CN105585855B - A kind of organic montmorillonite flame-retardant pitch and preparation method thereof - Google Patents

A kind of organic montmorillonite flame-retardant pitch and preparation method thereof Download PDF

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CN105585855B
CN105585855B CN201410563646.0A CN201410563646A CN105585855B CN 105585855 B CN105585855 B CN 105585855B CN 201410563646 A CN201410563646 A CN 201410563646A CN 105585855 B CN105585855 B CN 105585855B
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retardant
montmorillonite
pitch
organo
fire
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CN105585855A (en
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宣根海
徐青柏
陈杰
石君章
宁爱民
李志军
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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Abstract

The present invention provides a kind of organic montmorillonite flame-retardant pitch, by weight includes: 100 parts of basic asphalt;2~15 parts of organo-mineral complexing fire retardant.Wherein organo-mineral complexing fire retardant is the organo-mineral complexing fire proofing with nucleocapsid structure that montmorillonite particle surface coats polyphosphoric acids amine salt.This organo-mineral complexing fire proofing with nucleocapsid structure improves dispersibility and uniformity of the montmorillonite inorganic powder particle in pitch, reduces the loading of fire retardant, realize the mutual supplement with each other's advantages between organic fire-retardant and inorganic fire retardants.

Description

A kind of organic montmorillonite flame-retardant pitch and preparation method thereof
Technical field
The invention belongs to flame-retardant pitch technical fields, and in particular to a kind of organic montmorillonite flame-retardant pitch and its preparation side Method.
Background technique
Pitch is had the characteristics that inflammable by the organic high molecular compound that carbon, hydrogen are that essential element forms.Pitch burning Process, melt, drip first, trickling, followed by bead burning, trickling unrestrained by the bead that burns again, causing fire spreading Expand.The burning of pitch is the chemical process of a heat release, decomposition, and hydrogen, methane, benzene and the easy combustion gas of alkanes are decomposited in burning Body, the burning of these gases can further accelerate the thermal decomposition of pitch, especially in tunnel, once fire occurs, fire Gesture extension is fast, range is wide, loss is big.The increase of vcehicular tunnel continued to bring out with tunnel traffic amount, the frequency that tunnel fire hazard occurs Rate can be also gradually increased.Due to the closure in tunnel, once fire incident occurs, consequence is hardly imaginable.China is built at present Cause anxiety at the tunnel safety measure come into operation, security risk is very big.The massive losses of tunnel fire hazard accident, cause people couple The safety in tunnel and the very big concern of fire problem.These road surfaces need to have preferable flame retardant property, to guarantee safety.Perhaps The research that tunnel fire hazard is prevented and treated is classified as important project by multinational family.China also has begun attention to tunnel fire in recent years The research of calamity is tried hard to bottom out the danger of tunnel fire hazard with loss.And the anti-flammability of pitch is improved, making flame-retardant pitch Concrete road surface is one of Asphalt Pavement Fire casualties and the important measures of material damage in current reduction tunnel.
Common fire retardant has halogen system, phosphorus system, nitrogen system, antimonial class, boron compound class, magnesium compound class, calorize to close Species etc..If Chinese patent CN101817936A discloses a kind of composite fire retardant used for asphalt mixture and preparation method thereof, Wherein contain organic bromide fire retardant.Such organic fire-retardant (such as halogen contained compound) flame retardant effect is preferable, but it is in high temperature When can discharge toxic irritative gas, this is proposed very high want not only for the production and construction of hot-mix asphalt mixture It asks, and personnel health is also very unfavorable to construction personnel and in the future in operational process.Currently, fire retardant is just towards Halogen, low The direction of malicious, low cigarette is developed.Wherein, metal hydroxides has fire-retardant, suppression cigarette, the secondary dirt of reduction as environment friendly flame retardant The features such as dye, is widely used.However, there is also certain disadvantage when metal hydroxides is applied as fire retardant, Such as additive amount is needed to show apparent flame retardant effect compared with Gao Caineng.
