CN111171424B - High-fluidity black master batch for PA engineering plastic and preparation method thereof - Google Patents
High-fluidity black master batch for PA engineering plastic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-fluidity black master batch for PA engineering plastics, which comprises the following components in percentage by weight: 29.5 to 50 percent of polyolefin resin; 5-20% of maleic anhydride grafted polyolefin; 20-50% of carbon black; 5-20% of aniline black; 5-20% of nano silicon carbide; 5-15% of a rheological agent; 0.5 to 2 percent of silane coupling agent. The invention also discloses a preparation method of the high-fluidity black master batch for the PA engineering plastic. The high black master batch can effectively improve the fluidity and the pigment dispersibility of PA plastic; thereby improving the blackness, the glossiness and the wear resistance of the surface of the product, improving the 'floating fiber' on the surface of the reinforced nylon, and solving the problems that the existing black master is difficult to meet the higher processability and surface requirements of the high-filling nylon engineering plastic, and the like; the preparation method is simple and low in cost.
Description
The technical field is as follows:
the invention relates to the technical field of high polymer materials, in particular to a high-flow black master batch for PA engineering plastics and a preparation method thereof.
The background art comprises the following steps:
the PA has excellent performance as an engineering plastic with wide application, can be further improved after being modified by filling, strengthening, toughening, flame retarding and the like, and is widely applied to the industries of automobiles, electronics and electrics, packaging, machinery, furniture, building materials, sports and leisure articles, articles for daily use, toys and the like. The coloring of the modified nylon material is an indispensable part in the processing process of the nylon product, and the coloring of the nylon product is mainly black.
The current black master batch used for nylon coloring is mainly universal black master batch, and is obtained by melting and extruding polyolefin and carbon black. When the universal black master batch is applied to high-filling nylon, the problems of difficult dispersion of carbon black, overlarge extrusion current, more surface defects of products and the like can occur. To address the above problems, many nylon modification plants reduce the screw extrusion rate and add more other additives such as mold release agents, dispersants, etc. However, the addition of too much auxiliary agent introduces more processing procedures, which leads to the reduction of production efficiency, the increase of errors in production of ingredients and the serious unqualified product performance.
The invention content is as follows:
one of the technical problems to be solved by the invention is to provide a high-flow black master batch for PA engineering plastics, aiming at the defects of the prior art, wherein the high-flow black master batch can effectively improve the fluidity and the pigment dispersibility of the PA plastics; thereby improving the blackness, the glossiness and the wear resistance of the surface of the product, improving the 'floating fiber' on the surface of the reinforced nylon, and solving the problems that the existing black master is difficult to meet the higher processability and the surface requirement of the high-filling nylon engineering plastic, and the like.
The second technical problem to be solved by the invention is to provide a preparation method of the high-flow black master batch for PA engineering plastics, aiming at the defects of the prior art, the method is simple to operate, the preparation cost is low, and the prepared black master batch has excellent performance.
In order to better solve the first technical problem, the invention adopts the following technical scheme:
a high-flow black master batch for PA engineering plastics comprises the following components in percentage by weight:
as a preferred technical scheme, the polyolefin is one or a mixture of PP, PE, POE and EVA; more preferably, the polyolefin resin is one or a mixture of PE and POE, and the performance of the polyolefin resin is preferably that the melt index of 190 ℃/2.16Kg is 5-100g/10min. The higher fluidity of the matrix resin contributes to an increase in the amount of toner filling and dispersion.
As a preferable technical scheme, the maleic anhydride grafted polyolefin is one or a mixture of PP-g-MAH, PE-g-MAH, POE-g-MAH and EVA-g-MAH. Further preferred is one or a mixture of PE-g-MAH and POE-g-MAH. The grafting ratio of the maleic anhydride grafted polyolefin is 1-10%, and the grafting ratio is preferably 5-10%. The maleic anhydride grafted polyolefin is beneficial to improving the compatibility of matrix resin and toner, is beneficial to improving the compatibility of the black master matrix resin and PA resin when the high-flow black master is applied to PA engineering plastics, and solves the problems of surface peeling and the like caused by incompatibility of the matrix resin and PA.
As a preferable technical scheme, the particle size of the carbon black is 5-200nm. Further preferred is high-pigment carbon black having a particle diameter of 5 to 20 nm. The smaller the particle diameter of the carbon black, the stronger the coloring power.
As a preferable technical scheme, the nigrosine is oil-soluble nigrosine and alcohol-soluble nigrosine. Further preferably oil-soluble aniline black, and the temperature resistance is more than 280 ℃. The aniline black has good compatibility with PA, strong tinting strength and good covering property when applied to PA engineering plastics, and is beneficial to improving the surface glossiness, smoothness and mechanical property maintenance of the modified nylon.
