Methods of preparing a polymeric material composite Number:7,041,780 from the United States Patent and Trademark Office (PTO) owispatent Methods to prepare a poly(arylene ether) and poly(alkenyl aromatic) polymeric material having reduced levels of particulate impurities are described. The polymeric material prepared is suitable for use in data storage media applications.<H composite, polymeric, Methods, of, prep, 7041780.html, Patent, pto, 7041780

Title: Methods of preparing a polymeric material composite

Abstract: Methods to prepare a poly(arylene ether) and poly(alkenyl aromatic) polymeric material having reduced levels of particulate impurities are described. The polymeric material prepared is suitable for use in data storage media applications.

Patent Number: 7,041,780 Issued on 05/09/2006 to Buckley, et al.

Inventors: Buckley; Paul W. (Scotia, NY); Dong; Jiawen (Rexford, NY); Giammattei; Mark H. (Selkirk, NY); Guo; Hua (Selkirk, NY); Hossan; Robert John (Delmar, NY); Lietzau; Christian (Delmar, NY); Silvi; Norberto (Clifton Park, NY)
Assignee: General Electric (Pittfield, MA)

Appl. No.: 648640

Filed: August 26, 2003

Current U.S. Class: 528/501 ; 159/2.2; 523/348; 525/132; 528/493; 528/499; 528/502A

Current International Class: C08F 6/06 (20060101)

Field of Search: 528/493,501,502A 525/132

References Cited [Referenced By]

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Primary Examiner: Zimmer; Marc S.

Claims

The invention claimed is:

1. A method of preparing a polymeric material, comprising: reacting a monohydroxy aromatic compound in the presence of a catalyst, oxygen, and a solvent to form a reaction mixture, wherein the monohydroxy aromatic compound, the solvent, or a combination of the foregoing is optionally purified prior to reacting; adding water and a chelating agent to the reaction mixture to form an aqueous phase and an organic phase, and separating the aqueous phase from the organic phase, wherein the organic phase comprises poly(arylene ether); optionally filtering the organic phase through a first filtration system to remove particulate impurities; isolating poly(arylene ether) from the organic phase; combining the poly(arylene ether) with a poly(alkenyl aromatic) to form a mixture, wherein the mixture is optionally purified; optionally purifying the poly(alkenyl aromatic) prior to the combining; obtaining a polymeric material from the mixture, wherein the polymeric material comprises poly(arylene ether) and poly(alkenyl aromatic); and wherein the polymeric material is substantially free of visible particulate impurities.

2. The method of claim 1, wherein the poly(alkenyl aromatic) is in the form of a solution, melt, or solid.

3. The method of claim 1, wherein the poly(arylene ether) is in the form of a solution, melt, or solid.

4. The method of claim 1, wherein the first filtration system comprises a filter having a pore size of about 0.01 to about 50 micrometers.

5. The method of claim 1, wherein the first filtration system comprises a sintered metal filter, a cloth filter, a fiber filter, a paper filter, a pulp filter, a metal mesh filter, a ceramic filter, or a combination comprising at least one of the foregoing filters.

6. The method of claim 1, wherein the first filtration system comprises a filter having a geometry that is cone, pleated, candle, stack, flat, wraparound, or a combination comprising at least one of the foregoing geometries.

7. The method of claim 1, further comprising washing the organic phase with an aqueous solvent.

8. The method of claim 1, further comprising concentrating the organic phase by removing solvent to form a concentrated organic phase.

9. The method of claim 8, further comprising filtering the concentrated organic phase through a second filtration system to remove particulate impurities.

10. The method of claim 1, wherein the poly(arylene ether) is in the form of a solid, and wherein the solid poly(arylene ether) is a powder formed by precipitation of poly(arylene ether) from the organic phase.

11. The method of claim 10, further comprising reslurrying the precipitated poly(arylene ether) with a solvent prior to isolating.

12. The method of claim 10, further comprising drying the poly(arylene ether) powder formed by precipitation.

13. The method of claim 12, wherein the poly(arylene ether) is precipitated, collected, and dried in an environment substantially free of particulate impurities.

14. The method of claim 1, further comprising transporting and storing the poly(arylene ether) in an environment substantially free of particulate impurities.

15. The method of claim 1, filtering the poly(arylene ether), poly(alkenyl aromatic), or both to remove particulate impurities prior to the combining step.

