CN106188835A - A kind of inorganic filler modified polypropylene material and preparation method thereof - Google Patents
A kind of inorganic filler modified polypropylene material and preparation method thereof Download PDFInfo
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- CN106188835A CN106188835A CN201610538646.4A CN201610538646A CN106188835A CN 106188835 A CN106188835 A CN 106188835A CN 201610538646 A CN201610538646 A CN 201610538646A CN 106188835 A CN106188835 A CN 106188835A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of inorganic filler modified polypropylene material, it is made up of the raw material of following weight parts: diethylene glycol dibenzoate 24, polypropylene 100 130, bisphenol A type epoxy resin 14 20, cabaltous nitrate hexahydrate 35, Nickelous nitrate hexahydrate 46, Fe(NO3)39H2O 57, 4, 4 diaminodiphenyl-methanes 0.8 1, molybdenum bisuphide 79, magnesium stearate 45, lauric acid amide of ethanol 0.5 1, antimony oxide 12, tetramethylolmethane 34, polyacrylamide 0.6 1, tetrabutyl ammonium bromide 0.3 1, ten difluoro heptyl propyl trimethoxy silicanes 0.1 0.2.The material surface intensity of the present invention is high, and hardness is good, and excellent in cushion effect, combination property is superior.
Description
Technical field
The present invention relates to polypropylene material technical field, particularly relate to a kind of inorganic filler modified polypropylene material and system thereof
Preparation Method.
Background technology
It is known that the main color of key factor affecting Polymer inorganic nanocomposite performance includes: (1) inorganic nano
Capacitive between particle and polymeric matrix；(2) nanoparticle dispersity in polymeric matrix；(3) between the two interface
And interaction.But, due to the reuniting effect of nanoparticle self, cause it to be difficult to be evenly dispersed in polymeric matrix
Form nano composite material.Therefore, in order to improve inorganic nano-particle dispersion in polymeric matrix and detain interaction between interface
Firmly, it usually needs inorganic nano-particle agriculture face is carried out covalently or non-covalently key functional modification.Covalent bond functional modification
Being presently the most method of modifying extensive, effective, be compared to non-covalent bond modified, modifier molecules is mainly made by covalent bond
Linking together with inorganic nano-particle, it interacts strong, Stability Analysis of Structures.Simultaneously can also be by covalent modification in nothing
Machine nanoparticle surface introduces active function groups or site, prepares polymer nanocomposite by grafting or in-situ polymerization further
Composite, is conducive to obtaining that good dispersion, interaction force be strong, the polymer nanocomposites of excellent performance.
The MoS2 stable chemical nature of structural integrity, surface is chemical inertness, with the interaction force of other reaction mediums
More weak, and can there is Van der Waals force between higher and lamella in nanometer MoS_2 surface, easily cause reunion so that it is be difficult to conventional
Solvent Cao forms good dispersion, to the preparation of MOS2 based polyalcohol nano composite material, studies and application causes greatly tired
Difficult.And the various excellent properties of MoS2 only could embody completely when its sheet keeps fine dispersion state.In order to fill
The excellent properties of MOS2 0 body is waved in distribution, and improves its dissolubility and the dispersibility etc. at polymeric matrix Cao thereof simultaneously, it is necessary to
MoS2 surface is carried out effective functional modification.Method modified for MoS2 is broadly divided into covalent modification and non-covalent bond changes
Property.
The most conventional preferable inorganic combustion inhibitor of flame retardant effect mainly includes phosphorus flame retardant and nitrogenated flame retardant, nitrogen system
Fire retardant, general by gas phase fire retardant mechanism performance fire retardation, it is fire-retardant that organic phosphorus flame retardant then lays particular emphasis on condensed phase.Greatly
Quantity research result shows, adds single nitrogen system or phosphorus flame retardant is difficult to obtain gratifying flame retardant effect.And ring three phosphorus
Nitrile fire retardant is main flame-retardant composition with phosphorus, nitrogen, in conjunction with nitrogen system and the advantage of phosphorus flame retardant, plays the collaborative resistance of phosphorus-nitrogen
Combustion effect, its fire retardant mechanism is commonly considered as the comprehensive function of gas phase and condensed phase, mainly shows as phosphazene compound and is heated point
Solve and generate the flame retardancy gas such as ammonia and nitrogen, dilute that material surface is flammable, the concentration of combustion-supporting gas reduce the table of material
Surface temperature, suppression burning.Metaphosphoric acid and poly-Metaphosphoric acid that meanwhile phosphazene compound generates in thermal degradation process can make material
Material dehydration carbonization, forms fine and close and solid layer of charcoal, can effectively interrupt heat exchange, the diffusion stoping imflammable gas and effusion
And stop oxygen to spread to base material simultaneously, delay the degraded of polymeric material, thus play fire retardation.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of inorganic filler modified polypropylene material and
Its preparation method.
