CN103408828A - Preparation method of halogen-free flame-retardant polyethylene (PE) pipe - Google Patents
Preparation method of halogen-free flame-retardant polyethylene (PE) pipe Download PDFInfo
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- CN103408828A CN103408828A CN2013103965308A CN201310396530A CN103408828A CN 103408828 A CN103408828 A CN 103408828A CN 2013103965308 A CN2013103965308 A CN 2013103965308A CN 201310396530 A CN201310396530 A CN 201310396530A CN 103408828 A CN103408828 A CN 103408828A
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Abstract
The invention belongs to the technical field of flame-retardant polyethylene (PE) pipes and in particular relates to a preparation method of a halogen-free flame-retardant PE pipe. The preparation method comprises the following steps: a, drying and modifying super-fine calcium carbonate to prepare activated modified super-fine calcium carbonate powder; b, drying and modifying magnesium hydroxide to prepare activated modified magnesium hydroxide powder; c, throwing high-density PE, the activated modified super-fine calcium carbonate powder, the activated modified magnesium hydroxide powder, pentaerythritol stearyl amine, an antioxidant 1010 and an auxiliary antioxidant 168 into a high-speed mixing machine, stirring at 80 to 100 DEG C for 5 to 10 minutes to obtain mixed raw materials, and throwing the mixed raw materials into a double-screw extruder and pelleting to obtain PE master batches; and d, extruding, sizing, drawing, cooling and sizing, and cutting the PE master batches by using a pipe forming machine to prepare the pipe. The preparation method has the beneficial effects that flame-retardant efficiency is high; the adding amount of a halogen-free flame retardant is reduced; the excellent comprehensive mechanical properties of the PE pipe are guaranteed.
Description
Technical field
The invention belongs to fire-retardant PE Manifold technology field, be specifically related to a kind of preparation method of halogen-free flameproof PE pipe.
Background technology
The PE(polyethylene) pipeline is one of modal pipeline, and it has low-temperature impact resistance, resistance to chemical attack, the advantage such as wear-resisting, all is used widely in feedwater, draining, heat supply, for combustion gas, agricultural irrigation, hydro project and various full scale plant.Polyethylene is combustible polymers, and oxygen index is 17-18%, and combustion heat value belongs to the higher person in polymer materials, be 45.9MJ/kg.Poly thermal degradation reaction is in random scission and molecule and the intermolecular transfer reaction, high-temperature heating is degraded into low molecular weight substance, propagating flame very easily, initiation fire, so must reach fire-retardant purpose by PE, adding fire retardant, resin fire retardant commonly used is addition type and response type at present, halogenated flame retardant especially brominated flame-retardant and antimonous oxide composite, PE is had to fire retardation preferably, but forbidden by European Union due to the environmental problem of fire retardant itself, use at home is also to reduce gradually, progressively studied the friendly type halogen-free flameproof of environment for use PE, but existing halogen-free flameproof PE also exists flame retardant effect poor, the halogen-free flame retardants addition causes greatly the defect of PE pipe mechanical properties decrease, hindered promoting the use of of halogen-free flameproof PE pipe.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the halogen-free flameproof PE pipe that a kind of halogen-free flame retardants addition is little.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of preparation method of halogen-free flameproof PE pipe, comprise the steps:
A, by calcium carbonate superfine powder drying and modification, make activation modification calcium carbonate superfine powder powder;
B, by magnesium hydroxide drying and modification, make the activation modification magnesium hydrate powder;
C, will high density polyethylene(HDPE), activation modification calcium carbonate superfine powder powder, activation modification magnesium hydrate powder, tetramethylolmethane Stearyl Amine, antioxidant 1010, auxiliary antioxidant 168 drop in high-speed mixers and stir and obtained mixing raw material in 5-10 minute at 80-100 ℃, mixing raw material is dropped into to granulation in twin screw extruder, obtain the polyethylene master batch;
D, the polyethylene master batch is extruded-sizing-traction-cooling and shaping-cutting by tube forming mill, made tubing.
