United States Environmental Protection Agency Industrial Environmental Research Laboratory Research Triangle Park NC 27711 Research and Development EPA-600/S2-80-209 July 1981 Project Summary Textile Warp Size Reclamation Using Thermal Precipitation W. S. Perkins, R. P. Walker, and L J. Hirth The report describes a novel method for reclaiming size based on precipita- tion of the size material by heating the desize washwater. The method uses hydroxypropyl cellulose (HPC) or hydroxypropyl methylcellulose (HPMC) which are soluble in cool water but insoluble in warm water. Reclaiming size would eliminate most of the BOD typically resulting from sizing and desizing. Since maximum system temperature with HPC is about 50°C, compared to 95°C for a conventional system, considerable energy is conserved. Strength and elongation of yarns sized with virgin HPC and with reclaimed HPC were not significantly different from those of yarns sized with the conventional size, polyvinyl alcohol (PVA), at similar add-on levels. Abrasion resistance of yarns sized with HPC was lower than that of yarns sized with PVA at similar add-on levels. Weaving of HPC-sized 50/50 polyester/cotton yarns in the laboratory was successful. In produc- tion weaving of percale sheeting, HPC accumulated on the shuttle caused poor weaving efficiency. The capital investment for reclaiming HPC using thermal precipitation is much lower than for reclaiming PVA using ultra- filtration. Operating costs for recover- ing HPC by thermal precipitation and for recovering PVA by ultrafiltration represent a savings over conventional sizing and desizing without reclaiming size. This Project Summary was develop- ed by EPA's Industrial Environmental Research Laboratory, Research Tri- angle Park, NC, to announce key find- ings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back). Introduction Virtually all textile yarns which are to be woven into the lengthwise direction (warp) in a fabric are coated with a protective material, called size, during the slashing process. The purpose of this size is to improve the performance of the yarn in the weaving process. In most cases the size material is removed from the woven fabric in the finishing plant. Published data indicate that 45% to 75% of the BOD load from a woven fabrics finishing plant results from this warp size which is removed from the fabric. A process to recover and recycle the warp size used in textile processes has the potential to lower the BOD and COD of textile finishing plant effluents more than any other single change in textile processing. Such a process has been the objective of much development work in recent years. The following are specific examples of approaches to size recovery and recycle: (1) Recovery of carboxymethyl cellu- lose by chemical precipitation from the desize wastewater has been studied but not commercial- ized. (2) Recovery of polyvinyl (PVA) by chemical precipitation has also been subject to investigation. ------- (3) Studies of recovery of warp size via solvent sizing and desizing have been made. A solvent sizing and solvent desizing system has been developed by two Italian machinery companies. (4) Recovery of polyvinyl alcohol (PVA)by ultrafiltration of the de- size wastewater has been subject to considerable development, and commercial processes have now been operating for several years. The tremendous interest of the U.S. textile industry in recycle of warp size is understandable since the economic outlook for such a development is as favorable as are the environmental considerations. The size material adds no value to the product (fabric), since it is normally removed in desizing and disposed of in a wastewater treatment facility. Therefore, the size material it- self adds to the cost of fabric production. A process for recovery and reuse of size material may prove profitable to the textile mill through reduced fabric production cost if a high degree of recovery of the size material is obtained. Therefore, a size reclamation process offers the potential for a modification from which the mill may realize a direct return on investment. This approach should be considerably more attractive to management than the prospect of construction of additional treatment facilities which may become obsolete as the 1983 Effluent Guidelines are imple- mented. Further, size recycling will allow the industry room for expansion and growth without great capital invest- ment for wastewater treatment facilities since recovery and recycle of warp sizes will allow increases in production without large increases in effluent loads. The size reclamation system which is the subject of this report uses a size material selected from a group of polymers having the unusual property of being soluble in water at room temperature but insoluble at some higher temperature. Hydroxypropyl- cellulose (HPC) is such a polymer. HPC is soluble in water at temperatures below 43°C (109°F) but becomes almost completely insoluble in water at temperatures above 45°C (113°F). Hydroxypropylmethylcellulose (HPMC) also exhibits this "reverse solubility" property but at a higher precipitation temperature than is required for HPC. Most of the work done in this project was concerned with HPC rather than HPMC and except where otherwise specified the discussions pertain to HPC rather than HPMC. Precipitation of HPC or HPMC from desize wastewater can be accomplished by heating the desize wastewater. A schematic diagram of the desizing and recovery system is shown in Figure 1. Application of the size material to the warp yarn in slashing and washing of the size material from the woven fabric in desizing is done with water at a temperature {lower than 43°C. The desize washwater containing HPC at a concentration of 0.5 to 1.5% by weight is filtered to remove insoluble impurities and heated to above 45°C to precipitate the HPC. The precipitated HPC is then separated from most of the water. The HPC redissolves when cooled to yield a solution concentrated enough to reuse in