CN109054015A - A kind of light heat-resisting fire proofing material and preparation method thereof - Google Patents
A kind of light heat-resisting fire proofing material and preparation method thereof Download PDFInfo
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- CN109054015A CN109054015A CN201810866316.7A CN201810866316A CN109054015A CN 109054015 A CN109054015 A CN 109054015A CN 201810866316 A CN201810866316 A CN 201810866316A CN 109054015 A CN109054015 A CN 109054015A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of light heat-resisting fire proofing materials, it is composed of the following raw materials by weight: ammonium persulfate 0.4-0.5, caprolactam 280-300, cumyl peroxide 3-4, methylcellulose 20-30, glucose 10-16, graphene oxide 30-40, ammonium polyphosphate 1-4, sodium acrylate 15-20, pentaerythrite 10-13, phosphorus trichloride 10-15, chlorinated paraffin 5-7, catalyst 0.01-0.02, the present invention can form uniform and stable carbon-coating in burning, to play heat-insulating, fire-preventing performance, and phosphate can then play the fire protecting performance of collaboration, anti-flammability is thought to further improve finished product, the present invention be graphene can in polycaprolactam stable dispersion, so as to improve the mechanics and fire protecting performance of finished product.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of light heat-resisting fire proofing material and preparation method thereof.
Background technique
Nylon has very strong vitality, it is modified to essentially consist in it as most important kind maximum in engineering plastics
Realize high performance, the followed by requirement high performance to product of the industries itself such as automobile, electric appliance, communication, electronics, machinery increasingly
Strongly；
But nylon is there is also disadvantage, its chemical structure is mainly carbon and hydrogen composition, nylon be it is highly combustible,
Big calorimetric can be discharged rapidly when burning in a short time, is burnt along with dense smoke, and discharge CO, CO2, HCN, NH3, CH4, C2H6
Etc. toxic or inflammable gas；And since nylon melt intensity is lower, thus easily generation largely has flame dissolved drip in combustion
Cause the fire spreads quickly；Meanwhile material light after can discharge big calorimetric in a short time, easily cause second-time burning.From microcosmic
From the point of view of structure, combustion process is explained are as follows: nylon is heated under flame interaction first, when temperature reaches 220 DEG C or so nylon crystalline substances
Lattice are entirely destroyed, and material gradually softens melting, and with the further raising of temperature, material starts thermal oxide decomposition, macromolecule
It is broken at the weak bond of chain, is attacked first by free radical on strand with the hydrogen on nitrogen-atoms on the α methylene being connected at first
Oxidation generates hydroperoxides, makes nylon backbone breaking therewith, and molecular weight reduces, thermal stability decline.And after backbone breaking
The free radical attack that methylene on the segment of the low molecular weight of formation can also be dissociated, decomposes it thoroughly.Generate acyl in oneself
The fuel gas such as amine, benzene are simultaneously spread to surrounding, continue to provide raw material for burning, exist in daily life and production latent
Fire hazard.Nylon can generate a large amount of toxic, mordant flue gases in combustion, cause in a fire serious
Consequence；Therefore, the fire protecting performance for how improving nylon material, just seems very necessary.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of light heat-resisting fire proofing material and its
Preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of light heat-resisting fire proofing material, it is composed of the following raw materials by weight:
Ammonium persulfate 0.4-0.5, caprolactam 280-300, cumyl peroxide 3-4, methylcellulose 20-30, Portugal
Grape sugar 10-16, graphene oxide 30-40, ammonium polyphosphate 1-4, sodium acrylate 15-20, pentaerythrite 10-13, phosphorus trichloride 10-
15, chlorinated paraffin 5-7, catalyst 0.01-0.02.
The catalyst is p-methyl benzenesulfonic acid.
The degree of substitution DS of the methylcellulose is 1.5-2.
