CN114213832A - Black master batch with high color dispersion and preparation method thereof - Google Patents
Black master batch with high color dispersion and preparation method thereof Download PDFInfo
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- CN114213832A CN114213832A CN202111680282.0A CN202111680282A CN114213832A CN 114213832 A CN114213832 A CN 114213832A CN 202111680282 A CN202111680282 A CN 202111680282A CN 114213832 A CN114213832 A CN 114213832A
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- black
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- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 97
- 239000006185 dispersion Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000006229 carbon black Substances 0.000 claims abstract description 106
- 229920005989 resin Polymers 0.000 claims abstract description 70
- 239000011347 resin Substances 0.000 claims abstract description 70
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000000314 lubricant Substances 0.000 claims abstract description 13
- 229920008347 Cellulose acetate propionate Polymers 0.000 claims abstract description 11
- 229920002545 silicone oil Polymers 0.000 claims abstract description 11
- 229920001661 Chitosan Polymers 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- -1 carbon black-modified carbon Chemical class 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 5
- 150000001721 carbon Chemical class 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000945 filler Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 10
- 239000011118 polyvinyl acetate Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 229920000573 polyethylene Polymers 0.000 claims description 7
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 238000005453 pelletization Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 3
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 3
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 3
- 239000001993 wax Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000004328 sodium tetraborate Substances 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 235000021355 Stearic acid Nutrition 0.000 claims 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims 1
- 239000008117 stearic acid Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 235000019241 carbon black Nutrition 0.000 description 92
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 241001391944 Commicarpus scandens Species 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/14—Mixed esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2455/00—Characterised by the use of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08J2423/00 - C08J2453/00
- C08J2455/02—Acrylonitrile-Butadiene-Styrene [ABS] polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5425—Silicon-containing compounds containing oxygen containing at least one C=C bond
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Abstract
The application relates to the technical field of master batches, in particular to a black master batch with high chromatic dispersion and a preparation method thereof, wherein the black master batch is prepared from the following raw materials in parts by weight: the carbon black-modified carbon black composite material comprises carbon black, modified carrier resin, a dispersing agent, a lubricating agent and a filling material, wherein each part of the modified carrier resin is prepared from the following components in parts by weight: carrier resin, chitosan, cellulose acetate propionate, silicone oil and a silane coupling agent. The black master batch prepared from the raw materials has high chromatic dispersion, good gloss, uniform color distribution, easy dispersion and good fluidity, and can keep better gloss for a long time.
Description
Technical Field
The application relates to the technical field of black master batches, in particular to a black master batch with high color dispersion and a preparation method thereof.
Background
Carbon black is one of the main components for producing the black master batch, and the dispersion degree of the carbon black plays a great role in the quality of the black master batch, because various groups on the primary particle size, the structure and the surface of the carbon black can greatly influence the dispersion capacity of the black master batch. In general, carbon black has small primary particle size, low structure, low volatile matter dispersion difficulty and easy agglomeration, so that the black master batch has weak chromatic dispersion, and simultaneously, carbon black stripes and spot areas without chromatic dispersion can be obviously displayed, so that the quality of the black master batch is poor. Therefore, manufacturers generally choose to use some resin carriers and carbon black to prepare black masterbatch, so that the carbon black can be further dispersed in the black masterbatch system, and the dispersion capability of the black masterbatch is improved, thereby improving the dyeing quality of the black masterbatch, but the carbon black carrying capability of the carrier resin is limited by the carrier resin material, so that the carbon black is still difficult to be uniformly dispersed in the black masterbatch, and the color dispersion of the black masterbatch is poor, so that improvement is needed.
Disclosure of Invention
In order to improve the problem of the color dispersion of the black master batch, the application provides the black master batch with high color dispersion and a preparation method thereof.
In a first aspect, the present application provides a black masterbatch with high dispersion, which adopts the following technical scheme:
a black master batch with high chromatic dispersion is prepared from the following raw materials in parts by weight:
30-60 parts of carbon black
20-40 parts of modified carrier resin
15-25 parts of dispersant
5-10 parts of lubricant
5-20 parts of filler
Each part of the modified carrier resin is prepared from the following components in parts by weight:
40-60 parts of carrier resin
15-20 parts of chitosan
2-5 parts of cellulose acetate propionate
10-20 parts of silicone oil
5-10 parts of a silane coupling agent.
