TH70853B - Polyester polymers in the molten phase with a high intrinsic viscosity that provide acceptable acetaldehyde production rates. - Google Patents

Abstract

------ 09/07/2018 ------ (OCR) page 1 of the number 1 page summary of invention The process for producing solid polyester polymers containing a) the constituents of polyester polymers in a molten state with Components of a condensed polymerization catalyst containing antimony constituents b) continuity in condensed polymerization of components. Polyester polymers in a molten state to obtain It.v. values from 0.68 dpi / g or more and c) after It.v. of 0.68 dpi / g or more. Add stabilizer and / or antimony catalyst moderator. Of molten polymers In particular, phosphorus-containing compounds and d) after It.v. with a value of 0.68 dpi l / g or more, the molten solids form a polyester polymer particle with no digestants. Dissolves acital dehike intra in another form After the solidification of polyester from Polymerization in the molten phase e) The content of the acitaldehyde in solid particles was reduced to 10 ppm or less in the solid state by It.v. of the particle. No more than 0.03 deci l / g Particles with an acitaldehyde (AA) generation rate of 20 ppm or less, depending on their exposure. Molten after solidification, followed by production in the molten cycle and the degree of Free acitaldehyde that is reduced after processing in the molten phase to 10 ppm or less is taken in the blaze of the melting process to form a molding material, such as the preform of a vial with a substance level. Acceptable solids of acital khiheke ------------ A process for producing solid polyester polymer particles containing (a) polyester polymer components in The melted state available Components of condensed polymerization catalysts containing antimony constituents (b) continuity in condensed polymerization of components. Polyester polymers in molten state to obtain It.V. with values from 0.68 dL / g or more and (c) after It.V. with a value of 0.68 dL / g or more. Stabilizes and / or moderators of antimony agitators Of molten polymers In particular, phosphorus-containing compounds, and (d) after It.V. with a value of 0.68 dL / g or more, the molten solids form polyester polymer particles, which do not contain amorphous degradation. Organic citaldehyde in another look. After the solidification of polyester from Polymerization process In the molten phase (e), the amount of acetaldehyde residue in solid particles was reduced to a level of 10 ppm or less in the solid state, where It.V. of No particles added more than 0.03 dl / g Particles with an AA formation rate (acetaldehyde) of 20 ppm or less, depending on It was melted after solidification followed by production in the molten phase and the degree of free AA decreased after the molten phase was produced to 10 ppm or less by being taken in the molten zone to form the material. Forming like The preform of the bottle contains Acceptable level of acetaldehyde residue.

Claims (6)

Disclaimer (all) which will not appear on the advertisement page: EDIT 23/07/2019 No disclaimers ---------- ------ 09/07 / 2018-- ---- (OCR) Page 1 of 4 pages. Disclaimer 1. Methods for producing solid polymeric particles, including: a) polycondensing, polyester polymer composition. That melted in the existence of The polycondensation catalyst composition consists of an antimony-containing type. B) The polycondensation of the molten polyester composition to obtain an I tv at 0.68 dl / g. And c) after reaching I tv at 0.68 dL / g or more, adding stabilizer and / or moderator of antimony catalyst to the molten polymer and d) after To I tv at 0.68 dL / g or more, moltenization Solids to particles are solid polyester polymers without organic acetaldehyde degradation, where the method for determining I t. V. Is expressed in units. Deciliter / gram The inherent viscosity was calculated from the inherent viscosity. The flanges were measured at 25? ใน in 60% thenel and 1,1,2,2-tetrachloroethane by 40% by weight. Claim 1 where solid particles have an acetylkehyde production rate of 20 ppm or less 3. Method of claim 2 where solid particles have an acetaldehyde rate of 16 ppm. 4. Method of claim 1 where the polycondensing catalyst consists of an antimony type 5. Method of claim 1 where the amount of antimony in the molten polymer has Range from 150 ppm to 300 ppm 6. Claim Method 1 whereby agile titanium-containing polyconscious solvent. 7. Clause method. 1 where polycondensation is continued up to I t. V. At least 0.70 dL / g. 8. Method of claim. 1 where polycondensation is continued up to I t. V. At least 0.72 dL / g 9. Method of claim. 