CN107586452A - A kind of phosphatization fiber intercalation modifying nylon material and preparation method thereof - Google Patents
A kind of phosphatization fiber intercalation modifying nylon material and preparation method thereof Download PDFInfo
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- CN107586452A CN107586452A CN201710820834.0A CN201710820834A CN107586452A CN 107586452 A CN107586452 A CN 107586452A CN 201710820834 A CN201710820834 A CN 201710820834A CN 107586452 A CN107586452 A CN 107586452A
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Abstract
The invention discloses a kind of phosphatization fiber intercalation modifying nylon material, it is made up of the raw material of following weight parts：Expansible graphite 18 20, stannous sulfide 0.1 0.2, nylon 130 150, string 25 30, chlorinated paraffin 34, acrylamide 24, phosphorus trichloride 35, three ammonium molybdates 0.4 1, allyl polyglycol 35, magnesium stearate 12, ZPT 0.5 1, maleic anhydride 10 16, MTES 13, calcium ricinoleate 0.4 1, castor oil acid 12, ammonium persulfate 0.6 1, potassium permanganate 35, material of the present invention is in burning, fibers carbonization, carbonized stock is distributed between graphene layer, graphene can improve carbonation intension, the direct calcination of flame is completely cut off, the conduction of heat is obstructed, serve good synergy, extend the resistance to combustion time, improve the fire protecting performance of finished product.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of phosphatization fiber intercalation modifying nylon material and preparation method thereof.
Background technology
Because nylon has the advantages that good mechanical performance and processability, heat resistance, corrosion resistance and self lubricity,
It is widely used in the every field such as telecommunications, textile, chemical industry manufacture.But there is also shortcoming, its chemistry for nylon
Structure is mainly carbon and hydrogen composition, and nylon is highly combustible, potential fire be present in daily life and production
Hidden danger, nylon can produce a large amount of poisonous, mordant flue gases, cause serious consequence in a fire in combustion.Mirror
In this, current many countries all attach great importance to the flame-retardant modified of nylon, are directed to developing and produce each based flame retardant；
In recent years, with state's manufacturing industry high speed development at this stage, all trades and professions product up-gradation speed is further frequent, to product material
Performance propose higher requirement, therefore the further performance of lifting nylon and to expand its use range imperative；Together
When constantly strengthening with the environmental consciousness of people, it is also increasingly harsh to the flame-retardancy requirements of nylon；Currently in order to improve nylon
Fire protecting performance, a variety of inorganic fire-retarded fillers are often added, these fillers are easily formed in nylon reunites, and causes the power of finished product
Hydraulic performance decline is learned, meanwhile, lifting of the inorganic filler for finished product fire resistance is more single, it is impossible to it is anti-to play collaboration from many aspects
The effect of fire.
The content of the invention
It is an object of the invention to easily be formed to reunite in nylon for filler in the prior art, the mechanics of finished product is caused
Hydraulic performance decline, meanwhile, lifting of the inorganic filler for finished product fire resistance is more single, it is impossible to plays collaboration fire prevention from many aspects
Effect the problem of, there is provided a kind of phosphatization fiber intercalation modifying nylon material and preparation method thereof.
To achieve the above object, the present invention uses following technical scheme：
A kind of phosphatization fiber intercalation modifying nylon material, it is made up of the raw material of following weight parts：
Expansible graphite 18-20, stannous sulfide 0.1-0.2, nylon 130-150, string 25-30, chlorinated paraffin 3-4, third
Acrylamide 2-4, phosphorus trichloride 3-5, three ammonium molybdate 0.4-1, allyl polyglycol 3-5, magnesium stearate 1-2, ZPT
0.5-1, maleic anhydride 10-16, MTES 1-3, calcium ricinoleate 0.4-1, castor oil acid 1-2, ammonium persulfate
0.6-1, potassium permanganate 3-5.
Described string is sisal fiber.