The present invention is achieved by the following technical solutions:
A kind of inorganic filler modified polypropylene material, it is made up of the raw material of following weight parts:
Diethylene glycol dibenzoate 2-4, polypropylene 100-130, bisphenol A type epoxy resin 14-20, cabaltous nitrate hexahydrate 3-5, six
Nitric hydrate nickel 4-6, Fe(NO3)39H2O 5-7,4,4-diaminodiphenyl-methane 0.8-1, molybdenum bisuphide 7-9, magnesium stearate
4-5, lauric acid amide of ethanol 0.5-1, antimony oxide 1-2, tetramethylolmethane 3-4, polyacrylamide 0.6-1, tetrabutyl bromine
Change ammonium 0.3-1, ten difluoro heptyl propyl trimethoxy silicane 0.1-0.2.
The preparation method of a kind of described inorganic filler modified polypropylene material, comprises the following steps:
(1) by above-mentioned cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, Fe(NO3)39H2O mixing, compound weight 100-is joined
The deionized water of 110 times, joins in reactor, is passed through nitrogen, stirring mixing 30-35 minute, the hydrogen of dropping 1.7-2mol/l
Sodium hydroxide solution, regulation pH is 10-11, rises high-temperature and is 96-98 DEG C, and constant temperature 20-25 hour adds above-mentioned tetrabutyl phosphonium bromide
Ammonium, antimony oxide, stir, discharging, by product sucking filtration, precipitation washing 3-4 time, is vacuum dried 1-2 little at 50-60 DEG C
Time, join the deionized water of its weight 60-70 times, ultrasonic 3-5 minute, obtain inorganic fire-retarded suspension；
(2) above-mentioned molybdenum bisuphide is joined in its weight 100-130 times, 40-46% isopropanol water solution, at 300-
Supersound process 6-7 hour under 350w, 1500-1600 rev/min centrifugal 17-20 minute, obtains molybdenum bisuphide suspension；
(3) above-mentioned polyacrylamide is joined in the deionized water of its weight 17-20 times, stirs, add magnesium stearate,
Insulated and stirred 4-10 minute at 50-60 DEG C, obtains amide aqueous solution；
(4) taking above-mentioned molybdenum bisuphide suspension, mix with inorganic fire-retarded suspension, amide aqueous solution, magnetic agitation 10-12 is little
Time, stand 2-3 hour, filter, dry at 80-85 DEG C will be deposited in, obtain inorganic sulphide Mo；
(5) being joined by above-mentioned lauric acid amide of ethanol in the acetone of its weight 10-14 times, stir, rising high-temperature is
60-67 DEG C, add ten difluoro heptyl propyl trimethoxy silicanes, insulated and stirred 3-10 minute, obtain silane acetone solution；
(6) above-mentioned inorganic sulphide Mo is joined in the acetone of its weight 70-80 times, ultrasonic 4-10 minute, add above-mentioned
Bisphenol A type epoxy resin, insulated and stirred 5-7 hour at 90-95 DEG C, it is sent in the oil bath of 100-105 DEG C, insulated and stirred
20-25 hour, by above-mentioned 4,4-diaminodiphenyl-methane added after adding heat fusing, stirs, and discharging, at 130-140 DEG C
Lower solidification 100-120 minute, adds above-mentioned silane acetone solution, and stirring, to room temperature, obtains epoxide modified inorganic composite materials；
(7) above-mentioned epoxide modified inorganic composite materials is mixed with remaining each raw material, stir, melt extrude, cooling, i.e.
?.
