CN107619520B - Blue-phase black master batch for polyethylene or polypropylene and preparation method thereof - Google Patents
Blue-phase black master batch for polyethylene or polypropylene and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a blue-phase black master batch for polyethylene or polypropylene, which is prepared from the following raw materials in percentage by mass: 40-75% of LLDPE resin, 25-40% of carbon black, 0-5% of dispersing agent, 0-2% of lubricating agent and 0-12% of inorganic filler. The invention selects LLDPE resin with a melt index less than 10, and further matches pigment carbon black with proper particle size and iodine absorption value and oil absorption value, thus being capable of obviously improving the glossiness and blackness of PE and PP products in PE and PP injection molding and enabling the products to show blue phase black; the manufacturing cost is low, and the working procedure is simple; compared with the imported color master batch, the black color master batch with the same amount is added in the PE and PP injection molding, the displayed black color phase is more blue, and the method has wide application prospect and market competitiveness.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a blue-phase black master batch for polyethylene or polypropylene and a preparation method thereof.
Background
As the surface gloss of the black soft rubber products is brighter and the blackness thereof is stronger, the quality thereof is higher, and thus many producers and designers seek a high-black plastic surface effect. Theoretically, coloring with high-pigment carbon black gives a better blackness, but high-pigment carbon black is difficult to disperse, and the hue expressed in the final product has a large relationship with the dispersibility of carbon black, the quality of the base material, the structure of the screw, the surface gloss of the mold, the injection pressure, and other factors.
The multi-purpose toner for achieving the high black effect on the market is matched colors, the color matching cost is higher, the production equipment and the production field are polluted, the storage time is short, the timeliness is very strong, the traditional coloring master batch is mostly red when soft rubber products such as PE and PP are injected, and the dispersion effect and the quality are obviously poor relative to the color matching effect.
Therefore, the production of a color master batch product with high blackness is a difficult problem to solve in the prior art.
Disclosure of Invention
The invention solves the problem of black coloring not according to the traditional thinking, but adopts technical means to solve the problems of light diffusion and reflection by researching the principle of light scattering and reflection. By adopting the special dilution and dispersion performance of the color master batch in the plastic product, more visible light absorption effects are realized, and finally, the black color presents a blue phase, so that the plastic product has the texture.
The invention aims to provide the blue-phase black master batch for polyethylene or polypropylene, which has the advantages of low manufacturing cost, simple process and good use effect.
The technical scheme adopted by the invention is as follows: a blue-phase black master batch for polyethylene or polypropylene is prepared from the following raw materials in percentage by mass:
preferably, the LLDPE resin has a melt index of less than 10, and preferably, the LLDPE resin has a melt index of 0.5 to 6.
When the LLDPE resin with the melt index higher than 10 is selected, the prepared black master batch has no blue phase effect in injection molding, but shows a red-yellow phase.
Preferably, the carbon black has an iodine absorption value of more than 110g/Kg and a DBP absorption value of less than 105X 10-5M3In terms of/kg. The preferred range of iodine absorption value of carbon black is 120-300g/Kg and the range of DBP absorption value is 50-105X 10-5M3In terms of/kg. When the iodine absorption value of the selected carbon black is less than 110g/Kg, the blackness of the prepared black master batch in injection molding is not enough, and the DBP absorption value is less than 105 multiplied by 10-5M3The amount of the dispersant used per kg of carbon black can be controlled to be as small as possible, thereby increasing the blue phase effect.
Preferably, the particle size of the carbon black is 11 to 50 nm.
Preferably, the dispersant is one or more of polyethylene wax (PE wax), ethylene stearamide (EBS) and EVA wax.
Preferably, the lubricant is one or more of zinc stearate and calcium stearate.
Preferably, the particle size of the inorganic filler is 10-10000nm, and the inorganic filler is selected from one or more of calcium carbonate, barium sulfate, glass beads, kaolin, wollastonite, talcum powder, mica, montmorillonite, aluminum hydroxide, magnesium hydroxide, diatomite and silicon dioxide; more preferably, the inorganic filler has a particle size of 50 to 3000 nm.
