CN111471255B - Silica-graphene modified color master batch and preparation method thereof - Google Patents
Silica-graphene modified color master batch and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silica-graphene modified color master batch and a preparation method thereof, wherein the silica-graphene modified color master batch is prepared from the following raw materials in parts by mass: 25-35 parts of silicon dioxide-graphene modified polyvinyl chloride carrier, 50-60 parts of pigment toner and 12-18 parts of dispersing agent. The color master batch disclosed by the invention is subjected to modification treatment aiming at a polyvinyl chloride carrier, and is subjected to secondary modification by using graphene and silicon dioxide respectively, so that the migration rate of the pigment is reduced, the overall stability of the color master batch is improved, and the color retention time of the pigment is longer.
Description
Technical Field
The invention belongs to the technical field of color master batches, and particularly relates to a silica-graphene modified color master batch and a preparation method thereof.
Background
The color master batch is a common plastic colorant and has the following advantages: 1. the pigment has better dispersibility in products; 2. the chemical stability of the pigment is favorably maintained: when the pigment is directly used, the pigment directly contacts air in the storage and use processes, so that the pigment can absorb water, oxidize and the like, and after the pigment is prepared into the color master batch, the resin carrier isolates the pigment from the air and moisture, so that the quality of the pigment can be kept unchanged for a long time; 3. guarantee of the color stability of the product: the color master batch is similar to the resin particles, so that the metering is more convenient and accurate, the color master batch cannot be adhered to a container during mixing, and the color master batch and the resin are mixed more uniformly, so that the stable addition can be ensured, and the stable color of the product is ensured; 4. protecting the health of the operator: the pigment is generally powder, is easy to fly during adding and mixing, and can affect the health of operators after being inhaled by human bodies; 5. the environment is kept clean, and vessels are not polluted; 6. simple process, easy color conversion, and saved time and raw materials.
The existing preparation method of the color master batch is generally to simply mix a carrier, a colorant, a dispersant and other additives, and because the mode is simpler, the product still has the defects of uneven coloring, lower pigment load, large color difference and high cost; at present, the color master batch manufacturing mode in China mostly adopts double-screw mixing extrusion, banburying kneading and a double-roller open mill, and the processing technologies are generally suitable for processing low-concentration toner dispersion; when the content of titanium dioxide in the color master batch is higher than 40%, the color master batch which is processed and molded by a conventional method singly has the problems of uneven macro dispersion, unstable color and the like when coloring a base material. Therefore, the carrier matrix of the color master batch is improved, so that the overall performance of the color master batch is improved, and the color master batch has a good use value.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a silica-graphene modified color master batch and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the silica-graphene modified color master batch is prepared from the following raw materials in parts by mass: 25-35 parts of silicon dioxide-graphene modified polyvinyl chloride carrier, 50-60 parts of pigment toner and 12-18 parts of dispersing agent.
Further, the preparation method of the silica-graphene modified polyvinyl chloride carrier comprises the following steps:
(1) dispersing graphene in absolute ethyl alcohol, adding a silane coupling agent with half of the mass of the graphene, carrying out ultrasonic reaction for 2-4 hours at the temperature of 50 ℃ at 500W, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(2) dissolving nano silicon dioxide in absolute ethyl alcohol, adding a silane coupling agent with the mass of 3-5% of the nano silicon dioxide after shearing and dispersing, shearing at a high speed for 30 minutes at 75-85 ℃, then performing ultrasonic dispersion for 30 minutes at 500W and 50 ℃, performing vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(3) mixing the materials obtained in the steps 1 and 2 with polyvinyl chloride according to the mass ratio of (1-2): (2-3): (95-97) weighing, feeding the polyvinyl chloride preheated to 110-130 ℃ into a plastic mixing machine, melting, passing through a wrapping roller, adding the graphene and silicon dioxide materials, and uniformly mixing.
Further, the roller distance of the plastic refining machine in the step 3 is controlled to be 0.8-1.2mm, and the roller temperature is controlled to be 130-150 ℃.
Preferably, the pigment toner is selected from any one of cadmium red, cadmium yellow, iron oxide red, iron oxide black, carbon black, titanium dioxide, chrome green, phthalocyanine red, phthalocyanine blue, phthalocyanine green and azoic red.
Preferably, the dispersant is any one selected from the group consisting of polyethylene low molecular wax, polyurethane polymer, stearate, imidazole and derivatives thereof.