By adopting the technical scheme, the prepared black master batch has high degree of dispersion, good gloss, uniform color distribution, easy dispersion and good fluidity, and can keep better gloss for a long time. The carbon black mainly endows the black master batch with black with high saturation, but the carbon black is easy to agglomerate, is difficult to disperse, has weak dispersion capability and poor coloring effect, the modified carrier resin has better fluidity and compatibility, can be used as a carrier to bear the carbon black, so that the carbon black is uniformly dispersed in the black master batch system, the dispersion capability of the black master batch is improved, the coloring effect is improved, the carbon black is compounded with other raw materials for use, the possibility of occurrence of carbon black stripes and spots can be reduced, the dispersing agent can improve the mixing uniformity of the carbon black, the modified carrier resin and the filling material, so that the prepared black master batch has better dispersion, impact resistance and glossiness, the lubricating agent separates the raw material particles, the carbon black is difficult to agglomerate, and the carbon black can be uniformly dispersed and can be used in the black master batch system to obtain the black master batch with higher dispersion, and the filling material can improve the impact resistance of the black master batch, so that the material is not easy to break.
The modified carrier resin is prepared from carrier resin, chitosan, cellulose acetate propionate, silicone oil and a silane coupling agent, has better fluidity and compatibility, can be uniformly mixed with other raw materials, reduces the possibility of carbon black agglomeration, is used for preparing black master batch, so that the black master batch has higher chromatic dispersion, the carrier resin has better physical properties of PC, ABS, TPU and other resins, but has poorer compatibility and fluidity, the chitosan has excellent dispersibility, fluidity and compatibility, the modified carrier resin is prepared by being used together with the carrier resin, the capability of the modified carrier resin for bearing carbon black is improved, the carbon black can be uniformly distributed in the black master batch, the chromatic dispersion of the black master batch is high, the color is bright, the uniformity is good, the dispersibility, the fluidity and the impact strength of the modified carrier resin can be improved, the weather resistance of the cellulose acetate propionate is good, the modified carrier resin is added with a certain amount of cellulose acetate propionate for preparing the black master batch, so that the black master batch can keep long-term bright color and high stability, the silicone oil can improve the lubricity of the modified carrier resin and improve the dispersion uniformity of the modified carrier resin and other raw materials, so that the black master batch has uniform black, the silane coupling agent can improve the dispersibility and adhesive force of chitosan, cellulose acetate propionate and silicone oil in the resin, and the modified carrier resin can improve the dispersibility of the modified carrier resin and the connection stability between the filler, carbon black and the modified carrier resin, so that the prepared modified carrier resin has better dispersion capability and impact resistance.
Preferably, the modified carrier resin is prepared by the following steps:
s1, weighing 40-60 parts of carrier resin, 15-20 parts of chitosan and 2-5 parts of cellulose acetate propionate according to parts by weight, stirring and mixing uniformly, putting into a weightlessness balance bin of main feeding, and then mixing 10-20 parts of silicone oil and 5-10 parts of silane coupling agent uniformly and putting into a weightlessness balance bin of side feeding;
s2, discharging in a weightless scale, extruding in a double screw rod, and granulating to obtain the modified carrier resin, wherein the melting temperature is 200-250 ℃.
By adopting the technical scheme, the prepared modified carrier resin has better compatibility and fluidity, is easy to combine with the carbon black, reduces the possibility of agglomeration of the carbon black, and enables the carbon black to be uniformly distributed in the black master batch, so that the prepared black master batch has better dispersion capacity, the carrier resin, the chitosan and the cellulose acetate propionate are all solids which are easy to be uniformly mixed, and the silicone oil and the silane coupling agent are liquid which are easy to be uniformly mixed, so that the silicone oil and the silane coupling agent are respectively mixed firstly, and then sequentially added into a weightless scale bin, so that all raw materials can be fully mixed, and then extrusion granulation is carried out, so that the prepared modified carrier resin has better fluidity and dispersibility, and is easy to combine with the carbon black.
