CN114874537B - Antistatic PP composite material with high heat resistance and high dimensional stability, and preparation method and application thereof - Google Patents
Antistatic PP composite material with high heat resistance and high dimensional stability, and preparation method and application thereof Download PDFInfo
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- CN114874537B CN114874537B CN202210320894.7A CN202210320894A CN114874537B CN 114874537 B CN114874537 B CN 114874537B CN 202210320894 A CN202210320894 A CN 202210320894A CN 114874537 B CN114874537 B CN 114874537B
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 31
- 239000010445 mica Substances 0.000 claims abstract description 25
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 12
- 239000002482 conductive additive Substances 0.000 claims abstract description 8
- 239000004743 Polypropylene Substances 0.000 claims description 43
- 239000012752 auxiliary agent Substances 0.000 claims description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 239000000314 lubricant Substances 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 7
- 229920000570 polyether Polymers 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- -1 polypropylene Polymers 0.000 claims description 6
- 239000012745 toughening agent Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 229920001940 conductive polymer Polymers 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000005022 packaging material Substances 0.000 claims description 2
- 229920000092 linear low density polyethylene Polymers 0.000 abstract description 3
- 239000004707 linear low-density polyethylene Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002216 antistatic agent Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention relates to an antistatic PP composite material with high heat resistance and high dimensional stability, a preparation method and application thereof. The composite material comprises the following components in parts by weight: 70-90 parts of PP resin; 5-10 parts of LLDPE; 2-20 parts of a conductive additive; 20-35 parts of mica powder; 1-5 parts of flake graphite; 0.5 to 2 parts of IDP resin. The composite material has better heat resistance, dimensional stability and conductivity.
Description
Technical Field
The invention belongs to the technical field of thermoplastic materials, and particularly relates to an antistatic PP composite material with high heat resistance and high dimensional stability, and a preparation method and application thereof.
Background
In the field of antistatic materials, a great application direction is electronic bearing and packaging, such as IC trays and the like. In general, such application scenarios have high requirements on the heat resistance and dimensional stability of the material. The heat-resistant antistatic materials which are economically available at present are usually amorphous materials with high glass transition temperature, such as Polycarbonate (PC), polyphenyl ether (PPE) and the like, and the materials have good heat resistance, are usually easy to reach the HDT temperature of more than 120 ℃ and have good dimensional stability. However, the materials have certain defects, such as reduced fluidity, difficult processing and higher material cost after the conductive filler is added, and limit the application of the materials in partial scenes. In addition, the existing antistatic material also has improved thermal stability by adding a filler, for example, chinese patent CN111171456a discloses a polypropylene composite material and a preparation method thereof, and the composite material has certain properties such as antistatic property and thermal stability by adding a mineral filler, an antistatic agent, a processing aid and the like into polypropylene resin, but the composite material has poor conductivity and heat resistance, and the composite material has poor dimensional stability, and cannot meet the application scenario with high requirements on conductivity, heat resistance and dimensional stability.
Disclosure of Invention
The invention aims to solve the technical problem of providing an antistatic PP composite material with high heat resistance and high dimensional stability, and a preparation method and application thereof, so as to overcome the defect of poor conductivity, heat resistance and dimensional stability of the PP composite material in the prior art.
The invention provides an antistatic PP composite material with high heat resistance and high dimensional stability, which comprises the following components in parts by weight:
preferably, the composite material comprises the following components in parts by weight:
preferably, the PP resin has a melt index of 5-20g/10min at 230 ℃/2.16 kg. The melt index is tested in accordance with ISO 1133-1-2011. PP resin base materials with different fluidity have different wettability to the conductive auxiliary agent, and PP resin with poor fluidity can cause that the conductive auxiliary agent aggregate cannot be dispersed to form physical defects.
Preferably, the conductive auxiliary agent comprises one or more of conductive carbon black, carbon fiber and carbon nano tube.