As a preferable technical scheme, the particle size of the nano silicon carbide is 20-500nm, and more preferably 20-100nm. The nano silicon carbide has high purity, high hardness and good compatibility with PA resin, and can obviously improve the wear resistance and tensile strength of products when added into PA engineering plastics.
As a preferred technical scheme, the rheological agent is one or a mixture of two of saturated monocarboxylic acid and saturated dicarboxylic acid. More preferably saturated dicarboxylic acid, specifically one or more of adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, dodecanedioic acid, tetradecanedioic acid, hexadecanedioic acid, octadecanedioic acid and eicosanedioic acid. Under melting, the acid can destroy hydrogen bonds formed between long-chain amido bonds of the PA and also has a certain hydrolysis effect on the amido bonds of the PA, so that the processing flowability of the filled nylon is improved.
As a preferable technical scheme, the silane coupling agent is one or a mixture of KH550, KH560 and KH 570; further preferred is KH550 or KH560 or a mixture of both. The silane coupling agent can react with surface hydroxyls such as carbon black, nano silicon carbide and the like to form bonds and can also interact with long chains of polymers, so that the compatibility of the carbon black, the nano silicon carbide and the aniline black with resin is improved, the dispersity is improved, and the phenomenon that the carbon black and the nano silicon carbide are not well dispersed and are agglomerated in a final product is avoided.
In order to better solve the second technical problem, the invention adopts the following technical scheme:
a preparation method of a high-flow black master batch for PA engineering plastics comprises the following steps:
(1) Respectively and uniformly mixing carbon black, aniline black and nano silicon carbide with dimethylbenzene, adding a silane coupling agent, stirring and mixing, heating to 60-80 ℃, reacting for 4-6 hours, performing rotary evaporation and concentration after the reaction is finished, drying, and grinding the solid obtained by drying to obtain modified carbon black, modified aniline black and modified nano silicon carbide;
(2) Uniformly mixing the prepared modified carbon black, modified aniline black and modified nano silicon carbide, and then feeding the mixture into a double-screw extruder from a side feeding port; and uniformly mixing the polyolefin resin, the maleic anhydride grafted polyolefin and the rheological agent in a high-speed mixer, feeding the mixture into a double-screw extruder from a main feeding port, and performing melt extrusion, cooling, granulating and drying to obtain the high-fluidity black master batch.
As a preferable technical scheme, in the step (2), the temperature of the melt extrusion is 120-280 ℃.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the high-flow black master batch for the PA engineering plastic, which is prepared by the invention, is applied to the high-filling PA engineering plastic, can obviously improve the dispersion effect of fillers such as carbon black and the like in resin, improve the processing fluidity of the PA engineering plastic, improve the processing efficiency, improve the blackness, the glossiness and the wear resistance of the surface of a product and improve the 'floating fiber' on the surface of reinforced nylon.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to be limiting.
EXAMPLE 1
A high-flow black master batch for PA engineering plastics comprises the following components in percentage by weight:
LDPE MG70 33％；
PE-g-MAH 15％；
25% of high-pigment carbon black;
oil-soluble black 7%;
10% of nano silicon carbide;
5% of tetradecanedioic acid;
silane coupling agent KH550 percent;
the preparation method comprises the following steps:
(1) Respectively and uniformly mixing high-color carbon black, oil-soluble black 7 and nano silicon carbide with dimethylbenzene, adding a silane coupling agent KH550, stirring and mixing, heating to 80 ℃, reacting for 4 hours, carrying out rotary evaporation and concentration at 75 ℃ after the reaction is finished, drying, and grinding solids obtained by drying at 105 ℃ to obtain modified high-color carbon black, modified oil-soluble black 7 and modified nano silicon carbide respectively;
(2) Uniformly mixing the prepared modified high-pigment carbon black, modified oil-soluble black 7 and modified nano silicon carbide, and feeding the mixture into a double-screw extruder from a side feeding port; uniformly mixing LDPE MG70 (Kataler petrochemical, melt index 190 ℃/2.16Kg).
