescent Retardant System to pure cotton fabric. But because pitch is high sticky, its rheological property is poor, make the compatibility of itself and imvite poor, affect dispersiveness and the uniformity of imvite, affect flame retardant effect.
Summary of the invention
For the deficiencies in the prior art, object of object of the present invention is to provide a kind of organic montmorillonite flame-retardant pitch. Another object of the present invention is to further improve the strong polarity on imvite surface, thereby improve dispersiveness and the uniformity of imvite inorganic powder particle in pitch, reduce the loading of fire retardant, realized the mutual supplement with each other's advantages between organic fire-retardant and inorganic combustion inhibitor. The road asphalt that a kind of fire resistance is good is finally provided.
The invention provides a kind of organic montmorillonite flame-retardant pitch, comprise by weight:
Basic asphalt 100;
The compound fire retardant 2～15 of organic-inorganic;
Wherein the compound fire retardant of organic-inorganic is the compound fire proofing of the organic-inorganic with nucleocapsid structure of the coated polyphosphoric acids amine salt in montmorillonite particle surface. Taking imvite, polyphosphoric acids (PPA) and aminated compounds as raw material, by the compound fire retardant of imvite organic-inorganic with nucleocapsid structure prepared by micron order montmorillonite particle surface modification and coated polyphosphoric acids amine salt. Wherein the weight content of each material is:
Imvite: 10%～25%
Polyphosphoric acids: 20%～40%
Amine: 35%～55%
Described montmorillonite particle is micron order phyllosilicate, and smectite content is greater than 96%. Its particle diameter is preferably 5um to 20um. The degree of polymerization of wherein said polyphosphoric acids is less than 1000.
In the present invention, aminated compounds can be one or more in lauryl amine, cetylamine, octadecylamine, ethylenediamine, sec-butylamine, trioctylamine, propionamide, butyramide, cyclohexylamine, p-phenylenediamine (PPD) etc.
In road fire-resistant modified pitch of the present invention, basic asphalt can specifically be determined according to the requirement using, as No. 70 pitches, No. 90 pitches etc.
In road fire-resistant modified pitch of the present invention, the preparation scheme of the compound fire retardant of organic-inorganic is as follows:
(1) under the condition of high-speed stirred (1000～1500r/min), adds rapidly polyphosphoric acids ethanolic solution by imvite, lasting stirring as at least 20min, preferably 25min-60min, suction filtration.
(2) filter cake in step (1) is added to amine ethanolic solution, after having fed in raw material, stir again 30min～80min, suction filtration.
(3) washing, vacuum drying, finally obtain the compound fire retardant of graininess organic-inorganic.
Organically-modified or inorganic-organic hybrid modified montmorillonoid has good dispersiveness, for example organic matter is coated on to imvite powder surface by chemical bond, form a kind of compound fire retardant of hydrophobicity organic-inorganic with nucleocapsid structure, thereby change the strong polarity on imvite surface. Can improve dispersiveness and the uniformity of imvite inorganic powder particle in pitch, reduce the loading of fire retardant, realize the mutual supplement with each other's advantages between organic fire-retardant and inorganic combustion inhibitor. Overcome the shortcoming of traditional inorganics filled pitch simultaneously, given mechanical property, anti-fatigue performance, dimensional stability and the gas barrier properties etc. of material excellence.
In the inventive method, the composition principle of the compound fire retardant of organic-inorganic is at micron order imvite surface grafting polyphosphoric acids long-chain, make its surface introduce multiple acid hydroxy groups, then add amine generation acid-base reaction to obtain the compound fire retardant of organic-inorganic of the coated polyphosphoric acid amine in surface. Its reaction mechanism:
The present invention provides a kind of preparation method of organic montmorillonite flame-retardant pitch simultaneously, comprising:
(1) prepare organic inorganic composite flame retardants;
(2) the compound fire retardant of organic-inorganic prepared step (1) is joined and in pitch, obtain organic montmorillonite flame-retardant pitch of the present invention.
