CN102731996A - Preparation method of calcium sulfate whisker filled flame-retardant polyamide high polymer material - Google Patents
Preparation method of calcium sulfate whisker filled flame-retardant polyamide high polymer material Download PDFInfo
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- CN102731996A CN102731996A CN2012101979871A CN201210197987A CN102731996A CN 102731996 A CN102731996 A CN 102731996A CN 2012101979871 A CN2012101979871 A CN 2012101979871A CN 201210197987 A CN201210197987 A CN 201210197987A CN 102731996 A CN102731996 A CN 102731996A
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- calcium sulfate
- parts
- preparation
- sulfate crystal
- crystal whiskers
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Belonging to the technological field of high polymer material preparation, the invention relates to a preparation method of a calcium sulfate whisker filled flame-retardant polyamide high polymer material. The method comprises the steps of: firstly weighing, by weight, 350-400 parts of nylon 610 resin, 100-120 parts of nylon 6 resin, 3.5-5.2 parts of a coupling agent, 70-100 parts of calcium sulfate whiskers, and 30-45 parts of an organic flame retardant, and putting them into a mixing machine for mixing, then putting 1.6-3.5 parts of an antioxidant and 130-170 parts of a chopped glass fiber weighted by weight into the mixing machine for further mixing so as to obtain a granulation material; and putting the granulation material into a twin-screw extruder for melt extrusion, and setting the extrusion temperature of each area, thus obtaining the calcium sulfate whisker filled flame-retardant polyamide high polymer material. The calcium sulfate whisker filled flame-retardant polyamide high polymer material prepared by the method of the invention has a tensile strength more than 130MPa, a bending strength over 260MPa, an izod notched impact strength greater than 23kj/m<2>, a melt index greater than 18g/10min, a heat deflection temperature greater than 230DEG C, and flame retardance up to V-0.
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of preparation method of Flameproof polyamide macromolecular material of calcium sulfate crystal whiskers filling
Background technology
calcium sulfate crystal whiskers receives people's favor with its high cost performance; Calcium sulfate crystal whiskers joined in the polyamide material can significantly improve the material heat resistance; But when being applied to thin goods, because the flame retardant resistance of material can not reach requirement.Thereby limited the purposes of material to a certain extent.Therefore be necessary to explore rational preparation technology and preferred raw material and proportioning thereof and use and under the prerequisite of not losing due mechanical property, ensure to have excellent flame-retardant performance and temperature tolerance, the technical scheme that will introduce below produces under this background
Summary of the invention
task of the present invention is to provide the preparation method of the Flameproof polyamide macromolecular material that a kind of calcium sulfate crystal whiskers fills; This method process procedure is few and be prone to satisfy the industrialized mass production requirement, and the material that obtains has excellent flame and temperature tolerance.
Task of the present invention is accomplished like this, and the preparation method of the Flameproof polyamide macromolecular material that a kind of calcium sulfate crystal whiskers is filled may further comprise the steps:
A) preparation granulation material; 350～40 parts of the NYLON610 resins that will take by weighing by weight earlier, 100～120 parts of Nylon 6s, 3.5～5.2 parts of coupling agents, 70～100 parts of calcium sulfate crystal whiskers and organic fire-retardant are put into for 30～45 parts and are mixed 20-30min in the mixing machine; The rotating speed of mixing machine is 700-1200n/min; Drop into 1.6～3.5 parts in the oxidation inhibitor take by weighing by weight and 130～170 parts of short glass fibers again, continue to mix 2-6min, obtain the granulation material;
B) granulation will be by steps A) the granulation material that obtains drops in the twin screw extruder and melt extrudes, and extrusion temperature is set to: 235 ℃ in a district; 240 ℃ in two districts, 250 ℃ in three districts, 250 ℃ in four districts; 252 ℃ in five districts, 255 ℃ in six districts, 257 ℃ in seven districts; 260 ℃ in eight districts, 250 ℃ in nine districts obtain the Flameproof polyamide macromolecular material that calcium sulfate crystal whiskers is filled.