A kind of preparation method of phosphatization fiber intercalation modifying nylon material, comprises the following steps：
（1）String is taken, is added in the ammonium sulfite solution that concentration is 0.7-1mol/l, stirs 2-3 hours, add castor-oil plant
Oleic acid, rise temperature is 60-65 DEG C, insulated and stirred 30-40 minutes, obtains activated fiber solution；
（2）Calcium ricinoleate is taken, is added in the absolute ethyl alcohol of 10-17 times of its weight, chlorinated paraffin is added, is protected at 85-90 DEG C
Temperature stirring 20-30 minutes, MTES is added, stirs to normal temperature, obtains solution of silane；
（3）Phosphorus trichloride is taken, is added in the deionized water of 30-40 times of its weight, stirs, adds maleic anhydride, stirring
Uniformly, it is sent in reactor, is passed through nitrogen, regulation temperature of reaction kettle is 75-80 DEG C, adds ammonium persulfate, insulated and stirred 3-4
Hour, obtain phosphatization polymer solution；
（4）Above-mentioned activated fiber solution, the mixing of phosphatization polymer solution are taken, stirs, is sent in boiling water bath, insulated and stirred
1-2 hours, discharging, obtain phosphatization polymer fiber solution；
（5）Expansible graphite is taken, in sulfuric acid solution that be added to 10-14 times of its weight, 96-98%, is stirred, rise temperature
Spend for 46-50 DEG C, add potassium permanganate, insulated and stirred 6-9 hours, filtering, precipitation is washed, dried at 90-95 DEG C of vacuum
Entirely, expansion graphite oxide is obtained；
（6）Expansion graphite oxide is taken, is added in the deionized water of 20-37 times of its weight, adds acrylamide, ultrasonic 10-20
Minute, it is added in above-mentioned phosphatization polymer fiber solution, rise temperature is 65-70 DEG C, insulated and stirred 3-4 hours, obtains phosphatization
Fiber intercalated graphite alkene solution；
（7）Above-mentioned phosphatization fiber intercalated graphite alkene solution, solution of silane mixing are taken, is stirred, addition allyl polyglycol,
Stannous sulfide, ultrasonic 30-40 minutes, ethanol is distilled off, 1-2 hours are dehydrated at 180-190 DEG C, air drying, are obtained organic
Phosphatization fiber intercalated graphite alkene；
（8）Above-mentioned organophosphor chemical fibre dimension intercalated graphite alkene is taken, is mixed with remaining each raw material, is stirred, be sent in extruder,
Melting extrusion, cooling granulation, produce the phosphatization fiber intercalation modifying nylon material.
Advantages of the present invention：
The present invention is first using maleic anhydride as monomer, and ammonium persulfate is initiator, and phosphorus trichloride is dopant, under nitrogen effect
Polymerization, obtains phosphatization polymer solution, and then itself and activated fiber is blended, obtains phosphatization fiber solution, then with inflatable
Graphite is raw material, is handled by potassium permanganate oxidation, obtained expansion graphite oxide is mixed with phosphatization fiber solution, with propylene
Acid amides is intercalator, obtains phosphatization fiber intercalated graphite alkene solution, it is compatible between polymer can effectively to improve graphene
Property, reduce and reunite, improve the mechanical property of finished product, for material of the present invention in burning, fibers carbonization, carbonized stock is distributed to graphene
Interlayer, graphene can improve carbonation intension, completely cut off the direct calcination of flame, obstructed the conduction of heat, serve very well
Synergy, extend the resistance to combustion time, improve the fire protecting performance of finished product, while phosphatization material can be urged in burning by dehydration
Carbon is melted into, plays a part of heat-insulated, oxygen barrier to the material below carbon-coating, hinders the material under carbon-coating further to thermally decompose, has
Good gas phase fire retardation, improve the fire resistance of finished product.
Embodiment
Embodiment 1
A kind of phosphatization fiber intercalation modifying nylon material, it is made up of the raw material of following weight parts：
Expansible graphite 20, stannous sulfide 0.2, nylon 150, string 30, chlorinated paraffin 4, acrylamide 4, phosphorus trichloride
3-5, three ammonium molybdates 1, allyl polyglycol 5, magnesium stearate 2, ZPT 1, maleic anhydride 16, methyltriethoxy silane
Alkane 3, calcium ricinoleate 1, castor oil acid 2, ammonium persulfate 1, potassium permanganate 5.
