CN105038191B - A kind of halogen-free flame-retardant thermoplastic elastomer and preparation method thereof - Google Patents
A kind of halogen-free flame-retardant thermoplastic elastomer and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to thermoplastic elastomer (TPE) technical field, and in particular to a kind of halogen-free flame-retardant thermoplastic elastomer and preparation method thereof, includes the raw material of following parts by weight：1.3 3 parts of 75 110 parts of polyurethane elastomer, 12 30 parts of phosphorus flame retardant, 5 35 parts of phosphorus-nitrogen containing flame retardant, 13 parts of inorganic salts fire retardant, 5 12 parts of plasticizer and lubricant.The present invention solves the problems, such as that the existing elastomer containing halogen flame can produce toxicity and corrosive gas, and greatly can control smoke amount in elastomer naked light combustion process.The halogen-free flame-retardant thermoplastic elastomer of the present invention strictly controls the weight proportion of each raw material, good flame retardation effect by using above-mentioned raw materials, fire-retardant rank can reach UL94 V0 levels, and fire line is good, and smoke is few, with low precipitation, anti-drip, high electrical property and excellent heat resistance；And excellent in abrasion resistance, ozone resistance are fabulous, hardness is big, intensity is high, elasticity is good, excellent combination property.
Description
Technical field
The present invention relates to thermoplastic elastomer (TPE) technical field, and in particular to a kind of halogen-free flame-retardant thermoplastic elastomer and its system
Preparation Method.
Background technology
Elastomeric material has excellent mechanical property, and he had both had the elasticity and deformation rate close to rubber.There is heat again
The advantage of the easy processing of thermoplastic plastic, temperature in use section is big, can -50 ~ 120 DEG C of temperature range normal use again, especially
The use in automobile, electronic product, household material, increase year by year, for the purpose of safety, either automobile,
Electronics, the material of household industry requires is fire-retardant, and it is in bullet to need by certain fire-retardant rank, traditional method
Elastomer material addition halogen flame arranges in pairs or groups antimony oxide to reach fire-retardant demand, but the use of halogen flame, has
The release of toxicity, corrosive gas, existing relevant laws and regulations have begun to the use for forbidding halogen containing flame-retardant progressively, the present invention
Novel halogen-free flame-retardant elastomeric material is the fire proofing synergistic use by using a variety of environment-friendly types, and the elastomer of preparation reaches
The requirement of a variety of fire-retardant ranks such as UL94-V0.
The content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of halogen-free flameproof heat
Thermoplastic elastic, solve the problems, such as that the existing elastomer containing halogen flame can produce toxicity and corrosive gas, and
Greatly smoke amount can be controlled in elastomer naked light combustion process.
Another object of the present invention is to provide a kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, the preparation method
Technique is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low, can large-scale industrial production.
The purpose of the present invention is achieved through the following technical solutions：A kind of halogen-free flame-retardant thermoplastic elastomer, including following weight
Measure the raw material of part：
Polyurethane elastomer 75-110 parts
Phosphorus flame retardant 12-30 parts
Phosphorus-nitrogen containing flame retardant 5-35 parts
Inorganic salts fire retardant 1-3 parts
Plasticizer 5-12 parts
Lubricant 1.3-3 parts.
The present invention solves the problems, such as that the existing elastomer containing halogen flame can produce toxicity and corrosive gas, and
And greatly it can control smoke amount in elastomer naked light combustion process.
The halogen-free flame-retardant thermoplastic elastomer good flame retardation effect of the present invention, fire-retardant rank can reach UL94-V0 levels, prevent fires
Property it is good, smoke is few, have low precipitation, anti-drip, high electrical property and excellent heat resistance；And excellent in abrasion resistance, ozone resistance pole
Well, hardness is big, intensity is high, elasticity is good, low temperature resistant, has good oil resistant, chemical-resistant resistance and environmental resistance, combination property
It is excellent.