Preferably, the oil absorption value of the conductive carbon black is 120-180cm 3 100g, specific surface area of 40-80m 2 And/g, the particle size is 25-45nm. The conductive carbon black in the range has excellent dispersibility, and can effectively reduce stress defects caused by poor dispersion of the carbon black. The oil absorption value was measured as TS 2583-1977. The particle size of the conductive carbon black in the PP composite material is the same as that of the conductive carbon black as a raw material, and the particle size of the conductive carbon black as the raw material is unchanged after the conductive carbon black is melted and extruded by a double-screw extruder, so that the conductive carbon black is the minimum physical dimension in the production of the carbon black.
Preferably, the mica powder has a particle size of 125-1250 mesh, more preferably 325-500 mesh. Mica powder having a smaller particle size has a better stabilizing effect on the size, but the smaller particle size is not suitable for processing. Too little mica powder content has limited dimensional stabilizing effect, too high content can not be processed smoothly, and the mechanical strength of the material is greatly reduced.
Preferably, the flake graphite is synthetic graphite; the grain diameter of the flake graphite D50 is 40-80 um.
Preferably, the IDP resin is a polyether type high-molecular conductive polymer, the polyether type high-molecular conductive polymer is a polypropylene polyether block copolymer, and the surface resistivity is 10 6 ～10 8 Ω/sq。
Preferably, the PP composite material further comprises 0-10 parts of an additive.
Preferably, the additive comprises one or more of an antioxidant, a lubricant, mineral powder and a toughening agent.
Preferably, the antioxidant comprises one or more of hindered phenol antioxidants, hindered amine antioxidants and phosphite antioxidants.
Preferably, the lubricant comprises one or more of an ester lubricant, an amide lubricant and a polyethylene lubricant.
Preferably, the mineral powder comprises one or more of talcum powder, calcium carbonate and mica.
Preferably, the toughening agent comprises one or more of POE type toughening agent, SEBS type toughening agent and EXA type toughening agent.
The invention also provides a preparation method of the antistatic PP composite material with high heat resistance and high dimensional stability, which comprises the following steps:
and mixing the conductive auxiliary agent with all components except the mica powder, and feeding the obtained mixture, the conductive auxiliary agent and the mica powder into a double-screw extruder for extrusion granulation to obtain the antistatic PP composite material with high heat resistance and high dimensional stability.
Preferably, the twin screw extruder has an aspect ratio of 40 to 60:1, the processing temperature is 180-250 ℃.
The invention also provides an application of the antistatic PP composite material with high heat resistance and high dimensional stability in electronic appliances or packaging materials, such as IC trays, floor washers and the like.
The IDP resin of the present invention is an intrinsic conductive polymer, such as PP-PEO structure (polypropylene polyether block copolymer), with surface resistivity of 10 6 ～10 8 Ω/sq。
In the invention, due to the lamellar structure of the mica powder, the transverse and longitudinal shrinkage rate of the composite material can be reduced, so that the dimensional stability of the material is improved, but the effect of rivets in the resin is only exerted, and the shrinkage difference caused by crystallization of a resin phase cannot be changed. According to the invention, a small amount of flake graphite is added to form a synergistic effect with the conductive auxiliary agent, so that the heat conducting property of the composite material is rapidly improved, the heat released by PP resin crystallization is rapidly diffused and homogenized in the injection molding process of the material, the regularity of a PP crystallization area is improved, and the dimensional stability of a resin phase is improved. Through the cooperation of mica powder, conductive auxiliary agent and crystalline flake graphite, the stability of different phases can be improved simultaneously, thereby achieving the synergistic effect of stable size.
The IDP resin is added, so that the IDP resin can be enriched around the conductive auxiliary agent due to the characteristic of strong polarity, and the connecting paths of the conductive auxiliary agents are increased, so that the material resistance is further greatly reduced by a small amount of the IDP resin.