The particle size of the inorganic filler is controlled within a reasonable range, for example, 10 to 10000nm, and if the particle size is too small, dispersion is not facilitated, and if the particle size is too large, the surface of the product may be rough.
The invention also provides a preparation method of the blue-phase black master batch for polyethylene or polypropylene, which comprises the following steps:
1) mixing LLDPE resin, inorganic filler, carbon black, dispersant and lubricant in a high-speed mixer for 8-12 minutes according to the proportion to obtain a mixed material;
2) putting the mixed materials into an internal mixer, mixing until the plastic is completely melted, pouring out, cooling and crushing;
3) and (3) extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, and granulating by using a water ring to obtain the blue-phase black master batch for polyethylene or polypropylene.
Preferably, the temperature of the internal mixer in the step 2) is controlled below 180 ℃, and the extrusion temperature in the step 3) is controlled to be 135-180 ℃.
In the injection molding process, only a small amount of the blue-phase black master batch can be added to color the plastic product to have blue tone, so that the plastic product has higher blackness and the aesthetic feeling of the product is improved.
The color development principle of the present invention is to utilize carbon black with specific conditions (iodine absorption value greater than 110g/Kg and DBP absorption value less than 105X 10)-5M3Kg) and a dispersant with a specific proportion, the obtained black master batch has a special effect beyond a specified range, the hue and the blackness of the prepared black master batch cannot reach the effect of blue phase high black, and an inorganic filler (10nm-10000nm) with a proper particle size can play a role in synergy and dispersion promotion.
The invention has the beneficial effects that: the invention selects LLDPE resin with a melt index less than 10, and further matches pigment carbon black with proper particle size (11-50nm) iodine absorption value and oil absorption value, which can obviously improve the glossiness and blackness of PE and PP products in PE and PP injection molding and can make the products show blue phase black; the manufacturing cost is low, and the working procedure is simple; compared with the imported color master batch, the blue-phase black master batch with the same amount is added in the PE and PP injection molding, the displayed black color phase is more blue, and the blue-phase black master batch has wide application prospect and market competitiveness.
Detailed Description
In order to better explain the present invention, the following detailed description of the invention is given in conjunction with specific embodiments.
Example 1
60% by mass of an LLDPE resin having a melt index of 8, 12% by mass of calcium carbonate having an average particle diameter of 200nm, 25% by mass of carbon black having an iodine absorption value of 134g/Kg and a DBP absorption value of 95X 10-5M3Mixing carbon black/kg, polyethylene wax (PE wax) 1% and zinc stearate 2% in a high-speed mixer for 10 minutes, banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using water in an annular manner to obtain the blue-phase black master batch for polyethylene or polypropylene.
Example 2
62% by mass of an LLDPE resin having a melt index of 5, 5% by mass of a calcium carbonate having an average particle diameter of 500nm, 30% by mass of a carbon black having an iodine absorption value of 188g/Kg and a DBP absorption value of 68X 10-5M3Mixing carbon black/kg, polyethylene wax (PE wax) 1.5% and calcium stearate 1.5% in a high-speed mixer for 8 minutes, banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using a water ring to obtain the blue-phase black master batch for polyethylene or polypropylene.
Example 3
61.5% by mass of an LLDPE resin having a melt index of 3 and 35% by mass of a carbon black having an iodine absorption value of 222g/Kg and a DBP valueAbsorption value of 55X 10-5M3Mixing carbon black/kg, 1.5 percent ethylene stearamide (EBS) and 2 percent zinc stearate in a high-speed mixer for 10 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 130-.
Example 4
57% by mass of an LLDPE resin having a melt index of 2.2, 40% by mass of a carbon black having an iodine absorption value of 256g/Kg and a DBP absorption value of 52X 10-5M3Mixing carbon black/kg, 2% polyethylene wax (PE wax) and 1% zinc stearate in a high-speed mixer for 12 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using water in an annular manner to obtain the blue-phase black master batch for polyethylene or polypropylene.