The wherein described organic inorganic composite flame retardants of preparation of step (1), comprising:
(1) under the condition of 1000～1500r/min high-speed stirred, imvite is added rapidly to polyphosphoric acids ethanolic solution, continue stirring until few 20min, preferably 25min-60min, suction filtration;
(2) filter cake in step (1) is added to amine ethanolic solution, after having fed in raw material, stir again 30min～80min, suction filtration;
(3) washing, vacuum drying, finally obtain the compound fire retardant of graininess organic-inorganic.
The process that the described compound fire retardant of organic-inorganic of step (2) joins in pitch is: compound described organic-inorganic fire retardant is joined in the pitch of 120 DEG C～160 DEG C, at 3000～4000r/min down cut 20min～60min, obtain organic montmorillonite flame-retardant pitch of the present invention with high-speed shearing machine. Wherein organic montmorillonite fire retardant and pitch addition are: 100 parts of basic asphalts; 2～15 parts of the compound fire retardants of organic modification montmonrillonite organic-inorganic.
Compared with prior art, advantage of the present invention is as follows:
1, in the present invention, the layer structure of imvite can be improved rheological property and the ageing resistace of pitch well, increases the hardness of pitch, improves thermo oxidative aging and the anti-light oxygen aging ability of pitch. Inorganic imvite is after organic intercalation, and interlamellar spacing can obviously increase, and the compatibility of imvite and pitch is improved, and modified effect is more excellent.
2, the present invention is by having prepared the compound fire proofing of organic-inorganic with nucleocapsid structure at the coated polyphosphoric acids amine salt of micron order montmorillonite particle Surface Creation chemical bond, improve dispersiveness and the uniformity of imvite inorganic powder particle in pitch, reduce the loading of fire retardant, realized the mutual supplement with each other's advantages between organic fire-retardant and inorganic combustion inhibitor.
3, in the present invention, polyphosphoric acid amine is a kind of organic expander type fire retardant efficiently, and loading can reach outstanding fire resistance in the time of lO%～20% conventionally. Iff imvite and the simple physical mixed of polyphosphoric acid amine are applied in pitch, due to the strong polarity on imvite surface and and pitch between compatibility poor, can greatly reduce the stability of modified pitch.
4, in the present invention, imvite has certain fire resistance, after being coated with, cooperatively interacts with polyphosphoric acid amine, cooperative flame retardant by surface grafting, has good fire-retardant and smoke suppressing effect. Flame-retardant pitch oxygen index (OI) of the present invention is high, does not produce the toxic gases such as hydrogen halides when burning, little to human respiratory tract and the injury of other organs. Preparation technology is simple, produces pollution-freely, and production cost is lower.
Detailed description of the invention
Now describe the present invention in conjunction with specific embodiments, but therefore do not limit the present invention.
Embodiment 1
The preparation of the compound fire retardant of organic-inorganic:
Wherein in imvite, smectite content is greater than 97%, and its particle diameter is 10um. The degree of polymerization of polyphosphoric acids is 100.
(1) under the condition of high-speed stirred (1000～1500r/min), imvite is added rapidly to polyphosphoric acids ethanolic solution, continue to stir 20min, suction filtration.
(2) filter cake in step (1) is added to lauryl amine ethanolic solution, after having fed in raw material, stir again lh, suction filtration.
(3) washing, vacuum drying, finally obtain particle dispersion good, the fluffy compound fire retardant of organic-inorganic that does not need grinding.
Wherein, wherein the weight content of each material is:
Imvite: 25%
Polyphosphoric acids: 25%
Lauryl amine: 50%
Being prepared as follows of organic-inorganic flame-retardant pitch:
The organic montmorillonite fire retardant of above-mentioned preparation is joined in the 70# pitch of 150 DEG C, at 3000～4000r/min down cut 30min, obtain organic montmorillonite flame-retardant pitch with high-speed shearing machine. Wherein the weight ratio of organic montmorillonite fire retardant and pitch is 1:10.