16. The method of claim 1, wherein the polymeric material is substantially free of particulate impurities greater than about 15 micrometers.

17. The method of claim 1, wherein the mixture is formed by melt blending poly(arylene ether) and poly(alkenyl aromatic) to form a melt mixture.

18. The method of claim 17, further comprising melt filtering the melt mixture through a melt filtration system.

19. The method of claim 18, wherein the melt filtration system comprises a sintered metal filter, a metal mesh filter, a fiber metal felt filter, a ceramic filter, or a combination of the foregoing filters.

20. The method of claim 18, wherein the melt filtration system comprises a filter having a geometry that is cone, pleated, candle, stack, flat, wraparound, or a combination comprising at least one of the foregoing geometries.

21. The method of claim 18, wherein the melt filtration system comprises a filter having a pore size of about 0.5 to about 200 micrometers.

22. The method of claim 18, wherein the melt filtration system is maintained at a temperature of about 260.degree. C. to about 380.degree. C.

23. The method of claim 18, wherein the melt blending occurs in a twin screw counter-rotating extruder, a twin screw co-rotating extruder, a single screw extruder, a single screw reciprocating extruder, or a ring extruder.

24. The method of claim 23, wherein the extruder has a specific throughput rate of about 0.5 kg/cm.sup.3 to about 8 kg/cm.sup.3.

25. The method of claim 23, wherein the extruder further comprises a melt pump.

26. The method of claim 23, wherein the melt has a residence time in the extruder of less than or equal to about 1 minute.

27. The method of claim 18, further comprising compounding the poly(arylene ether) and poly(alkenyl aromatic) prior to melt blending.

28. The method of claim 27, wherein the compounding is performed in a counterrotating conical extruder, or a counterrotating extruder.

29. The method of claim 1, wherein the mixture is formed by combining poly(arylene ether), poly(alkenyl aromatic), and a solvent to form a solution mixture.

30. The method of claim 1, wherein the mixture is formed by combining poly(arylene ether) powder and poly(alkenyl aromatic) powder to form a powder mixture.

31. The method of claim 1, wherein the combining is performed in an environment substantially free of particulate impurities.

32. The method of claim 1, wherein the combining is performed under an inert atmosphere.

33. The method of claim 1, wherein the mixture is filtered using a third filtration system to remove particulate impurities.

34. The method of claim 33, wherein the third filtration system comprises a filter having a pore size of about 0.01 to about 50 micrometers.

35. The method of claim 33, wherein the third filtration system comprises a sintered metal filter, a cloth filter, a fiber filter, a paper filter, a pulp filter, a metal mesh filter, a ceramic filter, or a combination comprising at least one of the foregoing filters.

36. The method of claim 33, wherein the third filtration system comprises a filter having a geometry that is cone, pleated, candle, stack, flat, wraparound, or a combination comprising at least one of the foregoing geometries.

37. The method of claim 1, wherein the mixture is a solution, melt, or powder.

38. The method of claim 1, wherein the polymeric material is obtained from the mixture by precipitation, or by the removal of solvent using a devolatilization extruder, a flash vessel, a distillation system, or a combination comprising at least one of the foregoing.

39. The method of claim 1, wherein the mixture further comprises a solvent, superheating the mixture; filtering the superheated mixture to form a superheated filtrate; feeding the superheated filtrate to an extruder, wherein the extruder comprises an upstream vent and a downstream vent; removing solvent from the filtrate via the upstream vent and the downstream vent; and obtaining a polymeric material.

40. The method of claim 39, wherein to polymeric material is obtained in the form of a pellet.

41. The method of claim 1, wherein an organic phase of the reaction mixture comprising the poly(arylene ether) in fed into a devolatilization extruder and the poly(alkylene aromatic) is fed to the extruder via a side feeder to form the mixture.

42. The method of claim 1, wherein the polymeric material is obtained in an environment substantially free of particulate impurities.

43. The method of claim 42, further comprising packaging, storing, or packaging and storing the polymeric material in an environment substantially free of particulate impurities.