Preferably, the carbon black is modified carbon black, and the modified carbon black is prepared by the following steps:
1) weighing 20-50 parts by weight of carbon black, soaking the carbon black in a nitric acid solution with the mass fraction of 50-60%, performing ultrasonic treatment for 0.5-1 h, performing reflux heating for 1-2 h, filtering, washing with water, and drying to obtain acidified carbon black;
2) mixing the acidified carbon black obtained in the step 1) with 30-50 parts by weight of polyvinyl acetate, putting the mixture into 10-20 parts by weight of ethyl acetate solution, adding 0.1-0.2 part by weight of dibenzoyl peroxide, carrying out reflux heating at 50-60 ℃, stirring, heating for 1-2 hours, filtering while hot, and drying to obtain the modified carbon black.
By adopting the technical scheme, the prepared modified carbon black is easy to combine with modified carrier resin, the carbon black can be uniformly dispersed in the black master batch, the dispersion capacity of the black master batch is improved, the nitric acid solution with the mass fraction of 50-60% can oxidize the surface of the carbon black, oxygen-containing functional groups on the surface of the carbon black are greatly improved, polyvinyl acetate is combined with the oxygen-containing functional groups on the surface of the carbon black under the action of dibenzoyl peroxide to obtain the modified carbon black, and the modified carbon black is difficult to aggregate, has good dispersibility, is easy to combine with the modified carrier resin, can be uniformly dispersed in the black master batch, and has better dispersion capacity and bright color.
Preferably, the weight ratio of the carbon black to the polyvinyl acetate is (3-4): (4-4.5).
By adopting the technical scheme, the weight ratio of the carbon black to the polyvinyl acetate is further optimized, so that the prepared modified carbon black has better dispersibility, is not easy to agglomerate, is easy to combine with modified carrier resin, is uniformly dispersed in the black master batch, and further improves the dispersion capacity of the black master batch.
Preferably, the dispersant is one of oxidized polyethylene, zinc stearate, borax or mica powder.
The dispersant has good dispersibility and fluidity, can be used for preparing the black master batch, can uniformly disperse the filler, the modified carrier resin and the modified carbon black in the whole system, and reduces the agglomeration of the filler, the modified carrier resin and the modified carbon black, thereby improving the dispersion capability, the impact resistance and the glossiness of the black master batch.
Preferably, the filler is at least one of silicon dioxide, precipitated calcium carbonate, barium sulfate or pottery clay.
The filler has better strength, can improve the shock resistance of the black master batch, and ensures that the black master batch is not easy to break. The silicon dioxide has good hardness, can improve the shock resistance of the black master batch, enables the black master batch not to be broken easily, has low cost and easy obtainment of precipitated calcium carbonate and argil, and can improve the processing performance of the black master batch besides the function of incremental filling; the barium sulfate has stable chemical property and good heat resistance, and can be used for preparing the black master batch and enhancing the chemical corrosion resistance and the heat resistance of the black master batch.
Preferably, the lubricant is one of paraffin, polyethylene wax or oleamide.
The lubricant has good lubricity and fluidity, so that the raw materials for preparing the black master batch are separated, the agglomeration of the carbon black is reduced, the carbon black can be uniformly dispersed in a black master batch system to obtain the black master batch with high dispersion, the paraffin wax and the polyethylene wax have good middle-stage and later-stage lubricating effects, the possibility that the raw materials are mutually bonded and agglomerated can be reduced, the oleamide has good lubricating performance, the processing and forming performance of the black master batch can be improved, and meanwhile, the antistatic effect is realized, and the dust can be reduced to be attached to the surface of the black master batch.
In a second aspect, the application provides a preparation method of a high-dispersion black master batch, which adopts the following technical scheme:
a preparation method of a high-dispersion black master batch comprises the following steps:
A) weighing 30-60 parts of carbon black, 20-40 parts of modified carrier resin, 15-20 parts of dispersing agent, 5-10 parts of lubricant and 5-20 parts of filler according to parts by weight, uniformly mixing, and banburying to obtain a mixture;
B) and crushing the mixture, extruding, bracing, granulating, pelletizing, dehydrating, air-drying, and polishing by a high-speed polishing machine to obtain the black master batch.