A kind of preparation method of light heat-resisting fire proofing material, comprising the following steps:
(1) glucose, methylcellulose mixing are taken, is added in the deionized water of 30-40 times of mixture weight, stirring is equal
It is even, graphene oxide is added, it is 1-2 hours ultrasonic, it is dehydrated, is then fed into retort at 200-250 DEG C, vacuum calcining: true
Reciprocal of duty cycle is 8-10Pa, and heating rate is 70-90 DEG C/min, and heat preservation roasting 10-12h, naturally cold after being warming up to 1050-1200 DEG C
But, carbonizing and modifying graphene is obtained；
(2) take above-mentioned carbonizing and modifying graphene, mixed with phosphorus trichloride, be added to 30-40 times of mixture weight go from
In sub- water, increasing temperature is 50-55 DEG C, insulated and stirred 1-2 hours, obtains phosphatization graphene dispersing solution；
(3) ammonium persulfate is taken, is added in the deionized water of 10-18 times of its weight, stirs evenly；
(4) sodium acrylate is taken, is added in above-mentioned phosphatization graphene dispersing solution, is stirred evenly, be sent in reaction kettle, is led to
Enter nitrogen, adjusting temperature of reaction kettle is 60-75 DEG C, and above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, season is added
Penta tetrol, increasing temperature is 90-96 DEG C, catalyst is added, insulated and stirred 1-2 hours, discharging cooling obtained phosphide doped graphene
Dispersion liquid；
(5) cumyl peroxide is taken, is added in the dehydrated alcohol of 6-9 times of its weight, stirs evenly, it is molten to obtain initiator
Liquid；
(6) caprolactam is taken, above-mentioned phosphide doped graphene dispersion liquid is added to, stirs evenly, be sent in reaction kettle,
It is passed through nitrogen, adjusting temperature of reaction kettle is 60-75 DEG C, and above-mentioned initiator solution is added, and insulated and stirred 3-5 hours, discharging cooled down,
It filters, filter cake is washed, air drying, mixed with remaining each raw material, stir evenly, be sent in extruder, melting extrusion is cold
But to get the light heat-resisting fire proofing material.
Advantages of the present invention:
The present invention is first using glucose, methylcellulose as carbon source, by being carbonized after dispersion is blended with graphene oxide, from
And the graphene of carbon load has been obtained, hydrolysis is blended with phosphorus trichloride later, then be blended with sodium acrylate monomers, makees in initiator
With lower polymerization, the graphene of Sodium Polyacrylate intercalation is obtained, is then blended with pentaerythrite, high temperature esterification, so as to improve stone
The reactivity of black alkene, so as to improve its dispersion compatibility between polycaprolactam, the present invention uses after being loaded by carbon
Polyalcohol intercalation can improve stability of the carbon between graphene layer, can form uniform and stable carbon-coating in burning, thus
Play heat-insulating, fire-preventing performance, and phosphate can then play the fire protecting performance of collaboration, thus further improve finished product think it is fire-retardant
Property, the present invention be graphene can in polycaprolactam stable dispersion, so as to improve the mechanics and fire protecting performance of finished product.
Specific embodiment
Embodiment 1
A kind of light heat-resisting fire proofing material, it is composed of the following raw materials by weight:
Ammonium persulfate 0.5, caprolactam 300, cumyl peroxide 4, methylcellulose 30, glucose 16, oxidation stone
Black alkene 40, ammonium polyphosphate 4, sodium acrylate 20, pentaerythrite 13, phosphorus trichloride 15, chlorinated paraffin 7, catalyst 0.02.
The catalyst is p-methyl benzenesulfonic acid.
The degree of substitution DS of the methylcellulose is 2.