Montmorillonite is relatively chiefly used in the fire-retardant of the materials such as textile, nylon as a kind of common fire proofing.Specially such as China Sharp CN201110427336 discloses a kind of nano flame retardant nylon, and CN201310211318 discloses a kind of Intumescent Retardant System pair The flame-retardant finishing method of pure cotton fabric.But due to the feature that pitch height glues, rheological property is poor, makes its compatibility with montmorillonite Difference influences the dispersibility and uniformity of montmorillonite, influences flame retardant effect.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention one is designed to provide a kind of fire-retardant drip of organic montmorillonite It is green.Another object of the present invention is to further increase the highly polar of montmorillonite surface, to improve montmorillonite inorganic particle Dispersibility and uniformity of the grain in pitch, reduce the loading of fire retardant, realize organic fire-retardant and inorganic fire retardants Between mutual supplement with each other's advantages.A kind of road asphalt of excellent flame retardancy is finally provided.
The present invention provides a kind of organic montmorillonite flame-retardant pitch, includes: by weight
Basic asphalt 100;
Organo-mineral complexing fire retardant 2~15;
Wherein organo-mineral complexing fire retardant is montmorillonite particle surface cladding polyphosphoric acids amine salt with nucleocapsid structure Organo-mineral complexing fire proofing.I.e. using montmorillonite, polyphosphoric acids (PPA) and aminated compounds as raw material, by micron Grade montmorillonite particle surface is modified and coats the montmorillonite organo-mineral complexing with nucleocapsid structure of polyphosphoric acids amine salt preparation Fire retardant.The wherein weight content of each substance are as follows:
Montmorillonite: 10%~25%
Polyphosphoric acids: 20%~40%
Amine: 35%~55%
The montmorillonite particle is micron order phyllosilicate, and smectite content is greater than 96%.Its partial size is preferably 5um To 20um.Wherein the degree of polymerization of the polyphosphoric acids is less than 1000.
In the present invention, aminated compounds can be lauryl amine, cetylamine, octadecylamine, ethylenediamine, sec-butylamine, trioctylamine, third One of amide, butyramide, cyclohexylamine, p-phenylenediamine etc. are a variety of.
In road fire-resistant modified pitch of the present invention, basic asphalt can specifically be determined according to the requirement used, such as No. 70 drips Blueness, No. 90 pitch etc..
In road fire-resistant modified pitch of the present invention, the preparation method of organo-mineral complexing fire retardant is as follows:
(1) under conditions of high-speed stirred (1000~1500r/min), that montmorillonite is rapidly added polyphosphoric acids ethyl alcohol is molten Liquid, lasting stirring such as at least 20min, preferably 25min-60min, filters.
(2) amine ethanol solution is added in filter cake in step (1), is stirred for 30min~80min after the completion of charging, filtered.
(3) it washs, be dried in vacuo, finally obtain graininess organo-mineral complexing fire retardant.
Organically-modified or inorganic-organic hybrid modified montmorillonoid has good dispersibility, such as by passing through of organic matter It learns key and is coated on montmorillonite powder surface, form a kind of hydrophobicity organo-mineral complexing fire retardant with nucleocapsid structure, thus Change the highly polar of montmorillonite surface.Dispersibility and uniformity of the montmorillonite inorganic powder particle in pitch can be improved, reduce The loading of fire retardant, realizes the mutual supplement with each other's advantages between organic fire-retardant and inorganic fire retardants.Traditional nothing is overcome simultaneously The shortcomings that machine object filled bitumen, assigns material excellent mechanical property, anti-fatigue performance, dimensional stability and gas barrier properties Deng.
