CN102875888B - A kind of modified graphite master batch and preparation method thereof - Google Patents
A kind of modified graphite master batch and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to materials science field, disclose a kind of modified graphite master batch and preparation method thereof.Modified graphite master batch disclosed by the invention comprises following component and mass percent: the Graphite Powder 99 of 33 ~ 76%, the inorganic powder of 1.65 ~ 28%, 0.11 ~ 4% coupling agent, the resin-oatmeal of 15 ~ 40%, the initiator of 0.5 ~ 3% and 0.5 ~ 5% grafts.The invention also discloses the preparation method of above-mentioned graphite master batch.Graphite master batch of the present invention is dispersed and com-patibilising effect is good.
Description
Technical field
The invention belongs to materials science field, relate to a kind of modified graphite master batch and preparation method thereof.
Background technology
Graphite performance, heat conductivility are excellent, and temperature tolerance is good, and nontoxicity, non-scaling, not pollution medium can make the plastics with excellent properties with resin compounded.But, because the volume of graphite own is little, lightweight, easily disperse, in the processing of traditional blending extrusion, when addition is larger (quality > 20%), no matter be disposable common blanking or side feeding with resin, graphite all can occur at feed opening putty, blanking velocity is uneven, the phenomenons such as the course of processing is unstable, have had a strong impact on process velocity, product properties.And in order to the high filler loading capacity that realizes graphite so as to utilize its excellent high heat conduction, high connductivity, antiwear characteristic, general way adopts thermofixation casting.For the resin extruded injection moulding of high filler loading capacity graphite, still not to effective method of modifying of Graphite Powder 99.
Summary of the invention
For graphite light weight, blanking difficulty when screw extrusion press is processed, in resin, the shortcoming such as difficult dispersion, the object of this invention is to provide a kind of modified graphite master batch, this graphite master batch dispersiveness and com-patibilising effect good.
Another object of the present invention is to provide a kind of preparation method of above-mentioned modified graphite master batch.
Technical scheme of the present invention is as follows:
The invention provides a kind of modified graphite master batch, this modified graphite master batch comprises following component and mass percent:
Graphite Powder 99 33 ~ 76%,
Inorganic powder 1.65 ~ 28%,
Coupling agent 0.11 ~ 4%,
Resin-oatmeal 15 ~ 40%,
Initiator 0.5 ~ 3%,
Grafts 0.5 ~ 5%.
Described Graphite Powder 99 is the crystalline graphite powder that oilness and plasticity-are higher, 200 order ~ 1500 orders.
Described inorganic powder is selected from one or more the mixture in polynite, aluminum oxide, magnesium oxide or titanium dioxide.
Described coupling agent is selected from the mixture of one or more in γ-aminopropyl triethoxysilane (KH-550), γ-methacryloxypropyl trimethoxy silane (KH-570), γ-mercaptopropyl trimethoxysilane (KH-590), isopropyl triisostearoyl titanate (TTS), three (dodecyl benzenesulfonyl) isopropyl titanate (9S) or isopropyl tri (dioctylphosphato)titanate (TTOP-12).Described resin-oatmeal be selected from polypropylene (PP), polyethylene (PE), polystyrene (PS), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyoxymethylene (POM), polycarbonate (PC), polycaprolactam (PA6), polymethylmethacrylate (PMMA), the poly-conventional general-purpose plastics resin such as hexanediamine hexanodioic acid (PA66) or acrylic nitrile-butadiene-styrene (ABS) or engineering plastic resin one or more, and be all extrusion grade or injection grade.
Described initiator is selected from the mixture of one or more in dicumyl peroxide, benzoyl peroxide, the peroxidation trimethylacetic acid tert-butyl ester, Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile).
Described grafts is selected from the compound containing anhydride group, epoxy group(ing) or isocyanato active group, is preferably MALEIC ANHYDRIDE, dodecenylsuccinic acid acid anhydride, maleic anhydride acrylic copolymer or diphenylmethane diisocyanate etc.