A kind of preparation method of light heat-resisting fire proofing material, includes following steps:
(1) glucose, methylcellulose mixing are taken, is added in 40 times of mixture weight of deionized water, stirs evenly,
Graphene oxide is added, ultrasound 2 hours is dehydrated at 250 DEG C, is then fed into retort, vacuum calcining: vacuum degree is
10Pa, heating rate are 90 DEG C/min, and heat preservation roasting 12h, natural cooling obtain carbonizing and modifying graphene after being warming up to 1200 DEG C；
(2) above-mentioned carbonizing and modifying graphene is taken, is mixed with phosphorus trichloride, 40 times of mixture weight of deionized water is added to
In, increasing temperature is 55 DEG C, insulated and stirred 2 hours, obtains phosphatization graphene dispersing solution；
(3) ammonium persulfate is taken, is added in the deionized water of 18 times of its weight, stirs evenly；
(4) sodium acrylate is taken, is added in above-mentioned phosphatization graphene dispersing solution, is stirred evenly, be sent in reaction kettle, is led to
Enter nitrogen, adjusting temperature of reaction kettle is 75 DEG C, and above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, Ji Wusi is added
Alcohol, increasing temperature is 96 DEG C, catalyst is added, insulated and stirred 1-2 hours, discharging cooling obtained phosphide doped graphene dispersion liquid；
(5) cumyl peroxide is taken, is added in the dehydrated alcohol of 9 times of its weight, is stirred evenly, it is molten to obtain initiator
Liquid；
(6) caprolactam is taken, above-mentioned phosphide doped graphene dispersion liquid is added to, stirs evenly, be sent in reaction kettle,
It is passed through nitrogen, adjusting temperature of reaction kettle is 75 DEG C, and above-mentioned initiator solution is added, and insulated and stirred 5 hours, discharging cooling filtered,
Filter cake is washed, air drying, mixed with remaining each raw material, stir evenly, be sent in extruder, melting extrusion is cooling, i.e.,
Obtain the light heat-resisting fire proofing material.
Embodiment 2
A kind of light heat-resisting fire proofing material, it is composed of the following raw materials by weight:
Ammonium persulfate 0.4, caprolactam 280, cumyl peroxide 3, methylcellulose 20, glucose 10-16, oxidation
Graphene 30, ammonium polyphosphate 1, sodium acrylate 15, pentaerythrite 10, phosphorus trichloride 10, chlorinated paraffin 5, catalyst 0.01.
The catalyst is p-methyl benzenesulfonic acid.
The degree of substitution DS of the methylcellulose is 1.5-2.
A kind of preparation method of light heat-resisting fire proofing material, comprising the following steps:
(1) glucose, methylcellulose mixing are taken, is added in 30 times of mixture weight of deionized water, stirs evenly,
Graphene oxide is added, ultrasound 1 hour is dehydrated at 200 DEG C, is then fed into retort, vacuum calcining: vacuum degree 8Pa,
Heating rate is 70 DEG C/min, and heat preservation roasting 10h, natural cooling obtain carbonizing and modifying graphene after being warming up to 1050-1200 DEG C；
(2) above-mentioned carbonizing and modifying graphene is taken, is mixed with phosphorus trichloride, 30 times of mixture weight of deionized water is added to
In, increasing temperature is 50 DEG C, insulated and stirred 1 hour, obtains phosphatization graphene dispersing solution；
(3) ammonium persulfate is taken, is added in the deionized water of 10 times of its weight, stirs evenly；
(4) sodium acrylate is taken, is added in above-mentioned phosphatization graphene dispersing solution, is stirred evenly, be sent in reaction kettle, is led to
Enter nitrogen, adjusting temperature of reaction kettle is 60 DEG C, and above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3 hours, Ji Wusi is added
Alcohol, increasing temperature is 90 DEG C, catalyst is added, insulated and stirred 1 hour, discharging cooling obtained phosphide doped graphene dispersion liquid；
(5) cumyl peroxide is taken, is added in the dehydrated alcohol of 6 times of its weight, is stirred evenly, it is molten to obtain initiator
Liquid；
(6) caprolactam is taken, above-mentioned phosphide doped graphene dispersion liquid is added to, stirs evenly, be sent in reaction kettle,
It is passed through nitrogen, adjusting temperature of reaction kettle is 60 DEG C, and above-mentioned initiator solution is added, and insulated and stirred 3 hours, discharging cooling filtered,
Filter cake is washed, air drying, mixed with remaining each raw material, stir evenly, be sent in extruder, melting extrusion is cooling, i.e.,
Obtain the light heat-resisting fire proofing material.