Described string is sisal fiber.
A kind of preparation method of phosphatization fiber intercalation modifying nylon material, comprises the following steps：
（1）String is taken, is added in the ammonium sulfite solution that concentration is 1mol/l, stirs 3 hours, add castor oil acid,
It is 65 DEG C to raise temperature, insulated and stirred 40 minutes, obtains activated fiber solution；
（2）Calcium ricinoleate is taken, is added in the absolute ethyl alcohol of 17 times of its weight, adds chlorinated paraffin, the insulated and stirred at 90 DEG C
30 minutes, MTES is added, stirs to normal temperature, obtains solution of silane；
（3）Phosphorus trichloride is taken, is added in the deionized water of 30-40 times of its weight, stirs, adds maleic anhydride, stirring
Uniformly, it is sent in reactor, is passed through nitrogen, regulation temperature of reaction kettle is 80 DEG C, addition ammonium persulfate, insulated and stirred 4 hours,
Obtain phosphatization polymer solution；
（4）Above-mentioned activated fiber solution, the mixing of phosphatization polymer solution are taken, stirs, is sent in boiling water bath, insulated and stirred
1-2 hours, discharging, obtain phosphatization polymer fiber solution；
（5）Expansible graphite is taken, is added in 14 times of its weight, 98% sulfuric acid solution, stirs, rise temperature is 50
DEG C, potassium permanganate is added, insulated and stirred 9 hours, filtering, precipitation is washed, it is dry complete at 95 DEG C of vacuum, oxidation stone must be expanded
Ink；
（6）Expansion graphite oxide is taken, is added in the deionized water of 37 times of its weight, acrylamide is added, ultrasound 20 minutes, adds
Enter into above-mentioned phosphatization polymer fiber solution, rise temperature is 70 DEG C, insulated and stirred 4 hours, obtains phosphatization fiber intercalated graphite
Alkene solution；
（7）Above-mentioned phosphatization fiber intercalated graphite alkene solution, solution of silane mixing are taken, is stirred, addition allyl polyglycol,
Stannous sulfide, ultrasound 40 minutes, is distilled off ethanol, is dehydrated 2 hours at 190 DEG C, air drying, obtains organophosphor chemical fibre dimension and inserts
Layer graphene；
（8）Above-mentioned organophosphor chemical fibre dimension intercalated graphite alkene is taken, is mixed with remaining each raw material, is stirred, be sent in extruder,
Melting extrusion, cooling granulation, produce the phosphatization fiber intercalation modifying nylon material.
Embodiment 2
A kind of phosphatization fiber intercalation modifying nylon material, it is made up of the raw material of following weight parts：
Expansible graphite 18, stannous sulfide 0.1, nylon 130, string 25, chlorinated paraffin 3, acrylamide 2, phosphorus trichloride
3rd, three ammonium molybdates 0.4, allyl polyglycol 3, magnesium stearate 1, ZPT 0.5, maleic anhydride 10, methyl triethoxy
Silane 1, calcium ricinoleate 0.4, castor oil acid 1, ammonium persulfate 0.6, potassium permanganate 3.
Described string is sisal fiber.