Example 5
56% by mass of an LLDPE resin having a melt index of 1.3, 40% by mass of a carbon black having an iodine absorption value of 288g/Kg and a DBP absorption value of 50X 10-5M3Mixing carbon black/kg, 3% polyethylene wax (PE wax) and 1% zinc stearate in a high-speed mixer for 8 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, finally extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using water in a ring manner to obtain the blue-phase black master batch for polyethylene or polypropylene.
Example 6
By mass, 48% of LLDPE resin having a melt index of 8, 9% of glass beads having an average particle diameter of 800nm, 40% of carbon black having an iodine absorption value of 132g/Kg and a DBP absorption value of 98X 10-5M3Perkg of carbon black, 1% of dispersant (0.6% of polyethylene wax + 0.4% of EVA wax), 2% of lubricant (1% of zinc stearate + 1% of calcium stearate), mixed in a high-speed mixer for 10 minutes, then banburying in an internal mixer until the plastics are completely melted(the temperature is controlled at 170 ℃), the mixture is crushed after being cooled and melted, and then is extruded and granulated by a double-screw extruder with the length-diameter ratio of 44:1, the extrusion temperature is 135-180 ℃, and water ring granulation is carried out to prepare the blue-phase black master batch for polyethylene or polypropylene.
Example 7
60% by mass of LLDPE resin having a melt index of 9, 12% of talc having an average particle diameter of 200nm, 28% of carbon black having an iodine absorption value of 188g/Kg and a DBP absorption value of 65X 10-5M3And mixing the carbon black/kg in a high-speed mixer for 8 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using a water ring to obtain the blue-phase black master batch for polyethylene or polypropylene.
Comparative example 1
60% by mass of an LLDPE resin having a melt index of 20, 12% of calcium carbonate having an average particle diameter of 200nm, 25% of carbon black having an iodine absorption value of 134g/Kg and a DBP absorption value of 95X 10-5M3Mixing carbon black/kg, polyethylene wax (PE wax) 1% and zinc stearate 2% in a high-speed mixer for 10 minutes, banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using water in a ring manner to obtain the black master batch for polyethylene or polypropylene.
Comparative example 2
62% by mass of an LLDPE resin having a melt index of 5, 5% by mass of a calcium carbonate having an average particle diameter of 15000nm, 30% by mass of a carbon black having an iodine absorption value of 188g/Kg and a DBP absorption value of 68X 10-5M3Mixing carbon black/kg, polyethylene wax (PE wax) 1.5% and calcium stearate 1.5% in a high-speed mixer for 8 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using a water ring to obtain the black master batch for polyethylene or polypropylene.
Comparative example 3
61.5% by mass of an LLDPE resin having a melt index of 3, 35% by mass of a carbon black having an iodine absorption value of 85g/Kg and a DBP absorption value of 55X 10-5M3Mixing carbon black/kg, ethylene stearamide (EBS) 1.5% and zinc stearate 2% in a high-speed mixer for 10 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 150 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 160 ℃, and granulating by using a water ring to obtain the black master batch for polyethylene or polypropylene.
Comparative example 4
By mass, 48% of LLDPE resin having a melt index of 8, 9% of glass beads having an average particle diameter of 800nm, 40% of carbon black having an iodine absorption value of 132g/Kg and a DBP absorption value of 112X 10-5M3Mixing 1% of dispersing agent (0.6% of polyethylene wax + 0.4% of EVA wax) and 2% of lubricating agent (1% of zinc stearate + 1% of calcium stearate) in a high-speed mixer for 10 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using a water ring to obtain the black master batch for polyethylene or polypropylene.
Comparative example 5
49% by mass of an LLDPE resin having a melt index of 1.3, 40% by mass of a carbon black having an iodine absorption value of 288g/Kg and a DBP absorption value of 50X 10-5M3Mixing 10% of polyethylene wax (PE wax) and 1% of zinc stearate in a high-speed mixer for 8 minutes, then banburying in an internal mixer until the plastic is completely molten (the temperature is controlled at 170 ℃), cooling and melting, crushing, finally extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, wherein the extrusion temperature is 135-180 ℃, and granulating by using water in a ring manner to obtain the black master batch for polyethylene or polypropylene.