Comparative example:
It by the nylon 6 of 280 parts by weight, is blended with the graphene oxide of 30 parts by weight, melting extrusion obtains contrast product.
Performance test:
The light heat-resisting fire proofing material of the embodiment of the present invention 1:
Tensile strength: 81.3Mpa, bending strength 101.3Mpa, oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, ratio
Weight is 0.94g/cm3；
The light heat-resisting fire proofing material of the embodiment of the present invention 2:
Tensile strength: 77.7Mpa, bending strength 91.5Mpa, oxygen index (OI) 31, V-0 grades of vertical combustion grade UL-94, ratio
Weight is 0.89g/cm3；
The product of comparative example:
Tensile strength: 63.0Mpa, bending strength 60.7Mpa, oxygen index (OI) 29, V-2 grades of vertical combustion grade UL-94, ratio
Weight is 0.11g/cm3。
Claims (4)
1. a kind of light heat-resisting fire proofing material, which is characterized in that it is composed of the following raw materials by weight:
Ammonium persulfate 0.4-0.5, caprolactam 280-300, cumyl peroxide 3-4, methylcellulose 20-30, glucose
10-16, graphene oxide 30-40, ammonium polyphosphate 1-4, sodium acrylate 15-20, pentaerythrite 10-13, phosphorus trichloride 10-15,
Chlorinated paraffin 5-7, catalyst 0.01-0.02.
2. a kind of light heat-resisting fire proofing material according to claim 1, which is characterized in that the catalyst is to methyl
Benzene sulfonic acid.
3. a kind of light heat-resisting fire proofing material according to claim 1, which is characterized in that the methylcellulose takes
It is 1.5-2 for degree DS.
4. a kind of preparation method of light heat-resisting fire proofing material as described in claim 1, which comprises the following steps:
(1) glucose, methylcellulose mixing are taken, is added in the deionized water of 30-40 times of mixture weight, stirs evenly,
Graphene oxide is added, it is 1-2 hours ultrasonic, it is dehydrated, is then fed into retort at 200-250 DEG C, vacuum calcining: vacuum degree
For 8-10Pa, heating rate is 70-90 DEG C/min, and heat preservation roasting 10-12h, natural cooling obtain after being warming up to 1050-1200 DEG C
Carbonizing and modifying graphene；
(2) above-mentioned carbonizing and modifying graphene is taken, is mixed with phosphorus trichloride, the deionized water of 30-40 times of mixture weight is added to
In, increasing temperature is 50-55 DEG C, insulated and stirred 1-2 hours, obtains phosphatization graphene dispersing solution；
(3) ammonium persulfate is taken, is added in the deionized water of 10-18 times of its weight, stirs evenly；
(4) sodium acrylate is taken, is added in above-mentioned phosphatization graphene dispersing solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen
Gas, adjusting temperature of reaction kettle is 60-75 DEG C, and above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, Ji Wusi is added
Alcohol, increasing temperature is 90-96 DEG C, catalyst is added, insulated and stirred 1-2 hours, discharging cooling obtained the dispersion of phosphide doped graphene
Liquid；
(5) cumyl peroxide is taken, is added in the dehydrated alcohol of 6-9 times of its weight, stirs evenly, obtain initiator solution；
(6) caprolactam is taken, above-mentioned phosphide doped graphene dispersion liquid is added to, stirs evenly, be sent in reaction kettle, be passed through
Nitrogen, adjusting temperature of reaction kettle is 60-75 DEG C, above-mentioned initiator solution is added, insulated and stirred 3-5 hours, discharging cooling was taken out
Filter, filter cake is washed, air drying, is mixed with remaining each raw material, is stirred evenly, be sent in extruder, melting extrusion is cold
But to get the light heat-resisting fire proofing material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862534A (en) * | 2019-11-13 | 2020-03-06 | 安徽微威减震降噪技术研究院 | Intercalation reinforced polyamide material and preparation method thereof |
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Application publication date: 20181221 |