Advantageous effects
The invention adopts the compounding of the conductive auxiliary agent, the mica powder and the crystalline flake graphite, so that the PP composite material has better heat resistance and dimensional stability.
The invention adopts the compounding of the conductive additive and the IDP resin, and can obviously improve the conductivity of the PP composite material.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Reagent source:
PP resin 1: PP SP179, petrochemical, melt index at 230 ℃/2.16kg at 8.0g/10min;
PP resin 2: PP K9017, taiwan, has a melt index of 19.0g/10min at 230 ℃/2.16 kg;
PP resin 3: k8003, a melt index of 2g/10min at 230 ℃/2.16 kg;
PP resin 4: PP BX3920, korean SK, melt index 100g/10min at 230 ℃/2.16 kg;
PA resin: PA6 resin, PA6 YH400, baling petrochemical;
LLDPE: LLDPE 7042, a luxury petrochemical product;
conductive auxiliary agent:
conductive additive 1: conductive carbon black with oil absorption value of 171cm 3 100g, specific surface area 62m 2 Per gram, the particle size is 40nm, the carbon black Ensaco 250G and the density is high;
conductive auxiliary 2: conductive carbon black with oil absorption value of 114cm 3 100g, specific surface area 115m 2 Per gram, particle size 22nm, N220, black cat black;
conductive auxiliary agent 3: carbon fiber, PX35CA0250-65, dongli, diameter 7um;
conductive auxiliary agent 4: carbon nanotubes, GC-21, shandong, large scale;
mica powder 1: wet mica, 125 mesh, rimamine mineral;
mica powder 2: wet mica, 325 mesh, guangzhou jia;
mica powder 3: wet mica, 500 mesh, guangzhou jia;
mica powder 4: wet mica, 1250 mesh, guangzhou jia;
flake graphite 1: synthetic graphite with D50 particle size of 44um, KS44 and Yirui stone;
flake graphite 2: synthetic graphite with D50 particle size of 150um, KS150, yirui stone;
IDP resin: PELECTRON resin, pelecstat-230, surface resistivity 5 x 10 7 Omega/sq, three oceans.
Additive:
an antioxidant: hindered phenols, commercially available;
and (3) a lubricant: amides, commercially available.
The additives (antioxidants, lubricants) used in the examples and comparative examples are the same commercial products.
The preparation method of the PP composite material comprises the following steps:
according to the proportions of table 1, table 2 and table 3, the conductive auxiliary agent and the components except the mica powder are mixed, and the obtained mixture, the conductive auxiliary agent and the mica powder are fed into a double-screw extruder for extrusion granulation, so that the antistatic PP composite material is obtained. Wherein, the length-diameter ratio of the twin-screw extruder is 52:1, the processing temperature is 180-250 ℃.
Performance test:
(1) Injection molding 100 x 1mm square plates, horizontally placing on a plane workbench, searching a gap between the square plates and a platform, measuring the maximum gap between the square plates and the platform by using a feeler gauge to obtain the warpage deformation quantity of the material, and testing the surface resistivity by using an RT-1000 surface resistance meter;
(2) Injecting 200mm shrinkage rate sample bars, testing the shrinkage rate of materials, measuring the length of the sample bars by using a two-dimensional optical imager, and calculating to obtain the shrinkage rate;
(3) 100 x 1mm square and 200mm shrinkage bars were baked at 120 ℃ for 2 hours, respectively, and the warpage deformation and shrinkage were measured according to the above-described methods.
Table 1 examples 1-10 proportions (parts by weight)
Table 2 examples 11-15 proportions (parts by weight)
Table 3 comparative example ratio (parts by weight)
As can be seen from tables 1 to 3, comparative example 1 was free from the addition of conductive additive, comparative example 2 was free from the addition of mica powder, comparative example 3 was free from the addition of crystalline flake graphite, comparative example 4 was PA resin, and comparative examples 1 to 4 were larger in shrinkage, warpage deformation, shrinkage after baking and warpage deformation after baking than example 1, and thus it was found that the addition of conductive additive, mica powder and crystalline flake graphene to PP resin was compounded to improve heat resistance and dimensional stability of PP resin composite material.