In the method for the present invention, the composition principle of organo-mineral complexing fire retardant is montmorillonite surface grafting poly in the micron-scale Phosphoric acid long-chain makes its surface introduce multiple acid hydroxy groups, adds amine generation acid-base reaction and obtains surface cladding polyphosphoric acid amine Organo-mineral complexing fire retardant.Its reaction mechanism:
Invention also provides a kind of preparation methods of organic montmorillonite flame-retardant pitch, comprising:
(1) organic inorganic composite flame retardants are prepared;
(2) organo-mineral complexing fire retardant prepared by step (1) is added in pitch and is organised up to of the invention Montmorillonite flame-retardant pitch.
Wherein organic inorganic composite flame retardants are prepared described in step (1), comprising:
(1) under conditions of 1000~1500r/min high-speed stirred, it is molten that montmorillonite is rapidly added polyphosphoric acids ethyl alcohol Liquid continues stirring until few 20min, preferably 25min-60min, filters;
(2) amine ethanol solution is added in filter cake in step (1), is stirred for 30min~80min after the completion of charging, filtered;
(3) it washs, be dried in vacuo, finally obtain graininess organo-mineral complexing fire retardant.
Organo-mineral complexing fire retardant described in step (2) is added to the process in pitch are as follows: by the organic-inorganic Composite flame-retardant agent is added in 120 DEG C~160 DEG C of pitch, shears 20min at 3000~4000r/min with high-speed shearing machine ~60min to get arrive organic montmorillonite flame-retardant pitch of the present invention.Wherein organic montmorillonite fire retardant and pitch additive amount Are as follows: 100 parts of basic asphalt;2~15 parts of organic modification montmonrillonite organo-mineral complexing fire retardant.
Compared with prior art, advantages of the present invention is as follows:
1, the layer structure of montmorillonite can improve the rheological property and anti-aging property of pitch well in the present invention, Increase pitch hardness, improve pitch thermo oxidative aging and anti-light oxygen aging ability.Inorganic montmorillonite after organic intercalation, Interlamellar spacing can significantly increase, so that the compatibility of montmorillonite and pitch improves, modified effect is more excellent.
2, the present invention coats polyphosphoric acids amine salt by montmorillonite particle Surface Creation chemical bond in the micron-scale and prepares Organo-mineral complexing fire proofing with nucleocapsid structure improves dispersibility of the montmorillonite inorganic powder particle in pitch And uniformity, the loading of fire retardant is reduced, the mutual supplement with each other's advantages between organic fire-retardant and inorganic fire retardants is realized.
3, polyphosphoric acid amine is a kind of efficient organic expander type fire retardant in the present invention, the amount of being generally filled with lO%~ It can reach outstanding flame retardant property when 20%.If only montmorillonite and the simple physical mixed of polyphosphoric acid amine are applied to In pitch, the poor compatibility due to the highly polar of montmorillonite surface and between pitch will be greatly reduced the stability of modified pitch.
4, montmorillonite has certain flame retardant property in the present invention, after being coated with by surface grafting, with polyphosphoric acid amine It cooperates, cooperative flame retardant, there is good fire-retardant and smoke suppressing effect.Flame-retardant pitch oxygen index (OI) of the present invention is high, and when burning does not produce The toxic gases such as raw hydrogen halides are small to human respiratory tract and other organ damages.Preparation process is simple, produces pollution-free, production Cost is relatively low.
Specific embodiment
Now in conjunction with specific embodiment, the present invention will be described in detail, but is not so limited the present invention.
Embodiment 1
The preparation of organo-mineral complexing fire retardant:
Wherein smectite content is greater than 97% in montmorillonite, partial size 10um.The degree of polymerization of polyphosphoric acids is 100.
(1) under conditions of high-speed stirred (1000~1500r/min), it is molten that montmorillonite is rapidly added polyphosphoric acids ethyl alcohol Liquid persistently stirs 20min, filters.
(2) lauryl amine ethanol solution is added in filter cake in step (1), is stirred for lh after the completion of charging, filtered.