44. The method of claim 1, wherein the obtaining is performed under an inert atomosphere.

45. The method of claim 1, wherein the poly(arylene ether) comprises a plurality of structural units of the structure ##STR00004## wherein for each Q.sup.1 is independently halogen, primary or secondary C.sub.1 C.sub.7 alkyl, phenyl, haloalkyl, aminoalkyl, hydrocarbonoxy, or halohydrocarbonoxy wherein at least two carbon atoms separate the halogen and oxygen atoms; and each Q.sup.2 is independently hydrogen, halogen, primary or secondary lower alkyl, phenyl, haloalkyl, hydrocarbonoxy, or halohydrocarbonoxy wherein at least two carbon atoms separate the halogen and oxygen atoms.

46. The method of claim 45, wherein the poly(arylene ether) has an intrinsic viscosity of about 0.10 to about 0.60 deciliters per gram as measured in chloroform at 25.degree. C.

47. The method of claim 1, wherein the poly(arylene ether) is salicylate capped poly(arylene ether).

48. The method of claim 1, wherein the poly(alkenyl aromatic) contains at least 25% by weight of structural units derived from an alkenyl aromatic monomer of the formula ##STR00005## wherein R.sup.1 is hydrogen, C.sub.1 C.sub.8 alkyl, or halogen; Z.sup.1 is vinyl, halogen or C.sub.1 C.sub.8 alkyl; and p is 0 to 5.

49. The method of 1, wherein the poly(alkenyl aromatic) is atactic crystal polystyrene.

50. The method of claim 1, wherein the polymeric material comprises about 90 to about 10 percent by weight of the poly(arylene ether) and about 10 to about 90 percent by weight of the poly(alkenyl aromatic).

51. The method of claim 1, wherein the polymeric material comprises about 60w about 30 percent by weight of the poly(arylene ether) and about 40 to about 70 percent by weight of the poly(alkenyl aromatic).

52. The method of claim 1, wherein the polymeric material further comprises flame retardants, mold release agents, lubricants, antioxidants, thermal stabilizers, ultraviolet stabilizers, pigments, dyes, colorants, anti-static agents, conductive agents, or a combination comprising at least one of the foregoing additives.

53. The method of claim 1, wherein the solvent is a halogenated aromatic solvent, a halogenated aliphatic solvent, a non-halogenated aromatic solvent, a non-halogenated aliphatic solvent, or a combination comprising at least one of the foregoing solvents.

54. The method of claim 1, wherein the solvent is ortho-dichlorobenzene or toluene.

55. The method of claim 1, wherein the polymeric material is obtained in the form of a pellet powder, or flake.

56. An article comprising the polymeric material prepared by the method of claim 1, wherein the article is formed by injection molding, direct injection molding, blow molding, extrusion, sheet extrusion, film extrusion, profile extrusion, pultrusion, compression molding, thermoforming, pressure forming, hydroforming, or vacuum forming.

57. A data storage medium comprising the polymeric material prepared by the method of claim 1.

58. A method of preparing a polymeric material, comprising: combining poly(arylene ether) and poly(alkenyl aromatic) to form a mixture, wherein the poly(arylene ether) prior to combining, the poly(alkenyl aromatic) prior to combining, the mixture, or a combination of the foregoing is purified; wherein the poly(arylene ether), poly(alkenyl aromatic), and the mixture are independently in the form of a solution, melt, or solid, and when in the form of a solution, the solution is filtered through a filtration system to remove particulate impurities; and wherein the filtration system comprises a filter having a geometry that is cone, pleated, candle, stack, flat, wraparound, or a combination comprising at least one of the foregoing geometries; obtaining a polymeric material from the mixture wherein the polymeric material comprises poly(arylene ether) and poly(alkenyl aromatic), wherein the polymeric material is optionally purified; packaging, storing, or packaging and storing the polymeric material, wherein the polymeric material is substantially free of visible particulate impurities; and wherein the combining, the obtaining, the purifying, or a combination of the foregoing steps is performed under an inert atmosphere.

59. The method of claim 58, wherein the combining, the obtaining, the packaging, or a combination of the foregoing steps is performed in an environment substantially free of particulate impurities.

60. The method of claim 58, wherein the filtration system comprises a filter having a pare size of about 0.01 to about 50 micrometers.

61. The method of claim 58, wherein the filtration system comprises a sintered metal filter, a cloth filter, a fiber filter, a paper filter, a pulp filter, a metal mesh filter, a ceramic filter, or a combination of the foregoing filters.

62. The method of claim 58, wherein the poly(arylene ether), poly(alkenyl aromatic), and the mixture are independently in the form of a melt, and wherein the melt is filtered through a melt filtration system.

63. The method of claim 62, wherein the melt filtration system comprises a sintered metal filter, a metal mesh filter, a fiber metal felt filter, a ceramic filter, or a combination comprising at least one of the foregoing filters.

64. The method of claim 62, wherein the melt filtration system comprises a filter having a geometry that is cone, pleated, candle, stack, flat, wraparound, or a combination comprising at least one of the foregoing geometries.

65. The method of claim 62, wherein the melt filtration system comprises a filter having a pore size of about 0.5 to about 200 micrometers.

66. A method of preparing a polymeric material, comprising: combining poly(arylene ether) and poly(alkenyl aromatic) to form a mixture, wherein, prior to combining, the poly(arylene ether), the poly(alkenyl aromatic), or both are purified and/or the mixture is purified subsequent to combining wherein the mixture is formed by melt blending the poly(arylene ether) and poly(alkenyl aromatic) to form a melt; wherein the melt blending occurs in a twin screw counter-rotating extruder, a twin screw co-rotating extruder, a single screw extruder, a single screw reciprocating extruder, or a ring extruder; wherein the extruder further comprises a melt pump; obtaining a polymeric material from the mixture wherein the polymeric material comprises poly(arylene ether) and poly(alkenyl aromatic), wherein the polymeric material is optionally purified; packaging, storing, or packaging and storing the polymeric material, wherein the polymeric material is substantially free of visible particulate impurities.

67. The method of claim 66, wherein the extruder has a specific throughput rate of about 0.5 kg/cm.sup.3 to about 8 kg/cm.sup.3.

68. The method of claim 67, wherein the melt has a residence time in the extruder of less than or equal to 1 minute.

69. The method of claim 67, further comprising compounding the poly(arylene ether) and poly(alkenyl aromatic) prior to melt blending.

70. The method of claim 69, wherein the compounding is performed in a counterrotating conical extruder, or a counterrotating extruder.

71. The method of claim 58, wherein the mixture is formed by combining poly(arylene ether) and poly(alkenyl aromatic) to form a solution mixture comprising poly(arylene ether), poly(alkenyl aromatic), and solvent.

72. The method of claim 58, wherein the mixture is formed by combining poly(arylene ether) powder and poly(alkenyl aromatic) powder to form a powder mixture.

73. The method of claim 58, wherein the combining is performed in an environment substantially free of particulate impurities.

74. The method of claim 58, wherein the combining is performed under an inert atmosphere.

75. The method of claim 58, wherein the polymeric material is obtained from the mixture by precipitation or by the removal of solvent using a devolatilization extruder, a flash vessel, a distillation system, or a combination comprising at least one of the foregoing.

76. The method of claim 71, further comprising superheating the solution mixture; filtering the superheated mixture to form a superheated filtrate; feeding the superheated filtrate to an extruder, wherein the extruder comprises an upstream vent and a downstream vent; removing solvent from the filtrate via the upstream vent and the downstream vent; and obtaining a polymeric material.

77. The method of claim 71, further comprising filtering the solution mixture to form a filtrate; superheating the filtrate; feeding the superheated filtrate to an extruder, wherein the extruder comprises an upstream vent and a downstream vent; removing solvent from the filtrate via the upstream vent and the downstream vent; and obtaining a polymeric material.

78. The method of claim 58, wherein the poly(arylene ether) is in the form of a solution fed to a devolatilization extruder mad the poly(alkenyl aromatic) is added to the devolatilization extruder via a non-vented side feeder to form the mixture.

79. The method of claim 58, wherein the polymeric material is obtained in the form of a pellet.

80. The method of claim 58, wherein the polymeric material is obtained in an environment substantially free of particulate impurities.

81. The method of claim 58, wherein the packaging storing, or packaging and storing is performed in an environment substantially free of particulate impurities.

82. The method of claim 58, wherein the obtaining is performed under an inert atomosphere.

83. The method of claim 58, wherein the poly(arylene ether) comprises a plurality of structural units of the structure ##STR00006## wherein for each structural wilt, each Q.sup.1 is independently halogen, primary or secondary C.sub.1 C.sub.7 alkyl, phenyl, haloalkyl, aminoalkyl, hydrocarbonoxy, or halohydrocarbonoxy wherein at least two carbon atoms separate the halogen and oxygen atoms; and each Q.sup.2 is independently hydrogen, halogen, primary or secondary lower alkyl, phenyl, haloalkyl, hydrocarbonoxy, or halohydrocarbonoxy wherein at least two carbon atoms separate the halogen and oxygen atoms.

84. The method of claim 83, wherein the poly(arylene ether) has an intrinsic viscosity of about 0.10 to about 0.60 deciliters per gram as measured in chloroform at 25.degree. C.

85. The method of claim 58, wherein the poly(arylene ether) is salicylate capped poly(arylene ether).

86. The method of claim 58, wherein the poly(alkenyl aromatic) contains at least 25% by weight of structural units derived from an alkenyl aromatic monomer of the formula ##STR00007## wherein R.sup.1 is hydrogen C.sub.1 C.sub.8 alkyl, or halogen; Z.sup.1 is vinyl, halogen or C.sub.1 C.sub.8 alkyl; and p is 0 to 5.

87. The method of 58, wherein the poly(alkenyl aromatic) is atactic crystal polystyrene.

88. The method of claim 58, wherein the polymeric material comprises about 90 to about 10 percent by weight of the poly(arylene ether) and about 10 to about 90 percent by weight of the poly(alkenyl aromatic).

89. The method of claim 58, wherein the polymeric material comprises about 60 to about 30 percent by weight of the poly(arylene ether) and about 40 to about 70 percent by weight of the poly(alkenyl aromatic).

90. The method of claim 58, wherein the polymeric material further comprises flame retardants, mold release agents, lubricants, antioxidants, thermal stabilizers, ultraviolet stabilizers, pigments, dyes, colorants, anti-static agents, conductive agents, or a combination comprising at least one of the foregoing additives.

91. The method of claim 71, wherein the solvent is a halogenated aromatic solvent, a halogenated aliphatic solvent, a non-halogenated aromatic solvent, a non-halogenated aliphatic solvent, or a combination comprising at least one of the foregoing solvents.

92. The method of claim 71, wherein the solvent is ortho-dichlorobenzene or toluene.

93. The method of claim 58, wherein the polymeric material is obtained in the form of a pellet, powder, or flake.

94. An article comprising the polymeric material prepared by the method of claim 58, wherein the article is formed by injection molding, direct injection molding, blow molding, extrusion, sheet extrusion, film extrusion, profile extrusion, pultrusion, compression molding, thermoforming, pressure forming, hydroforming, or vacuum forming.

95. A data storage medium comprising the polymeric material prepared by the method of claim 58.

96. A method of preparing a polymeric material, comprising: reacting a monohydroxy aromatic compound in the presence of a catalyst, oxygen, and a solvent to form a reaction mixture comprising a poly(arylene ether), wherein the monohydroxy aromatic compound prior to reacting, the solvent prior to reacting, the reaction mixture, or a combination of the foregoing optionally purified; isolating and purifying the poly(arylene ether); combining the poly(arylene ether) with a poly(alkenyl aromatic) to form a mixture, wherein the poly(alkenyl aromatic) is purified prior to combining and/or the mixture is purified subsequent to combining; obtaining a polymeric material from the mixture, wherein the polymeric material is substantially free of visible particulate impurities and comprises poly(arylene ether) and poly(alkenyl aromatic), wherein the polymeric material is optionally purified; packaging or storing the polymeric material, wherein the packaging storing, or packaging and storing of the polymeric material is performed in an environment substantially free of particulate impurities.

97. A method of preparing a polymeric material, comprising: reacting a monohydroxy aromatic compound in the presence of a catalyst, oxygen, and a solvent to form a reaction mixture comprising a poly(phenylene ether); precipitating the poly(arylene ether) from the reaction mixture to obtain poly(phenylene ether) powder; mixing the poly(phenylene ether) powder and polystyrene in a solvent to form a mixture, wherein the amount of poly(phenylene ether) powder and polystyrene in the solvent is less then or equal to about 75 weight percent based on the total weight of poly(phenylene ether) powder, polystyrene, and solvent; superheating the mixture and filtering the superheated mixture through a filtration system comprising sintered metal filters to form a filtrate; concentrating the filtrate by removal of solvent from the filtrate to form a concentrated filtrate; introducing the concentrated filtrate to an extruder, wherein the extruder comprises en upstream vent and a downstream vent; removing solvent from the concentrated filtrate via the upstream vent and the downstream vent; and isolating a polymeric material from the concentrated filtrate; wherein the polymeric material comprises poly(phenylene ether) and polystyrene.

98. The method of claim 97, wherein the extruder operation is characterized by a ratio of a feed rate in kilograms per hour to an extruder screw speed in revolutions per minute, the ratio being about 0.045 to about 45.

99. The method of claim 97, wherein the concentrated filtrate is pressurized and introduced to the extruder via a pressure control valve.

100. The method of claim 97, wherein the extruder further comprises a side feeder, wherein the side feeder comprises a side feeder vent operated at about 750 mm of Hg or greater or at about 750 of Hg or less; and wherein the upstream vent is operated at about 750 mm of Hg or greater or about 750 mm of Hg or less, and wherein the downstream vent is operated at about 750 mm of Hg or less.

101. The method of claim 100, wherein the concentrated filtrate is introduced to the extruder via a pressure control valve located on the side feeder.

Description

BACKGROUND OF INVENTION

Optical, magnetic and magneto-optic media are primary sources of high performance storage technology that enable high storage capacity coupled with a reasonable price per megabyte of storage. Areal density, typically expressed as billions of bits per square inch of disk surface area (gigabits per square inch (Gbits/in.sup.2)), is equivalent to the linear density (bits of information per inch of track) multiplied by the track density in tracks per inch. Improved areal density has been one of the key factors in the price reduction per megabyte, and further increases in areal density continue to be demanded by the industry.

In the area of optical storage, advances focus on access time, system volume, and competitive costing. Increasing areal density is being addressed by focusing on the diffraction limits of optics (using near-field optics), investigating three dimensional storage, investigating potential holographic recording methods and other techniques.

Polymeric data storage media have been employed in areas such as compact disks (CD) and recordable or re-writable compact discs (e.g., CD-RW), and similar relatively low areal density devices, e.g. less than about 1 Gbits/in.sup.2, which are typically read-through devices requiring the employment of a good optical quality substrate having low birefringence.

Unlike the CD, storage media having high areal density capabilities, typically up to or greater than about 5 Gbits/in.sup.2, employ first surface or near field read/write techniques in order to increase the areal density. For such storage media, although the optical quality of the substrate is not relevant, the physical and mechanical properties of the substrate become increasingly important. For high areal density applications, including first surface applications, the surface quality of the storage media can affect the accuracy of the reading device, the ability to store data, and replication qualities of the substrate.

While there are materials presently available for use in data storage media, there remains a need for additional polymeric materials possessing the combined attributes necessary to satisfy the increasingly exacting requirements for data storage media applications.

SUMMARY OF INVENTION

In one embodiment a method of preparing a polymeric material comprises reacting a monohydroxy aromatic compound in the presence of a catalyst, oxygen, and a solvent to form a poly(arylene ether); combining the poly(arylene ether) with a poly(alkenyl aromatic) to form a mixture; obtaining a polymeric material from the mixture, wherein the polymeric material comprises poly(arylene ether) and poly(alkenyl aromatic); and purifying the monohydroxy aromatic compound, the solvent, the reaction mixture, the poly(arylene ether), the poly(alkenyl aromatic), the mixture, the polymeric material, or a combination of the foregoing to result in the polymeric material substantially free of visible particulate impurities.

In another embodiment, a method of preparing a polymeric material comprises combining poly(arylene ether) and poly(alkenyl aromatic) to form a mixture; obtaining a polymeric material from the mixture wherein the polymeric material comprises poly(arylene ether) and poly(alkenyl aromatic); purifying the poly(arylene ether), the poly(alkenyl aromatic), the mixture, the polymeric material, or a combination of the foregoing; and packaging, storing, or packaging and storing the polymeric material, wherein the polymeric material is substantially free of visible particulate impurities.

Other embodiments, including articles made from the polymeric material, are described below.

BRIEF DESCRIPTION OF DRAWINGS

FIG. 1 illustrates a general scheme to prepare clean polymeric material comprising poly(arylene ether) and poly(alkenyl aromatic);

FIG. 2 illustrates an embodiment to prepare poly(phenylene ether);

FIGS. 3 5 illustrate various embodiments to prepare clean polymeric material comprising poly(phenylene ether) and polystyrene; and

FIG. 6 illustrates an embodiment of a devolatilization extruder.

DETAILED DESCRIPTION

Due to the surface quality requirements of high areal density storage media, it is desirable that current data storage media are prepared from materials containing limited quantities of particulate impurities, whether inorganic or organic. Visible particulate impurities, such as gels and carbonized polymeric material (black specks), are undesirable as an aesthetic defect resulting in a consumer's perception of an inferior quality product. Particles having sizes larger than about 50 micrometers may act as stress concentrators in molded articles, thereby reducing the impact strength of these articles. Particulate impurities about 1 micrometer in size may contribute to an increase in haze which can affect the transmittance of light through or transparency of articles molded from material containing such impurities. Most importantly, particulate impurities may affect surface quality of storage media thereby affecting read accuracy, data storage, and replication.

Visible particulates or black specks and microscopic particulates are often present in poly(arylene ether) compositions as the poly(arylene ether) is subject to oxidative degradation at high temperatures. Poly(arylene ether)s tend to form carbonized black specks when processed at high shear rates and/or high temperatures. The amine compounds of catalyst systems employed in the preparation of poly(arylene ether)s may also contribute to the formation of black specks. Furthermore, when copper is used as a catalyst in the process to produce the poly(arylene ether), it is suspected that the copper contributes to the corrosion of stainless steel present in processing equipment. The corrosion results in the formation of black specks. It is theorized that iron from the stainless steel equipment is oxidized by the copper according to the formula: Cu.sup.+2+Fe.fwdarw.Fe.sup.+2+Cu. Therefore, upon isolation of a poly(arylene ether) product from the reaction mixture used to prepare the poly(arylene ether), it is preferable to remove substantially all of the catalyst and corresponding amine portion.

Furthermore, colorless organic impurities such as gels may also be formed when producing or processing poly(arylene ether)s. Gels include high molecular weight polymers or crosslinked material caused by a number of factors, for example processing the poly(arylene ether) at high heat, degradation of additives present in the poly(arylene ether) that have poor thermal stability, remaining catalyst residue after poly(arylene ether) production, and other organic or inorganic contamination present in the poly(arylene ether). Finally, it is also suspected that the methyl groups of methyl substituted poly(arylene ether)s may oxidize in the reaction solution to a carboxylic acid. The carboxylic acid in turn may couple with the catalyst used in the preparation of the poly(arylene ether) or catalyst decomposition products to form a crosslinked polyamide structure manifesting itself as a black speck or a gel.

Poly(arylene ether)s exhibit physical and mechanical properties desirable for a number of applications. By combining poly(arylene ether) and another polymer, it is possible to obtain a material possessing qualities of each polymer. A preferred combination is a composite of poly(arylene ether) and poly(alkenyl aromatic). Any known method of blending or combining poly(arylene ether) and another polymer may be used to form a composite material. As the poly(arylene ether) is combined with other polymeric material, black specks, gels, and other impurities may be formed or collected during the process to form the composite. Accordingly, the composite may be processed to remove particulate impurities present in the starting components or impurities that form during the combining process. Alternatively, if the composite is prepared from clean starting components, care can then be taken not to introduce impurities into clean composite through processing or handling. Finally, conditions of isolating, collecting, and storing clean composite polymeric materials are preferably controlled to minimize the contamination of the composite from impurities from the surroundings.

As used herein, the term an environment substantially free of particulate impurities is defined as an environment the meets or exceeds ISO 14644-1 class rating of 10,000. A clean room rating of 10,000 is equivalent to the maximum number of particles (10,000) having a size greater than or equal to 0.5 micrometer per cubic foot.

As used herein, the term substantially free of visible particulate impurities means that a ten gram sample of a polymeric material dissolved in fifty milliliters of chloroform (CHCl.sub.3) exhibits fewer than 5 visible specks when viewed in a light box. Particles visible to the naked eye are typically those greater than 40 micrometers in diameter.

As used herein, the term substantially free of particulate impurities greater than about 15 micrometers means that of a forty gram sample of polymeric material dissolved in 400 milliliters of CHCl.sub.3, the number of particulates per gram having a size of about 15 micrometers is less than 50, as measured by a Pacific Instruments ABS2 analyzer based on the average of five samples of twenty milliliter quantities of the dissolved polymeric material that is allowed to flow through the analyzer at a flow rate of one milliliter per minute (plus or minus five percent).