in one embodiment of the invention, described NYLON610 resin is that fusing point is at 220 ℃ of resins.
in another embodiment of the present invention, described Nylon 6 is 210 ℃ of resins of fusing point.
in yet another embodiment of the present invention, described coupling agent is the 3-aminopropyltriethoxywerene werene.
in another embodiment of the present invention, described calcium sulfate crystal whiskers be surface treated length-to-diameter ratio be 80～120 and length be 5 microns calcium sulfate crystal whiskers.
also have among the embodiment of the present invention, and described organic fire-retardant is a TDE.
are more of the present invention and among embodiment, described oxidation inhibitor is (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester.
in of the present invention and then embodiment, described short glass fiber is the alkali-free short glass fiber for length 3mm.
The tensile strength of the Flameproof polyamide macromolecular material that the calcium sulfate crystal whiskers of the inventive method preparation is filled is greater than 130MPa, and flexural strength is greater than 260MPa, and the socle girder notched Izod impact strength is greater than 23kj/m
2
, melting index is greater than 18g/10min, and heat-drawn wire is greater than 230 ℃, and flame retardant resistance reaches V-0 (UL-94-1.6mm).
Embodiment
Embodiment 1:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is 350 parts of NYLON610 resins at 220 ℃ resin; Fusing point is 110 parts of Nylon 6s at 210 ℃ resin, and coupling agent is 3.5 parts of 3-aminopropyltriethoxywerene werene, surface treated length-to-diameter ratio be 80～120 and length be that 80 parts of calcium sulfate crystal whiskers and the organic fire-retardant of 5 μ m is that TDE is put into for 30 parts and mixed 30min in the mixing machine; The mixing machine rotating speed is 700n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is 2 parts of (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol esters, and length 3mm is 130 parts of alkali-free short glass fibers; Continue to mix 2min, obtain the granulation material;
B) granulation will be by steps A) the granulation material that obtains drops in the twin screw extruder and melt extrudes, and the screw rod extrusion temperature is: 235 ℃ in a district; 240 ℃ in two districts, 250 ℃ in three districts, 250 ℃ in four districts; 252 ℃ in five districts, 255 ℃ in six districts, 257 ℃ in seven districts; 260 ℃ in eight districts, 250 ℃ in nine districts obtain the Flameproof polyamide macromolecular material that calcium sulfate crystal whiskers is filled.
Embodiment 2:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is 380 parts of NYLON610 resins at 220 ℃ resin; Fusing point is 100 parts of Nylon 6s at 210 ℃ resin, and coupling agent is 4 parts of 3-aminopropyltriethoxywerene werene, surface treated length-to-diameter ratio be 80～120 and length be that 100 parts of calcium sulfate crystal whiskers and the organic fire-retardant of 5 μ m is that TDE is put into for 35 parts and mixed 20min in the mixing machine; The mixing machine rotating speed is 1200n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is 1.6 parts of (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol esters, and length 3mm is 170 parts of alkali-free short glass fibers; Continue to mix 3min, obtain the granulation material.All the other are all with the description to embodiment 1.
Embodiment 3:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is 400 parts of NYLON610 resins at 220 ℃ resin; Fusing point is 120 parts of Nylon 6s at 210 ℃ resin, and coupling agent is 4.5 parts of 3-aminopropyltriethoxywerene werene, surface treated length-to-diameter ratio be 80～120 and length be that 90 parts of calcium sulfate crystal whiskers and the organic fire-retardant of 5 μ m is that TDE is put into for 45 parts and mixed 25min in the mixing machine; The mixing machine rotating speed is 1000n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is 3 parts of (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol esters, and length 3mm is 160 parts of alkali-free short glass fibers; Continue to mix 6min, obtain the granulation material.All the other are all with the description to embodiment 1.