Preferably, described step a comprises: calcium carbonate superfine powder: 94-97%, aluminium titanium composite coupler: 2-3%, silane coupling agent by weight percentage: 1-3% weighs, calcium carbonate superfine powder is dropped in high-speed mixer, stirring is warmed to 100-110 ℃ of dehydration 10-20 minute, then aluminium titanium composite coupler and silane coupling agent are dropped into to mix and blend 10-20 minute in high-speed mixer, make water ratio lower than 0.8% activation modification calcium carbonate superfine powder powder.
Preferably, described step b comprises: magnesium hydroxide 97-99%, silane coupling agent 1-3% weigh by weight percentage, magnesium hydroxide is dropped in high-speed mixer, stirring is warmed to 100-110 ℃ of dehydration 10-20 minute, then silane coupling agent is dropped into to mix and blend 10-20 minute in high-speed mixer, make water ratio lower than 0.8% activation modification magnesium hydrate powder.
Preferably, in described step c, the weight proportion of each raw material is:
High density polyethylene(HDPE): 60-78%
Magnesium hydrate powder: 15-28%
Calcium carbonate superfine powder powder: 4-9%
Tetramethylolmethane Stearyl Amine: 1%
Antioxidant 1010: 0.5-1%
Auxiliary antioxidant 168:1-2%.
The invention has the beneficial effects as follows that flame retarding efficiency is high, the addition of halogen-free flame retardants greatly reduces, and has guaranteed that simultaneously the comprehensive mechanical property of PE pipe is good.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described in detail.
The preparation method of a kind of halogen-free flameproof PE pipe of embodiment mono-, comprise
Step a: calcium carbonate superfine powder by weight percentage: 94%, aluminium titanium composite coupler: 3%, silane coupling agent: 3% weighs, calcium carbonate superfine powder is dropped in high-speed mixer, stirring is warmed to 100 ℃ of dehydrations 10 minutes, then aluminium titanium composite coupler and silane coupling agent were dropped in high-speed mixer to mix and blend 10 minutes, and made water ratio lower than 0.8% activation modification calcium carbonate superfine powder powder.
Step b: magnesium hydroxide 97%, silane coupling agent 3% are weighed by weight percentage, magnesium hydroxide is dropped in high-speed mixer, stirring is warmed to 100 ℃ of dehydration 10 clocks, then silane coupling agent was dropped in high-speed mixer to mix and blend 10 minutes, and made water ratio lower than 0.8% activation modification magnesium hydrate powder.
Step c: high density polyethylene(HDPE), activation modification calcium carbonate superfine powder powder, activation modification magnesium hydrate powder, tetramethylolmethane Stearyl Amine, antioxidant 1010, auxiliary antioxidant 168 are dropped in high-speed mixer and stir and obtained mixing raw material in 5 minutes at 80 ℃, mixing raw material is dropped into to granulation in twin screw extruder, obtain the polyethylene master batch; Wherein the weight proportion of each raw material is:
High density polyethylene(HDPE): 64%
Magnesium hydrate powder: 26%
Calcium carbonate superfine powder powder: 7%
Tetramethylolmethane Stearyl Amine: 1%
Antioxidant 1010: 1%
Auxiliary antioxidant 168:1%.
Material after granulation is extruded-sizing-traction-cooling and shaping-cutting by tube forming mill, made tubing.
After tested, the tensile strength of this halogen-free flameproof PE pipe is 12.62Mpa, and tensile elongation is 157%, and outer sightseeing is white, and oxygen index is 30%.
The preparation method of a kind of halogen-free flameproof PE pipe of embodiment bis-, comprise
Step a: calcium carbonate superfine powder by weight percentage: 97%, aluminium titanium composite coupler: 2%, silane coupling agent: 1% weighs, calcium carbonate superfine powder is dropped in high-speed mixer, stirring is warmed at 1100 temperature dewatered 20 minutes, then aluminium titanium composite coupler and silane coupling agent were dropped in high-speed mixer to mix and blend 20 minutes, and made water ratio lower than 0.8% activation modification calcium carbonate superfine powder powder.