Preferably, the polyurethane elastomer includes PAUR elastomer 40-60 parts and EU bullet
Property body 35-50 parts.
The present invention is by using PAUR elastomer and EU elastomer as polyurethane elastomer
Compounding use, and it is 8-12 to control its weight ratio：7-10 is obtained halogen-free flame-retardant thermoplastic elastomer excellent in abrasion resistance, resistance to smelly
Oxygen is fabulous, hardness is big, intensity is high, elasticity is good, low temperature resistant, has good oil resistant, chemical-resistant resistance and environmental resistance, comprehensive
Close excellent performance.
Preferably, the phosphorus flame retardant includes boron phosphate 1-7 parts, ferric pyrophosphate 1-8 parts and microencapsulated powder oil 10-15
Part.
The present invention by using boron phosphate, ferric pyrophosphate and microencapsulated powder oil as phosphorus flame retardant compounding use, and
It is 1-7 to control its weight ratio：1-8：10-15, phosphorus flame retardant can produce the more stable crosslinking shape solids of structure when heated
On the one hand matter or carburization zone, the formation of carburization zone can prevent polymer from being further pyrolyzed, on the other hand can prevent its internal heat
It is few into gas phase participation combustion process, obtained halogen-free flame-retardant thermoplastic elastomer good flame retardation effect, smoke to decompose generation.
Preferably, the phosphorus-nitrogen containing flame retardant includes APP 5-10 parts and microencapsulation APP 0-25 parts.
The present invention, as phosphorus-nitrogen containing flame retardant, there is phosphorus, nitrogen to assist by using APP and microencapsulation APP
Fire retardation is imitated, has that gas phase is fire-retardant and the fire-retardant mechanism of condensed phase concurrently, when being heated, surface can generate one layer of uniform carbonaceous foam
Layer, play a part of heat-insulated, oxygen barrier, suppression cigarette, and prevent molten drop phenomenon, therefore there is good anti-flammability, good flame retardation effect,
Heat endurance is good, obtained halogen-free flame-retardant thermoplastic elastomer good flame retardation effect, and smoke is few.
Preferably, the inorganic salts fire retardant includes at least one of Firebrake ZB, antifungin and line borate.
The present invention is used as inorganic salts fire retardant by using at least one of Firebrake ZB, antifungin and line borate, can
To effectively improve fire resistance, the generation of smog when reducing burning, and can with the chemistry of regulation elasticity body, the side such as mechanically and electrically
The performance in face, obtained halogen-free flame-retardant thermoplastic elastomer good flame retardation effect, smoke are few.More there are preferable, the inorganic salts
Based flame retardant is to compare 0.8-1.2 by Firebrake ZB, antifungin and line borate with weight：1.5-2.5：The mixture of 1 composition.
Preferably, the plasticizer is phosphate plasticizer.
The present invention by using phosphate plasticizer, have it is excellent be plasticized, be fire-retardant, be wear-resisting, antibacterial action, both can be with
Use as plasticizer, can be used again as fire retardant, obtained halogen-free flame-retardant thermoplastic elastomer good flame retardation effect.
Preferably, the phosphate plasticizer includes triphenyl phosphate and/or tricresyl phosphate.The present invention is by adopting
By the use of triphenyl phosphate and/or tricresyl phosphate as plasticizer, the anti-flammability of halogen-free flame-retardant thermoplastic elastomer can be improved
Energy.It is more highly preferred to, the phosphate plasticizer is to compare 2-4 by triphenyl phosphate and tricresyl phosphate with weight：1 composition
Mixture.
Preferably, the lubricant includes pentaerythritol ester 0.5-1.0 parts and high-carbon fatty acid ester 0.8-2.0 parts.
The present invention, as lubricant compounding use, and controls its weight by using pentaerythritol ester and high-carbon fatty acid ester
Than for 0.5-1.0：0.8-2.0, two kinds of mix lubricant uses can improve the mobility of elastomer in process and take off
Mould.
