CN103992436B - A kind of high strength and high impact resistance low content alloy material and preparation method thereof - Google Patents
A kind of high strength and high impact resistance low content alloy material and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29B9/00—Making granules
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7461—Combinations of dissimilar mixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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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
- B29C48/25—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
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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
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- 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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Abstract
The invention discloses a kind of high strength and high impact resistance low content PA6/LLDPE alloy material, include that following components forms according to parts by weight: linear low density polyethylene (LLDPE) 60 ~ 90 parts, polyamide (PA6) 10 ~ 40 parts, maleic anhydride (MAH) 2 ~ 8 parts, montmorillonite 2 ~ 10 parts.The invention also discloses the preparation method of above-mentioned high strength and high impact resistance low content PA6/LLDPE alloy material.The present invention can make two kinds of incompatible resin raw material PA6 and LLDPE well merge, the introducing of LLDPE significantly improves PA6 low temperature impact properties, graft reaction is there is in the molten state in pre-irradiation LLDPE with MAH, strengthen the compatibility of LLDPE Yu PA6, LLDPE and the PA6 boundary that is added in of montmorillonite plays the effect of intercalation, can obtain the PA6/LLDPE alloy material with bicontinuous structure.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of high strength and high impact resistance low content alloy material and preparation method thereof.
Background technology
Linear low density polyethylene (LLDPE) has excellent low-temperature impact, environmental stress cracking resistance；But there is also the problems such as intensity is little, rigidity is low.If carrying out enhancing is blended to LLDPE with engineering plastics PA6, high performance alloys material can be formed.Owing to PA6 with LLDPE cannot be the most compatible, needing to add compatilizer and improve both compatibilitys, polyolefinic introducing can improve the impact property of polyamide (PA), and a small amount of PA can also improve polyolefinic barrier properties for gases and solvent resistance.But, owing to PA and polyolefin are thermodynamics Immiscible Polymer Blends, when by External Force Acting, the stress in its blend cannot transmit effectively between matrix and dispersion phase, thus causes performance seriously to reduce.So blend must be carried out effective increase-volume, to improve water ratio limit power.And economically viable method is by adding reactive compatibilizers at extrusion situ generation graft copolymer in industrialized production, phase size can be stablized, reduce interfacial tension thus realize the enhancing of water ratio limit power, the generation of this reactive compatibilizers graft reaction, it is generally required to carry out initiation grafting by initiator, arises that efficiency of initiation is the highest, graft reaction is uncontrollable causes occurring the problems such as crosslinking in various degree.
Summary of the invention
Goal of the invention: first technical problem to be solved by this invention there is provided a kind of high strength and high impact resistance low content PA6/LLDPE alloy material.Second technical problem to be solved by this invention there is provided the preparation method of above-mentioned alloy material.The present invention is by using the generation of pre-irradiation initiation grafting reaction, dosage and time by pre-irradiation control to produce living radical concentration, and then control graft reaction efficiency and percent grafting, LLDPE and the PA6 compatibility is well strengthened, and the method that this polyolefin is blended with engineering plastics is to prepare high-performance composite materials to provide new thinking.The present invention uses pre-irradiation technology, in air atmosphere, LLDPE is carried out pre-irradiation, the LLDPE of pre-irradiation produces polymeric peroxide on its strand, using the polymeric peroxide of generation on LLDPE strand as initiator, by through the LLDPE of pre-irradiation, PA6, MAH, montmorillonite mixing, carry out reactive blending extrusion, prepare PA6/LLDPE alloy material.The PA6/LLDPE alloy material compatibility obtained is good, mobility is excellent, comprehensive physical good mechanical property, and the especially performance in terms of intensity and shock resistance is obviously improved.
Technical scheme: for solving above-mentioned technical problem, the invention provides a kind of high strength and high impact resistance low content PA6/LLDPE alloy material, include that following components forms according to parts by weight: linear low density polyethylene 60 ~ 90 parts, polyamide 10 ~ 40 parts, maleic anhydride 2 ~ 8 parts, montmorillonite 2 ~ 10 parts.