Preferably, the silica-graphene modified color master batch can be added with a flame retardant, a brightening agent and an antioxidant according to the product performance requirements.
The invention also provides a preparation method of the silica-graphene modified color master batch, which comprises the following steps:
(1) sequentially adding the silicon dioxide-graphene modified polyvinyl chloride carrier, the pigment toner and the dispersing agent into a stirrer, and stirring and mixing for 4-6 minutes at the speed of 100-150 revolutions per minute to obtain a mixture;
(2) feeding the mixture into a mixing roll, and shearing and mixing at high speed of 400-500 r/min at the temperature of 60-80 ℃ to obtain a high-dispersion polymer material;
(3) and (3) feeding the polymerization material into a double-screw extruder, extruding and granulating, and dehydrating, drying and screening the obtained master batch to obtain the master batch.
Further, the temperature zones of the twin-screw extruder in the step 3 are sequentially set to 160-.
The invention has the advantages that:
the color master batch is used for modifying a polyvinyl chloride carrier, and is secondarily modified by the graphene and the silicon dioxide respectively, wherein the graphene modification utilizes the good heat conduction and stretching performances of the graphene, the interlayer spacing is increased by the reaction of a silane coupling agent and oxygen-containing groups on the surface of the graphene, the graphene is promoted to be dispersedly coated by polyvinyl chloride in the subsequent mixing process, the binding property of the graphene is improved, and further the mechanical property of the carrier is enhanced; and on the other hand, the silicon dioxide can also be used as an interface modifier and can form a relatively stable silicon-oxygen metal chemical bond with the pigment toner, so that a firm silicon dioxide film is formed on the surface of the toner, the contact between the toner and water and air is reduced, the aging resistance of the toner is improved, the color stability is improved during coloring, and the color difference is small.
The product of the invention has the advantages of nontoxic and environment-friendly preparation process, simple and convenient process, saving of manpower, electric power, equipment and production field, good aging resistance and migration resistance of the obtained product, namely, improved color stability during coloring, small color difference, and suitability for automatic and continuous production in the production process, and can generate better economic benefit.
Detailed Description
The technical scheme of the invention is further explained by combining the specific examples as follows:
example 1
The silica-graphene modified color master batch is prepared from the following raw materials in parts by mass: 25kg of silicon dioxide-graphene modified polyvinyl chloride carrier, 50kg of cadmium red toner, 12kg of polyethylene low molecular wax and 3kg of flame retardant.
The preparation method of the silicon dioxide-graphene modified polyvinyl chloride carrier comprises the following steps:
(1) dispersing graphene in absolute ethyl alcohol, adding a silane coupling agent with half of the mass of the graphene, carrying out ultrasonic reaction for 2 hours at the temperature of 50 ℃ at 500W, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(2) dissolving nano silicon dioxide in absolute ethyl alcohol, adding a silane coupling agent with the mass of 3% of the nano silicon dioxide after shearing and dispersing, shearing at a high speed for 30 minutes at 75 ℃, then ultrasonically dispersing for 30 minutes at 500W and 50 ℃, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(3) mixing the materials obtained in the steps 1 and 2 with polyvinyl chloride according to the mass ratio of 1: 2: 97, feeding the polyvinyl chloride preheated to 110 ℃ into a plastic mixing mill, controlling the roller distance to be 0.8mm and the roller temperature to be 150 ℃, melting, then thinly passing through a wrapping roller, adding graphene and silicon dioxide materials, and uniformly mixing.
The preparation method of the silica-graphene modified color master batch comprises the following steps:
(1) sequentially adding the silicon dioxide-graphene modified polyvinyl chloride carrier, the cadmium red toner, the polyethylene low molecular wax and the flame retardant into a stirrer, and stirring and mixing for 6 minutes at a speed of 100 revolutions per minute to obtain a mixture;
(2) feeding the mixture into a mixing roll, and shearing and mixing at a high speed of 500 revolutions per minute at the temperature of 60 ℃ to obtain a high-dispersion polymer material;
(3) and (2) feeding the polymerization material into a double-screw extruder, setting temperature zones to be 160 ℃, 165 ℃, 175 ℃ and 180 ℃ in sequence, controlling the rotating speed of a main engine to be 600 revolutions per minute, extruding and granulating, and dehydrating, drying and screening the obtained master batch to obtain the master batch of the embodiment.