(3) it washs, be dried in vacuo, finally obtain that particle dispersion is good, the fluffy organo-mineral complexing for not needing grinding Fire retardant.
Wherein, wherein the weight content of each substance are as follows:
Montmorillonite: 25%
Polyphosphoric acids: 25%
Lauryl amine: 50%
Preparing for organic-inorganic flame-retardant pitch is as follows:
The organic montmorillonite fire retardant of above-mentioned preparation is added in 150 DEG C of 70# pitch, is existed with high-speed shearing machine 30min is sheared under 3000~4000r/min, obtains organic montmorillonite flame-retardant pitch.Wherein organic montmorillonite fire retardant and The weight ratio of pitch is 1:10.
Embodiment 2
The preparation of organo-mineral complexing fire retardant:
Wherein smectite content is greater than 97% in montmorillonite, partial size 10um.The degree of polymerization of polyphosphoric acids is 100.
(1) under conditions of high-speed stirred (1000~1500r/min), it is molten that montmorillonite is rapidly added polyphosphoric acids ethyl alcohol Liquid persistently stirs 20min, filters.
(2) cetylamine ethanol solution is added in filter cake in step (1), is stirred for lh after the completion of charging, filtered.
(3) it washs, be dried in vacuo, finally obtain that particle dispersion is good, the fluffy organo-mineral complexing for not needing grinding Fire retardant.
Wherein, wherein the weight content of each substance are as follows:
Montmorillonite: 25%
Polyphosphoric acids: 30%
Cetylamine: 45%
Preparing for organic-inorganic flame-retardant pitch is as follows:
The organic montmorillonite fire retardant of above-mentioned preparation is added in 150 DEG C of 70# pitch, is existed with high-speed shearing machine 30min is sheared under 3000~4000r/min, obtains organic montmorillonite flame-retardant pitch.Wherein organic montmorillonite fire retardant and The weight ratio of pitch is 3:20.
Embodiment 3
The preparation of organo-mineral complexing fire retardant:
Wherein smectite content is greater than 97% in montmorillonite, partial size 10um.The degree of polymerization of polyphosphoric acids is 100.
(1) under conditions of high-speed stirred (1000~1500r/min), it is molten that montmorillonite is rapidly added polyphosphoric acids ethyl alcohol Liquid persistently stirs 20min, filters.
(2) octadecylamine ethanol solution is added in filter cake in step (1), is stirred for lh after the completion of charging, filtered.
(3) it washs, be dried in vacuo, finally obtain that particle dispersion is good, the fluffy organo-mineral complexing for not needing grinding Fire retardant.
Wherein, wherein the weight content of each substance are as follows:
Montmorillonite: 25%
Polyphosphoric acids: 35%
Octadecylamine: 45%
Preparing for organic-inorganic flame-retardant pitch is as follows:
The organic montmorillonite fire retardant of above-mentioned preparation is added in 150 DEG C of 70# pitch, is existed with high-speed shearing machine 30min is sheared under 3000~4000r/min, obtains organic montmorillonite flame-retardant pitch.Wherein organic montmorillonite fire retardant and The weight ratio of pitch is 1:5.
Comparison array 1
Montmorillonite is added in 150 DEG C of pitch, shears 30min at 3000~4000r/min with high-speed shearing machine, Obtain flame-retardant pitch.Wherein the weight ratio of montmorillonite and pitch is 4:10.
Comparison array 2
Aluminium hydroxide is added in 150 DEG C of pitch, is sheared at 3000~4000r/min with high-speed shearing machine 30min obtains flame-retardant pitch.Wherein the weight ratio of aluminium hydroxide and pitch is 3:10.
The performance indicator of 1 fire-retardant modified asphalt of table
As it can be seen from table 1 the oxygen that organic montmorillonite fire retardant of the invention can effectively improve flame-retardant pitch refers to Number.After organically-modified to montmorillonite progress, hence it is evident that reduce its dosage, improve its compatibility.By covering in the micron-scale It is fire-retardant that de- soil particle Surface Creation chemical bond cladding polyphosphoric acids amine salt has prepared the organo-mineral complexing with nucleocapsid structure Material improves dispersibility and uniformity of the montmorillonite inorganic powder particle in pitch, reduces the loading of fire retardant, real The mutual supplement with each other's advantages between organic fire-retardant and inorganic fire retardants is showed.