Embodiment 2
The preparation of the compound fire retardant of organic-inorganic:
Wherein in imvite, smectite content is greater than 97%, and its particle diameter is 10um. The degree of polymerization of polyphosphoric acids is 100.
(1) under the condition of high-speed stirred (1000～1500r/min), imvite is added rapidly to polyphosphoric acids ethanolic solution, continue to stir 20min, suction filtration.
(2) filter cake in step (1) is added to cetylamine ethanolic solution, after having fed in raw material, stir again lh, suction filtration.
(3) washing, vacuum drying, finally obtain particle dispersion good, the fluffy compound fire retardant of organic-inorganic that does not need grinding.
Wherein, wherein the weight content of each material is:
Imvite: 25%
Polyphosphoric acids: 30%
Cetylamine: 45%
Being prepared as follows of organic-inorganic flame-retardant pitch:
The organic montmorillonite fire retardant of above-mentioned preparation is joined in the 70# pitch of 150 DEG C, at 3000～4000r/min down cut 30min, obtain organic montmorillonite flame-retardant pitch with high-speed shearing machine. Wherein the weight ratio of organic montmorillonite fire retardant and pitch is 3:20.
Embodiment 3
The preparation of the compound fire retardant of organic-inorganic:
Wherein in imvite, smectite content is greater than 97%, and its particle diameter is 10um. The degree of polymerization of polyphosphoric acids is 100.
(1) under the condition of high-speed stirred (1000～1500r/min), imvite is added rapidly to polyphosphoric acids ethanolic solution, continue to stir 20min, suction filtration.
(2) filter cake in step (1) is added to octadecylamine ethanolic solution, after having fed in raw material, stir again lh, suction filtration.
(3) washing, vacuum drying, finally obtain particle dispersion good, the fluffy compound fire retardant of organic-inorganic that does not need grinding.
Wherein, wherein the weight content of each material is:
Imvite: 25%
Polyphosphoric acids: 35%
Octadecylamine: 45%
Being prepared as follows of organic-inorganic flame-retardant pitch:
The organic montmorillonite fire retardant of above-mentioned preparation is joined in the 70# pitch of 150 DEG C, at 3000～4000r/min down cut 30min, obtain organic montmorillonite flame-retardant pitch with high-speed shearing machine. Wherein the weight ratio of organic montmorillonite fire retardant and pitch is 1:5.
Comparison array 1
Imvite is joined in the pitch of 150 DEG C, at 3000～4000r/min down cut 30min, obtain flame-retardant pitch with high-speed shearing machine. Wherein the weight ratio of imvite and pitch is 4:10.
Comparison array 2
Aluminium hydroxide is joined in the pitch of 150 DEG C, at 3000～4000r/min down cut 30min, obtain flame-retardant pitch with high-speed shearing machine. Wherein the weight ratio of aluminium hydroxide and pitch is 3:10.
The performance indications of table 1 fire-retardant modified asphalt
As can be seen from Table 1, organic montmorillonite fire retardant of the present invention can improve the oxygen index (OI) of flame-retardant pitch effectively. To imvite carry out organically-modified after, obviously reduced its consumption, improved its compatibility. By having prepared the compound fire proofing of organic-inorganic with nucleocapsid structure at the coated polyphosphoric acids amine salt of micron order montmorillonite particle Surface Creation chemical bond, improve dispersiveness and the uniformity of imvite inorganic powder particle in pitch, reduce the loading of fire retardant, realized the mutual supplement with each other's advantages between organic fire-retardant and inorganic combustion inhibitor.
Claims (10)
1. an organic montmorillonite flame-retardant pitch, is characterized in that: comprise by weight:
100 parts of basic asphalts;
2～15 parts of the compound fire retardants of organic-inorganic;
Wherein the compound fire retardant of organic-inorganic is the compound fire proofing of the organic-inorganic with nucleocapsid structure of the coated polyphosphoric acids amine salt in montmorillonite particle surface.