By adopting the technical scheme, the operation is simple and convenient, the prepared black master batch has good chromatic dispersion, good color gloss and strong stability, and the dispersion degree of the carbon black is further improved by combining the modified carbon black with the modified carrier resin in the banburying process, so that the chromatic dispersion capability and the fluidity of the black master batch are improved; in the banburying process, the carbon black, the modified carrier resin, the dispersing agent, the lubricating agent and the filler are fully and uniformly mixed, so that the subsequent granulation is facilitated, and the dispersion capacity, the flowability and the impact resistance of the prepared black master batch are improved.
Preferably, the banburying temperature in the step A) is 200-280 ℃, the modified carrier resin is firstly added, the filler, the dispersant and the lubricant are added after the modified carrier resin is melted, the mixture is uniformly stirred, and the carbon black is added in 3-5 times.
By adopting the technical scheme, the raw materials can be fully and uniformly mixed, the carbon black can be uniformly distributed in the black master batch, the carbon black is a substance which is easy to agglomerate, the carbon black needs to spend longer time for mixing in one-time addition, the time for uniformly mixing in batch addition is short, and the time cost is saved.
Preferably, the extrusion temperature in the step B) is 240-280 ℃.
The temperature is a better temperature range for granulation, and if the temperature is lower than 240 ℃, granular substances exist in the black master batch, so that the black master batch is unqualified; if the temperature is higher than 280 ℃, the modified carrier resin is easy to coke and is difficult to combine with the carbon black, so that the carbon black is not uniformly dispersed, and the dispersion capacity of the black master batch is poor.
In summary, the present application has the following beneficial effects:
1. the black master batch prepared from the carbon black, the modified carrier resin, the dispersing agent, the lubricating agent and the filler in a reasonable ratio has high chromatic dispersion, good gloss, uniform color distribution, easy dispersion and good fluidity, and can keep better gloss for a long time.
2. According to the application, after the carbon black is soaked in a nitric acid solution with the mass fraction of 50-60%, the carbon black reacts with polyvinyl acetate under the action of dibenzoyl peroxide to prepare the modified carbon black, the modified carbon black is easy to combine with modified carrier resin, the carbon black can be uniformly dispersed in the black master batch, and the dispersion capacity of the black master batch is improved.
Detailed Description
The present application will be described in further detail with reference to examples and comparative examples. The starting materials in this application are all commercially available, and the following are the types of sources of some of the starting materials in this application, as shown in table 1:
TABLE 1 sources and types/models of part of the raw materials
Preparation example of modified Carrier resin
A modified carrier resin prepared by the following method:
s1, 40-60 parts of carrier resin, 15-20 parts of chitosan and 2-5 parts of cellulose acetate propionate, stirring and mixing uniformly, putting into a weightlessness scale bin of main feeding, and then mixing uniformly 10-20 parts of silicone oil and 5-10 parts of silane coupling agent, and putting into a weightlessness scale bin of side feeding;
s2, discharging in a weightless scale, and extruding and granulating in a double screw rod to obtain the modified carrier resin, wherein the melting temperature is 200-280 ℃. The components and the amounts of the modified carrier resins prepared in preparation examples 1 to 3 are shown in Table 2:
TABLE 2 Components and amounts for preparing modified support resins
Preparation of modified carbon Black
Preparation example 4
A modified carbon black prepared by the following method:
1) weighing 2kg of carbon black, soaking the carbon black in 1kg of nitric acid solution with the mass fraction of 50%, performing ultrasonic treatment for 0.5h, performing reflux heating for 1h, filtering, washing with water, and drying to obtain acidified carbon black;
2) mixing the acidified carbon black obtained in the step 1) with 3kg of polyvinyl acetate, putting the mixture into 1kg of ethyl acetate solution, adding 0.01kg of dibenzoyl peroxide, heating under reflux at 50 ℃, stirring, heating for 1h, filtering while hot, and drying to obtain the modified carbon black.
Preparation example 5
A modified carbon black prepared by the following method:
1) weighing 3kg of carbon black, soaking the carbon black in 1.5kg of nitric acid solution with mass fraction of 55%, performing ultrasonic treatment for 0.45h, performing reflux heating for 1.5h, filtering, washing with water, and drying to obtain acidified carbon black;
2) mixing the acidified carbon black obtained in the step 1) with 4kg of polyvinyl acetate, putting the mixture into 1.5kg of ethyl acetate solution, adding 0.015kg of dibenzoyl peroxide, heating the mixture under reflux at 55 ℃, stirring the mixture at the same time, heating the mixture for 1.5 hours, filtering the mixture while the mixture is hot, and drying the mixture to obtain the modified carbon black.