Preferably, the pentaerythritol ester includes pentaerythritol stearate and/or PETO.The present invention is logical
Cross using pentaerythritol stearate and/or PETO as lubricant, the intermolecular of elastomer melt can be reduced
Friction, improve elastomer mobility in process and release property.It is more highly preferred to, the pentaerythritol ester is by season penta
Tetrol stearate and PETO compare 0.8-1.2 with weight：The mixture of 1 composition.
The high-carbon fatty acid ester includes butyl stearate, stearic acid monoglyceride, glycerol trioleate, the palmitic acid of glycerine three
At least one of ester and glycerol tristearate.The present invention, as lubricant, can drop by using above-mentioned high-carbon fatty acid ester
The intermolecular friction of low elasticity body melt, improve elastomer mobility in process and release property.It is more highly preferred to, institute
It is with weight ratio 1 by butyl stearate and stearic acid monoglyceride to state high-carbon fatty acid ester：1.4-2.2 the mixture of composition.
A kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, above-mentioned raw materials input high-speed mixer is weighed by weight
In, 3-4min is mixed, obtains mixture；Mixture is passed through into single screw extrusion machine or double screw extruder extruding pelletization, extrusion
The extruder temperature of machine is arranged on 160-185 DEG C, and halogen-free flame-retardant thermoplastic elastomer is made.
The preparation method technique of the present invention is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low,
Can large-scale industrial production.
The beneficial effects of the present invention are：The present invention, which solves the existing elastomer containing halogen flame, can produce toxicity
And the problem of corrosive gas, and greatly can control smoke amount in elastomer naked light combustion process.
The halogen-free flame-retardant thermoplastic elastomer good flame retardation effect of the present invention, fire-retardant rank can reach UL94-V0 levels, prevent fires
Property it is good, smoke is few, have low precipitation, anti-drip, high electrical property and excellent heat resistance；And excellent in abrasion resistance, ozone resistance pole
Well, hardness is big, intensity is high, elasticity is good, low temperature resistant, has good oil resistant, chemical-resistant resistance and environmental resistance, combination property
It is excellent.
The preparation method technique of the present invention is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low,
Can large-scale industrial production.
Embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1
A kind of halogen-free flame-retardant thermoplastic elastomer, include the raw material of following parts by weight：
75 parts of polyurethane elastomer
12 parts of phosphorus flame retardant
5 parts of phosphorus-nitrogen containing flame retardant
1 part of inorganic salts fire retardant
5 parts of plasticizer
1.3 parts of lubricant.
The polyurethane elastomer includes 35 parts of 40 parts of PAUR elastomer and EU elastomer.
The phosphorus flame retardant includes 10 parts of 1 part of boron phosphate, 1 part of ferric pyrophosphate and microencapsulated powder oil.
The phosphorus-nitrogen containing flame retardant includes 5 parts of APP.
The inorganic salts fire retardant is Firebrake ZB.
The plasticizer is phosphate plasticizer.
The phosphate plasticizer is triphenyl phosphate.
The lubricant includes 0.8 part of 0.5 part of pentaerythritol ester and high-carbon fatty acid ester.
The pentaerythritol ester is pentaerythritol stearate；The high-carbon fatty acid ester is butyl stearate or stearic acid
Monoglyceride.
A kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, above-mentioned raw materials input high-speed mixer is weighed by weight
In, 3min is mixed, obtains mixture；Mixture is passed through into single screw extrusion machine or double screw extruder extruding pelletization, extruder
Extruder temperature be arranged on 160-185 DEG C, be made halogen-free flame-retardant thermoplastic elastomer.
Embodiment 2
A kind of halogen-free flame-retardant thermoplastic elastomer, include the raw material of following parts by weight：
83 parts of polyurethane elastomer
15 parts of phosphorus flame retardant
14 parts of phosphorus-nitrogen containing flame retardant
1.5 parts of inorganic salts fire retardant
6 parts of plasticizer
1.7 parts of lubricant.