Step b: magnesium hydroxide 99%, silane coupling agent 1% are weighed by weight percentage, magnesium hydroxide is dropped in high-speed mixer, stirring is warmed at 110 ° of temperature dewatered 20 minutes, then silane coupling agent was dropped in high-speed mixer to mix and blend 20 minutes, and made water ratio lower than 0.8% activation modification magnesium hydrate powder.
Step c: high density polyethylene(HDPE), activation modification calcium carbonate superfine powder powder, activation modification magnesium hydrate powder, tetramethylolmethane Stearyl Amine, antioxidant 1010, auxiliary antioxidant 168 are dropped in high-speed mixer and stir and obtained mixing raw material in 10 minutes at 100 ℃, mixing raw material is dropped into to granulation in twin screw extruder, obtain the polyethylene master batch; Wherein the weight proportion of each raw material is:
High density polyethylene(HDPE): 60%
Magnesium hydrate powder: 28%
Calcium carbonate superfine powder powder: 9%
Tetramethylolmethane Stearyl Amine: 1%
Antioxidant 1010: 0.5%
Auxiliary antioxidant 168:1.5%.
Material after granulation is extruded by tube forming mill---sizing---traction---cooling and shaping---be cut into tubing.
After tested, the tensile strength of this halogen-free flameproof PE pipe is 13.00Mpa, and tensile elongation is 81.6%, and outer sightseeing is white, and oxygen index is 31%.
The preparation method of a kind of halogen-free flameproof PE pipe of embodiment tri-, comprise
Step a: calcium carbonate superfine powder by weight percentage: 95%, aluminium titanium composite coupler: 2%, silane coupling agent: 3% weighs, calcium carbonate superfine powder is dropped in high-speed mixer, stirring is warmed to 105 ℃ of dehydrations 15 minutes, then aluminium titanium composite coupler and silane coupling agent were dropped in high-speed mixer to mix and blend 15 minutes, and made water ratio lower than 0.8% activation modification calcium carbonate superfine powder powder.
Step b: magnesium hydroxide 98%, silane coupling agent 2% are weighed by weight percentage, magnesium hydroxide is dropped in high-speed mixer, stirring is warmed to dehydration 10-20 minute under 105 ℃, then silane coupling agent is dropped into to mix and blend 10-20 minute in high-speed mixer, make water ratio lower than 0.8% activation modification magnesium hydrate powder.
Step c: high density polyethylene(HDPE), activation modification calcium carbonate superfine powder powder, activation modification magnesium hydrate powder, tetramethylolmethane Stearyl Amine, antioxidant 1010, auxiliary antioxidant 168 are dropped in high-speed mixer and stir and obtained mixing raw material in 8 minutes at 90 ℃, mixing raw material is dropped into to granulation in twin screw extruder, obtain the polyethylene master batch; Wherein the weight proportion of each raw material is:
High density polyethylene(HDPE): 70%
Magnesium hydrate powder: 21%
Calcium carbonate superfine powder powder: 6%
Tetramethylolmethane Stearyl Amine: 1%
Antioxidant 1010: 1%
Auxiliary antioxidant 168:1%.
Material after granulation is extruded-sizing-traction-cooling and shaping-cutting by tube forming mill, made tubing.
After tested, the tensile strength of this halogen-free flameproof PE pipe is 28.09Mpa, and tensile elongation is 215%, and smooth in appearance is white, and oxygen index is 24%.
The preparation method of a kind of halogen-free flameproof PE pipe of embodiment tetra-, comprise
Step a: calcium carbonate superfine powder by weight percentage: 96%, aluminium titanium composite coupler: 2%, silane coupling agent: 2% weighs, calcium carbonate superfine powder is dropped in high-speed mixer, stirring is warmed to 105 ℃ of dehydrations 13 minutes, then aluminium titanium composite coupler and silane coupling agent were dropped in high-speed mixer to mix and blend 16 minutes, and made water ratio lower than 0.8% activation modification calcium carbonate superfine powder powder.
