CN108864698A - A kind of protective metal shell fire proofing material and preparation method thereof - Google Patents
A kind of protective metal shell fire proofing material and preparation method thereof Download PDFInfo
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- CN108864698A CN108864698A CN201810837702.3A CN201810837702A CN108864698A CN 108864698 A CN108864698 A CN 108864698A CN 201810837702 A CN201810837702 A CN 201810837702A CN 108864698 A CN108864698 A CN 108864698A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical & Material Sciences (AREA)
- 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)
Abstract
The invention discloses a kind of protective metal shell fire proofing materials, it is made of the raw material of following weight parts：Tributyl phosphate 10-13, diethylenetriamine 4-6, aluminum oxide 0.1-0.12, modified caprolactam 170-200, initiator 3-4, calcium stearate 2-4, Adipoyl Chloride 3-5, pyridine 0.01-0.02, superfine silicon dioxide aeroge 20-30; it adopts and invents imidazoline modified tributyl phosphate; the fire retardant performance of finished product not only can be improved; but also the corrosion resistance of metal can be improved, improve the protecting effect to metal base.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of protective metal shell fire proofing material and preparation method thereof.
Background technique
Currently, halogen flame is still used to the fire-retardant research of glass fiber reinforced nylon 6 both at home and abroad, however, halogen flame retardant
Noxious material is generated when agent is burnt for glass fiber reinforced nylon 6 composite material and seriously affects people's lives and health, simultaneously
Environmental requirement is not achieved in the problem of environmental pollution of generation, therefore present many industries and department are all being limited or are being forbidden to use
Halogen flame, and the sheath material of metal only focuses on its mechanical property mostly at present, studies very the Corrosion Protection of metal
Few, protective metal shell material some since leakproofness is poor is easy for that various gases, liquid, high/low temperature etc. is caused to cause metal
Corrosion, and even if leakproofness good sheath material again, it is also difficult to guarantee to play various gases, liquid, high/low temperature anti-well
Property, meanwhile, once sheath material is destroyed, after exposed metal/bare metal, corrosion rate quickly, therefore, if inside sheath material
The effect that can carry out anticorrosive protection to metal is introduced, then can play better protectiveness.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of protective metal shell fire proofing material and its
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of protective metal shell fire proofing material, it is made of the raw material of following weight parts：
Tributyl phosphate 10-13, diethylenetriamine 4-6, aluminum oxide 0.1-0.12, modified caprolactam 170-200,
Initiator 3-4, calcium stearate 2-4, Adipoyl Chloride 3-5, pyridine 0.01-0.02, superfine silicon dioxide aeroge 20-30.
The initiator is one of cumyl peroxide, dibenzoyl peroxide.
What the modification caprolactam was made of the raw material of following weight parts：
Caprolactam 100-110, lignin 13-20, oxalic acid 8-10, chloroform 40-50, pyridine 0.01-0.02.
The preparation method of the modification caprolactam, includes the following steps：
(1) lignin is taken, in sodium hydroxide solution that be added to 5-6 times of its weight, 0.7-1mol/l, it is small to impregnate 2-3
When, it is sent in baking oven, is dried at 80-90 DEG C to constant weight, discharging cooling obtains activation lignin；
(2) oxalic acid is taken, is added in chloroform, is stirred evenly, caprolactam is added, increasing temperature is 50-55 DEG C, and heat preservation is stirred
It mixes 2-3 hours, above-mentioned activation lignin is added, stirs evenly, is sent in ice-water bath, pyridine is added, it is small to be stirred to react 6-10
When, it discharges, revolving removes chloroform to get the modified caprolactam.