Example 2
The silica-graphene modified color master batch is prepared from the following raw materials in parts by mass: 35kg of silicon dioxide-graphene modified polyvinyl chloride carrier, 60kg of iron oxide yellow powder, 18kg of polyurethane polymer and 7kg of antioxidant.
The preparation method of the silicon dioxide-graphene modified polyvinyl chloride carrier comprises the following steps:
(1) dispersing graphene in absolute ethyl alcohol, adding a silane coupling agent with half of the mass of the graphene, carrying out ultrasonic reaction for 4 hours at the temperature of 50 ℃ at 500W, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(2) dissolving nano silicon dioxide in absolute ethyl alcohol, adding a silane coupling agent with the mass of 5% of the nano silicon dioxide after shearing and dispersing, shearing at a high speed for 30 minutes at 85 ℃, then ultrasonically dispersing for 30 minutes at 500W and 50 ℃, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(3) mixing the materials obtained in the steps 1 and 2 with polyvinyl chloride according to the mass ratio of 2: 3: and after 95 measurement and weighing, feeding the polyvinyl chloride preheated to 130 ℃ into a plastic mixing machine, controlling the roller distance to be 1.2mm and the roller temperature to be 130 ℃, melting, then thinly passing through a wrapping roller, adding graphene and silicon dioxide material, and uniformly mixing.
The preparation method of the silica-graphene modified color master batch comprises the following steps:
(1) sequentially adding the silicon dioxide-graphene modified polyvinyl chloride carrier, the ferric oxide yellow powder, the polyurethane polymer and the antioxidant into a stirrer, and stirring and mixing for 4 minutes at a speed of 150 revolutions per minute to obtain a mixture;
(2) feeding the mixture into a mixing roll, and shearing and mixing at a high speed of 400 r/min at 80 ℃ to obtain a high-dispersion polymer material;
(3) and (2) feeding the polymerization material into a double-screw extruder, setting temperature zones to be 165 ℃, 175 ℃, 185 ℃ and 190 ℃ in sequence, controlling the rotating speed of a main engine to be 500 revolutions per minute, extruding and granulating, and dehydrating, drying and screening the obtained master batch to obtain the master batch of the embodiment.
Example 3
The silica-graphene modified color master batch is prepared from the following raw materials in parts by mass: 30kg of silicon dioxide-graphene modified polyvinyl chloride carrier, 55kg of titanium dioxide and 15kg of calcium stearate.
The preparation method of the silicon dioxide-graphene modified polyvinyl chloride carrier comprises the following steps:
(1) dispersing graphene in absolute ethyl alcohol, adding a silane coupling agent with half of the mass of the graphene, carrying out ultrasonic reaction for 3 hours at the temperature of 50 ℃ at 500W, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(2) dissolving nano silicon dioxide in absolute ethyl alcohol, adding a silane coupling agent with the mass of 4% of the nano silicon dioxide after shearing and dispersing, shearing at a high speed for 30 minutes at 80 ℃, then ultrasonically dispersing for 30 minutes at 500W and 50 ℃, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(3) mixing the materials obtained in the steps 1 and 2 with polyvinyl chloride according to the mass ratio of 1.5: 2.5: 96, weighing, feeding the polyvinyl chloride preheated to 120 ℃ into a plastic mixing machine, controlling the roller distance to be 1.0mm and the roller temperature to be 140 ℃, melting, then thinly passing through a wrapping roller, adding graphene and silicon dioxide materials, and uniformly mixing.
The preparation method of the silica-graphene modified color master batch comprises the following steps:
(1) sequentially adding the silicon dioxide-graphene modified polyvinyl chloride carrier, the titanium dioxide and the calcium stearate into a stirrer, and stirring and mixing for 5 minutes at a speed of 120 revolutions per minute to obtain a mixture;
(2) feeding the mixture into a mixing roll, and shearing and mixing at a high speed of 450 revolutions per minute at 70 ℃ to obtain a high-dispersion polymer material;
(3) and (2) feeding the polymerization material into a double-screw extruder, setting temperature zones to be 160 ℃, 170 ℃, 175 ℃, 180 ℃ and 185 ℃ in sequence, controlling the rotating speed of a main engine to be 550 revolutions per minute, extruding and granulating, and dehydrating, drying and screening the obtained master batch to obtain the master batch of the embodiment.