1 where the polycondensation is continued up to I t. V. At least 0.80 dL / g 1 0. Clause 1 method where stabilizers or retardants of The catalyst contains phosphorus compounds that have been added to make the weight generation. Molecular molecules of molten polymers are actually formed. Page 2 of the number 4. Page 1 1. Method of claim 10, whereby stabilizers or retardants of The catalyst consists of an acidic phosphorus compound 1 2. Method of claim 11 where the acidic phosphorus compound contains phosphoric acid; Pyrophosphoric acid; Polyphosphoric acid or mono or di-ester acid Phos, father Rick with ethylene glycol; Diethylene glycol; Triethylene glycol or 2-ethyl-! - hexanol; Phosphate ester acidic pyrophosphoric acid with ethylene glycol; Diethylene glycol, triethylene glycol or 2-ethyl hexanol; Phosphate ester acidic of polyphosphoric acid. With ethylene glycol, diethylene glycol, triethylene glycol or 2-ethyl hexanol or mixtures of each substance 1 3. Method of holding Rights 11 Where stabilizers or retarders of The catalyst is composed of phosphoric acid 1 4. Method of claim 1 where the catalyst retardant is composed of The phosphorus compounds contained in the stoichiometry ratio of phosphorus to antimony were at least 0.5: 1 1 1. 1 6. Method of claim 14 where the stoichiometry ratio ranged from 1: 1 to 2.5: 1 1 7. Method of claim 1 where the organic pigment is added to the molten polymer 1 8. The method of claim 1 where the color value L * The value of the crystalline particle is at least 73, where the method for determining the color L * is measured on the side of the flask 1 9. The claim 1 method consists of a valid preform. Derived from such particles, Pornformang has a L * value of at least 70, where the method for determining L * is measured on the side of the vial 2 0. Method of claim 1 where the color b * Of crystalline particles is at least 3.0 or less and L * is 76 or greater, where the method for determining the color b * and L * is measured on the side of the bottle 2 1. Method of Claim 1, which further includes e) Reduction of the amount of acetaldehyde deposited in solid particles to a level of 10 ppm or less in the solid state without increasing the I tv of the particles. T Low 0.03 dcs l / g 2 2. Method of claim 21 wherein the level of residual acitaldehyde in solid particles is treated. Decrease in solid state to 5 ppm or less 2. 3. Method of claim 21 wherein residual acitaldehyde in solid particles is reduced in Solid state up to 2 ppm or less, page 3 of number 4, page 2 4. Method of claim 21 where the residual acetaldehyde of the ball particles was reduced by The particles are introduced into the container to form a particle bed inside the reaction vessel. And touch the bed with the current The gas flow rate was not greater than 70.79 h 3 s \ '1 (standard conditions) per 0.45359237 kg of particles per hour (0.15 SCFM per lb. of particles per hour) and finished particle extraction. The end of the reaction vessel with a reduced residual acetaldehyde content 2 5. Method of claim 24 where the gas was introduced at a temperature less than 7 (7? C 2 6. Method Of claim 24, where the ingested gas is air 2 7. Method of claim 21 where, where the level of the residual acetaldehyde in the particles before The reduction procedure is at a value of at least 10 ppm. 2. 8. Methods for the manufacture of composite items with a method for the production of poly particles. Solid polymers according to claim 1 and include (i) imports of solid polymer polymers with I tv with a value of at least 0.68 dL / g obtained in the polymers. In the molten phase, the crystallinity level is at least 20%, the residual acetaldehyde level of 10 ppm or less, the residue of the polycondensate catalyst composition. The steep slopes consisted of Antimony The oxidation rate of acetaldehyde is less than 20 ppm, and there is no hydrolysis of acetaldehyde in it. In the zone where the melting process is performed And melting particles to form Molten polyester compositions; and (ii) the creation of a fabrication consisting of sheets, ropes, stressed fibers or parts formed from the molten polymer composition, whereby methods for determining I tv is shown in units. Deciliter / gram Calculated from inherent viscosity measured at 25? C in 60% phenol and 1,1,2,2-tetrachloroethane 40% by weight 2 9. Method of claim 28 where item is the preform of vial 3 0. Method of claim 29 where vial preform contains \ 'residual acetaldehyde content of 10 ppm or less. Over 3. 1. Method of claim 30 where the flask blessing contains 8 ppm or less of the acetaldehyde residue 3. 