A kind of preparation method of protective metal shell fire proofing material, includes the following steps：
(1) initiator is taken, is added in the isopropanol of 20-30 times of its weight, stirs evenly；
(2) tributyl phosphate, calcium stearate mixing are taken, is added in the chloroform of 6-8 times of mixture weight, stirs evenly,
Obtain ester dispersion liquid；
(3) diethylenetriamine is taken, is added in above-mentioned ester dispersion liquid, aluminum oxide is added, is sent in reaction kettle, is led to
Enter nitrogen, increasing temperature is 140-146 DEG C, insulated and stirred 3-5 hours, continues to increase temperature to be 200-210 DEG C, reacts 100-
110 minutes, discharging obtained ester modified imidazoline；
(4) superfine silicon dioxide aeroge, Adipoyl Chloride mixing are taken, is added in the chloroform of 2-3 times of mixture weight,
It insulated and stirred 1-2 hours at 50-60 DEG C, is mixed with above-mentioned ester modified imidazoline, stirs evenly, be sent in ice-water bath, be added
Pyridine is stirred to react 3-4 hours, is discharged, revolving, removes chloroform, and drying 1-2 hours at 60-70 DEG C of vacuum, discharging cooling obtains
Organically-modified aeroge；
(5) above-mentioned organically-modified aeroge is taken, is mixed with modified caprolactam, is stirred evenly, be sent in reaction kettle, add
Enter above-mentioned initiator solution, be passed through nitrogen, adjusting temperature of reaction kettle is 60-75 DEG C, insulated and stirred 3-5 hours, is filtered, by filter cake
Washing, air drying is to get the protective metal shell fire proofing material.
Advantages of the present invention：
The present invention uses naoh treatment lignin first, later by caprolactam chloride, promotes under cryogenic conditions
Phenolic hydroxyl group and acyl chlorides react in lignin, so as to improve the compatibility of lignin and caprolactam monomer, and then improve
Dispersibility of the lignin between polymer improves the toughness and intensity of finished product；The present invention passes through using tributyl phosphate as raw material
It is reacted after imidazoline modified with the Adipoyl Chloride solution blending of aeroge, so as to improve the surface-active of aeroge, Zhi Houyu
The caprolactam monomer blending polymerization of lignin modification, so as to improve dispersion compatibility of the aeroge in finished-product material, into
One step improves the mechanical property of finished product, while using imidazoline modified tributyl phosphate, and the fire prevention of finished product not only can be improved
Flame retardant property, and can interact to form protective layer with the unpaired electron of metal surface, the anti-corruption of metal can be improved
Corrosion energy improves the protection effect to metal base.
Specific embodiment
Embodiment 1
A kind of protective metal shell fire proofing material, it is made of the raw material of following weight parts：
Tributyl phosphate 13, diethylenetriamine 6, aluminum oxide 0.12, modified caprolactam 200, initiator 4, tristearin
Sour calcium 4, Adipoyl Chloride 5, pyridine 0.02, superfine silicon dioxide aeroge 30.
The initiator is dibenzoyl peroxide.
What the modification caprolactam was made of the raw material of following weight parts：
Caprolactam 110, lignin 20, oxalic acid 10, chloroform 50, pyridine 0.02.
The preparation method of the modification caprolactam, includes the following steps：
(1) lignin is taken, in sodium hydroxide solution that be added to 6 times of its weight, 1mol/l, impregnates 3 hours, is sent to
In baking oven, dried at 90 DEG C to constant weight, discharging cooling obtains activation lignin；
(2) oxalic acid is taken, is added in chloroform, is stirred evenly, caprolactam is added, increasing temperature is 55 DEG C, insulated and stirred 3
Hour, above-mentioned activation lignin is added, stirs evenly, is sent in ice-water bath, pyridine is added, is stirred to react 10 hours, discharges,
Revolving removes chloroform to get the modified caprolactam.
A kind of preparation method of protective metal shell fire proofing material, includes the following steps：
(1) initiator is taken, is added in the isopropanol of 30 times of its weight, stirs evenly；
(2) tributyl phosphate, calcium stearate mixing are taken, is added in 8 times of mixture weight of chloroform, is stirred evenly, obtain
Ester dispersion liquid；
(3) diethylenetriamine is taken, is added in above-mentioned ester dispersion liquid, aluminum oxide is added, is sent in reaction kettle, is led to
Enter nitrogen, increasing temperature is 146 DEG C, insulated and stirred 5 hours, continues to increase temperature to be 210 DEG C, react 110 minutes, discharging obtains
Ester modified imidazoline；
(4) superfine silicon dioxide aeroge, Adipoyl Chloride mixing are taken, is added in 3 times of mixture weight of chloroform, 50
Insulated and stirred 2 hours at DEG C mix with above-mentioned ester modified imidazoline, stir evenly, be sent in ice-water bath, and pyridine is added, stirs
Reaction 4 hours is mixed, is discharged, revolving removes chloroform, and drying 2 hours at 70 DEG C of vacuum, discharging cooling obtains organically-modified aeroge；
(5) above-mentioned organically-modified aeroge is taken, is mixed with modified caprolactam, is stirred evenly, be sent in reaction kettle, add
Enter above-mentioned initiator solution, is passed through nitrogen, adjusting temperature of reaction kettle is 75 DEG C, it insulated and stirred 5 hours, filters, filter cake is washed,
Air drying is to get the protective metal shell fire proofing material.