Embodiment 4:
A) preparation granulation material; The fusing point that will take by weighing by weight earlier is 390 parts of NYLON610 resins at 220 ℃ resin; Fusing point is 110 parts of Nylon 6s at 210 ℃ resin, and coupling agent is 5.2 parts of 3-aminopropyltriethoxywerene werene, surface treated length-to-diameter ratio be 80～120 and length be that 95 parts of calcium sulfate crystal whiskers and the organic fire-retardant of 5 μ m is that TDE is put into for 40 parts and mixed 20min in the mixing machine; The mixing machine rotating speed is 1100n/min; Dropping into the oxidation inhibitor that takes by weighing by weight again is 3.5 parts of (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol esters, and length 3mm is 145 parts of alkali-free short glass fibers; Continue to mix 4min, obtain the granulation material.All the other are all with the description to embodiment 1.
The Flameproof polyamide macromolecular material that the calcium sulfate crystal whiskers that is obtained by the foregoing description 1-4 is filled has the technique effect shown in the following table through test:
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength MPa | 130 | 133 | 136 | 139 |
| Flexural strength MPa | 260 | 265 | 269 | 273 |
| Socle girder notched Izod impact strength kj/m 2 | 23.0 | 23.4 | 23.7 | 24.2 |
| Melting index g/10min | 18 | 18.3 | 18.6 | 19.1 |
| Heat-drawn wire ℃ | 230 | 235 | 236 | 238 |
| Flame retardant resistance (UL-94-1 .6mm) | V-0 | V-0 | V-0 | V-0 |
Claims (8)
1.
The preparation method of the Flameproof polyamide macromolecular material that a kind of calcium sulfate crystal whiskers is filled is characterized in that may further comprise the steps:
A) preparation granulation material; 350～400 parts of the NYLON610 resins that will take by weighing by weight earlier, 100～120 parts of Nylon 6s, 3.5～5.2 parts of coupling agents, 70～100 parts of calcium sulfate crystal whiskers and organic fire-retardant are put into for 30～45 parts and are mixed 20-30min in the mixing machine; The rotating speed of mixing machine is 700-1200n/min; Drop into 1.6～3.5 parts in the oxidation inhibitor take by weighing by weight and 130～170 parts of short glass fibers again, continue to mix 2-6min, obtain the granulation material;
B) granulation will be by steps A) the granulation material that obtains drops in the twin screw extruder molten disputing and extrudes, and extrusion temperature is set to: 235 ℃ in a district; 240 ℃ in two districts, 250 ℃ in three districts, 250 ℃ in four districts; 252 ℃ in five districts, 255 ℃ in six districts, 257 ℃ in seven districts; 260 ℃ in eight districts, 250 ℃ in nine districts obtain the Flameproof polyamide macromolecular material that calcium sulfate crystal whiskers is filled.
2. the preparation method of the Flameproof polyamide macromolecular material of
calcium sulfate crystal whiskers filling according to claim 1 is characterized in that described NYLON610 resin is that fusing point is at 220 ℃ of resins.
3. the preparation method of the Flameproof polyamide macromolecular material of
calcium sulfate crystal whiskers filling according to claim 1 is characterized in that described Nylon 6 is 210 ℃ of resins of fusing point.
4. the preparation method of the Flameproof polyamide macromolecular material of
calcium sulfate crystal whiskers filling according to claim 1 is characterized in that described coupling agent is the 3-aminopropyltriethoxywerene werene.
5. the preparation method of
calcium sulfate crystal whiskers according to claim 1 Flameproof polyamide macromolecular material of filling, it is characterized in that described calcium sulfate crystal whiskers be surface treated length-to-diameter ratio be 80～120 and length be 5 microns calcium sulfate crystal whiskers.
6. the preparation method of the Flameproof polyamide macromolecular material of
calcium sulfate crystal whiskers filling according to claim 1 is characterized in that described organic fire-retardant is a TDE.
7. the preparation method of the Flameproof polyamide macromolecular material of
calcium sulfate crystal whiskers filling according to claim 1 is characterized in that described oxidation inhibitor is (3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester.
8.