Comparative example 1 does not add a conductive additive, comparative example 5 does not add an IDP resin, and the surface resistances of comparative example 1 and comparative example 5 are significantly greater than those of example 1, and it can be seen that the conductivity of the composite material can be significantly improved by compounding the conductive additive and the IDP resin.
Claims (9)
1. The antistatic PP composite material with high heat resistance and high dimensional stability is characterized by comprising the following components in parts by weight:
the melt index of the PP resin is 5-20g/10min under the conditions of 230 ℃/2.16 kg;
the grain diameter of the flake graphite D50 is 40-80 um;
the IDP resin is a polyether type high-molecular conductive polymer, and the polyether type high-molecular conductive polymer is a polypropylene polyether block copolymer.
2. The PP composite material of claim 1, wherein the composite material comprises, in parts by weight:
3. the PP composite material of claim 1, wherein the conductive additive comprises one or more of conductive carbon black, carbon fiber, and carbon nanotubes; the oil absorption value of the conductive carbon black is 120-180cm 3 100g, specific surface area of 40-80m 2 And/g, the particle size is 25-45nm.
4. The PP composite of claim 1 wherein the mica powder has a particle size of 125-1000 mesh.
5. The PP composite material of claim 1 wherein the flake graphite is synthetic graphite; the grain diameter of the flake graphite D90 is 48-65 um; IDP resin having surface resistivity of 10 6 ～10 8 Ω/sq。
6. The PP composite of claim 1, further comprising 0-10 parts of an additive; the additive comprises one or more of an antioxidant, a lubricant, mineral powder and a toughening agent.
7. A process for the preparation of a PP composite material as defined in any one of claims 1 to 6, comprising the steps of:
and mixing the conductive auxiliary agent with all components except the mica powder, and feeding the obtained mixture, the conductive auxiliary agent and the mica powder into a double-screw extruder for extrusion granulation to obtain the antistatic PP composite material with high heat resistance and high dimensional stability.
8. The method of claim 7, wherein the twin screw extruder has an aspect ratio of 40 to 60:1, the processing temperature is 180-250 ℃.
9. Use of a PP composite material as defined in any one of claims 1 to 6 in an electronic appliance or packaging material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210320894.7A CN114874537B (en) | 2022-03-22 | 2022-03-22 | Antistatic PP composite material with high heat resistance and high dimensional stability, and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210320894.7A CN114874537B (en) | 2022-03-22 | 2022-03-22 | Antistatic PP composite material with high heat resistance and high dimensional stability, and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN114874537A CN114874537A (en) | 2022-08-09 |
| CN114874537B true CN114874537B (en) | 2024-01-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH07238214A (en) * | 1994-03-01 | 1995-09-12 | Plus Teku Kk | Heat-resistant, electrically-conductive resin composition and heat-resistant ic tray using the same |
| CN102643480B (en) * | 2012-05-04 | 2014-05-14 | 浙江三威防静电装备有限公司 | Anti-static alloy composite material and preparation method thereof |
| JP5582586B2 (en) * | 2012-10-10 | 2014-09-03 | 株式会社ジェイエスピー | Polyolefin resin foamed molded body |
| CN106046550A (en) * | 2016-06-28 | 2016-10-26 | 邵炯 | High-temperature-resistant, aging-resistant and impact-resistant heat-conduction polypropylene material and preparing method thereof |
| CN107082951A (en) * | 2017-04-17 | 2017-08-22 | 广东圆融新材料有限公司 | A kind of antistatic low warp glass fiber strengthens weather-proof PP materials and preparation method thereof |
| KR102236413B1 (en) * | 2018-11-30 | 2021-04-05 | 롯데첨단소재(주) | Thermoplastic resin composition and article produced therefrom |
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