Embodiment 2
A kind of protective metal shell fire proofing material, it is made of the raw material of following weight parts：
Tributyl phosphate 10, diethylenetriamine 4, aluminum oxide 0.1, modified caprolactam 170, initiator 3, stearic acid
Calcium 2, Adipoyl Chloride 3, pyridine 0.01, superfine silicon dioxide aeroge 20.
The initiator is cumyl peroxide.
What the modification caprolactam was made of the raw material of following weight parts：
Caprolactam 100, lignin 13, oxalic acid 8, chloroform 40, pyridine 0.01.
The preparation method of the modification caprolactam, includes the following steps：
(1) lignin is taken, in sodium hydroxide solution that be added to 5 times of its weight, 0.7mol/l, impregnates 2 hours, is sent into
Into baking oven, dried at 80 DEG C to constant weight, discharging cooling obtains activation lignin；
(2) oxalic acid is taken, is added in chloroform, is stirred evenly, caprolactam is added, increasing temperature is 50 DEG C, insulated and stirred 2
Hour, above-mentioned activation lignin is added, stirs evenly, is sent in ice-water bath, pyridine is added, is stirred to react 6 hours, discharges,
Revolving removes chloroform to get the modified caprolactam.
A kind of preparation method of protective metal shell fire proofing material, includes the following steps：
(1) initiator is taken, is added in the isopropanol of 20 times of its weight, stirs evenly；
(2) tributyl phosphate, calcium stearate mixing are taken, is added in 6 times of mixture weight of chloroform, is stirred evenly, obtain
Ester dispersion liquid；
(3) diethylenetriamine is taken, is added in above-mentioned ester dispersion liquid, aluminum oxide is added, is sent in reaction kettle, is led to
Enter nitrogen, increasing temperature is 140 DEG C, insulated and stirred 3 hours, continues to increase temperature to be 200 DEG C, react 100 minutes, discharging obtains
Ester modified imidazoline；
(4) superfine silicon dioxide aeroge, Adipoyl Chloride mixing are taken, is added in 2 times of mixture weight of chloroform, 50
Insulated and stirred 1 hour at DEG C mixes with above-mentioned ester modified imidazoline, stirs evenly, be sent in ice-water bath, and pyridine is added, stirs
Reaction 3 hours is mixed, is discharged, revolving removes chloroform, and drying 1 hour at 60 DEG C of vacuum, discharging cooling obtains organically-modified aeroge；
(5) above-mentioned organically-modified aeroge is taken, is mixed with modified caprolactam, is stirred evenly, be sent in reaction kettle, add
Enter above-mentioned initiator solution, is passed through nitrogen, adjusting temperature of reaction kettle is 60 DEG C, it insulated and stirred 3 hours, filters, filter cake is washed,
Air drying is to get the protective metal shell fire proofing material.