The preparation method of a kind of high strength and high impact resistance low content PA6/LLDPE alloy material, comprises the following steps:
1) linear low density polyethylene is carried out pre-irradiation process；
2) preparation of PA6/LLDPE alloy material: the linear low density polyethylene processed through pre-irradiation and polyamide, montmorillonite, maleic anhydride (MAH) are joined according to certain ratio of weight and number and is uniformly mixed so as to obtain mixed material in super mixer, mixed material is put in the hopper of double screw extruder and is extruded under the conditions of 180 ~ 240 DEG C, extruded, check rod, cooling, pelletize, obtain low content PA6/LLDPE alloy material.
Wherein, above-mentioned steps 1) in pre-irradiation to process be to load in the cloth bag that is of moderate size by linear low density polyethylene, after tiling, thickness is 3 ~ 10mm, use electron accelerator as irradiation bomb, with β ray, linear low density polyethylene being carried out pre-irradiation process, pre-irradiation dosage range is 2KGy-50KGy
, the time of pre-irradiation is 5 ~ 60s.
In described step 2) before, polyamide is dried 8 ~ 12 hours in 90 DEG C of vacuum drying ovens.
Wherein, above-mentioned steps 2) LLDPE, PA6, MAH, the ratio of weight and number of montmorillonite be: 60 ~ 90:10 ~ 40:2 ~ 8:2 ~ 10.
Wherein, above-mentioned steps 2) in double screw extruder engine speed be 50 ~ 600rpm/min, feeding rotating speed is 15 ~ 50rpm/min.
Wherein, above-mentioned steps 2) in double screw extruder a diameter of 65, draw ratio is 36:1 ~ 44:1.
Wherein, above-mentioned steps 2) in double screw extruder charge door to each section of temperature of mouth die be: 170 ~ 190 DEG C, 170 ~ 190 DEG C, 170 ~ 190 DEG C, 180 ~ 200 DEG C, 180 ~ 200 DEG C, 190 ~ 210 DEG C, 190 ~ 215 DEG C, 200 ~ 220 DEG C, 200 ~ 230 DEG C, 210 ~ 240 DEG C.
The high strength and high impact resistance low content PA6/LLDPE alloy material that above-mentioned preparation method prepares.
Beneficial effect: compared with prior art, the invention have the advantages that polymeric peroxide concentration that the present invention uses pre-irradiation technology to make to produce on LLDPE strand, suitable (peroxide concentrations is the lowest, and grafting efficiency and percent grafting all can reduce；Peroxide concentrations is the highest, crosslinking in various degree can be produced, also can reduce grafting efficiency and percent grafting), be evenly distributed, avoid MAH homopolymerization and the side reaction such as crosslinked polymer or degraded that initiator causes, effectively reduce interfacial tension thus realize the enhancing of water ratio limit power, and stable phase size can be obtained；The present invention can make two kinds of incompatible resin raw material PA6 and LLDPE well merge, the introducing of LLDPE significantly improves PA6 low temperature impact properties, graft reaction is there is in the molten state in pre-irradiation LLDPE with MAH, the graft generated can reduce the interfacial tension between LLDPE and PA6, thus strengthen the compatibility of LLDPE Yu PA6, and pre-irradiation initiation grafting reacts compared to initiator initiation grafting, percent grafting and grafting efficiency are higher, reaction controllability is higher, LLDPE and the PA6 boundary that is added in of montmorillonite plays the effect of intercalation, the PA6/LLDPE alloy material with bicontinuous structure can be obtained, this alloy material physical and mechanical properties is excellent, intensity, the mechanical properties such as impact are good.