The blue phase black master batches prepared in examples 1 to 7 and the black master batches prepared in comparative examples 1 to 5 were added to PP and PE in an amount of 1% by mass of PP or 1% by mass of PE, respectively, and the results are shown in tables 1 and 2.
TABLE 1 Black masterbatch hue test results (1% addition to PP)
TABLE 2 Black masterbatch hue test (1% addition to PE)
| Item | Value of L | a value | b value |
| Example 1 | 23.9 | -1.3 | -0.8 |
| Example 2 | 23.7 | -0.9 | -2.1 |
| Example 3 | 23.5 | -3.6 | -1.2 |
| Example 4 | 23.1 | -1.77 | -0.9 |
| Example 5 | 23.8 | -0.8 | -1.1 |
| Example 6 | 24.2 | -0.8 | -2.2 |
| Example 7 | 24.6 | -0.9 | -1.7 |
| Comparative example 1 | 26.1 | -0.2 | +2.5 |
| Comparative example 2 | 25.0 | +1.1 | +0.9 |
| Comparative example 3 | 26.8 | -0.2 | +1.8 |
| Comparative example 4 | 25.9 | +2.1 | +0.6 |
| Comparative example 5 | 27.0 | +1.28 | +1.1 |
As is apparent from tables 1 and 2, when 1% of the blue-phase black master batches prepared in examples 1 to 7 were added to PP and PE, the results of the color measurement by a colorimeter showed that the L values were all 25 or less, and the smaller the L value, the higher the blackness, and the negative values of the a value and the b value, respectively, indicating that the hue of the product was bluish. And observed by naked eyes under a D65 light source (no color blindness and color weakness in 30 standard observers aged 18-40 years, 29 people gave consistent blue phase conclusions). As can be seen from tables 1 and 2, the blue phase black masterbatches prepared in examples 1 to 7 exhibited a blue phase with a high brightness, whereas the black masterbatches prepared in comparative examples 1 to 5 exhibited a red-yellow phase with no blue phase effect and the change in filler fineness had the least effect on hue.
Claims (6)
1. The blue-phase black master batch for polyethylene or polypropylene is characterized by being prepared from the following raw materials in percentage by mass:
the LLDPE resin has a melt index of less than 10; the carbon black has iodine absorption value of more than 110g/Kg and DBP absorption value of less than 105 x 10-5M3/kg。
2. The blue phase black masterbatch for polyethylene or polypropylene according to claim 1, wherein the dispersant is one or more of polyethylene wax, ethylene stearamide and EVA wax.
3. The blue phase black master batch for polyethylene or polypropylene according to claim 1, wherein the lubricant is one or more of zinc stearate and calcium stearate.
4. The blue-phase black master batch for polyethylene or polypropylene according to claim 1, wherein the particle size of the inorganic filler is 10-10000nm, and the inorganic filler is one or more selected from calcium carbonate, barium sulfate, glass beads, kaolin, wollastonite, talcum powder, mica, montmorillonite, aluminum hydroxide, magnesium hydroxide, diatomite and silica.
5. Process for the preparation of the blue phase black masterbatch for polyethylene or polypropylene according to any of claims 1 to 4, characterized in that it comprises the following steps:
1) mixing LLDPE resin, inorganic filler, carbon black, dispersant and lubricant in a high-speed mixer for 8-12 minutes according to the proportion to obtain a mixed material;
2) putting the mixed materials into an internal mixer, internally mixing until the plastic is completely melted, pouring out, cooling and crushing,
3) and (3) extruding and granulating by using a double-screw extruder with the length-diameter ratio of 44:1, and granulating by using a water ring to obtain the blue-phase black master batch for polyethylene or polypropylene.
6. The method as claimed in claim 5, wherein the temperature of the internal mixer in the step 2) is controlled to be 180 ℃ or lower, and the extrusion temperature in the step 3) is controlled to be 135-180 ℃.
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