The polyurethane elastomer includes 38 parts of 45 parts of PAUR elastomer and EU elastomer.
The phosphorus flame retardant includes 11 parts of 2 parts of boron phosphate, 2 parts of ferric pyrophosphate and microencapsulated powder oil.
The phosphorus-nitrogen containing flame retardant includes 8 parts of 6 parts of APP and microencapsulation APP.
The inorganic salts fire retardant is with weight ratio 0.8 by Firebrake ZB, antifungin and line borate：1.5：1 composition mixes
Compound.
The plasticizer is phosphate plasticizer.
The phosphate plasticizer is with weight ratio 2 by triphenyl phosphate and tricresyl phosphate：The mixing of 1 composition
Thing.
The lubricant includes 1.1 parts of 0.6 part of pentaerythritol ester and high-carbon fatty acid ester.
The pentaerythritol ester is with weight ratio 0.8 by pentaerythritol stearate and PETO：1 composition
Mixture；The high-carbon fatty acid ester is with weight ratio 1 by butyl stearate and stearic acid monoglyceride：The mixture of 1.4 compositions.
A kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, above-mentioned raw materials input high-speed mixer is weighed by weight
In, 3.5min is mixed, obtains mixture；Mixture is passed through into single screw extrusion machine or double screw extruder extruding pelletization, extrusion
The extruder temperature of machine is arranged on 160-185 DEG C, and halogen-free flame-retardant thermoplastic elastomer is made.
Embodiment 3
A kind of halogen-free flame-retardant thermoplastic elastomer, include the raw material of following parts by weight：
92 parts of polyurethane elastomer
20 parts of phosphorus flame retardant
23 parts of phosphorus-nitrogen containing flame retardant
2 parts of inorganic salts fire retardant
8 parts of plasticizer
2.2 parts of lubricant.
The polyurethane elastomer includes 42 parts of 50 parts of PAUR elastomer and EU elastomer.
The phosphorus flame retardant includes 12 parts of 4 parts of boron phosphate, 4 parts of ferric pyrophosphate and microencapsulated powder oil.
The phosphorus-nitrogen containing flame retardant includes 15 parts of 8 parts of APP and microencapsulation APP.
The inorganic salts fire retardant is with weight ratio 1 by Firebrake ZB, antifungin and line borate：2：The mixture of 1 composition.
The plasticizer is phosphate plasticizer.
The phosphate plasticizer is with weight ratio 3 by triphenyl phosphate and tricresyl phosphate：The mixing of 1 composition
Thing.
The lubricant includes 1.4 parts of 0.8 part of pentaerythritol ester and high-carbon fatty acid ester.
The pentaerythritol ester is with weight ratio 1 by pentaerythritol stearate and PETO：1 composition mixes
Compound；The high-carbon fatty acid ester is with weight ratio 1 by butyl stearate and stearic acid monoglyceride：The mixture of 1.8 compositions.
A kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, above-mentioned raw materials input high-speed mixer is weighed by weight
In, 3.5min is mixed, obtains mixture；Mixture is passed through into single screw extrusion machine or double screw extruder extruding pelletization, extrusion
The extruder temperature of machine is arranged on 160-185 DEG C, and halogen-free flame-retardant thermoplastic elastomer is made.
Embodiment 4
A kind of halogen-free flame-retardant thermoplastic elastomer, include the raw material of following parts by weight：
101 parts of polyurethane elastomer
26 parts of phosphorus flame retardant
29 parts of phosphorus-nitrogen containing flame retardant
2.5 parts of inorganic salts fire retardant
10 parts of plasticizer
2.6 parts of lubricant.
The polyurethane elastomer includes 46 parts of 55 parts of PAUR elastomer and EU elastomer.