Detailed description of the invention
Embodiment 1: the preparation of high strength and high impact resistance low content PA6/LLDPE alloy material
LLDPE carrying out pre-irradiation process in advance: being loaded in the cloth bag being of moderate size by LLDPE, after tiling, thickness is 3mm, use electron accelerator as irradiation bomb, with β ray, linear low density polyethylene is carried out pre-irradiation process, pre-irradiation dosage range is 2KGy
, the time of pre-irradiation is 60s；The LLDPE weight portion 90 parts processed through pre-irradiation is joined in super mixer mix with the PA6 weight portion 10 parts of dry 8 hours in 90 DEG C of vacuum drying ovens, MAH weight portion 3 parts, montmorillonite weight portion 3 parts, mixed material is put in the hopper of double screw extruder, twin screw extrusion process parameter arrange be engine speed be 50rpm/min, feeding rotating speed is 15rpm/min；A diameter of the 65 of extruder, draw ratio is 36:1, and from charge door to die temperature, each section of temperature is: 180,180,190,190,200,210,220,220,225,225 DEG C of reaction masses are extruded under the conditions of 180 ~ 240 DEG C by double screw extruder, draw, are cooled down, pelletize, obtain PA6/LLDPE alloy material.Pure LLDPE notch impact strength is 11KJ/m2, hot strength is 9.8MPa, and the PA6/LLDPE alloy notch impact strength obtained by Formulation Implementation above is from 11KJ/m2Bring up to 40KJ/m2, hot strength brings up to 12MPa from 9.8MPa.
Embodiment 2: the preparation of high strength and high impact resistance low content PA6/LLDPE alloy material
In advance linear low density polyethylene is carried out pre-irradiation process: loaded by LLDPE in the cloth bag being of moderate size, after tiling, thickness is 10mm, using electron accelerator as irradiation bomb, with β ray, LLDPE is carried out pre-irradiation process, pre-irradiation dosage range is 50KGy
, the time of pre-irradiation is 5s；The LLDPE weight portion 60 parts processed through pre-irradiation is joined in super mixer mix with the PA6 weight portion 40 parts of dry 12 hours in 90 DEG C of vacuum drying ovens, MAH weight portion 6 parts, montmorillonite weight portion 6 parts, mixed material is put in the hopper of double screw extruder, twin screw extrusion process parameter arrange be engine speed be 600rpm/min, feeding rotating speed is 50rpm/min；A diameter of the 65 of extruder, draw ratio is 40:1, and from charge door to die temperature, each section of temperature is: 180,180,190,190,200,210,220,220,225,225 DEG C, reaction mass is extruded under the conditions of 180 ~ 240 DEG C by double screw extruder, draws, is cooled down, pelletize, obtains PA6/LLDPE alloy material.The PA6/LLDPE alloy notch impact strength obtained by Formulation Implementation above is 8KJ/m2, hot strength reaches 15MPa.Compared with Example 1, the increase of PA6 content, the hot strength of LLDPE/PA6 alloy material increased, and this is owing to the intensity of PA6 itself is higher, makes the respective performances of system increase.When PA6 increases to 40%, the compatibility poor of system, impact strength is minimum have decreased to 7KJ/m2。
Embodiment 3: the preparation of high strength and high impact resistance low content PA6/LLDPE alloy material
In advance LLDPE is carried out pre-irradiation process: loaded by LLDPE in the cloth bag being of moderate size, after tiling, thickness is 6mm, uses electron accelerator as irradiation bomb, with β ray, LLDPE is carried out pre-irradiation process, pre-irradiation dosage range is 26KGy, and the time of pre-irradiation is 32s；The LLDPE weight portion 75 parts processed through pre-irradiation is joined in super mixer mix with the PA6 weight portion 25 parts of dry 10 hours in 90 DEG C of vacuum drying ovens, MAH weight portion 5 parts, montmorillonite weight portion 2 parts, mixed material is put in the hopper of double screw extruder, twin screw extrusion process parameter arrange be engine speed be 325rpm/min, feeding rotating speed is 32rpm/min；A diameter of the 65 of extruder, draw ratio is 44:1, and from charge door to die temperature, each section of temperature is: 180,180,190,190,200,210,220,220,225,225 DEG C, engine speed 150r/min, reaction mass is extruded under the conditions of 180 ~ 240 DEG C by double screw extruder, draws, is cooled down, pelletize, obtains PA6/LLDPE alloy material.The PA6/LLDPE alloy notch impact strength obtained by Formulation Implementation above is 27KJ/m2, hot strength is 21MPa.