The preparation method of the Flameproof polyamide macromolecular material that calcium sulfate crystal whiskers according to claim 1 is filled is characterized in that described short glass fiber is the alkali-free short glass fiber for length 3mm
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101979871A CN102731996A (en) | 2012-06-15 | 2012-06-15 | Preparation method of calcium sulfate whisker filled flame-retardant polyamide high polymer material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101979871A CN102731996A (en) | 2012-06-15 | 2012-06-15 | Preparation method of calcium sulfate whisker filled flame-retardant polyamide high polymer material |
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| CN102731996A true CN102731996A (en) | 2012-10-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012101979871A Pending CN102731996A (en) | 2012-06-15 | 2012-06-15 | Preparation method of calcium sulfate whisker filled flame-retardant polyamide high polymer material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214840A (en) * | 2013-04-16 | 2013-07-24 | 常熟市凯力达蜂窝包装材料有限公司 | Preparation method of glass-fiber-reinforced black halogen-free flame-retardant polyamide composite material |
| CN103214838A (en) * | 2013-04-16 | 2013-07-24 | 常熟市凯力达蜂窝包装材料有限公司 | Glass-fiber-reinforced black halogen-free flame-retardant polyamide composite material |
| CN103642227A (en) * | 2013-11-18 | 2014-03-19 | 安徽宜万丰电器有限公司 | Polyphenylene sulfide modified nylon material for automobile plastic members |
| WO2014079393A1 (en) * | 2012-11-26 | 2014-05-30 | 浙江盛元化纤有限公司 | Method for preparing flame-retardant melt droplet-resistant polyester |
| CN111892813A (en) * | 2020-07-28 | 2020-11-06 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
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| CN101942193A (en) * | 2009-07-10 | 2011-01-12 | 合肥杰事杰新材料有限公司 | Whisker-enhanced nylon composite |
| CN102061088A (en) * | 2010-12-10 | 2011-05-18 | 南京聚隆科技股份有限公司 | Nylon engineering plastics for high-speed transit railway track and manufacture method thereof |
| CN102108204A (en) * | 2009-12-24 | 2011-06-29 | 合肥杰事杰新材料有限公司 | Plastic case material for breaker and preparation method thereof |
| CN102321362A (en) * | 2011-08-05 | 2012-01-18 | 四川大学 | High-retardant polyamide |
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2012
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101942193A (en) * | 2009-07-10 | 2011-01-12 | 合肥杰事杰新材料有限公司 | Whisker-enhanced nylon composite |
| CN102108204A (en) * | 2009-12-24 | 2011-06-29 | 合肥杰事杰新材料有限公司 | Plastic case material for breaker and preparation method thereof |
| CN102061088A (en) * | 2010-12-10 | 2011-05-18 | 南京聚隆科技股份有限公司 | Nylon engineering plastics for high-speed transit railway track and manufacture method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014079393A1 (en) * | 2012-11-26 | 2014-05-30 | 浙江盛元化纤有限公司 | Method for preparing flame-retardant melt droplet-resistant polyester |
| GB2526441A (en) * | 2012-11-26 | 2015-11-25 | Zhejiang Shengyuan Chemical Fibre Co Ltd | Method for preparing flame-retardant melt droplet-resistant polyester |
| GB2526441B (en) * | 2012-11-26 | 2019-01-09 | Zhejiang Shengyuan Chemical Fibre Co Ltd | Method for preparing flame-retardant and melt droplet-resistant polyester |
| CN103214840A (en) * | 2013-04-16 | 2013-07-24 | 常熟市凯力达蜂窝包装材料有限公司 | Preparation method of glass-fiber-reinforced black halogen-free flame-retardant polyamide composite material |
| CN103214838A (en) * | 2013-04-16 | 2013-07-24 | 常熟市凯力达蜂窝包装材料有限公司 | Glass-fiber-reinforced black halogen-free flame-retardant polyamide composite material |
| CN103642227A (en) * | 2013-11-18 | 2014-03-19 | 安徽宜万丰电器有限公司 | Polyphenylene sulfide modified nylon material for automobile plastic members |
| CN111892813A (en) * | 2020-07-28 | 2020-11-06 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
| CN111892813B (en) * | 2020-07-28 | 2023-01-10 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
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Application publication date: 20121017 |