The phosphorus flame retardant includes 14 parts of 6 parts of boron phosphate, 6 parts of ferric pyrophosphate and microencapsulated powder oil.
The phosphorus-nitrogen containing flame retardant includes 20 parts of 9 parts of APP and microencapsulation APP.
The inorganic salts fire retardant is with weight ratio 1.2 by Firebrake ZB, antifungin and line borate：2.5：1 composition mixes
Compound.
The plasticizer is phosphate plasticizer.
The phosphate plasticizer is with weight ratio 4 by triphenyl phosphate and tricresyl phosphate：The mixing of 1 composition
Thing.
The lubricant includes 1.7 parts of 0.9 part of pentaerythritol ester and high-carbon fatty acid ester.
The pentaerythritol ester is with weight ratio 1.2 by pentaerythritol stearate and PETO：1 composition
Mixture；The high-carbon fatty acid ester is with weight ratio 1 by butyl stearate and stearic acid monoglyceride：The mixture of 2.2 compositions.
A kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, above-mentioned raw materials input high-speed mixer is weighed by weight
In, 3.5min is mixed, obtains mixture；Mixture is passed through into single screw extrusion machine or double screw extruder extruding pelletization, extrusion
The extruder temperature of machine is arranged on 160-185 DEG C, and halogen-free flame-retardant thermoplastic elastomer is made.
Embodiment 5
A kind of halogen-free flame-retardant thermoplastic elastomer, include the raw material of following parts by weight：
110 parts of polyurethane elastomer
30 parts of phosphorus flame retardant
35 parts of phosphorus-nitrogen containing flame retardant
3 parts of inorganic salts fire retardant
12 parts of plasticizer
3 parts of lubricant.
The polyurethane elastomer includes 50 parts of 60 parts of PAUR elastomer and EU elastomer.
The phosphorus flame retardant includes 15 parts of 7 parts of boron phosphate, 8 parts of ferric pyrophosphate and microencapsulated powder oil.
The phosphorus-nitrogen containing flame retardant includes 25 parts of 10 parts of APP and microencapsulation APP.
The inorganic salts fire retardant includes antifungin or line borate.
The plasticizer is phosphate plasticizer.
The phosphate plasticizer is tricresyl phosphate.
The lubricant includes 2.0 parts of 1.0 parts of pentaerythritol ester and high-carbon fatty acid ester.
The pentaerythritol ester is PETO；The high-carbon fatty acid ester is glycerol trioleate, glycerine three
Palmitate or glycerol tristearate.
A kind of preparation method of halogen-free flame-retardant thermoplastic elastomer, above-mentioned raw materials input high-speed mixer is weighed by weight
In, 4min is mixed, obtains mixture；Mixture is passed through into single screw extrusion machine or double screw extruder extruding pelletization, extruder
Extruder temperature be arranged on 160-185 DEG C, be made halogen-free flame-retardant thermoplastic elastomer.
The mechanical and physical performance of halogen-free flame-retardant thermoplastic elastomer is as shown in table 1 made from embodiment 1-5.
Table 1
| Test event | Standard value | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Tensile strength（MPa） | ≥15.0 | 32.7 | 34.8 | 36.1 | 36.5 | 33.6 |
| Bending strength（MPa） | ≥15.0 | 47.3 | 49.2 | 52.1 | 54.9 | 45.7 |
| Elongation at break（%） | ≥150 | 396 | 401 | 408 | 419 | 398 |
| Hardness/Shore D | ≥50 | 80 | 83 | 85 | 86 | 81 |
| Fire-retardant/UL94 | V2 | V0 | V0 | V0 | V0 | V0 |
| Smoke amount | It is less | Seldom | Seldom | Seldom | Seldom | Seldom |
As it can be seen from table 1 the halogen-free flame-retardant thermoplastic elastomer of the present invention solve it is existing containing halogen flame
Elastomer can produce the problem of toxicity and corrosive gas, and greatly can control smoke in elastomer naked light combustion process
Amount.