In the preparation of a polymeric material substantially free of particulate impurities, a number of points along the process chain to prepare the polymeric material may be controlled, from the purity of the starting materials to the type of packaging used to contain the final, clean polymeric material to prevent further contamination. A wide range of techniques may be used to prepare clean polymeric material such as filtration methods, temperature control, use of inert atmospheres, use of clean rooms, special packaging and storage methods, and the like may be used alone or in combination to provide a clean composite.

FIG. 1 illustrates a general schematic for the preparation of a clean polymeric material comprising poly(arylene ether) (PAE) and poly(alkenyl aromatic) (PAA). The individual components of poly(arylene ether) (10) and poly(alkenyl aromatic) (20) may be in any form, such as a powder, flake, pellet, in solution, as a melt, and the like. In an exemplary embodiment, the poly(arylene ether) is in solution and the poly(alkenyl aromatic) is in the form of a pellet added to the solution. In another exemplary embodiment, the poly(arylene ether) is in the form of a powder and the poly(alkenyl aromatic) is in the form of a pellet. Any combinations of forms are contemplated herein. In addition to the component form, the components, independently, may or may not have been purified prior to their being combined. Various purification methods will be described in more detail herein.

Combining (30) the two components may be effected by any methods known in the art to result in an intimate mixture of two polymeric components. Suitable methods include melt compounding, solution blending, powder mixing, and the like to result in a mixture of the components (40) in a variety of formats. Such formats of the mixture may include melts (90), solutions (80), and solid powder mixtures. The mixture may optionally be purified by filtration of the melt or solution. The polymeric material comprising poly(arylene ether) and poly(alkenyl aromatic) may be isolated and/or collected without further purification of the mixture.

The polymeric material (70) may be isolated (50) from the mixture and/or collected (60) using various techniques depending upon the format of the mixture. In an exemplary embodiment, the polymeric material may be isolated by precipitation from a solution of the mixture and collected. Alternatively, if the mixture is in the form of a melt, the melt may be extruded and collected as pellets comprising the polymeric material. The isolated or collected form of the polymeric material (70) may include any form such as pellets, powders, flakes, and the like. A further purification step may be accomplished prior to or during the isolation or collection step. For example, a melt comprising a poly(arylene ether) and poly(alkenyl aromatic) may be melt filtered as it is extruded from an extruder.

At any number of points along the general schematic in FIG. 1, the components and/or the mixture may be purified to provide a final clean composite polymeric material. The "P" in FIG. 1 indicates locations where a purification step may occur in the process to produce a clean composite. For instance, the poly(arylene ether) and/or poly(alkenyl aromatic) may be purified prior to being combined to form a mixture. A solution mixture of poly(arylene ether) and poly(alkenyl aromatic) itself may be purified, for example by filtration, before isolation or collection of the clean polymeric material. Also contemplated are any combinations of purification steps, including multiple purification steps, that will result in a composite polymeric material substantially free of particulate impurities. All possible permutations of preparing a clean composite polymeric material are contemplated herein, including any type and number of purification steps, any form of starting components, any method of mixing, any format of mixtures, any method of isolation or collection, any form of composite, and the like.

In a process to prepare a clean polymeric material, any and all combinations of options within the general scheme of FIG. 1 are contemplated herein. For example, the poly(arylene ether) may be in the form of a solution that has been filtered. The poly(alkenyl aromatic) may be in the form of a pellet added to the solution of poly(arylene ether) to form a mixture. The solvent may be removed from the mixture through a devolatilization process to result in clean polymeric material that can be pelletized under clean room conditions and stored in clean containers, such as a clean Super Sack.RTM. available from B.A.G. Corporation. Another example may include the previous example having the poly(alkenyl aromatic) in the form of a solution and the mixture of poly(arylene ether) and poly(alkenyl aromatic) is filtered prior to isolation of the polymeric material. The details of a method to prepare a clean composite polymeric material will now be discussed.

In one embodiment, the starting components of poly(arylene ether) and poly(alkenyl aromatic) used to prepare the polymeric material are independently prepared and/or purified to be substantially free of particula