A kind of preparation method of phosphatization fiber intercalation modifying nylon material, comprises the following steps：
（1）String is taken, is added in the ammonium sulfite solution that concentration is 0.7mol/l, stirs 2 hours, add castor oil
Acid, rise temperature is 60 DEG C, insulated and stirred 30 minutes, obtains activated fiber solution；
（2）Calcium ricinoleate is taken, is added in the absolute ethyl alcohol of 10 times of its weight, chlorinated paraffin is added, is incubated and stirs at 85-90 DEG C
Mix 20 minutes, add MTES, stir to normal temperature, obtain solution of silane；
（3）Phosphorus trichloride is taken, is added in the deionized water of 30 times of its weight, stirs, adds maleic anhydride, stirring is equal
It is even, it is sent in reactor, is passed through nitrogen, regulation temperature of reaction kettle is 75 DEG C, adds ammonium persulfate, insulated and stirred 3 hours, obtains
Phosphatization polymer solution；
（4）Above-mentioned activated fiber solution, the mixing of phosphatization polymer solution are taken, stirs, is sent in boiling water bath, insulated and stirred
1 hour, discharging, obtain phosphatization polymer fiber solution；
（5）Expansible graphite is taken, is added in 10 times of its weight, 96% sulfuric acid solution, stirs, rise temperature is 46-
50 DEG C, potassium permanganate is added, insulated and stirred 6 hours, filtering, precipitation is washed, it is dry complete at 90 DEG C of vacuum, oxidation must be expanded
Graphite；
（6）Expansion graphite oxide is taken, is added in the deionized water of 20 times of its weight, acrylamide is added, ultrasound 10 minutes, adds
Enter into above-mentioned phosphatization polymer fiber solution, rise temperature is 65 DEG C, insulated and stirred 3 hours, obtains phosphatization fiber intercalated graphite
Alkene solution；
（7）Above-mentioned phosphatization fiber intercalated graphite alkene solution, solution of silane mixing are taken, is stirred, addition allyl polyglycol,
Stannous sulfide, ultrasound 30 minutes, is distilled off ethanol, is dehydrated 1 hour at 180 DEG C, air drying, obtains organophosphor chemical fibre dimension and inserts
Layer graphene；
（8）Above-mentioned organophosphor chemical fibre dimension intercalated graphite alkene is taken, is mixed with remaining each raw material, is stirred, be sent in extruder,
Melting extrusion, cooling granulation, produce the phosphatization fiber intercalation modifying nylon material.
The phosphatization fiber intercalation modifying nylon material performance test of the embodiment of the present invention 1：
Tensile strength：23.7MPa；
Oxygen index (OI)：37；
Smog toxicity：1 grade of safety；
Smoke density grade（DSR）：16；
The phosphatization fiber intercalation modifying nylon material performance test of the embodiment of the present invention 2：
Tensile strength：27.9MPa；
Oxygen index (OI)：38；
Smog toxicity：1 grade of safety；
Smoke density grade（DSR）：19.5；
The performance test of conventional nylon material：
Tensile strength：14-18MPa；
Oxygen index (OI)：26；
Smog toxicity：2 grades of safety；
Smoke density grade（DSR）：36.1.
As can be seen that the material of the present invention has more preferable a mechanical property and fire retardant performance, security is good.
Claims (3)
1. a kind of phosphatization fiber intercalation modifying nylon material, it is characterised in that it is made up of the raw material of following weight parts：
Expansible graphite 18-20, stannous sulfide 0.1-0.2, nylon 130-150, string 25-30, chlorinated paraffin 3-4, third
Acrylamide 2-4, phosphorus trichloride 3-5, three ammonium molybdate 0.4-1, allyl polyglycol 3-5, magnesium stearate 1-2, ZPT
0.5-1, maleic anhydride 10-16, MTES 1-3, calcium ricinoleate 0.4-1, castor oil acid 1-2, ammonium persulfate
0.6-1, potassium permanganate 3-5.
2. a kind of phosphatization fiber intercalation modifying nylon material according to claim 1, it is characterised in that described plant is fine
Tie up as sisal fiber.