2. Method of claim 28 whereby particles are flown in. In the zone in which the process is performed Molten, not polymerized at solid state 3 3. Method of claim 28, composed of 4 pages of 4 pages (i) Imports of particles with I tv of at least 0.72. The deciliter / g was obtained in the crystallization process in the molten phase, the crystallinity level was at least 30%, the degree of azidaldehyde at 10 ppm or less, the residual residual. Of the polycondensation catalyst component, which includes Antimony The rate of acetaldehyde is less than 20 ppm, no degradation of acetaldehyde, organic. Stabilizer / stabilizer of phosphorus-containing catalysts and which are not polymerized at solid state. Go into the zone where the melting process is performed. And melting particles to form Molten polyester polymer composition and (ii) the construction of the bottle form from Molten polymer composition 3 4. Method of claim 33, wherein the residual acetaldehyde content of the impregnated particles In zones where the melting process is 7 ppm or less 3 5. Method of claim 33 where the retarder / stabilizer of the catalytic The phosphorus-containing reaction was obtained from the acidic phosphorus compound 3 6. Method of claim 33 where the vial preform contained 10 ppm or less acetaldehyde residue 3 7. Method Claim 33 where the vial form contains 8 ppm or less of acetaldehyde residue 3. 8. Method of claim 28 where the particles are free of acetal degradation. Formaldehyde ------------ 1. Method for the production of solid polymer particles including a) polycondensing, molten polyester composition. In the existence of A polycondensation catalyst composition consisting of an antimony type b) a continuous polycondensation of the molten polyester composition to obtain I tV at 0.68 dl / g. And c) after reaching I tV of 0.68 dL / g or more, adding stabilizer and / or moderator of antimony catalysts to the molten polymer and d). After reaching I tV of 0.68 dL / g or more, the moltenization was Solid to solid polyester polymer particles which do not contain organic acetaldehyde degradation, where the method for determining I tV is disclosed in the lecture 2. Process according to claim 1 where the particle The solids had an AA formation rate of 20 ppm or less. 3. Process according to claim 2, where solid particles had an AA formation rate of 16 ppm or less. 4. Process according to claim 1, whereby the poly catalytic Merise Sun Pattern Condensation consists of antimony compounds 5. Process according to claim 1 where the amount of antimony in the molten polymer is from 150 ppm to 300 ppm 6. Process according to claim 1 where the molten substance in the reaction Condensed polymerization without titanium reactant 7. Process according to claim 1, whereby the condensed polymerization The fur was at least 0.70 dL / g of I t.V. 8. Process according to claim 1 where the condensed polymerization The coat had a I t.V. at least 0.72 dL / g 9. Process according to claim 1 where the condensed polymerization The fur has at least an I t.V. 0.76 dL / g 1 0. Process according to claim 1 where the condensed polymerization The transport has an I t.V. at least 0.80 dL / g 1 1. Process according to claim 1, where the stabilizer is the catalyst. Or a catalyst retarder containing phosphorus compounds added to There is a large amount to complete the molecular weight formation of the molten polymer 1 2. Process according to claim 10, where catalytic stabilizers are Or the catalyst retarder contains acidic phosphorus compounds 1 3. Process according to claim 11 where acidic phosphorus compounds Contains phosphoric acid Pyrophosphoric acid Polyphosphoric acid or mono or di-ester of phosphoric acid With ethylene glycol Diethylene glycol Triethylene glycol or 2-ethyl-1-hexanol Phosphate ester acidic acid of pyrophosphoric acid with ethylene glycol. Diethylene glycol Triethylene glycol or or 2-ethyl hexanol Phosphate ester acidic polyphosphoric acid with ethylene glycol. Diethylene glycol Triethylene glycol or or 2-ethyl hexanol Or a mixture of each substance 1 4. Act in accordance with claim 12 where stabilizers are catalysts Or the catalyst stabilizer contains phosphoric acid 1 5. The act of claim 1, whereby the stabilizer that is the catalyst Or retarders of catalysts containing phosphorus compounds contained in The stoichiometric ratio of phosphorus to antimony was at least 0.5: 1 1 6. Process according to claim 14 where the stoichiometric ratio was at least 0.7: 1 1 7. Claim process 14 where The stoichiometric ratios ranged from 1: 1 to 2.5: 1 1 8. Process by claim 1 where at least part of the interaction Condensed polymerization was formed at temperatures greater than 280 ํ 1 9. Process according to claim 1 wherein the compound color enhancer is The organic matter is added to the molten polymer 2 0. Process according to claim 1 where the color L * of the crystalline particle is at least 73 2 1. The process according to claim 1 consists of a preform. Obtained from such particles Or the said preform has a L * value of at least 70 2. 