Step b: magnesium hydroxide 97%, silane coupling agent 3% are weighed by weight percentage, magnesium hydroxide is dropped in high-speed mixer, stirring is warmed to 105 ℃ of dehydrations 16 minutes, then silane coupling agent was dropped in high-speed mixer to mix and blend 17 minutes, and made water ratio lower than 0.8% activation modification magnesium hydrate powder.
Step c comprises: high density polyethylene(HDPE), activation modification calcium carbonate superfine powder powder, activation modification magnesium hydrate powder, tetramethylolmethane Stearyl Amine, antioxidant 1010, auxiliary antioxidant 168 are dropped in high-speed mixer and stir and obtained mixing raw material in 8 minutes at 85 ℃, mixing raw material is dropped into to granulation in twin screw extruder, obtain the polyethylene master batch; Wherein the weight proportion of each raw material is:
High density polyethylene(HDPE): 72%
Magnesium hydrate powder: 20%
Calcium carbonate superfine powder powder: 5%
Tetramethylolmethane Stearyl Amine: 1%
Antioxidant 1010: 0.5%
Auxiliary antioxidant 168:1.5%.
Material after granulation is extruded-sizing-traction-cooling and shaping-cutting by tube forming mill, made tubing.
After tested, the tensile strength of this halogen-free flameproof PE pipe is 26.17Mpa, and tensile elongation is 248%, and smooth in appearance is white, and oxygen index is 27%.
The halogen-free flameproof PE pipe produced according to four embodiment of the present invention has first carried out drying and modification to calcium carbonate superfine powder and magnesium hydroxide before manufacturing the polyethylene master batch, make flame retarding efficiency high, all meet the UL94 standard, the addition of halogen-free flame retardants greatly reduces, and has guaranteed that simultaneously the comprehensive mechanical property of PE pipe is good.
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (4)
1. the preparation method of a halogen-free flameproof PE pipe, is characterized in that, comprises the steps:
A, by calcium carbonate superfine powder drying and modification, make activation modification calcium carbonate superfine powder powder;
B, by magnesium hydroxide drying and modification, make the activation modification magnesium hydrate powder;
C, will high density polyethylene(HDPE), activation modification calcium carbonate superfine powder powder, activation modification magnesium hydrate powder, tetramethylolmethane Stearyl Amine, antioxidant 1010, auxiliary antioxidant 168 drop in high-speed mixers and stir and obtained mixing raw material in 5-10 minute at 80-100 ℃, mixing raw material is dropped into to granulation in twin screw extruder, obtain the polyethylene master batch;
D, the polyethylene master batch is extruded-sizing-traction-cooling and shaping-cutting by tube forming mill, made tubing.
2. a kind of preparation method of halogen-free flameproof PE pipe according to claim 1, it is characterized in that, described step a comprises: calcium carbonate superfine powder: 94-97%, aluminium titanium composite coupler: 2-3%, silane coupling agent by weight percentage: 1-3% weighs, calcium carbonate superfine powder is dropped in high-speed mixer, stirring is warmed to 100-110 ℃ of dehydration 10-20 minute, then aluminium titanium composite coupler and silane coupling agent are dropped into to mix and blend 10-20 minute in high-speed mixer, make water ratio lower than 0.8% activation modification calcium carbonate superfine powder powder.
3. a kind of preparation method of halogen-free flameproof PE pipe according to claim 1, it is characterized in that, described step b comprises: magnesium hydroxide 97-99%, silane coupling agent 1-3% weigh by weight percentage, magnesium hydroxide is dropped in high-speed mixer, stirring is warmed to 100-1100 ℃ of dehydration 10-20 minute, then silane coupling agent is dropped into to mix and blend 10-20 minute in high-speed mixer, make water ratio lower than 0.8% activation modification magnesium hydrate powder.
