CN109265751A - A kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating - Google Patents

A kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating Download PDF

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Publication number
CN109265751A
CN109265751A CN201810969988.0A CN201810969988A CN109265751A CN 109265751 A CN109265751 A CN 109265751A CN 201810969988 A CN201810969988 A CN 201810969988A CN 109265751 A CN109265751 A CN 109265751A
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China
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activated carbon
flame retardant
carbon fibre
composite nanometer
added
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CN201810969988.0A
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许涛
王斯文
张韩帅
夏文静
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Nanjing Forestry University
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Nanjing Forestry University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/12Adsorbed ingredients, e.g. ingredients on carriers
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/003Flushing
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12Treatment with organosilicon compounds

Abstract

It is an object of the present invention to provide a kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating, belong to technical field of flame retardant, solve the problems, such as that current bituminous pavement fire retardant volume is low, influence pitch routine service performance, release process is fast, flame retardant effect is poor.The present invention under the conditions of ultrasonic wave aid dispersion, activated carbon fibre is added in the mixed acid solution of the concentrated sulfuric acid and concentrated nitric acid first, carries out oxidation processes;Then, mixed acid solution is diluted, activated carbon fibre is placed on miillpore filter, cleaning active Carbon fibe, it is dry in baking oven;Activated carbon fibre is added in composite nanometer flame retardant ion salt solution again, ultrasonic disperse, be added ammonia precipitation process agent, continue to stir at room temperature, composite nanometer flame retardant be deposited in activated carbon fibre the hole in surface on;Finally, being added in silicone acrylic emulsion after dry, clad is formed on activated carbon fibre surface, fixed composite nanometer flame retardant particle improves bituminous pavement fire retardant volume, improves fire-retardant, smoke suppressing effect.