A kind of 3. preparation method of phosphatization fiber intercalation modifying nylon material as claimed in claim 1, it is characterised in that including
Following steps：
（1）String is taken, is added in the ammonium sulfite solution that concentration is 0.7-1mol/l, stirs 2-3 hours, add castor-oil plant
Oleic acid, rise temperature is 60-65 DEG C, insulated and stirred 30-40 minutes, obtains activated fiber solution；
（2）Calcium ricinoleate is taken, is added in the absolute ethyl alcohol of 10-17 times of its weight, chlorinated paraffin is added, is protected at 85-90 DEG C
Temperature stirring 20-30 minutes, MTES is added, stirs to normal temperature, obtains solution of silane；
（3）Phosphorus trichloride is taken, is added in the deionized water of 30-40 times of its weight, stirs, adds maleic anhydride, stirring
Uniformly, it is sent in reactor, is passed through nitrogen, regulation temperature of reaction kettle is 75-80 DEG C, adds ammonium persulfate, insulated and stirred 3-4
Hour, obtain phosphatization polymer solution；
（4）Above-mentioned activated fiber solution, the mixing of phosphatization polymer solution are taken, stirs, is sent in boiling water bath, insulated and stirred
1-2 hours, discharging, obtain phosphatization polymer fiber solution；
（5）Expansible graphite is taken, in sulfuric acid solution that be added to 10-14 times of its weight, 96-98%, is stirred, rise temperature
Spend for 46-50 DEG C, add potassium permanganate, insulated and stirred 6-9 hours, filtering, precipitation is washed, dried at 90-95 DEG C of vacuum
Entirely, expansion graphite oxide is obtained；
（6）Expansion graphite oxide is taken, is added in the deionized water of 20-37 times of its weight, adds acrylamide, ultrasonic 10-20
Minute, it is added in above-mentioned phosphatization polymer fiber solution, rise temperature is 65-70 DEG C, insulated and stirred 3-4 hours, obtains phosphatization
Fiber intercalated graphite alkene solution；
（7）Above-mentioned phosphatization fiber intercalated graphite alkene solution, solution of silane mixing are taken, is stirred, addition allyl polyglycol,
Stannous sulfide, ultrasonic 30-40 minutes, ethanol is distilled off, 1-2 hours are dehydrated at 180-190 DEG C, air drying, are obtained organic
Phosphatization fiber intercalated graphite alkene；
（8）Above-mentioned organophosphor chemical fibre dimension intercalated graphite alkene is taken, is mixed with remaining each raw material, is stirred, be sent in extruder,
Melting extrusion, cooling granulation, produce the phosphatization fiber intercalation modifying nylon material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047626A (en) * | 2018-01-30 | 2018-05-18 | 温州市赢创新材料技术有限公司 | A kind of expanded graphite crosslinking conductive material and preparation method thereof |
| CN108752794A (en) * | 2018-06-12 | 2018-11-06 | 台州学院 | A kind of carbon fiber and graphite alkene plastics pipe of high-strength light |
| CN109267328A (en) * | 2018-08-15 | 2019-01-25 | 杭州布源纺织有限公司 | A kind of nano flame retardant wall paper and preparation method thereof |
| CN109504079A (en) * | 2018-12-06 | 2019-03-22 | 朱莲华 | A kind of graphene fire-retardant nylon material and preparation method thereof |
| CN109608780A (en) * | 2018-12-31 | 2019-04-12 | 王爱绿 | A kind of flame-retardant expanded insulating board for building and preparation method thereof |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948396A (en) * | 2006-11-09 | 2007-04-18 | 四川大学 | Preparation method of nylon/montmorillonoid fire retarding composite material |
| CN107118549A (en) * | 2017-06-26 | 2017-09-01 | 陈霞 | A kind of environment friendly flame retardant fire-retardant Nylon 6 and preparation method thereof |
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2017
- 2017-09-13 CN CN201710820834.0A patent/CN107586452A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948396A (en) * | 2006-11-09 | 2007-04-18 | 四川大学 | Preparation method of nylon/montmorillonoid fire retarding composite material |
| CN107118549A (en) * | 2017-06-26 | 2017-09-01 | 陈霞 | A kind of environment friendly flame retardant fire-retardant Nylon 6 and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108047626A (en) * | 2018-01-30 | 2018-05-18 | 温州市赢创新材料技术有限公司 | A kind of expanded graphite crosslinking conductive material and preparation method thereof |
| CN108752794A (en) * | 2018-06-12 | 2018-11-06 | 台州学院 | A kind of carbon fiber and graphite alkene plastics pipe of high-strength light |
| CN109267328A (en) * | 2018-08-15 | 2019-01-25 | 杭州布源纺织有限公司 | A kind of nano flame retardant wall paper and preparation method thereof |
| CN109504079A (en) * | 2018-12-06 | 2019-03-22 | 朱莲华 | A kind of graphene fire-retardant nylon material and preparation method thereof |
| CN109608780A (en) * | 2018-12-31 | 2019-04-12 | 王爱绿 | A kind of flame-retardant expanded insulating board for building and preparation method thereof |
| 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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