Present invention also offers a kind of preparation method of above-mentioned modified graphite master batch, the method comprises the following steps:
(1) be the Graphite Powder 99 of 33 ~ 76% by mass percent, account for (1) use the per-cent of raw material total mass to be 60 ~ 95%; Mass percent is the inorganic powder of 1.65 ~ 28%, account for (1) use the per-cent of raw material total mass to be 3 ~ 35%; Mass percent is the coupling agent of 0.11 ~ 4%, account for (1) use the per-cent of raw material total mass to be 0.2 ~ 5%; At 90 ~ 130 DEG C, mix 15 ~ 30min, take out cool to room temperature, obtain mixed powder a;
(2) by mass percent be 55 ~ 80% mixed powder a, mass percent be 15 ~ 40% resin-oatmeal, mass percent be 0.5 ~ 3% initiator and mass percent be the grafts of 0.5 ~ 5%, stirring at normal temperature mixing 15 ~ 30min in high speed mixing smelting machine, take out cool to room temperature, obtain mixed powder b;
(3) mixed powder b is joined mixing 15 ~ 30min in rubber internal mixer;
(4) will be cut by the mixing gains of rubber internal mixer or pulverize, obtain graphite master batch.
Described rubber internal mixer temperature setting is identical with resin-oatmeal melt temperature.
Compared with the existing technology, tool has the following advantages and beneficial effect in the present invention:
1, in the present invention, Graphite Powder 99 and inorganic powder can accomplish high addition, and dispersion effect is good, meet the specific demand of engineering plastics to Graphite Powder 99 filler.Owing to adopting rubber internal mixer shear agitation, avoid the blanking difficulty in the course of processing, the difficult problems such as difficult mixing.
2, the present invention introduces the high-activity compounds such as coupling agent, initiator, grafts in the course of processing, through effectively processing graphite surface when being uniformly mixed, with mixed with resin plastify extrude time, improve dispersion effect, therefore have enhancement.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
A kind of modified graphite master batch and working method thereof, as described below:
By the 1000 order crystalline graphite powders of 950g, 30g titanium dioxide, 20g silane resin acceptor kh-550, mixes 30min at 90 DEG C, takes out cooling, obtains mixed powder a; By the PP resin-oatmeal of 1000g mixed powder a and 727g, 55g dicumyl peroxide, 36g maleic anhydride acrylic copolymer, in high speed mixing smelting machine, stirring at normal temperature mixing 30min, takes out cooling, obtains mixed powder b;
Mixed powder b is joined mixing 15min in rubber internal mixer, mixing roll temperature is 190 DEG C;
To be cut by the mixing gained block of rubber internal mixer or pulverize, obtain graphite master batch.
Embodiment 2
A kind of modified graphite master batch and working method thereof, as described below:
By the 800 order crystalline graphite powders of 600g, 350g polynite, 50g titanate coupling agent 9S, mixes 30min at 130 DEG C, takes out cooling, obtains mixed powder a; By the PET resin powder of 1000g mixed powder a, 209g, 6g 2,2'-Azobis(2,4-dimethylvaleronitrile), 35g diphenylmethane diisocyanate, in high speed mixing smelting machine, stirring at normal temperature mixing 20min, takes out cooling, obtains mixed powder b;
Mixed powder b is joined mixing 20min in rubber internal mixer, mixing roll temperature is set as 245 DEG C;
To be cut by the mixing gained block of rubber internal mixer or pulverize, obtain graphite master batch.
Embodiment 3
A kind of modified graphite master batch and working method thereof, as described below:
By the 500 order crystalline graphite powders of 780g, 218g aluminum oxide, 2g Silane coupling reagent KH-570, mixes 20min at 120 DEG C, takes out cooling, obtains mixed powder a; By the PBT resin powder of 1000g mixed powder a, 412g, 26.5g benzoyl peroxide, 32g MALEIC ANHYDRIDE, in high speed mixing smelting machine, stirring at normal temperature mixing 15min, takes out cooling, obtains mixed powder b;
Mixed powder b is joined mixing 30min in rubber internal mixer, mixing roll temperature is set as 230 DEG C;
To be cut by the mixing gained block of rubber internal mixer or pulverize, obtain graphite master batch.