2. according to organic montmorillonite flame-retardant pitch claimed in claim 1, it is characterized in that: the compound fire retardant of described organic-inorganic is for taking imvite, polyphosphoric acids and aminated compounds as raw material, by the compound fire retardant of imvite organic-inorganic with nucleocapsid structure prepared by micron order montmorillonite particle surface modification and coated polyphosphoric acids amine salt.
3. according to organic montmorillonite flame-retardant pitch claimed in claim 1, it is characterized in that: in the compound fire retardant of described organic-inorganic, the weight content of each material is:
Imvite: 10%～25%
Polyphosphoric acids: 20%～40%
Amine: 35%～55%.
4. according to organic montmorillonite flame-retardant pitch claimed in claim 3, it is characterized in that: described montmorillonite particle is micron order phyllosilicate, and smectite content is greater than 96%.
5. according to the organic montmorillonite flame-retardant pitch described in claim 3 or 4, it is characterized in that: described imvite particle diameter is 5um to 20um.
6. according to organic montmorillonite flame-retardant pitch claimed in claim 3, it is characterized in that: the degree of polymerization of described polyphosphoric acids is less than 1000.
7. according to organic montmorillonite flame-retardant pitch claimed in claim 1, it is characterized in that: the preparation scheme of the compound fire retardant of described organic-inorganic is as follows:
(1) under the condition of 1000～1500r/min high-speed stirred, imvite is added rapidly to polyphosphoric acids ethanolic solution, continue stirring until few 20min, preferably 25min-60min, suction filtration;
(2) filter cake in step (1) is added to amine ethanolic solution, after having fed in raw material, stir again 30min～80min, suction filtration;
(3) washing, vacuum drying, finally obtain the compound fire retardant of graininess organic-inorganic.
8. a preparation method for organic montmorillonite flame-retardant pitch described in claim 1-7, is characterized in that this preparation comprises:
(1) prepare organic inorganic composite flame retardants;
(2) the compound fire retardant of organic-inorganic prepared step (1) is joined and in pitch, obtain organic montmorillonite flame-retardant pitch of the present invention.
9. according to preparation method claimed in claim 8, it is characterized in that: the described organic inorganic composite flame retardants of preparation of step (1) comprises:
(1) under the condition of 1000～1500r/min high-speed stirred, imvite is added rapidly to polyphosphoric acids ethanolic solution, continue stirring until few 20min, preferably 25min-60min, suction filtration;
(2) filter cake in step (1) is added to amine ethanolic solution, after having fed in raw material, stir again 30min～80min, suction filtration;
(3) washing, vacuum drying, finally obtain the compound fire retardant of graininess organic-inorganic.
10. according to preparation method claimed in claim 8, it is characterized in that: the process that the described compound fire retardant of organic-inorganic of step (2) joins in pitch is: compound described organic-inorganic fire retardant is joined in the pitch of 120 DEG C～160 DEG C, with high-speed shearing machine at 3000～4000r/min down cut 20min～60min, obtain organic montmorillonite flame-retardant pitch of the present invention, wherein organic montmorillonite fire retardant and pitch addition are: 100 parts of basic asphalts; 2～15 parts of the compound fire retardants of organic modification montmonrillonite organic-inorganic.
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Cited By (2)
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| CN111501374A (en) * | 2020-04-30 | 2020-08-07 | 青岛悦浪建筑技术有限责任公司 | Modified asphalt waterproof coiled material with excellent flame retardant property and preparation method thereof |
| CN111501375A (en) * | 2020-04-30 | 2020-08-07 | 青岛悦浪建筑技术有限责任公司 | Flame-retardant modified asphalt waterproof coiled material and preparation method thereof |
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Cited By (2)
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| CN111501374A (en) * | 2020-04-30 | 2020-08-07 | 青岛悦浪建筑技术有限责任公司 | Modified asphalt waterproof coiled material with excellent flame retardant property and preparation method thereof |
| CN111501375A (en) * | 2020-04-30 | 2020-08-07 | 青岛悦浪建筑技术有限责任公司 | Flame-retardant modified asphalt waterproof coiled material and preparation method thereof |
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