Example 2
A high-flow black master batch for PA engineering plastics comprises the following components in percentage by weight:
POE 8200 33％；
POE-g-MAH 15％；
25% of high-pigment carbon black;
oil-soluble black 7%;
10% of nano silicon carbide;
5% of tetradecanedioic acid;
silane coupling agent KH 560%;
the preparation method comprises the following steps:
(1) Respectively and uniformly mixing high-pigment carbon black, oil-soluble black 7 and nano silicon carbide with dimethylbenzene, adding a silane coupling agent KH560, stirring and mixing, heating to 80 ℃, reacting for 4 hours, carrying out rotary evaporation concentration at 75 ℃ after the reaction is finished, drying, and grinding the solid obtained by drying at 105 ℃ to respectively obtain modified high-pigment carbon black, modified oil-soluble black 7 and modified nano silicon carbide;
(2) Uniformly mixing the prepared modified high-pigment carbon black, modified oil-soluble black 7 and modified nano silicon carbide, and feeding the mixture into a double-screw extruder from a side feeding port; POE 8200 (Dow DuPont, melt index 190 ℃/2.16Kg.
Example 3
A high-flow black master batch for PA engineering plastics comprises the following components in percentage by weight:
LDPE MG70 30％；
PE-g-MAH 15％；
25% of high-pigment carbon black;
oil-soluble black 7%;
10% of nano silicon carbide;
8% of tetradecanedioic acid;
silane coupling agent KH550 percent;
the preparation method comprises the following steps:
(1) Respectively and uniformly mixing high-pigment carbon black, oil-soluble black 7 and nano silicon carbide with xylene, adding a silane coupling agent KH550, stirring and mixing, heating to 80 ℃, reacting for 4 hours, performing rotary evaporation concentration at 75 ℃ after the reaction is finished, drying, and grinding the solid obtained by drying at 105 ℃ to respectively obtain modified high-pigment carbon black, modified oil-soluble black 7 and modified nano silicon carbide;
(2) Uniformly mixing the prepared modified high-pigment carbon black, modified oil-soluble black 7 and modified nano silicon carbide, and feeding the mixture into a double-screw extruder from a side feeding port; uniformly mixing LDPE MG70 (Kataler petrochemical, melt index 190 ℃/2.16Kg).
Example 4
A high-flow black master batch for PA engineering plastics comprises the following components in percentage by weight:
LDPE MG70 33％；
PE-g-MAH 10％；
20% of high-pigment carbon black;
oil-soluble black 7%;
20% of nano silicon carbide;
5% of tetradecanedioic acid;
silane coupling agent KH550 percent;
the preparation method comprises the following steps:
(1) Respectively and uniformly mixing high-color carbon black, oil-soluble black 7 and nano silicon carbide with dimethylbenzene, adding a silane coupling agent KH550, stirring and mixing, heating to 80 ℃, reacting for 4 hours, carrying out rotary evaporation and concentration at 75 ℃ after the reaction is finished, drying, and grinding solids obtained by drying at 105 ℃ to obtain modified high-color carbon black, modified oil-soluble black 7 and modified nano silicon carbide respectively;
(2) Uniformly mixing the prepared modified high-pigment carbon black, modified oil-soluble black 7 and modified nano silicon carbide, and feeding the mixture into a double-screw extruder from a side feeding port; uniformly mixing LDPE MG70 (Kataler petrochemical, melt index 190 ℃/2.16Kg).
Comparative example 1
The current general black master batch formula and the preparation method are adopted, wherein the black master batch comprises 50% of LDPE MG70 (Kataler petrochemical, melt index 190 ℃/2.16Kg). Adding the components into a mixer, mixing for 10min, feeding the uniformly mixed material into a double-screw extruder from a main feeding port, and carrying out melt extrusion, grain cutting and drying to prepare the black master batch.
Comparative example 2
The specific process is the same as that of example 1, except that no silane coupling agent is used for surface treatment of carbon black, aniline black and nano silicon carbide.
Comparative example 3
The process is the same as example 1 except that the nylon rheology agent tetradecanedioic acid is not included.
Comparative example 4
The specific process is the same as that of example 1, except that no nano silicon carbide is contained.
Application example 1
The PA6, the glass fiber 50%, the antioxidant 0.3% and the black master batch prepared in the examples and the comparative examples, which are 47.7% in mass fraction, are subjected to melt mixing extrusion granulation at 250 ℃ in a twin-screw extruder with an aspect ratio of 1 to 35, and the stable current during extrusion is recorded.
Application example 2
57.7% of PA6, 40% of talc, 0.3% of antioxidant and 2% of the black masterbatch prepared in examples and comparative examples were melt-mixed, extruded and pelletized at 250 ℃ in a twin-screw extruder having an aspect ratio of 1.
Drying the prepared filled PA6 particle material in a vacuum oven at 90-100 ℃ for 4 hours, then carrying out injection molding on the dried particle material on an injection molding machine to prepare a sample, and carrying out performance test.