Embodiment 4
A kind of modified graphite master batch and working method thereof, as described below:
By the 200 order crystalline graphite powders of 784g, 190g magnesium oxide, 26g titanate coupling agent TTOP-12, mixes 30min at 100 DEG C, takes out cooling, obtains mixed powder a; By the ABS resin powder of 1000g mixed powder a, 192g, the 25.6g peroxidation trimethylacetic acid tert-butyl ester, 64g dodecenylsuccinic acid acid anhydride, in high speed mixing smelting machine, stirring at normal temperature mixing 30min, takes out cooling, obtains mixed powder b;
Mixed powder b is joined mixing 30min in rubber internal mixer, mixing roll temperature is set as 210 DEG C;
To be cut by the mixing gained block of rubber internal mixer or pulverize, obtain graphite master batch.
Embodiment 5
A kind of modified graphite master batch and working method thereof, as described below:
By the 300 order crystalline graphite powders of 950g, 30g polynite, 20g silane coupling agent KH-590, mixes 15min at 120 DEG C, takes out cooling, obtains mixed powder a; By the PMMA resin-oatmeal of 1000g mixed powder a, 209g, the Diisopropyl azodicarboxylate of 6.3g, 35g MALEIC ANHYDRIDE, in high speed mixing smelting machine, stirring at normal temperature mixing 30min, takes out cooling, obtains mixed powder b;
Mixed powder b is joined mixing 20min in rubber internal mixer, mixing roll temperature is set as 230 DEG C;
To be cut by the mixing gained block of rubber internal mixer or pulverize, obtain graphite master batch.
Comparative example
By PP resin-oatmeal, aluminum oxide, 600 order crystalline graphite powders, silane resin acceptor kh-550, initiator dicumyl peroxide, grafts MALEIC ANHYDRIDE by weight ratio 600g: 30g: 350g: 5g: 7g: 8g normal temperature mixes, by Screw Extrusion granulation, extruder temperature section is set as 130 ~ 200 DEG C, and die temperature is 180 DEG C.
The graphite master batch obtained in above-described embodiment and resin, processing aid are mixed by weight 40%: 55 ~ 59%: 1 ~ 5%, all can through Screw Extrusion granulation, and pelletizing is even.According to the method then easy putty of comparative example, extrude instability.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (5)
1. a modified graphite master batch, is characterized in that: this modified graphite master batch comprises following component and mass percent,
Described inorganic powder is selected from one or more the mixture in polynite, aluminum oxide, magnesium oxide or titanium dioxide;
The preparation method of described modified graphite master batch comprises the following steps:
(1) be the Graphite Powder 99 of 33 ~ 76% by mass percent, account for (1) use the per-cent of raw material total mass to be 60 ~ 95%; Mass percent is the inorganic powder of 1.65 ~ 28%, account for (1) use the per-cent of raw material total mass to be 3 ~ 35%; Mass percent is the coupling agent of 0.11 ~ 4%, account for (1) use the per-cent of raw material total mass to be 0.2 ~ 5%; At 90 ~ 130 DEG C, mix 15 ~ 30min, take out cool to room temperature, obtain mixed powder a;
(2) by mass percent be 55 ~ 80% mixed powder a, mass percent be 15 ~ 40% resin-oatmeal, mass percent be 0.5 ~ 3% initiator and mass percent be the grafts of 0.5 ~ 5%, stirring at normal temperature mixing 15 ~ 30min in high speed mixing smelting machine, take out cool to room temperature, obtain mixed powder b;
(3) mixed powder b is joined mixing 15 ~ 30min in rubber internal mixer;
(4) will be cut by the mixing gains of rubber internal mixer or pulverize, obtain graphite master batch;
Described Graphite Powder 99 is crystalline graphite powder, 200 order ~ 1500 orders;
Described coupling agent is selected from the mixture of one or more in γ-aminopropyl triethoxysilane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, isopropyl triisostearoyl titanate, three (dodecyl benzenesulfonyl) isopropyl titanates or isopropyl tri (dioctylphosphato)titanate;
Described grafts is selected from MALEIC ANHYDRIDE, dodecenylsuccinic acid acid anhydride or maleic anhydride acrylic copolymer.