According to GB/T2406.2-2009 standard, limit oxygen index is surveyed：
The protective metal shell fire proofing material of the embodiment of the present invention 1：30；
The protective metal shell fire proofing material of the embodiment of the present invention 1：31；
Commercially available pure nylon 6：20-25；
Using testing vertical flammability：
Using blowtorch, flame height about 10mm is adjusted, applies burning 10s in testing bar bottom surface end after flame stabilization
(testing bar is height 30cm, bottom surface is 3cm × 3cm) is then withdrawn blowtorch, is recorded residual flame time a (s), after residual flame extinguishes
Apply flame 10s again and withdraw blowtorch, records residual flame time b (s), be placed with absorbent cotton in sample bottom, seen whether combustion
Burn the low absorbent cotton that ignites of object；Every group of testing bar is 5；
Survey the sum of the residual flame time a+ residual flame time b of every group of 5 testing bars (s)：
The protective metal shell fire proofing material of the embodiment of the present invention 1 is testing bar：80s；And absorbent cotton is without igniting；
The protective metal shell fire proofing material of the embodiment of the present invention 2 is testing bar：73s；And absorbent cotton is without igniting；
Commercially available pure nylon 6 is testing bar：243s；Absorbent cotton ignites；
Comparative example 1：
It by 13 parts by weight of lignin, 6 100 parts by weight of nylon, 20 parts by weight of superfine silicon dioxide aeroge, mixes, stirring
Uniformly, it is sent in extruder, melting extrusion, cooling granulation；
Comparative example 2：
By 6 100 parts by weight of nylon, 20 parts by weight of superfine silicon dioxide aeroge, mixing stirs evenly, is sent to extrusion
In machine, melting extrusion, cooling granulation；
Performance test：
According to ASTM G154, by the embodiment of the present invention 1, the protective metal shell fire proofing material of embodiment 2, commercially available nylon 6, right
Than the material of embodiment 1, the material of comparative example 2, it is placed in QUV (340nm) accelerated weathering accelerator, is measured after 1000h
Tensile strength retention rate；
The protective metal shell fire proofing material of the embodiment of the present invention 1：92.0%；
The protective metal shell fire proofing material of the embodiment of the present invention 2：93.1%；
Commercially available nylon 6：68.1%；
The material of comparative example 1：78.1%；
The material of comparative example 2：77.3%；
Tensile strength (Mpa)
The protective metal shell fire proofing material of the embodiment of the present invention 1：88.3；
The protective metal shell fire proofing material of the embodiment of the present invention 2：89.1；
Commercially available nylon 6：55-65；
The material of comparative example 1：79.7；
The material of comparative example 2：74.3；
Bending strength (Mpa)
The protective metal shell fire proofing material of the embodiment of the present invention 1：116.5；
The protective metal shell fire proofing material of the embodiment of the present invention 2：120.3；
Commercially available nylon 6：75-90；
The material of comparative example 1：103.4；
The material of comparative example 2：100.6.
Corrosion Protection test：
It selects iron steel pipe (40cm × 1cm × 1cm), using 6 sheath material of commercially available nylon, this hair of identical size, specification
Bright protective metal shell fire proofing material cladding, it is desirable that hermetic seal is fine, sample is respectively placed in water, 5% hydrochloric acid solution, 5%
It in sodium hydroxide solution, was taken out every 12 hours once, sheath is taken out whether observation iron steel pipe corrodes, if there is corruption
Erosion, then recording soaking time is t, does not occur corroding, and continues to cover upper jacket, be placed in coordinative solvent；
It measures；
Covering the iron steel pipe of commercially available 6 sheath material of nylon, t is 25 days in water, t is 48 hours in 5% hydrochloric acid solution,
T is 60 hours in 5% sodium hydroxide solution；
Being cased with the iron steel pipe of protective metal shell fire proofing material of the invention, t is 40 days in water, t is 6 in 5% hydrochloric acid solution
It, t is 7 days in 5% sodium hydroxide solution；
Said sample is tested using salt mist tester：
Salting liquid is the sodium chloride solution of 70g/l in experiment, and experiment the temperature inside the box is 35 DEG C, and spray pattern is continuous spray
Mist, salt fog deposition are 2.0ml/h80cm2, taken out every 12 hours once, sheath taken out whether observation iron steel pipe occurs
Corrosion then records if there is corrosion and carries out the salt spray test time as t, do not occur corroding, and continues to cover upper jacket, carries out salt fog
Test；
It measures：
The salt spray resistance t for being cased with the iron steel pipe of protective metal shell fire proofing material of the invention is 420 hours；
The salt spray resistance t for covering the iron steel pipe of commercially available 6 sheath material of nylon is 348 hours.
Claims (5)
1. a kind of protective metal shell fire proofing material, which is characterized in that it is made of the raw material of following weight parts：
Tributyl phosphate 10-13, diethylenetriamine 4-6, aluminum oxide 0.1-0.12, modified caprolactam 170-200, cause
Agent 3-4, calcium stearate 2-4, Adipoyl Chloride 3-5, pyridine 0.01-0.02, superfine silicon dioxide aeroge 20-30.
2. a kind of protective metal shell fire proofing material according to claim 1, which is characterized in that the initiator is peroxidating
One of diisopropylbenzene (DIPB), dibenzoyl peroxide.