Description

A kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating
Technical field
The present invention is a kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating, belongs to the fire-retardant skill of bituminous pavement Art field.
Background technique
In recent years, great-leap-forward development is presented in China's Transportation Infrastructure Construction, and building for vcehicular tunnel also accordingly increases, but That pitch combustibility is the major safety problems that tunnel sheet pavement faces, when fire occurs for tunnel, temperature sharply on Rise, bituminous pavement participates in burning, generate big calorimetric and poison gas, and tunnel due to the particularity of its position, space it is long and narrow Limitation brings very big difficulty to trapped person's escape and fire rescue, leads to great casualties and property loss.
In order to make bituminous pavement that can also reach road environment special in tunnel while giving full play to own advantages It is required that i.e. flame-retardancy requirements, researcher mainly takes adds various different flame retardants, the method for smoke suppressant in bituminous pavement Come the heat and poison gas for reducing or tunnel fire hazard process bituminous pavement being delayed to generate, reduces bituminous pavement to the greatest extent and thermally decompose and join With burning, tunnel sheet pavement fire safety is improved.
However, bituminous pavement flame-retarding means are mainly the more single fire retardant of direct addition component in pitch, association at present It is poor with fire retarding effect, fire retardation can only be played in some relatively narrow temperature range of pitch multistage thermal decomposition process, it is difficult to Multistage fire-retardant demand caused by adapting to because of pitch each component thermal decomposition temperature section difference;In view of mixed to pitch or pitch Closing material pavement performance influences, and fire retardant volume is limited;The biggish micron order fire retardant of partial size is mainly used in order to improve dispersibility, Flame retardant effect is poor, and the asphalt after leading to admixture fire retardant still can thermally decompose under high temperature environment, burn, and generates big Calorimetric and poison gas, it is difficult to meet bituminous pavement multistage, overall process flame-retardancy requirements.
As it can be seen that generating big calorimetric and poison gas because bituminous pavement thermally decomposes when reducing tunnel fire hazard, tunnel is improved Asphalt Pavement Fire safety needs to increase fire retardant volume, and will not generate negative shadow to bituminous pavement routine pavement performance It rings.Although the fire-retardant research of bituminous pavement at present obtains certain progress, bituminous pavement flame retardant constituent is more single, partial size compared with Greatly, single-stage load, directly admixture, shortage cooperative flame retardant, road surface self-extinguishment is poor, and there is also many problem in science needs are further Research.
Activated carbon fibre (ACF) is the third generation to grow up after powdery, grain dress active carbon in 1970's New function adsorbent material, activated carbon fibre have in terms of fire-retardant agent carrier because of its good absorption, filling and stability Good application prospect.The fire retardant of activated carbon fiber-loaded type can greatly improve anti-flammability, not only solve conventional resistance in this way The problem that agent specific surface area is small, flame retardant activity is low, release process is fast is fired, and also eliminates pure nano level flame retardant band easy to reunite The problem come.But it currently without the research being related to using activated carbon fiber-loaded composite nanometer flame retardant and method for coating, mentions The additive amount of fire retardant and fire-retardant, smoke suppressing effect in high bituminous pavement.The present invention proposes multiple using activated carbon fiber-loaded nanometer Fire-retardant agent method is closed, and activated carbon fibre is coated, the reinforcement material as bituminous pavement, fixed nano composite fire retardant Agent improves tunnel sheet pavement fire safety.
Summary of the invention
(1) technical problem
Activated carbon fiber-loaded composite nanometer flame retardant and method for coating, this method are used it is an object of the present invention to provide a kind of Nanoscale composite flame-retardant agent is loaded using activated carbon fibre and suitable covering material is selected to coat it, is solved Bituminous pavement fire retardant volume is low at present, influence bituminous pavement routine service performance, release process is fast, flame retardant effect is poor asks Topic improves fire retardant to the efficient inhibiting effect of pitch thermal decomposition process.
(2) technical solution
That there are fire retardant volumes is low, it is fast to influence bituminous pavement routine service performance, release process in view of current bituminous pavement, The problem of flame retardant effect difference, the present invention provide a kind of activated carbon fiber-loaded composite nanometer flame retardant of use and coat to it Method.Technical solution of the present invention is as follows: first under the conditions of ultrasonic wave aid dispersion, activated carbon fibre being added to the concentrated sulfuric acid In the mixed acid solution of concentrated nitric acid, it is aided with mechanical stirring and carries out oxidation processes;Then, mixed acid solution is diluted with deionized water, it will Activated carbon fibre is placed on miillpore filter, cleaning active carbon fiber surface impurity and residue, drying for standby in baking oven;Then, Activated carbon fibre is added in the salting liquid of composite nanometer flame retardant ion, ultrasonic disperse, ammonia precipitation process agent is added, in room temperature Under continue to stir, composite nanometer flame retardant be deposited in activated carbon fibre hole and surface on;Finally, drying in an oven, then It is added in silicone acrylic emulsion, forms clad on activated carbon fibre surface, the composite nanometer flame retardant in fixed activated carbon fibre Particle.To improve bituminous pavement fire retardant volume, reducing influences bituminous pavement routine service performance, reduction rate of release, Improve flame retardant effect.
(3) beneficial effect
In order to make bituminous pavement that can also reach road environment special in tunnel while giving full play to own advantages It is required that i.e. flame-retardancy requirements, when fire occurs in tunnel, bituminous pavement does not encourage fire.Using activity provided by the invention The method that Carbon fibe loads nanoscale composite flame-retardant agent and suitable material is selected to coat it can increase fire retardant and stablize Property, delay fire retardant to discharge, to improve the flame retardant property of fire retardant so that fire retardant each step that pitch burns have with Matched fire retardant play effectiveness, play better flame retardant effect.Solve current bituminous pavement fire retardant volume it is low, influence drip Green road surface routine service performance, the release problem that process is fast, flame retardant effect is poor.The patented technology provided according to the present invention, passes through Industry-university-research linkage can develop pitch efficient flame-retarding agent with independent intellectual property rights actively with relevant enterprise cooperation, use In vcehicular tunnel and Urban Underground Passage bituminous pavement, tunnel and Urban Underground Passage fire safety can be improved, for large size Theoretical foundation is provided using flame-retardant pitch road surface in tunnel, tunnel is improved and Urban Underground Passage bituminous pavement is used for a long time Performance improves Asphalt Pavement Fire safety and durability, saves operation cost, has preferable economic benefit.
Specific embodiment
The present invention is that a kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating, specific implementation step are as follows:
(1) under ultrasonic wave dispersion condition, 5 grams of activated carbon fibre is added to and fill the concentrated sulfuric acid and concentrated nitric acid volume ratio is In 3: 1 mixed acid solution, it is aided in the case of 300 revs/min of mechanical stirring and carries out oxidation processes 3 hours;
(2) mixed acid solution is diluted to pH with deionized water is 6, and it is 0.2 micron poly- that activated carbon fibre, which is placed on aperture, On tetrafluoroethene miillpore filter, with deionized water cleaning active carbon fiber surface impurity and residue, in 80 DEG C of vacuum drying oven Middle drying 24 hours spare;
(3) spare activated carbon fibre is added to the salting liquid of the composite nanometer flame retardant ion containing required load In, and it is dispersed in the solution to be added a certain amount of polyvinyl alcohol enhancing activated carbon fibre, ultrasonic disperse 10 minutes;
(4) ammonia precipitation process agent is added, adjusting pH value of solution is 10, continues stirring 12 hours at room temperature, reacts in the liquid phase Generate composite nanometer flame retardant, and be deposited in activated carbon fibre the hole in surface on;
(5) activated carbon fibre for loading composite nanometer flame retardant is 24 hours dry in 105 DEG C of baking oven, load is made The activated carbon fibre of composite nanometer flame retardant particle;
(6) activated carbon fibre for loading composite nanometer flame retardant particle is added in silicone acrylic emulsion, under the conditions of 80 DEG C Stirring 5 hours keeps the temperature 12 hours at 40 DEG C, 12 hours dry at 105 DEG C, forms clad on activated carbon fibre surface, fixed Composite nanometer flame retardant particle in activated carbon fibre delays fire retardant rate of release under high temperature.