The invention have the advantage that the MOS2 that the present invention adds can play physical barrier effect；Inorganic fire-retarded filler is dividing
Can absorb the partial heat of burning release in solution preocess, the discharged steam of inorganic fire-retarded filler decomposition simultaneously then can rise
Effect to dilution fuel gas；The existence of inorganic fire-retarded filler/M0S2 may advantageously facilitate epoxy resin formed finer and close and
Continuous print layer of charcoal, improves the degree of graphitization of layer of charcoal simultaneously, can effectively during retarded combustion polymeric material and air it
Between heat and mass exchange, it is possible to effectively interrupt heat exchange, stop the diffusion of imflammable gas and effusion and stop oxygen simultaneously
Gas spreads to base material, delays the degraded of polymeric material, thus plays fire retardation thus reduce HRR, suppression
The thermal degradation of polymeric material, improves the fire safety evaluating performance of material；
The addition of inorganic fire-retarded modifying agent makes the compatibility between epoxy resin and MoS2 nanoscale twins increase；Inorganic nano is filled out
Material can be uniformly adhered to MOS2 nanoscale twins surface, effectively suppresses the reunion of MOS2 lamella, improves molybdenum disulfide nano skin
Layer dispersibility in the epoxy, can play layer of charcoal enhancing or expansion in condensed phase, advantageously forms densification and steady
Fixed Char Residues Structure, the formation of layer of charcoal can effectively delay, suppress the conduction of heat and the diffusion of imflammable gas, thus play
Fire retardation；The material surface intensity of the present invention is high, and hardness is good, and excellent in cushion effect, combination property is superior.
Detailed description of the invention
A kind of inorganic filler modified polypropylene material, it is made up of the raw material of following weight parts:
Diethylene glycol dibenzoate 2, polypropylene 100, bisphenol A type epoxy resin 14, cabaltous nitrate hexahydrate 3, Nickelous nitrate hexahydrate
4, Fe(NO3)39H2O 5,4,4 diaminodiphenyl-methanes 0.8, molybdenum bisuphide 7, magnesium stearate 4, lauric acid amide of ethanol
0.5, antimony oxide 1, tetramethylolmethane 3, polyacrylamide 0.6, tetrabutyl ammonium bromide 0.3, ten difluoro heptyl propyl group trimethoxy
Base silane 0.1.
The preparation method of a kind of described inorganic filler modified polypropylene material, comprises the following steps:
(1) by above-mentioned cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, Fe(NO3)39H2O mixing, compound weight 100 times is joined
Deionized water, join in reactor, be passed through nitrogen, stirring mixing 30 minutes, the sodium hydroxide solution of dropping 1.7mol/l,
Regulation pH is 10, and rising high-temperature is 96 DEG C, constant temperature 20 hours, adds above-mentioned tetrabutyl ammonium bromide, antimony oxide, and stirring is all
Even, discharging, by product sucking filtration, precipitation washing 3 times, it is vacuum dried 1 hour at 50 DEG C, joins the deionization of its weight 60 times
Water, ultrasonic 3 minutes, obtains inorganic fire-retarded suspension；
(2) above-mentioned molybdenum bisuphide is joined in its weight 100 times, the isopropanol water solution of 40%, supersound process under 300w
6 hours, 1500 revs/min were centrifuged 17 minutes, obtain molybdenum bisuphide suspension；
(3) above-mentioned polyacrylamide is joined in the deionized water of its weight 17 times, stir, add magnesium stearate,
At 50 DEG C, insulated and stirred 4 minutes, obtain amide aqueous solution；
(4) take above-mentioned molybdenum bisuphide suspension, mix with inorganic fire-retarded suspension, amide aqueous solution, magnetic agitation 10 hours, quiet
Put 2 hours, filter, drying will be deposited at 80 DEG C, obtain inorganic sulphide Mo；
(5) being joined by above-mentioned lauric acid amide of ethanol in the acetone of its weight 10 times, stir, rising high-temperature is 60
DEG C, add ten difluoro heptyl propyl trimethoxy silicanes, insulated and stirred 3 minutes, obtain silane acetone solution；
(6) above-mentioned inorganic sulphide Mo is joined in the acetone of its weight 70 times, ultrasonic 4 minutes, add above-mentioned bisphenol A-type
Epoxy resin, insulated and stirred 5 hours at 90 DEG C, it is sent in the oil bath of 100 DEG C, insulated and stirred 20 hours, by above-mentioned 4,4 two
Aminodiphenylmethane adds after adding heat fusing, stirs, and discharging solidifies 100 minutes at 130 DEG C, adds above-mentioned silane
Acetone solution, stirring, to room temperature, obtains epoxide modified inorganic composite materials；
(7) above-mentioned epoxide modified inorganic composite materials is mixed with remaining each raw material, stir, melt extrude, cooling, i.e.
?.
Performance test:
Hot strength 28.6MPa；
Elongation at break 372%.