2. modified graphite master batch according to claim 1, it is characterized in that: described resin-oatmeal be selected from polypropylene, polyethylene, polystyrene, polyethylene terephthalate, polybutylene terephthalate, polyoxymethylene, polycarbonate, polycaprolactam, polymethylmethacrylate, poly-hexanediamine hexanodioic acid or acrylic nitrile-butadiene-styrene one or more, and be all extrusion grade or injection grade.
3. modified graphite master batch according to claim 1, is characterized in that: described initiator is selected from the mixture of one or more in dicumyl peroxide, benzoyl peroxide, the peroxidation trimethylacetic acid tert-butyl ester, Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile).
4. the preparation method of the arbitrary described modified graphite master batch of claims 1 to 3, is characterized in that: the method comprises the following steps,
(1) be the Graphite Powder 99 of 33 ~ 76% by mass percent, account for (1) use the per-cent of raw material total mass to be 60 ~ 95%; Mass percent is the inorganic powder of 1.65 ~ 28%, account for (1) use the per-cent of raw material total mass to be 3 ~ 35%; Mass percent is the coupling agent of 0.11 ~ 4%, account for (1) use the per-cent of raw material total mass to be 0.2 ~ 5%; At 90 ~ 130 DEG C, mix 15 ~ 30min, take out cool to room temperature, obtain mixed powder a;
(2) by mass percent be 55 ~ 80% mixed powder a, mass percent be 15 ~ 40% resin-oatmeal, mass percent be 0.5 ~ 3% initiator and mass percent be the grafts of 0.5 ~ 5%, stirring at normal temperature mixing 15 ~ 30min in high speed mixing smelting machine, take out cool to room temperature, obtain mixed powder b;
(3) mixed powder b is joined mixing 15 ~ 30min in rubber internal mixer;
(4) will be cut by the mixing gains of rubber internal mixer or pulverize, obtain graphite master batch.
5. the preparation method of modified graphite master batch according to claim 4, is characterized in that: described rubber internal mixer temperature setting is identical with resin-oatmeal melt temperature.
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| CN103724026B (en) * | 2013-12-30 | 2014-12-17 | 江苏苏嘉集团新材料有限公司 | Magnesium carbon-based castable |
| CN104119558A (en) * | 2014-07-02 | 2014-10-29 | 合肥和安机械制造有限公司 | Modified graphite used for wear-resistant high-pressure rubber hose materials and a preparing method of the modified graphite |
| CN109627618A (en) * | 2018-11-30 | 2019-04-16 | 朱莲华 | A kind of graphene polystyrene doped material and preparation method thereof |
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| CN101857689A (en) * | 2010-02-26 | 2010-10-13 | 广东联塑科技实业有限公司 | Material for preparing plastic pipeline with high thermal conductivity |
| CN101906225A (en) * | 2009-06-04 | 2010-12-08 | 合肥杰事杰新材料有限公司 | Thermal conductive high polymer material applied to pipes and preparation method thereof |
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| CN1908075A (en) * | 2006-08-02 | 2007-02-07 | 华侨大学 | Modified expanded graphite master batch and preparation method thereof |
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| CN101906225A (en) * | 2009-06-04 | 2010-12-08 | 合肥杰事杰新材料有限公司 | Thermal conductive high polymer material applied to pipes and preparation method thereof |
| CN101857689A (en) * | 2010-02-26 | 2010-10-13 | 广东联塑科技实业有限公司 | Material for preparing plastic pipeline with high thermal conductivity |
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Denomination of invention: Modified graphite masterbatch and preparation method thereof Effective date of registration: 20191202 Granted publication date: 20160210 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |