CA2457758A1 - Method for making masterbatch - Google Patents

Method for making masterbatch Download PDF

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Publication number
CA2457758A1
CA2457758A1 CA002457758A CA2457758A CA2457758A1 CA 2457758 A1 CA2457758 A1 CA 2457758A1 CA 002457758 A CA002457758 A CA 002457758A CA 2457758 A CA2457758 A CA 2457758A CA 2457758 A1 CA2457758 A1 CA 2457758A1
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CA
Canada
Prior art keywords
plastics material
colouring
components
powder
mixer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002457758A
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French (fr)
Inventor
George Leopold Archer
John Stewart Holmes
Neville Hugh Mckay
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gjn Polymers Ltd
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Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of CA2457758A1 publication Critical patent/CA2457758A1/en
Abandoned legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A process for producing a colouring agent (masterbatch) for colouring a polymers is provided, comprising the step of mixing a plastics material, carbon black and waste print powder. The maximum proportion of waste print powder is preferably 50 %. The process enables waste print powder to be recycled in a useful manner, thereby addressing the environmental problem of waste print powder pollution.

Description

METHOD FOR MAHING MASTERBATCH
The present invention relates to a process for producing a colouring agent for colouring a polymer, and in particular to a process for producing a masterbatch for use in extrusion processes and the like.
The development of polymer chemistry and its subsequent application to the production of industrial and household articles is one of the great success stories of the 2011' century. The result is that an enormous range of articles are now produced from plastics materials.
to Some of these were previously produced from alternative materials, and the production of some has only been possible because of the development of polymer chemistry.
Despite the fact that this technology is more than a century old, the scale of production of these articles is such that research into new and improved polymers and methods of 15 production continues apace.
The natural colour of most plastics materials is rather unattractive and variable, and accordingly a colouring agent has traditionally been added to the plastics material in order to produce a finished article of uniform colour. When the aesthetic appearance of the 2o article is not particularly important (for example in the production of dustbins or industrial components), then the article is often coloured black. However, it is possible to produce the full range of colours simply by varying the colouring agent in order to meet consumer demand.
25 The colouring agent is normally prepared by adding a dyestuff to a plastics material in order to produce a small amount of intensely coloured plastics material, and then by mixing the intensely coloured plastics material with a second plastics material (which may or may not be the same as the first) when the second plastics material is being formed into the finished article. The intensely coloured first plastics material is known as 30 "masterbatch".
Black masterbatch is generally formed by mixing carbon black with an appropriate polymer and optionally adding chalk dust as a filler in an extrusion machine.
The components are heated, mixed, extruded and pelletised to produce the masterbatch, which is then added in amounts of 0.1 to 25% by weight to the plastics material when it is being processed into the finished article (for example in a moulding or extrusion process).
If it is desired to produce a masterbatch of a different colour, then an appropriately coloured pigment is mixed with the polymer and chalk filler (normally without carbon black) and the process is carried out as before.
to Industry is always on the lookout for improved production processes, particularly in the field of polymer chemistry with its large scale of production and the consequently large cost savings available.
15 EP 0322555 (General Electric Company) discloses a method for colouring thermoplastic polymer resins using a masterbatch which is formed from a colorant such as carbon black and a polyetherimide ester elastomer. A wide variety of inorganic and organic colorants are disclosed. The masterbatch may be manufactured on high intensity high shear equipment such as compounding extruders, two-roll compounding mills and in Banbury 20 mixers.
WO 79/00406 (Akesson et al.) discloses a method for the preparation of a masterbatch to be added to a thermoplastic resin. The masterbatch is in the form of a colourant including colour pigment particles as an additive dispersed in a vehicle.
JP 08003322 (Canon KK) discloses compositions for colouring plastics comprised of thermoplastic polymers and pigments. The compositions give mouldings without unevenness or density difference of colour.
3o According to a first aspect of the present invention, there is provided a process for producing a colouring agent for colouring a polymer, comprising the step of mixing a plastics material and waste print resin. Optionally, pure carbon black and Iow density polyethylene may be added.
Print resin is a specific product used by the print industry to create print automatically and at high speed onto paper (or another substrate) without causing smudging.
Print resin is normally provided in powder form, and generally comprises at least some of the following components: carbon black, ferrous oxide, carranba wax, styrene acrylic polymer, polyester resin, zinc stearate, nigrazine dye and oxide famerete powder. A
1o variety of carrier polymers may be included depending on the brand. Ferrous oxide, carbon black and nigrazine dye are black colour enhancers, and one or two of the three may be omitted, depending on the shade of black or brand of powder employed.
If a different colour to black is required, then all three are omitted, and a pigment of appropriate colour is added.
Without wishing to be constrained by theory, it is thought that print powder also includes a component or number of components which stabilises the melting point of the composition. All waste print powders investigated by the applicants (including waste print powders obtained from Xerox, Canon, Ricoh, Hewlett-Packard and Osay) have a melting point close to 118°C.
As the temperature is raised above the melting point, the waste print powder hardens again.
Investigations have found that this solidification point is in all cases very close to 0.75°C
above the melting point, i.e. 118.75°C.
Print powder is normally provided in a sealed cartridge for use in computer printers and photocopying machines. The cartridge may have a sliding door or the like which opens when the cartridge is fitted into the printer in order to allow access to the waste print powder, and closes when the cartridge is removed from the printer in order to prevent the 3o escape of powder.

It is impractical to design a system which uses alI of the powder in a cartridge and inevitably somewhere in the region of 5% of the powder remains inaccessible in the cartridge when the printer shows the cartridge as having expired.
Even though the amount of powder remaining in a spent cartridge is relatively small, the total number of spent cartridges and therefore the total amount of waste powder produced by industry is substantial and growing rapidly.
The powder left in expired cartridges is a waste product which is very difficult to dispose l0 of. The powder is so finely divided (with particle sizes being in the order of 15~,m) that it tends to escape from landfill sites and find its way to the water supply, with serious environmental consequences. This is now of world-wide concern.
The inventive realisation of the present realisation is that this waste print powder can be 15 used to make masterbatch. Thus, a waste product which is extremely difficult to dispose of in an environmentally friendly way can be employed in the production of an industrially useful product.
A substantial amount of surplus or imperfect waste print powder is produced by print 2o manufacturers, and often this is difficult or expensive for the manufacturer to dispose o~
Accordingly, the powder employed in the present invention may be obtained from spent cartridges as described above, or may be obtained directly from the print manufacturer, who may have supplies which could not otherwise be used in print cartridges.
For example, waste powder for printer cartridges must be produced with having narrow 25 particle size distribution. Powder having particles which axe too small (in the order of 2 ~m or less) or too large (in the order of 10 ~m or more) cannot be employed in printer cartridges and is surplus to requirements. It is however perfectly suitable for the purposes of the present invention.
30 The preferred proportion by weight of the components in the inventive process is as follows:

Plastics materials - preferably from 5 to 95%, more preferably at least from 20 to 50%, most preferably about 25%.
Carbon black - preferably from 0.5 to 80%, more preferably from 20 to 40%, most 5 preferably about 25%.
Waste print powder - preferably from 5 to 80%, more preferably from 25 to 50%, most preferably about 40%.
to The ratio of plastics material to carbon black depends on the particle size of the carbon black. Thus the ratios of particularly preferred embodiments of the present invention are given in Table 1 below:

CARBON BLACK
DBP STRUCTURE CARBON BLACK PLASTICS WASTE PRINT
MATERIAL POWDER

137 22.5 32.5 45 The term "Carbon Black DBP Structure" refers to the grade of carbon black and is a definition well known in the industry.
If these ratios are not adhered to, the likelihood is that:
(1) the end product will be too brittle to be effective (2) the product will overheat during the process and the mixture will oxidise (3) if oxidation does occur the pigment transportation qualities of the product are reduced to below commercial value.
It has been found that the use of waste print powder on its own results in an end product which is too brittle to be effective.
The relative proportions of the various components is varied depending on how dark the masterbatch is required to be (the so-called "cover"). For example, if heavier cover is required than that given by the preferred proportions of 50% waste print powder, 25%
to carbon black and 25% polymer, then 45% waste print powder, 30% carbon black and 25%
polymer may be used. Ideally, the polymer is included at 25% by weight or more, which prevents the final product becoming brittle and difficult to handle during extrusion.
Other additives may be included to create and/or enhance the required end-product 15 specification.
In order to produce a non-black colouring agent, the appropriate coloured pigment (e.g.
coloured waste print powder) is mixed with the plastics material in accordance with the invention. The coloured powder may be supplemented with additional pigment and/or 20 other additives, in order to produce the desired final colour.
An effective masterbatch can be prepared by the following preferred process:
I. The components are mixed loosely in a drum.
25 2. The components are transferred by a variable speed feeder at a defined rate to a mixer and grinder where they are mixed, ground and amalgamated.
3. The resulting materials exit the pre-mixer in a rope form which is then fed by a time-sequenced pusher device at a constant rate into an extruder.
4. The mixture is mixed and extruded as a series of strands.

In a preferred embodiment, the components are mixed together and heated in a mixing machine such as a twin screw extruder, a single screw extruder, a two roll mill, or, preferably, a Farrel CP machine, a Banbury mixer, or any suitable mixer.
It has been found that it is advantageous to keep the entrance into the mixer relatively cool in order to avoid softening the waste print powder (which softening begins at about 90°C).
Keeping the entrance below about 90°C, preferably from 40 to 90°C and most preferably about 45°C, enables the waste print powder to be transported into a mixer in a stable condition. It is particularly desirable to control this temperature carefully in the case of mixers other than Banbury or Farrel CP machines. The advantage of using a Banbury or Farrel machine is that mixing of the components is more thorough and the entrance temperature is not so critical.
Processing temperatures within the mixer are fairly flexible, but preferably range from 135 to 230°C and are most preferably at about 150°C. At approximately 118°C, the waste print powder melts and then very rapidly hardens as the temperature rises by another degree or so. It is therefore necessary to use a mixer which is sufficiently powerful to grind the powder continuously to prevent it from conglomerating and hardening. The mixer should 2o be sufficiently powerful to mix the waste print powder and the carbon black into the Garner resin homogeneously. It has been discovered that the Banbury and Farrel machines are particularly effective at achieving this aim.
In a preferred embodiment, the components are mixed at a mixing rate of from 150 to 500 miri 1, preferably from 350 to 400 miri 1.
Because the processing temperature tends to range from 135 to 230°C, heat is transferred from the main body of the mixer to the mixer entrance. Accordingly, the mixer entrance may be artificially cooled, for example by circulating cooled water in a j acket around the 3o entrance, in order to maintain the entrance at the temperatures outlined above.

The components are fed into the mixer until the maximum safe operational amperage is reached. In the case of a Farrel CP 500, the maximum amperage is in the region of 90 to 95 amps and this equates to a rate of addition of the mix of from 500 to 550 kg per hour.
The plastics material may be selected by a skilled person to match the plastics material which is to be coloured by addition of the masterbatch. Suitably plastics material include polyethylene, polypropylene, EVA, EEA, ABS, PVC or any other type of polymer.
After the components have been mixed to form the masterbatch, the masterbatch may be to extruded and divided into pellets for use in the colouring of a second plastics material.
In accordance with a second aspect of the invention, there is provided a colouring agent for colouring a polymer which agent is obtainable by means of a process defined above.
15 In accordance with a third aspect of the invention, there is provided a process for forming a coloured object from a plastics material, comprising the steps of mixing said plastics material with a colouring agent obtainable by means of a process as defined above, and forming the coloured plastics material into said object. The object may be formed by means of an extrusion or moulding process.
The amount of masterbatch added to the plastics material generally varies from 1 to 25%
by weight. The precise amount will depend on the level of cover required, and from what the plastics material is formed. For example, if the plastics material is clear, then a relatively low amount of masterbatch is required (perhaps 1- 2%) in order to produce a good level of cover. If however plastics material is used which has been coloured white (with e.g. titanium dioxide), then perhaps 15-20% of masterbatch may be required in order to achieve the same level of cover. Cover is usually assessed by eye and the components of the subsequent process adjusted accordingly.
3o In a fourth aspect of the invention, there is provided an object formed from a plastics material, which material has been coloured by the addition of a colouring agent obtainable by means of a process as defined above.

The invention will now be illustrated by means of the following examples.
Example 1 Carbon black, print powder from expired printer cartridges and manufacturer's waste and polyethylene resin were weighed and loaded into a blender above an extruder in the following amount:
1o Carbon black - 25%
Print powder - 50%
Polyethylene - 25%
After being blended the mixture was fed into a Farrel CP 500 mixer at a feed rate of from 1s 350 to SSOKgph.
The entrance to the mixer as surrounded with a water-cooled jacket in order to maintain the temperature at about 60 to 70°C.
2o The components were mixed at high pressure within the Farrel CP S00 at approximately 150°C and at a mixing speed of from 350 to 400 revolutions per minute.
The resultant mix was discharged from the mixer in the form a continuous hot rope into a single screw extruder. It was then pushed through a dye to form separate strands, which 25 were fed into a pelletiser where pellets were formed and cooled.

Example 2 The process of Example 1 was carried out except that the proportions of the components were altered to the following in order to provide rnasterbatch with a heavier cover:
Carbon black - 30%
Waste print powder- 45%
Polyethylene - 25%
to Machine settings are within parameters as defined in Example 1.

Claims (14)

1. A process for producing a colouring agent for colouring a polymer, comprising the step of mixing from 20 to 50% plastics material, from 20 to 40% carbon black and from 25 to 50% waste print powder.
2. A process as claimed in claim 1, wherein the said proportions are about 25%
plastics material, about 25% carbon black and about 50% waste print powder.
3. A process as claimed in claim 1 or 2, wherein the components are added to a mixer, and wherein the entrance to the mixer maintained at a temperature of from 40 to 90°C to prevent softening of the waste print powder.
4. A process as claimed in claim 3, wherein the mixer entrance is maintained at about 45°C.
5. A process as claimed in any preceding claim, wherein the components are mixed at a temperature of from 135 to 230°C.
6. A process as claimed in claim 5, wherein the components are mixed at about 150°C.
7. A process as claimed in any preceding claim, wherein the components are mixed in a twin screw extruder, a Farrel CP machine, a Banbury mixer, a single screw extruder, or a two roll mill.
8. A process as claimed in claim 7, wherein the components are mixed at a mixing rate of from 150 to 500 min-1.
9. A process as claimed in any preceding claim, wherein after the components are mixed to form the colouring agent, said agent is extruded and divided into pellets for use in the colouring of a second plastics material.
10. A process as claimed in any preceding claim, wherein the waste print powder melts at about 118°C and solidifies at about 118.75°C.
11. A colouring agent for colouring a polymer which agent is obtainable by means of a process according to any preceding claim.
12. A process for forming a coloured object from a plastics material, comprising the steps of mixing said plastics material with a colouring agent as claimed in claim 11, and forming the coloured plastics material into said object.
13. A process as claimed in claim 12, wherein said object is formed by extruding said plastics material with said colouring agents.
14. An object formed from a plastics material, which material has been coloured by the addition of a colouring agent as claimed in claim 11.
CA002457758A 2001-08-14 2002-08-14 Method for making masterbatch Abandoned CA2457758A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB0119815.9 2001-08-14
GBGB0119815.9A GB0119815D0 (en) 2001-08-14 2001-08-14 Method for making masterbatch
PCT/GB2002/003780 WO2003025046A1 (en) 2001-08-14 2002-08-14 Method for making masterbatch

Publications (1)

Publication Number Publication Date
CA2457758A1 true CA2457758A1 (en) 2003-03-27

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CA002457758A Abandoned CA2457758A1 (en) 2001-08-14 2002-08-14 Method for making masterbatch

Country Status (5)

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US (1) US20040034949A1 (en)
EP (1) EP1419192A1 (en)
CA (1) CA2457758A1 (en)
GB (1) GB0119815D0 (en)
WO (1) WO2003025046A1 (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005054344A1 (en) * 2003-12-05 2005-06-16 John Scheirs Masterbatch
WO2008070916A1 (en) * 2006-12-14 2008-06-19 Close The Loop Technologies Pty Ltd Materials, systems and methods involving plastics material
AU2014231766B2 (en) * 2013-03-15 2017-11-09 Close The Loop Technologies Pty Ltd Asphalt including modified toner based additive
EP2915652A1 (en) 2014-03-03 2015-09-09 Ricoh Company, Ltd. Method and apparatus for producing masterbatch pellets from waste toner
EP2915837B1 (en) 2014-03-03 2017-05-03 Ricoh Company, Ltd. Method and apparatus for producing masterbatch from waste toner powders

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2500664C3 (en) * 1975-01-09 1978-08-17 Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt Process for the production of pigment / plastic concentrates containing carbon black
SE417622B (en) * 1977-12-19 1981-03-30 Tore Jan Borje Akesson DAMM-FREE SHIPPING CONCENTRATE FOR INSERTING THERMOPLASTIC MATERIAL
EP0322555A3 (en) * 1987-12-23 1991-01-30 General Electric Company Novel pigment carrier system
DE4405256A1 (en) * 1994-02-18 1995-08-24 Buna Gmbh Recycled plastic molding compound
JP3176220B2 (en) * 1994-06-27 2001-06-11 キヤノン株式会社 Colorant composition for adding molded plastic
US6113681A (en) * 1999-08-13 2000-09-05 Texas Department Of Transportation Toner-modified asphalt compositions

Also Published As

Publication number Publication date
EP1419192A1 (en) 2004-05-19
US20040034949A1 (en) 2004-02-26
WO2003025046A1 (en) 2003-03-27
GB0119815D0 (en) 2001-10-10

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