Comparative example
Compared with the example 3, the method does not use silica-graphene modified polyvinyl chloride as a carrier, only uses common commercial polyvinyl chloride as a carrier, and comprises the following specific steps:
the color master batch is prepared from the following raw materials in parts by mass: 30kg of polyvinyl chloride carrier, 55kg of titanium dioxide and 15kg of calcium stearate, and the preparation method comprises the following steps:
(1) sequentially adding the polyvinyl chloride carrier, the titanium dioxide and the calcium stearate into a stirrer, and stirring and mixing for 5 minutes at a speed of 120 revolutions per minute to obtain a mixture;
(2) feeding the mixture into a mixing roll, and shearing and mixing at a high speed of 450 revolutions per minute at 70 ℃ to obtain a high-dispersion polymer material;
(3) and (2) feeding the polymerization material into a double-screw extruder, setting temperature zones to be 160 ℃, 170 ℃, 175 ℃, 180 ℃ and 185 ℃ in sequence, controlling the rotating speed of a main engine to be 550 revolutions per minute, extruding and granulating, and dehydrating, drying and screening the obtained master batch to obtain the master batch of the comparative example.
The color master batches obtained in examples 1, 2 and 3 and the comparative example were subjected to quality testing, specifically as follows:
migration resistance test:
extruding the colored color master batch into a sheet shape, and mixing the color master batch with a PVC sheet containing 5% of different color powder at a ratio of 1kg/cm2After being closely adhered and placed at a temperature of 80 ℃ for 24 hours, the degree of contamination of the PVC sheet was observed and judged by a standard gray card. Grade 5 indicates no migration and grade 1 is severe, with the results shown in table 1:
TABLE 1
| Example 1 | Example 1 | Example 1 | Comparative example | |
| Migration rating | Grade 5 | Grade 5 | Grade 5 | Grade 3 |
As can be seen from table 1 above, after the polyvinyl chloride carrier is subjected to graphene and silica composite modification, the migration resistance of the obtained color master batch material is significantly improved.
And (3) testing heat resistance:
a weight loss analysis test is carried out by adopting a thermal weight loss analyzer: n is a radical of2The temperature rise rate is 10 ℃/min, the temperature rise interval is 30-600 ℃, and the results are shown in Table 2:
TABLE 2
| T5％(℃) | T50％(℃) | T90％(℃) | Tmax(℃) | |
| Example 1 | 208.6 | 295.4 | 593.5 | 294.1 |
| Example 2 | 206.5 | 294.8 | 592.4 | 294.0 |
| Example 3 | 209.1 | 295.7 | 594.0 | 294.3 |
| Comparative example | 184.7 | 288.5 | 489.2 | 288.6 |
As can be seen from table 2 above, after the polyvinyl chloride carrier is subjected to graphene and silicon dioxide composite modification, the decomposition temperatures are all higher than those of the unmodified material when the weight loss rates reach 5%, 50% and 90%, and the temperature corresponding to the maximum decomposition rate is also significantly increased, so that the heat resistance is improved, which indicates that the color stability is enhanced during coloring.
Testing the pressure value of the filter screen:
the polymer-based mixture containing 3% of pigment flows through an extruder provided with a melt pump and a filter screen assembly supported by a porous plate, a melt pressure sensor is installed at the front end of the filter screen assembly, the pressure difference between the initial pressure and the pressure measured by the pressure sensor in front of the filter screen assembly behind the melt pump is a filter screen pressure value (FPV), the dispersion effect of the color master is represented by the size of the FPV, and the smaller the FPV value is, the better the dispersibility is.
Extruder temperature profile: the conveying section is 200 ℃, and the rest sections are 240 ℃.
Extrusion amount: 53 g/min.