3. a kind of protective metal shell fire proofing material according to claim 1, which is characterized in that the modification caprolactam is
It is made of the raw material of following weight parts：
Caprolactam 100-110, lignin 13-20, oxalic acid 8-10, chloroform 40-50, pyridine 0.01-0.02.
4. a kind of protective metal shell fire proofing material according to claim 3, which is characterized in that the modification caprolactam
Preparation method includes the following steps：
(1) lignin is taken, in sodium hydroxide solution that be added to 2-3 times of its weight, 0.7-1mol/l, impregnates 2-3 hours, send
Enter into baking oven, is dried at 80-90 DEG C to constant weight, discharging cooling obtains activation lignin；
(2) oxalic acid is taken, is added in chloroform, is stirred evenly, caprolactam is added, increasing temperature is 50-55 DEG C, insulated and stirred 2-
3 hours, above-mentioned activation lignin is added, stirs evenly, is sent in ice-water bath, pyridine is added, is stirred to react 6-10 hours, out
Material, revolving remove chloroform to get the modified caprolactam.
5. a kind of preparation method of protective metal shell fire proofing material as described in claim 1, which is characterized in that include the following steps：
(1) initiator is taken, is added in the isopropanol of 20-30 times of its weight, stirs evenly；
(2) tributyl phosphate, calcium stearate mixing are taken, is added in the chloroform of 6-8 times of mixture weight, stirs evenly, obtain ester
Dispersion liquid；
(3) diethylenetriamine is taken, is added in above-mentioned ester dispersion liquid, aluminum oxide is added, is sent in reaction kettle, is passed through nitrogen
Gas, increasing temperature is 140-146 DEG C, insulated and stirred 3-5 hours, continues to increase temperature to be 200-210 DEG C, 100-110 points of reaction
Clock, discharging, obtains ester modified imidazoline；
(4) superfine silicon dioxide aeroge, Adipoyl Chloride mixing are taken, is added in the chloroform of 2-3 times of mixture weight, in 50-
It insulated and stirred 1-2 hours at 60 DEG C, is mixed with above-mentioned ester modified imidazoline, stirs evenly, be sent in ice-water bath, pyrrole is added
Pyridine is stirred to react 3-4 hours, is discharged, revolving, removes chloroform, and drying 1-2 hours at 60-70 DEG C of vacuum, discharging cooling must have
Machine modified aerogels；
(5) above-mentioned organically-modified aeroge is taken, is mixed with modified caprolactam, is stirred evenly, be sent in reaction kettle, in addition
Initiator solution is stated, nitrogen is passed through, adjusting temperature of reaction kettle is 60-75 DEG C, insulated and stirred 3-5 hours, is filtered, by filter cake water
It washes, air drying is to get the protective metal shell fire proofing material.
Priority Applications (1)
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| CN201810837702.3A CN108864698A (en) | 2018-07-26 | 2018-07-26 | A kind of protective metal shell fire proofing material and preparation method thereof |
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| CN201810837702.3A CN108864698A (en) | 2018-07-26 | 2018-07-26 | A kind of protective metal shell fire proofing material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826045A (en) * | 2020-07-30 | 2020-10-27 | 马鞍山市金韩防水保温工程有限责任公司 | Heat insulation coating for building exterior wall and preparation method thereof |
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| CN1631981A (en) * | 2004-11-19 | 2005-06-29 | 竺华锋 | Use of polyamide composite materials in preparation of pump or valve |
| CN103992636A (en) * | 2014-04-22 | 2014-08-20 | 天长市富信电子有限公司 | Nylon sheath material for power lines and preparation method thereof |
| CN104974510A (en) * | 2015-06-27 | 2015-10-14 | 青岛文晟汽车零部件有限公司 | High-performance fiber glass reinforced plastic composite material |
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2018
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|---|---|---|---|---|
| CN1631981A (en) * | 2004-11-19 | 2005-06-29 | 竺华锋 | Use of polyamide composite materials in preparation of pump or valve |
| CN103992636A (en) * | 2014-04-22 | 2014-08-20 | 天长市富信电子有限公司 | Nylon sheath material for power lines and preparation method thereof |
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| CN111826045A (en) * | 2020-07-30 | 2020-10-27 | 马鞍山市金韩防水保温工程有限责任公司 | Heat insulation coating for building exterior wall and preparation method thereof |
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Application publication date: 20181123 |