Embodiment 4: the preparation of high strength and high impact resistance low content PA6/LLDPE alloy material
LLDPE carrying out pre-irradiation process in advance: being loaded in the cloth bag being of moderate size by LLDPE, after tiling, thickness is 3 ~ 10mm, use electron accelerator as irradiation bomb, with β ray, LLDPE is carried out pre-irradiation process, pre-irradiation dosage range is 25KGy
, the time of pre-irradiation is 30s；The LLDPE weight portion 90 parts processed through pre-irradiation is joined in super mixer mix with the PA6 weight portion 10 parts of dry 9 hours in 90 DEG C of vacuum drying ovens, MAH weight portion 2 parts, montmorillonite weight portion 8 parts, mixed material is put in the hopper of double screw extruder, twin screw extrusion process parameter arrange be engine speed be 150rpm/min, feeding rotating speed is 30rpm/min；A diameter of the 65 of extruder, draw ratio is 40:1, and from charge door to die temperature, each section of temperature is: 180,180,190,190,200,210,220,220,225,225 DEG C, reaction mass is extruded under the conditions of 180 ~ 240 DEG C by double screw extruder, draws, is cooled down, pelletize, obtains PA6/LLDPE alloy material.The PA6/LLDPE alloy notch impact strength obtained by Formulation Implementation above is 45KJ/m2, hot strength is 12MPa.
The above is only the preferred embodiment of the present invention; it is noted that, to those of ordinary skill in the art; under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (4)
1. the preparation method of a high strength and high impact resistance low content PA6/LLDPE alloy material, it is characterised in that comprise the following steps:
1) linear low density polyethylene is carried out pre-irradiation process；It is to load in the cloth bag being of moderate size by linear low density polyethylene that pre-irradiation processes, after tiling, thickness is 3 ~ 10mm, use electron accelerator as irradiation bomb, with β ray, linear low density polyethylene is carried out pre-irradiation process, pre-irradiation dosage range is 2KGy-50KGy, and the time of pre-irradiation is 5 ~ 60s；
2) preparation of PA6/LLDPE alloy material: the linear low density polyethylene processed through pre-irradiation and polyamide, montmorillonite, maleic anhydride are joined and is uniformly mixed so as to obtain mixed material in super mixer, mixed material puts into the hopper extrusion of double screw extruder, extruded, check rod, cooling, pelletize, obtain low content PA6/LLDPE alloy material；Described linear low density polyethylene 60 ~ 90 parts, polyamide 10 ~ 40 parts, maleic anhydride 2 ~ 8 parts, montmorillonite 2 ~ 10 parts；
Described step 2) in double screw extruder charge door be 170 ~ 190 DEG C, 170 ~ 190 DEG C, 170 ~ 190 DEG C, 180 ~ 200 DEG C, 180 ~ 200 DEG C, 190 ~ 210 DEG C, 190 ~ 215 DEG C, 200 ~ 220 DEG C, 200 ~ 230 DEG C, 210 ~ 240 DEG C to each section of temperature of mouth die.
The preparation method of a kind of high strength and high impact resistance low content PA6/LLDPE alloy material the most according to claim 1, it is characterised in that in described step 2) before, polyamide is dried 8 ~ 12 hours in 70 DEG C ~ 100 DEG C vacuum drying ovens.
The preparation method of a kind of high strength and high impact resistance low content PA6/LLDPE alloy material the most according to claim 1, it is characterised in that described step 2) in double screw extruder engine speed be 50 ~ 600rpm/min, feeding rotating speed is 15 ~ 50rpm/min.
The preparation method of a kind of high strength and high impact resistance low content PA6/LLDPE alloy material the most according to claim 1, it is characterised in that described step 2) in double screw extruder a diameter of 65, draw ratio is 36:1 ~ 44:1.
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Inventor after: Lu Zhaojun Inventor after: Lu Pingcai Inventor after: Xu Jian Inventor after: Zhao Yinzhu Inventor before: Lu Pingcai Inventor before: Xu Jian Inventor before: Zhao Yinzhu |
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Effective date of registration: 20200108 Address after: 212400 opposite the traffic police team of West Ring Road, Jurong Development Zone, Zhenjiang City, Jiangsu Province Patentee after: Jurong Yuda Industrial Investment Co., Ltd Address before: 212400, No. 99 Huayang West Road, Zhenjiang, Jiangsu, Jurong Patentee before: Jiangsu Zhao Lam novel material limited-liability company |