4. a kind of preparation method of halogen-free flameproof PE pipe according to claim 1, is characterized in that, in described step c, the weight proportion of each raw material is:
High density polyethylene(HDPE): 60-78%
Magnesium hydrate powder: 15-30%
Calcium carbonate superfine powder powder: 4-9%
Tetramethylolmethane Stearyl Amine: 1%
Antioxidant 1010: 0.5-1%
Auxiliary antioxidant 168:1-2%.
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CN106967243A (en) * | 2017-04-06 | 2017-07-21 | 浙江伟豪能源科技有限公司 | A kind of preparation method of Graphene antibiosis PE pipes |
CN107081891A (en) * | 2017-05-16 | 2017-08-22 | 镇江宝塑高分子材料有限公司 | A kind of 90 DEG C of thermoplastic low-smoke halide-free material preparation single screw extrusion machines |
CN107118415A (en) * | 2017-04-06 | 2017-09-01 | 浙江伟豪能源科技有限公司 | A kind of preparation method of the fire-retardant PE pipes of graphene |
CN107141551A (en) * | 2017-04-06 | 2017-09-08 | 浙江伟豪能源科技有限公司 | A kind of preparation method of high reliability graphene PE pipes |
CN109265800A (en) * | 2018-09-04 | 2019-01-25 | 武汉升瑞通管业有限公司 | A kind of PE pipe and its production technology |
CN109774001A (en) * | 2018-11-27 | 2019-05-21 | 江西势通钙业有限公司 | A kind of preparation method of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane |
CN113502012A (en) * | 2021-07-21 | 2021-10-15 | 安徽万安环境科技股份有限公司 | Anti-aging termite-rat-proof flame-retardant PE pipeline |
CN113512247A (en) * | 2021-07-21 | 2021-10-19 | 安徽万安环境科技股份有限公司 | Preparation method of anti-aging termite-rat-proof nano self-cleaning flame-retardant PE pipeline |
CN116731397A (en) * | 2023-07-20 | 2023-09-12 | 浙江钦堂钙业有限公司 | Modified shell-core structure calcium carbonate with flame retardant function |
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Cited By (9)
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CN106967243A (en) * | 2017-04-06 | 2017-07-21 | 浙江伟豪能源科技有限公司 | A kind of preparation method of Graphene antibiosis PE pipes |
CN107118415A (en) * | 2017-04-06 | 2017-09-01 | 浙江伟豪能源科技有限公司 | A kind of preparation method of the fire-retardant PE pipes of graphene |
CN107141551A (en) * | 2017-04-06 | 2017-09-08 | 浙江伟豪能源科技有限公司 | A kind of preparation method of high reliability graphene PE pipes |
CN107081891A (en) * | 2017-05-16 | 2017-08-22 | 镇江宝塑高分子材料有限公司 | A kind of 90 DEG C of thermoplastic low-smoke halide-free material preparation single screw extrusion machines |
CN109265800A (en) * | 2018-09-04 | 2019-01-25 | 武汉升瑞通管业有限公司 | A kind of PE pipe and its production technology |
CN109774001A (en) * | 2018-11-27 | 2019-05-21 | 江西势通钙业有限公司 | A kind of preparation method of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane |
CN113502012A (en) * | 2021-07-21 | 2021-10-15 | 安徽万安环境科技股份有限公司 | Anti-aging termite-rat-proof flame-retardant PE pipeline |
CN113512247A (en) * | 2021-07-21 | 2021-10-19 | 安徽万安环境科技股份有限公司 | Preparation method of anti-aging termite-rat-proof nano self-cleaning flame-retardant PE pipeline |
CN116731397A (en) * | 2023-07-20 | 2023-09-12 | 浙江钦堂钙业有限公司 | Modified shell-core structure calcium carbonate with flame retardant function |
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