Preparation example 6
A modified carbon black prepared by the following method:
1) weighing 5kg of carbon black, soaking the carbon black in 2kg of nitric acid solution with the mass fraction of 50%, performing ultrasonic treatment for 1h, performing reflux heating for 2h, filtering, washing with water, and drying to obtain acidified carbon black;
2) mixing the acidified carbon black obtained in the step 1) with 5kg of polyvinyl acetate, putting the mixture into 2kg of ethyl acetate solution, adding 0.02kg of dibenzoyl peroxide, heating under reflux at 60 ℃, stirring, heating for 2 hours, filtering while hot, and drying to obtain the modified carbon black.
TABLE 3 raw materials and amounts used for preparing modified carbon blacks in preparation examples 4 to 6
Examples
Example 1
A black master batch with high dispersion is prepared by the following steps:
A) weighing 3kg of carbon black, 2kg of modified carrier resin from preparation example 1, 1.5kg of oxidized polyethylene, 0.5kg of paraffin and 5kg of silicon dioxide, uniformly mixing, adding into an internal mixer, and carrying out internal mixing at the temperature of 200 ℃ to obtain a mixture;
B) and crushing the mixture, extruding, bracing, granulating, pelletizing, dehydrating, air-drying, and polishing by a high-speed polishing machine to obtain the black master batch.
Example 2
A black master batch with high dispersion is prepared by the following steps:
A) adding 2kg of modified carrier resin from preparation example 1 into an internal mixer, adding 1.5kg of oxidized polyethylene, 0.5kg of paraffin and 5kg of silicon dioxide after the modified carrier resin is melted, uniformly stirring, adding 1kg of carbon black each time, and mixing at 200 ℃ to obtain a mixture;
B) and crushing the mixture, extruding, bracing, granulating, pelletizing, dehydrating, air-drying, and polishing by a high-speed polishing machine to obtain the black master batch.
Example 3
The present embodiment is different from embodiment 2 in that: the modified carbon black from preparation 4 was substituted for an equal amount of carbon black and the remaining amounts and procedure were in accordance with example 2.
The raw materials and the amounts used in examples 4 to 7 are partially different from those in example 2, and are shown in table 4:
TABLE 4 raw materials and amounts and banburying temperatures in examples 1-7
TABLE 5 sources of modified carbon blacks and modified support resins from examples 1-7
| Examples | Modified support resin | Modified carbon black |
| Example 1 | Preparation example 1 | Ordinary carbon black |
| Example 2 | Preparation example 1 | Preparation example 4 |
| Example 3 | Preparation example 1 | Preparation example 4 |
| Example 4 | Preparation example 2 | Preparation example 5 |
| Example 5 | Preparation example 3 | Preparation example 6 |
| Example 6 | Preparation example 1 | Preparation example 5 |
| Example 7 | Preparation example 2 | Preparation example 6 |
Comparative example
Comparative example 1
This comparative example differs from example 3 in that: the modified support resin from preparation 3 was replaced with an equal amount of PC, and the remaining amounts and procedures were the same as in example 3.
Comparative example 2
This comparative example differs from example 4 in that: the modified carrier resin from preparation 2 was replaced by the same amount of TPU, and the remaining amounts and procedures were the same as in example 4.
Comparative example 3
This comparative example differs from example 5 in that: the modified support resin from preparation 5 was replaced with the same amount of ABS as in example 5, except that the procedure was the same.
Performance test
And (4) measuring the mass flow rate of the black master batch melt.
And (4) measuring the dispersion size grade and the dispersion appearance grade of the black master batch.
And (4) measuring the blackness of the black master batch.
And (4) measuring the impact strength of the black master batch.
Detection method/test method
And (3) measuring the mass flow rate of the black master batch melt: testing according to ISO 1133 standard.
And (3) measuring the dispersion size grade and the dispersion appearance grade of the black master batch: tested according to the GB/T18251-2019 standard.
And (3) determining the blackness of the black master batch: the assay was performed according to GB/T7048-.
And (3) determining the impact strength of the black master batch: the measurement was carried out according to GB/T1843-2008.