Claims (1)

1. a kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating, it is characterised in that the specific steps of this method are such as Under:
(1) under ultrasonic wave dispersion condition, 5 grams of activated carbon fibre is added to and fill the concentrated sulfuric acid and concentrated nitric acid volume ratio as 3:1 Mixed acid solution in, be aided in the case of 300 revs/min of mechanical stirring and carry out oxidation processes 3 hours;
(2) mixed acid solution is diluted to pH with deionized water is 6, and activated carbon fibre is placed on the polytetrafluoro that aperture is 0.2 micron On ethylene miillpore filter, with deionized water cleaning active carbon fiber surface impurity and residue, done in 80 DEG C of vacuum drying oven Dry 24 hours spare;
(3) spare activated carbon fibre is added in the salting liquid of the composite nanometer flame retardant ion containing required load, and It is dispersed in the solution that a certain amount of polyvinyl alcohol enhancing activated carbon fibre is added, ultrasonic disperse 10 minutes;
(4) ammonia precipitation process agent is added, adjusting pH value of solution is 10, continues stirring 12 hours at room temperature, and reaction generates in the liquid phase Composite nanometer flame retardant, and be deposited in activated carbon fibre hole and surface on;
(5) activated carbon fibre for loading composite nanometer flame retardant is 24 hours dry in 105 DEG C of baking oven, load nanometer is made The activated carbon fibre of composite flame-retardant agent particle;
(6) activated carbon fibre for loading composite nanometer flame retardant particle is added in silicone acrylic emulsion, stirs 5 under the conditions of 80 DEG C Hour, 12 hours are kept the temperature at 40 DEG C, it is 12 hours dry at 105 DEG C, clad, fixed active carbon are formed on activated carbon fibre surface Composite nanometer flame retardant particle on fiber delays fire retardant rate of release under high temperature.
CN201810969988.0A 2018-08-21 2018-08-21 A kind of activated carbon fiber-loaded composite nanometer flame retardant and method for coating Pending CN109265751A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007070738A (en) * 2005-09-05 2007-03-22 Gun Ei Chem Ind Co Ltd Extra fine phenol resin fiber, its assembly and method for producing the same
CN103694657A (en) * 2013-12-24 2014-04-02 南京理工大学 Flame-retardant polylactic acid material of ternary composite flame-retardant system and preparation method thereof
CN104845346A (en) * 2015-04-28 2015-08-19 芜湖众力部件有限公司 High-efficiency modified PC (Polycarbonate) composite material loading composite fiber retardant with active carbon fiber and preparation method thereof
CN105097302A (en) * 2015-09-15 2015-11-25 江苏苏通碳纤维有限公司 Activated carbon fibers for supercapacitor and preparation method therefor
CN105199182A (en) * 2015-10-28 2015-12-30 辽宁石油化工大学 Polyolefin flame retardant

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007070738A (en) * 2005-09-05 2007-03-22 Gun Ei Chem Ind Co Ltd Extra fine phenol resin fiber, its assembly and method for producing the same
CN103694657A (en) * 2013-12-24 2014-04-02 南京理工大学 Flame-retardant polylactic acid material of ternary composite flame-retardant system and preparation method thereof
CN104845346A (en) * 2015-04-28 2015-08-19 芜湖众力部件有限公司 High-efficiency modified PC (Polycarbonate) composite material loading composite fiber retardant with active carbon fiber and preparation method thereof
CN105097302A (en) * 2015-09-15 2015-11-25 江苏苏通碳纤维有限公司 Activated carbon fibers for supercapacitor and preparation method therefor
CN105199182A (en) * 2015-10-28 2015-12-30 辽宁石油化工大学 Polyolefin flame retardant

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Application publication date: 20190125

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