Pressure sensor scale: kg/cm2。
TABLE 3
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Pressure value of filter screen | 0.36 | 0.38 | 0.35 | 1.17 |
As can be seen from table 3 above, after the polyvinyl chloride carrier is subjected to graphene and silicon dioxide composite modification, the pressure value of the filter screen of the color master batch is significantly reduced, which indicates that the dispersibility of the color master batch in the base material is enhanced.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The silica-graphene modified color master batch is characterized by being prepared from the following raw materials in parts by mass: 25-35 parts of silicon dioxide-graphene modified polyvinyl chloride carrier, 50-60 parts of pigment toner, 12-18 parts of dispersing agent,
the preparation method of the silicon dioxide-graphene modified polyvinyl chloride carrier comprises the following steps:
(1) dispersing graphene in absolute ethyl alcohol, adding a silane coupling agent with half of the mass of the graphene, carrying out ultrasonic reaction for 2-4 hours at the temperature of 50 ℃ at 500W, carrying out vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(2) dissolving nano silicon dioxide in absolute ethyl alcohol, adding a silane coupling agent with the mass of 3-5% of the nano silicon dioxide after shearing and dispersing, shearing at a high speed for 30 minutes at 75-85 ℃, then performing ultrasonic dispersion for 30 minutes at 500W and 50 ℃, performing vacuum filtration on the obtained dispersion liquid, washing to be neutral, and drying for later use;
(3) mixing the materials obtained in the steps 1 and 2 with polyvinyl chloride according to the mass ratio of (1-2): (2-3): (95-97) weighing, feeding the polyvinyl chloride preheated to 110-130 ℃ into a plastic mixing machine, melting, passing through a wrapping roller, adding graphene and silicon dioxide materials, and uniformly mixing,
in the step (3), the roller distance of the plastic refining machine is controlled to be 0.8-1.2mm, the roller temperature is controlled to be 130-,
the pigment toner is selected from any one of cadmium red, iron oxide yellow and titanium dioxide,
the dispersing agent is selected from any one of polyethylene low molecular wax, polyurethane polymer and calcium stearate.
2. The silica-graphene modified color masterbatch of claim 1, wherein a flame retardant, a brightener and an antioxidant can be added according to product performance requirements.
3. A method of preparing the silica-graphene modified color masterbatch according to any one of claims 1-2, comprising the steps of:
(1) sequentially adding the silicon dioxide-graphene modified polyvinyl chloride carrier, the pigment toner and the dispersing agent into a stirrer, and stirring and mixing for 4-6 minutes at the speed of 100-150 revolutions per minute to obtain a mixture;
(2) feeding the mixture into a mixing roll, and shearing and mixing at high speed of 400-500 r/min at the temperature of 60-80 ℃ to obtain a high-dispersion polymer material;
(3) and (3) feeding the polymerization material into a double-screw extruder, extruding and granulating, and dehydrating, drying and screening the obtained master batch to obtain the master batch.
4. The method for preparing silica-graphene modified color master batch according to claim 3, wherein the temperature zone of the twin-screw extruder in the step 3 is sequentially set to 160-.
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| CN101885885B (en) * | 2010-07-20 | 2012-05-16 | 广州市波斯塑胶颜料有限公司 | Color master batch for hard PVC and preparation method thereof |
| CN104844959A (en) * | 2014-05-13 | 2015-08-19 | 佛山市顺德区加合塑料颜料科技有限公司 | PVC imitation wood grain co-extruded color master batch making method |
| CN104072913B (en) * | 2014-07-09 | 2016-08-24 | 苏州亨利通信材料有限公司 | A kind of fastness master batch and manufacture method thereof |
| CN106147082A (en) * | 2016-08-17 | 2016-11-23 | 林炳祥 | A kind of PVC color masterbatch |
| CN106380720A (en) * | 2016-08-22 | 2017-02-08 | 浙江西大门新材料股份有限公司 | Anti-ultraviolet PVC color masterbatch |
| CN106751221A (en) * | 2016-12-31 | 2017-05-31 | 天津科彩塑料科技有限公司 | A kind of hard PVC color masterbatch and preparation method thereof |
| CN107663347A (en) * | 2017-09-18 | 2018-02-06 | 苏州武江新材料科技有限公司 | A kind of preparation method of high fire-retardance PVC Masterbatch |
| CN107722512A (en) * | 2017-11-16 | 2018-02-23 | 福建鑫邦新材料科技有限公司 | PVC Masterbatch and preparation method thereof |
| CN108047661A (en) * | 2017-12-05 | 2018-05-18 | 浙江金霞新材料科技有限公司 | A kind of graphene dacron master grain and preparation method thereof |
| CN108314890A (en) * | 2018-03-26 | 2018-07-24 | 石芮巾 | A kind of PVC Masterbatch |
| CN110372947A (en) * | 2019-09-05 | 2019-10-25 | 安徽省聚科石墨烯科技股份公司 | A kind of scratch-resistant graphene plastic matrix and preparation method thereof |
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