Table 6 performance testing experimental data
By combining examples 1-7 and comparative examples 1-3 and combining table 6, it can be seen that the black master batch in examples 1-7 has a high melt mass flow rate, a high dispersion size grade and a high dispersion appearance grade of the black master batch, and a good blackness. Comparing example 3 with comparative example 1, example 4 with comparative example 2, and example 5 with example 3, two by two, it can be seen that the black masterbatch prepared with the modified carrier resin has a higher melt mass flow rate, a high dispersion size grade and dispersion appearance grade of the black masterbatch, and a good blackness.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The black master batch with high color dispersion is characterized by being prepared from the following raw materials in parts by weight:
30-60 parts of carbon black
20-40 parts of modified carrier resin
15-25 parts of dispersant
5-10 parts of lubricant
5-20 parts of filler
Each part of the modified carrier resin is prepared from the following components in parts by weight:
40-60 parts of carrier resin
15-20 parts of chitosan
2-5 parts of cellulose acetate propionate
10-20 parts of silicone oil
5-10 parts of a silane coupling agent.
2. The black master batch with high dispersion degree according to claim 1, wherein: the modified carrier resin is prepared by the following steps:
s1, weighing 40-60 parts of carrier resin, 15-20 parts of chitosan and 2-5 parts of cellulose acetate propionate according to parts by weight, stirring and mixing uniformly, putting into a weightlessness balance bin of main feeding, and then mixing 10-20 parts of silicone oil and 5-10 parts of silane coupling agent uniformly and putting into a weightlessness balance bin of side feeding;
s2, discharging in a weightless scale, extruding in a double screw rod, and granulating to obtain the modified carrier resin, wherein the melting temperature is 200-280 ℃.
3. The black master batch with high dispersion degree according to claim 1, wherein: the carbon black is modified carbon black, and the modified carbon black is prepared by the following steps:
1) weighing 20-50 parts by weight of carbon black, soaking the carbon black in a nitric acid solution with the mass fraction of 50-60%, performing ultrasonic treatment for 0.5-1 h, performing reflux heating for 1-2 h, filtering, washing with water, and drying to obtain acidified carbon black;
2) mixing the acidified carbon black obtained in the step 1) with 30-50 parts by weight of polyvinyl acetate, putting the mixture into 10-20 parts by weight of ethyl acetate solution, adding 0.1-0.2 part by weight of dibenzoyl peroxide, carrying out reflux heating at 50-60 ℃, stirring, heating for 1-2 hours, filtering while hot, and drying to obtain the modified carbon black.
4. The black master batch with high dispersion degree according to claim 3, wherein: the weight ratio of the carbon black to the polyvinyl acetate is (3-4): (4-4.5).
5. The black master batch with high dispersion degree according to claim 1, wherein: the dispersant is one of oxidized polyethylene, zinc stearate, borax or mica powder.
6. The black master batch with high dispersion degree according to claim 1, wherein: the filling material is at least one of silicon dioxide, precipitated calcium carbonate, barium sulfate and argil.
7. The black master batch with high dispersion degree according to claim 1, wherein: the lubricant is one of paraffin, polyethylene wax, stearic acid or oleamide.
8. A process for the preparation of a high-dispersibility black masterbatch according to any one of claims 1 to 7, characterized in that it comprises the following steps:
A) weighing 30-60 parts of carbon black, 20-40 parts of modified carrier resin, 15-20 parts of dispersing agent, 5-10 parts of lubricant and 5-20 parts of filler according to parts by weight, uniformly mixing, and banburying to obtain a mixture;
B) and crushing the mixture, extruding, bracing, granulating, pelletizing, dehydrating, air-drying, and polishing by a high-speed polishing machine to obtain the black master batch.
9. The process for preparing a high-dispersion black master batch according to claim 8, wherein the process comprises the following steps: and B) banburying in the step A) at the temperature of 200-250 ℃, adding the modified carrier resin, adding the filler, the dispersant and the lubricant after the modified carrier resin is molten, uniformly stirring, and adding the modified carbon black by 3-5 times.
10. The process for preparing a high-dispersion black master batch according to claim 8, wherein the process comprises the following steps: the temperature of extrusion in the step B) is 240-280 ℃.
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