2. Process according to claim 1 where the color b * of the crystalline particle is at least 3.0 or less and L * is 76 or greater 2. 3. Process according to claim 1 with additional processes e) The amount of acetaldehyde residue in the solid particles was reduced to a level of 10 ppm or less in the solid state, with the I tV of the particles not added. Exceeding 0.03 dl / g 2 4. Process according to claim 22 where the level of acetaldehyde residue in the particle The solids were reduced to a solid state to 5 ppm or less 2. 5. Process according to claim 23, where the degree of acetaldehyde residue in the particles was reduced to 5 ppm or less. The solids were reduced to a solid state to 2 ppm or less 2. 6. Process according to claim 22, where the degree of acetaldehyde residue in the particle It is lowered in the reaction tank to form a path of the particles inside the reaction tank. And experience the line of The steam particles of the gas that begin to enter the gas flow rate are not greater than 0.15 SCFM per pound of particles per hour. And by pulling the last particle, the reaction tank containing the amount of substance Reduced acetaldehyde residue 2 7. Process according to claim 25, where the gas is introduced at less than 70 C 2 8. The process according to claim 25, wherein the imported gas is Air 2 9. Process according to claim 22, where, where the level of the acetaldehyde residue in Particles prior to the reduction step mentioned at a value of at least 10 ppm 3 0. Process according to claim 27 where, where the acetaldehyde residue level in Particles prior to the reduction process mentioned at a value of at least 20 ppm 3 1. Process according to claim 1, where the generation rate reduction process is reduced. The solid particle acetaldehyde is at least 10% or more. 3. 2. Process according to claim 29, where the reduction of the generation rate is reduced. The acetaldehyde of solid particles is at least 30% or more. 3. Process according to claim 30, where the reduction of the generation rate is reduced. The acetaldehyde of solid particles is at least 40% or more. 3. 4. Production process for forming agents containing (i) the feeding of solid polyester polymers with I tV with a certain value. At least 0.68 dL / g obtained from the process Polymerization in the molten phase The crystallinity level is not less than 20%, the level of acetaldehyde residue is 10 ppm or less than the residue of the catalyst component of the reaction. Polymerization that contains Antimony species, a reduction of at least 20% or 30% or more of acetaldehyde incidence, or an acetaldehyde incidence rate of 295 ํ for 5. The minute is more than 18 ppm and does not contain organic acetaldehyde degradation. In the zone of the annealing process And melting the particles causes Molten polyester and (ii) forming a sheet, stand, or fiber, or molded part of the polyester polymer composition that Melting 3 5. Process according to claim 34 where the molding material mentioned is the vial preform 3 6. Process according to claim 35 where the vial preform contains acetaldehyde residue. 10 ppm or less3 7. Process according to claim 36, where the vial preform contains acetaldehyde residue in the amount of 8 ppm or less3 8. Process according to claim 34 by Where particles are fed into the zone of The melting process was not polymerized at the solid state. 3. 9. Process according to claim 34 consisted of (i) the feeding of I t.V. particles with a value of at least 0.72 dL / g obtained by the process. Polymerization in the molten phase The crystallinity level is not lower than 30%, the degree of acetaldehyde residue 10 ppm or less than the residue of the polymer reaction catalyst component. Raises containing antimony (antimaony species) acetaldehyde rate less than 20 ppm, no organic acetaldehyde degradation agent. Catalyst / stabilizer containing phosphorus and no solid state polymerization. In the zone of the annealing process And the melting of the particles causes Molten polyester polymers and (ii) vial preform creation. From the molten polymer component 4 0. Process according to claim 39, where the acetaldehyde residue in the particles at Enter into the melting zone with a value of 7 ppm or less 4. 1. Process according to claim 39, where the catalyst / impregnation moderator has The phosphorus-containing stability is derived from the acidic phosphorus compound 4 2. Process according to claim 39, where the vial preform contains acetaldehyde residue in the amount of 10 ppm or less 4. 3. Process According to claim 39, where the vial preform contains acetaldehyde residue in the amount of 8 ppm or less 4 4. Process according to claim 34, where the particles do not contain any metal catalysts except Sb. 4 5. Process according to claim 34, where the particles do not contain any acetaldehyde degradation 4 6. Process according to claim 34 where the particles have a minimum I tV of 0.76 dl / g 4 7. Process according to claim 46, where the particles have a minimum I tV of 0.8 dl / g 4 8. The process of forming particles forming materials containing (i) the feeding of solid polyester polymers containing I tV at At least 0.68 dL / g obtained from the polymerization process. Sesun in the Molten Time The crystallinity level was not lower than 25%, the degree of acetaldehyde residue 10 ppm or less than the residue of the catalyst component of the reaction. Polymersuns containing antimony species do not contain organic acetaldehyde degradation. In the zone of the annealing process And the melting of the particles causes Molten polyester polymers and (ii) forming a sheet, strand or fiber, or a part formed from the polymer composition of polyester. Melted with the forming material having acetaldehyde residue less than 20 ppm 4 9. Process according to claim 48 where the molding material consists of a preform of a vial or a molded bottle with a blow molding. Stretch pull With the amount of acetaldehyde residue 14 ppm or less 5 0. Process according to claim 49 where the forming material has the acetaldehyde residue of 10 ppm or less 5. 1. Process according to claim 48, where the forming material is the bottle preform 5 2. Process according to claim 48, wherein the sector fed into the zone of Solid state non-polymerization process 5 3. Process according to claim 48 (i) Feeding polymer particles containing I t.V. with a value of at least 0.72 dL / g. Obtained from the process Polymerization in the molten phase The crystallinity level is not lower than 30%, the degree of acetaldehyde residue 10 ppm or less than the residue of the catalyst component of the reaction containing antimony species. Produces less than 20 ppm of acetaldehyde, does not contain organic acetaldehyde degradation. Contains non-polymerized phosphorus in the solid state in the zone. Of the annealing process And the melting of the region creates a polymeric component. Molten polystyrene and (ii) the formation of vial preforms. From the components of Molten polymer 5 4. Process according to claim 53 where the vial preform contains residue. Acetaldehyde 10 ppm or less 5. Final polyester polymer particles with I t.V. of at least 0.68 dl / g. Obtained from the polymerization process In the molten cycle The crystallinity level is not less than 20% of the antimony atom of phosphorus. The acetaldehyde generation rate is less than 20 ppm, no organic acetaldehyde degradation agent, and no solid state polymerization 5 6. The final particles of claim 55 by Where particles have a level of acetaldehyde residue of 10 ppm or less 5. 7. The final particle of claim 55, where the last particle mentioned consists of Bald Particulate 5. 8. Final Particle of claim 57, where Babald particle is contained in the carrier 5 9. Final Particle of Proposition 58, where the Babald Particle occupies a minimum volume of 10. Cubic meter 6 0. The final particle of claim 58 where the particle has an I tV value of at least 0.72 dL / g. Obtained from the polymerization process in the molten phase And level of The crystal is not less than 30% 6 1. The last particle of claim 55 where the particle has a color value b * of 3 or less and the color L * is 70 or greater 6. 2. The last particle of claim 55. Claim 55 where L * is 76 or greater 6. 3. The final particle of claim 55, where the quantity of antimony atoms is from 150 ppm to 300ppm 64. Such substances are free. Reactive titanium 6 5. The final particle of claim 55, where the particle has an I t.V. obtained from production. In the molten phase with a value of at least 0.70 dl / g 6 6. The final particle of claim 55 where the phosphorus atom is obtained from Acidic phosphorus compound 6 7. The final particle of claim 66 whereby the phosphorus atom is obtained from the phosphoric acid 6 8. The final particle of claim 66 where Moles of an atom The phosphorus per antimony atom was at least 1: 1. 6. 9. The final particle of claim 55, where the acetaldehyde residue level was 7 ppm or less, 7. The final particle. Of claim 55 with I tV of at least 0.68 dL / g. Obtained from the polymerization process In the molten cycle The crystallinity level is not less than 20% of the antimony atom of phosphorus. The acetaldehyde generation rate is less than 20 ppm, no organic acetaldehyde degradation agent, and no solid state polymerization.7 1. The final particles of claim 70 by Where the particle has an acetaldehyde residue level of 10 ppm or less 7. 