Claims (9)

1. a kind of organic montmorillonite flame-retardant pitch, it is characterised in that: include: by weight
100 parts of basic asphalt;
2~15 parts of organo-mineral complexing fire retardant;
The organo-mineral complexing fire retardant is using montmorillonite, polyphosphoric acids and aminated compounds as raw material, by being 5 to partial size μm to 20 μm of montmorillonite particle surfaces are modified and the organic and inorganic compound with nucleocapsid structure of cladding polyphosphoric acids amine salt preparation Close fire retardant;
The weight content of each substance in the organo-mineral complexing fire retardant are as follows:
Montmorillonite: 10%~25%
Polyphosphoric acids: 20%~40%
Aminated compounds: 35%~55%.
2. organic montmorillonite flame-retardant pitch described in accordance with the claim 1, it is characterised in that: the montmorillonite particle is micro- Meter level phyllosilicate, smectite content are greater than 96%.
3. organic montmorillonite flame-retardant pitch described in accordance with the claim 1, it is characterised in that: the polymerization of the polyphosphoric acids Degree is less than 1000.
4. organic montmorillonite flame-retardant pitch described in accordance with the claim 1, it is characterised in that: the organo-mineral complexing is fire-retardant The preparation method of agent is as follows:
(1) under conditions of 1000~1500r/min high-speed stirred, montmorillonite is rapidly added polyphosphoric acids ethanol solution, is held Continuous stirring at least 20min is filtered;
(2) aminated compounds ethanol solution is added in filter cake in step (1), is stirred for 30min~80min after the completion of charging, taken out Filter;
(3) it washs, be dried in vacuo, finally obtain graininess organo-mineral complexing fire retardant.
5. organic montmorillonite flame-retardant pitch according to claim 4, it is characterised in that: when persistently being stirred in step (1) Between be 25 min -60min.
6. a kind of preparation method of any one of claim 1-5 organic montmorillonite flame-retardant pitch, it is characterised in that the system It is standby to include:
(1) organic inorganic composite flame retardants are prepared;
(2) organo-mineral complexing fire retardant prepared by step (1) is added in pitch up to the fire-retardant drip of organic montmorillonite It is green.
7. preparation method according to claim 6, it is characterised in that: prepare organo-mineral complexing resistance described in step (1) Firing agent includes:
(1) under conditions of 1000~1500r/min high-speed stirred, montmorillonite is rapidly added polyphosphoric acids ethanol solution, is held Continuous stirring at least 20min is filtered;
(2) aminated compounds ethanol solution is added in filter cake in step (1), is stirred for 30min~80min after the completion of charging, taken out Filter;
(3) it washs, be dried in vacuo, finally obtain graininess organo-mineral complexing fire retardant.
8. preparation method according to claim 7, it is characterised in that: continuing mixing time in step (1) is 25 min- 60min。
9. preparation method according to claim 6, it is characterised in that: organo-mineral complexing fire retardant described in step (2) The process being added in pitch are as follows: the organo-mineral complexing fire retardant is added in 120 DEG C~160 DEG C of pitch, is used High-speed shearing machine shears 20min~60min at 3000~4000r/min to get organic montmorillonite flame-retardant pitch is arrived, wherein Organic montmorillonite fire retardant and pitch additive amount are as follows: 100 parts of basic asphalt;Organic modification montmonrillonite organo-mineral complexing is fire-retardant 2~15 parts of agent.
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CN111501375B (en) * 2020-04-30 2023-06-09 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
CN111501374B (en) * 2020-04-30 2023-03-28 山东普文特防水科技股份有限公司 Modified asphalt waterproof coiled material with excellent flame retardant property and preparation method thereof

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CN102757581A (en) * 2012-07-31 2012-10-31 华南理工大学 Intumescent flame retardant functional silicate and preparation method thereof
CN103102109A (en) * 2011-11-09 2013-05-15 中国石油化工股份有限公司 Phase-change energy storage floor tile and manufacturing method thereof
CN103467777A (en) * 2013-06-27 2013-12-25 石河子大学 Lanthanum-based organic acid montmorillonite and water phase one-step preparation technology thereof

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CN102604396A (en) * 2012-02-13 2012-07-25 长安大学 Synergic flame retardance asphalt material and preparation method thereof
CN102757581A (en) * 2012-07-31 2012-10-31 华南理工大学 Intumescent flame retardant functional silicate and preparation method thereof
CN103467777A (en) * 2013-06-27 2013-12-25 石河子大学 Lanthanum-based organic acid montmorillonite and water phase one-step preparation technology thereof

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