1. Melt index test:
the melt flow rate test was carried out according to ISO1133-2005 at 260 ℃ X2.16 Kg.
2. And (3) testing mechanical properties:
the tensile properties were measured according to ISO527-2 (1996) with specimen dimensions of 170X 10X 4mm and a tensile speed of 50mm/min; the bending property test is carried out according to ISO178-2003, the size of a sample is 80 multiplied by 10 multiplied by 4mm, the bending speed is 2mm/min, and the span is 64mm; the impact strength of the notch of the simply supported beam is carried out according to ISO179-2000, the size of a test sample is 80 multiplied by 6 multiplied by 4mm, and the depth of the notch is one third of the thickness of the test sample.
3. And (3) testing the wear resistance: the test results are expressed in units of mg/1000 revolutions on a Taber abrasion tester with a 500g load and a weight loss of 1000 revolutions of the wheel.
The test results are shown in table 1:
TABLE 1
From the test results, the black master batch prepared by the invention can be added into PA plastic to effectively improve the fluidity, mechanical property and wear resistance of matrix resin. The addition of the maleic anhydride grafted polyolefin and the nano silicon carbide can better improve the performance of the matrix resin.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is intended that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (7)
1. The high-flow black master batch for the PA engineering plastic is characterized by comprising the following components in percentage by weight:
29.5 to 50 percent of polyolefin resin;
5-20% of maleic anhydride grafted polyolefin;
20-50% of carbon black;
5-20% of aniline black;
5-20% of nano silicon carbide;
5-15% of rheological agent;
0.5 to 2 percent of silane coupling agent;
the rheological agent is tetradecanedioic acid; the polyolefin is one or a mixture of PP, PE, POE and EVA;
the preparation method comprises the following steps:
(1) Respectively and uniformly mixing carbon black, aniline black and nano silicon carbide with dimethylbenzene, adding a silane coupling agent, stirring and mixing, heating to 60-80 ℃, reacting for 4-6 hours, performing rotary evaporation and concentration after the reaction is finished, drying, and grinding the solid obtained by drying to obtain modified carbon black, modified aniline black and modified nano silicon carbide;
(2) Uniformly mixing the prepared modified carbon black, modified aniline black and modified nano silicon carbide, and then feeding the mixture into a double-screw extruder from a side feeding port; and uniformly mixing the polyolefin resin, the maleic anhydride grafted polyolefin and the rheological agent in a high-speed mixer, feeding the mixture into a double-screw extruder from a main feeding port, and performing melt extrusion, cooling, granulating and drying to obtain the high-fluidity black master batch.
2. The high-flow black master batch for PA engineering plastics as claimed in claim 1, wherein the maleic anhydride grafted polyolefin is one or more of PP-g-MAH, PE-g-MAH, POE-g-MAH and EVA-g-MAH.
3. The high-flow black master batch for PA engineering plastics as claimed in claim 1, wherein the particle size of the carbon black is 5-200nm.
4. The high-flow black master batch for PA engineering plastics according to claim 1, wherein the nigrosine is oil-soluble nigrosine or alcohol-soluble nigrosine.
5. The high-flow black master batch for PA engineering plastics as claimed in claim 1, wherein the nano silicon carbide has a particle size of 20-500nm.
6. The high-flow black master batch for PA engineering plastics according to claim 1, wherein the silane coupling agent is one or more of KH550, KH560 and KH 570.
7. The high-flow black master batch for PA engineering plastics, according to claim 1, is characterized in that in step (2), the temperature of melt extrusion is 120-280 ℃.
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|---|---|---|---|---|
| US4810733A (en) * | 1987-10-19 | 1989-03-07 | Toyo Ink Mfg Co., Ltd | Color concentrates |
| CN102838828A (en) * | 2011-06-20 | 2012-12-26 | 上海安凸塑料添加剂有限公司 | Bright-black functional black masterbatch for ABS engineering plastics and preparation method thereof |
| CN103360670A (en) * | 2013-06-03 | 2013-10-23 | 广东波斯科技股份有限公司 | Universal high-gloss black masterbatch |
| CN106189209A (en) * | 2016-08-24 | 2016-12-07 | 浙江佳华精化股份有限公司 | Polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds and preparation method thereof |
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Denomination of invention: A high flow black masterbatch for PA engineering plastics and its preparation method Effective date of registration: 20231009 Granted publication date: 20221202 Pledgee: Bank of China Limited Shangyu sub branch Pledgor: ZHEJIANG JAVA SPECIALTY CHEMICALS Co.,Ltd. Registration number: Y2023980060206 |