2. The final particle of claim 70, where the final particle mentioned consists of The bald region 7 3. The final particle of claim 70 where the babald particle is placed in the transport container 7 4. The final particle of claim 73 where the babald particle occupies a volume of space. At least 10 cubic meters 7 5. The final particle of claim 73 where the particle has an I tV value of at least 0.72 dL / g. The crystallinity of at least 30% 7 6. The final particle of claim 70, where the particle has a color b * of 3 or less and the color L * is 76 or greater 7 7 The last particle of claim 70 where the color L * is 73 or greater 7. 8. The final particle of claim 70, where the amount of antimony atoms is from 150 ppm to 300 ppm 7 9. Final particle Extreme of claim 70, where the particles are free of substances Reactive titanium 8 0. The final particle of claim 70, where the particle has an I t.V. obtained from production. In the molten phase with a value of at least 0.70 dL / g 8 1. The final particle of claim 70, where the phosphorus atom is obtained from Acidic phosphorus compound 8 2. The final particle of claim 81 where the phosphorus atom is derived from the phosphoric acid 8 3. The final particle of claim 81 where Moles of an atom The phosphorus per antimony atom was at least 1: 1. 8 4. The final particle of claim 70, where the acetaldehyde level of residue was 7 ppm or less 8. 5. The process of assembly. Accompanied by (i) conduction current flows into the zone of melting containing Phosphorus compounds and currents containing solid polyester particles with I t.V. of at least 0.72 dL / g. Obtained from the polymerization process In the molten cycle The crystallinity level was not less than 20%, the level of acetaldehyde residue 10 ppm or less than the residue of the catalyst component obtained from the reaction. Condensed polymerization contains Antimony secies do not contain organic acetaldehyde degradation. Does not polymerize in solid state. And (ii) the vial preform from molten polymer components. The bottle has a level of residue. Citaldehyde equal to 10 ppm or less 8. 7. Process according to claim 85 where the vial preform has a residue level. Citaldehyde equal to 8 ppm or less 8. 8. Process consisting of (i) conduction flow into the zone of melting containing Phosphorus compounds and currents containing solid polyester particles with I t.V. of at least 0.72 dL / g. Obtained from the polymerization process In the molten cycle The crystallinity level was not less than 20%, the level of acetaldehyde residue 10 ppm or less than the residue of the catalyst component obtained from the reaction. Condensed polymerization contains Antimony secies do not contain organic acetaldehyde degradation and do not polymerize in the solid state. And (ii) vial preforms from molten polymer components. 8 9. Process according to claim 85 where the preforms are formed. The bottle has a level of residue. Citaldehyde equal to 10 ppm or less 9 0. Process according to claim 85 where the vial preform has a residue level. Citaldehyde is 8 ppm or less than 9. 1. A process consisting of (i) conducting a flowing current into a zone of melting consisting of Phosphorus compounds and currents containing solid polyester particles with I t.V. of at least 0.72 dL / g. The crystallinity level is not less than 30%, the degree of acetaldehyde residue 10 ppm or less than the residue of the catalyst component obtained from the polymer reaction. Condensed rice sun contains Antimony secies do not contain organic acetaldehyde degradation. Does not polymerize in solid state. And particle melting to form molten polyester polymer components; and (ii) vial preforms from molten polymer components 9. 2. Process according to claim 91, where the vial preform has residue levels. Acetondehyde is 10 ppm or less than 9. 3. Process according to claim 91, where the vial preforms have residue levels. Acetangehyde is 8 ppm or less than 9. 4. A process consisting of (i) conducting a flowing current into a zone of melting consisting of Phosphorus compounds and currents containing solid polyester particles with I t.V. of at least 0.72 dL / g. Obtained from the polymerization process In the molten cycle The crystallinity level was not less than 20%, the level of acetaldehyde residue 10 ppm or less than the residue of the catalyst component obtained from the polymer reaction. Condensed rice sun contains Antimony secies do not contain organic acetaldehyde degradation. Does not polymerize in solid state. And (ii) vial preforms from molten polymer components. 9. 5. Process according to claim 94, where the vial preform has residue levels. Acetaldehyde is 10 ppm or less than 9. 6. Process according to claim 94, where the vial preforms have residue levels. Acetaldehyde is 8 ppm or less.