The halogen-free flame-retardant thermoplastic elastomer good flame retardation effect of the present invention, fire-retardant rank can reach UL94-V0 levels, prevent fires
Property it is good, smoke is few, have low precipitation, anti-drip, high electrical property and excellent heat resistance；And excellent in abrasion resistance, ozone resistance pole
Well, hardness is big, intensity is high, elasticity is good, low temperature resistant, has good oil resistant, chemical-resistant resistance and environmental resistance, combination property
It is excellent.
Above-described embodiment is the preferable implementation of the present invention, and in addition, the present invention can be realized with other manner,
Do not depart from and any on the premise of present inventive concept obviously replace within protection scope of the present invention.
Claims (5)
- A kind of 1. halogen-free flame-retardant thermoplastic elastomer, it is characterised in that：Include the raw material of following parts by weight：Polyurethane elastomer 75-110 partsPhosphorus flame retardant 12-30 partsPhosphorus-nitrogen containing flame retardant 14-35 partsInorganic salts fire retardant 1-3 partsPlasticizer 5-12 partsLubricant 1.3-3 parts；The phosphorus flame retardant includes boron phosphate 1-7 parts, ferric pyrophosphate 1-8 parts and microencapsulated powder oil 10-15 parts；The phosphorus-nitrogen containing flame retardant includes APP 6-10 parts and microencapsulation APP 8-25 parts；The inorganic salts fire retardant is to compare 0.8-1.2 by Firebrake ZB, antifungin and line borate with weight：1.5-2.5：1 composition Mixture；The lubricant includes pentaerythritol ester 0.5-1.0 parts and high-carbon fatty acid ester 0.8-2.0 parts；The pentaerythritol ester includes pentaerythritol stearate and/or PETO；The high-carbon fatty acid ester bag Include in butyl stearate, stearic acid monoglyceride, glycerol trioleate, palmitin and glycerol tristearate at least It is a kind of.
- A kind of 2. halogen-free flame-retardant thermoplastic elastomer according to claim 1, it is characterised in that：The polyurethane elastomer Including PAUR elastomer 40-60 parts and EU elastomer 35-50 parts.
- A kind of 3. halogen-free flame-retardant thermoplastic elastomer according to claim 1, it is characterised in that：The plasticizer is phosphoric acid Ester plasticizer.
- A kind of 4. halogen-free flame-retardant thermoplastic elastomer according to claim 3, it is characterised in that：The phosphoric acid ester plasticising Agent includes triphenyl phosphate and/or tricresyl phosphate.
- A kind of 5. preparation method of halogen-free flame-retardant thermoplastic elastomer as described in claim any one of 1-4, it is characterised in that： Weigh by weight in above-mentioned raw materials input high-speed mixer, mix 3-4min, obtain mixture；Mixture is passed through into single screw rod Extruder or double screw extruder extruding pelletization, the extruder temperature of extruder are arranged on 160-185 DEG C, and halogen-free flameproof thermoplastic is made Property elastomer.
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| CN107286637B (en) * | 2017-07-31 | 2020-06-12 | 广东安拓普聚合物科技有限公司 | Low-smoke halogen-free flame-retardant ceramic thermoplastic polyurethane elastomer composite material and preparation method and application thereof |
| CN108003600A (en) * | 2017-12-22 | 2018-05-08 | 芜湖环瑞汽车内饰件有限公司 | A kind of flame retardant automotive inside gadget material and preparation method thereof |
| CN109401275A (en) * | 2018-09-11 | 2019-03-01 | 苏州市雄林新材料科技有限公司 | A kind of high fire-retardance softness TPU film and preparation method thereof |
| CN111696720B (en) * | 2020-04-24 | 2021-10-29 | 上海蓝昊电气股份有限公司 | Lightweight reel high-voltage cable and preparation method thereof |
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