Claims (2)
1. an inorganic filler modified polypropylene material, it is characterised in that it is made up of the raw material of following weight parts:
Diethylene glycol dibenzoate 2-4, polypropylene 100-130, bisphenol A type epoxy resin 14-20, cabaltous nitrate hexahydrate 3-5, six
Nitric hydrate nickel 4-6, Fe(NO3)39H2O 5-7,4,4-diaminodiphenyl-methane 0.8-1, molybdenum bisuphide 7-9, magnesium stearate
4-5, lauric acid amide of ethanol 0.5-1, antimony oxide 1-2, tetramethylolmethane 3-4, polyacrylamide 0.6-1, tetrabutyl bromine
Change ammonium 0.3-1, ten difluoro heptyl propyl trimethoxy silicane 0.1-0.2.
2. the preparation method of an inorganic filler modified polypropylene material as claimed in claim 1, it is characterised in that include with
Lower step:
(1) by above-mentioned cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, Fe(NO3)39H2O mixing, compound weight 100-is joined
The deionized water of 110 times, joins in reactor, is passed through nitrogen, stirring mixing 30-35 minute, the hydrogen of dropping 1.7-2mol/l
Sodium hydroxide solution, regulation pH is 10-11, rises high-temperature and is 96-98 DEG C, and constant temperature 20-25 hour adds above-mentioned tetrabutyl phosphonium bromide
Ammonium, antimony oxide, stir, discharging, by product sucking filtration, precipitation washing 3-4 time, is vacuum dried 1-2 little at 50-60 DEG C
Time, join the deionized water of its weight 60-70 times, ultrasonic 3-5 minute, obtain inorganic fire-retarded suspension；
(2) above-mentioned molybdenum bisuphide is joined in its weight 100-130 times, 40-46% isopropanol water solution, at 300-
Supersound process 6-7 hour under 350w, 1500-1600 rev/min centrifugal 17-20 minute, obtains molybdenum bisuphide suspension；
(3) above-mentioned polyacrylamide is joined in the deionized water of its weight 17-20 times, stirs, add magnesium stearate,
Insulated and stirred 4-10 minute at 50-60 DEG C, obtains amide aqueous solution；
(4) taking above-mentioned molybdenum bisuphide suspension, mix with inorganic fire-retarded suspension, amide aqueous solution, magnetic agitation 10-12 is little
Time, stand 2-3 hour, filter, dry at 80-85 DEG C will be deposited in, obtain inorganic sulphide Mo；
(5) being joined by above-mentioned lauric acid amide of ethanol in the acetone of its weight 10-14 times, stir, rising high-temperature is
60-67 DEG C, add ten difluoro heptyl propyl trimethoxy silicanes, insulated and stirred 3-10 minute, obtain silane acetone solution；
(6) above-mentioned inorganic sulphide Mo is joined in the acetone of its weight 70-80 times, ultrasonic 4-10 minute, add above-mentioned
Bisphenol A type epoxy resin, insulated and stirred 5-7 hour at 90-95 DEG C, it is sent in the oil bath of 100-105 DEG C, insulated and stirred
20-25 hour, by above-mentioned 4,4-diaminodiphenyl-methane added after adding heat fusing, stirs, and discharging, at 130-140 DEG C
Lower solidification 100-120 minute, adds above-mentioned silane acetone solution, and stirring, to room temperature, obtains epoxide modified inorganic composite materials；
(7) above-mentioned epoxide modified inorganic composite materials is mixed with remaining each raw material, stir, melt extrude, cooling, i.e.
?.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109518293A (en) * | 2018-11-23 | 2019-03-26 | 深圳市欧科力科技有限公司 | A kind of high tenacity flame-retardant polypropelene material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670109A (en) * | 2014-11-21 | 2016-06-15 | 神华集团有限责任公司 | Polypropylene composition, preparation method thereof, and polypropylene material prepared therethrough |
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2016
- 2016-07-11 CN CN201610538646.4A patent/CN106188835A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670109A (en) * | 2014-11-21 | 2016-06-15 | 神华集团有限责任公司 | Polypropylene composition, preparation method thereof, and polypropylene material prepared therethrough |
Non-Patent Citations (1)
| Title |
|---|
| 黄锐、王旭、李忠明 编著: "《纳米塑料——聚合物/纳米无机复合材料研制、应用与进展》", 31 January 2002, 中国轻工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109518293A (en) * | 2018-11-23 | 2019-03-26 | 深圳市欧科力科技有限公司 | A kind of high tenacity flame-retardant polypropelene material and preparation method thereof |
| CN109518293B (en) * | 2018-11-23 | 2021-02-12 | 上海阜泰实业有限公司 | High-toughness flame-retardant polypropylene material and preparation method thereof |
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