slashing. The recovered water can be cooled to below 43°C and reused in the desize washer. This report describes both laboratory and in-plant work concerned with the development of a process utilizing HPC as the warp size with the objective of reclaiming the HPC using the thermal precipitation principle. Work was per- formed in the following areas: Fabric in (1) Utility and performance of HPC as\ a textile warp size. (2) Design and operation of a thermal precipitation size reclamation system. (3) Economics of size reclamation by thermal precipitation. Conclusions Hydroxypropylcellulose (HPC) is soluble in water at room temperature but becomes virtually insoluble in water at a temperature greater than about 43°C. HPC can be precipitated from water by heating the water to above the precipitation temperature. The HPC can then be separated from most of the water by settling, filtration, or centrifu- gation. Therefore, a dilute solution such as is obtainable in a conventional desize washer can be concentrated to the extent required for use of the material in a conventional slashing process. More than 90% of the HPC in a 1.0% solution of desize washwater can be obtained at up to 25% concentration in the re- claimed solution using a recovery system based on settling of the HPC in warm water. Hydroxypropylmethylcel-| lulose (HPMC) also exhibitsthistherman Fabric out Desize Washwaste 11.0% size) Desize water at 40°C Reclaimed Water Filter for fiber and \insoluble impurities] Fresh Water \fapprox. 10% of total) Cooling of reclaimed} water Heats to 45°C Water/ Size Separator Reclaimed Water Concentrated size to slasher (8 - 10%) Figure 1. Schematic of desize and recovery system. ------- precipitation phenomenon, but at about 65°C. Textile yarns consisting of 100% cotton or 50% polyester and 50% cotton can be sized with HPC or HPMC. The physical properties of yarns sized with HPC or HPMC are adequate for the yarns to be woven into fabric. The tensile strength of yarn sized with HPC is appreciably higher than that of un- sized yarn and is not significantly differ- ent from the tensile strength of yarns sized with the conventional size, polyvinyl alcohol (PVA), at the same size add-on. The abrasion resistence of yarns sized with HPC is higher than that of unsized yarns. The magnitude of the improvement in abrasion resistance depends on the size add-on level. The abrasion resistance of yarns sized with PVA is higher than that of yarns sized with HPC at the same add-on level. Clear flexible films are formed upon evaporation of the water from aqueous solutions of HPC. Clear films are pro- duced even when the temperature is higher than that which causes the HPC to precipitate from water. The strength of HPC films is similar to that of conven- tional sizes such as starch and carboxy- methylcellulose. The elongation of films of HPC is intermediate between that of conventional size, starch, and PVA. Yarns sized with HPC can be woven into fabric. On 50-inch wide looms weaving at 215 filling insertions per minute, the contact of the shuttle with the yarn results in an accumulation of HPC on the shuttle. The accumulation of HPC on the shuttle is undesirable be- cause it eventually interferes with the passage of the shuttle into the yarn shed causing excessive yarn breaks near the sides of the loom. The accumulated size material may also be periodically stripped away from the shuttle and become woven into the fabric causing a fabric defect. This accumulation of HPC on the shuttle does not occur to a dis- ruptive degree on 24-inch looms weav- ing at 175 filling insertions per minute. Whether this accumulation of size on the shuttle also occurs with HPMC on 50-inch looms is not known, but the accumulation of HPMC does not occur to a disruptive degree on 24-inch looms weaving at 175 filling insertions per minute. HPC reclaimed from woven fabric has tensile strength and elongation not appreciably different from that of virgin HPC. Yarns sized with reclaimed HPC have abrasion resistance not appreci- ably different from that of similar yarns sized with virgin HPC. Pure HPC may be more flexible than is desirable in a size material. HPC softens dramatically at high relative humidity, and its effec- tiveness as a warp size deteriorates. Fabrics containing HPC can be rapidly desized using room-temperature water. The rate of removal of HPC from a poly- ester/cotton fabric is as rapid at 25°C (77°F) as the removal of PVA at 95°C (203°F). Water used for desizing and subsequently separated from the HPC in the recovery system is suitable for reuse in desizing. The content of impurities in desize washwater increases with each reuse cycle. A steady state level of impurities is reached if a fraction of the desize washwater is discharged at each cycle. Thermally precipitated HPC particles have a negative zeta potential in water. Consequently, coagulation and settling of HPC particles is enhanced by addition of cations such as Ca+* or Al+++. The addition of cations does not have an appreciable effecton the settling rate of particles of thermally precipitated HPMC. Virgin HPC is resistant to biodegrada- tion and solutions can be stored for long periods. Reclaimed HPC solutions are subject to biodegradation because of the presence of natural impurities removed from the fabric. Reclaimed HPC solutions can be preserved with agents typically used for preservation of textile chemicals. HPC is stable for long periods at the temperature necessary for its reclamation. The capital investment for reclama- tion of HPC by thermal precipitation is about one-third of that for reclamation of polyvinyl alcohol by ultrafiltration. The operating costs including size material costs for a system based on reclamation of HPC by thermal precipi- tation is slightly higher than for a system based on reclamation by PVA by ultrafiltration. The payback period for a thermal precipitation system is about one-third of that for an ultrafiltration system. Because of the value of the re- claimed material, size reclamation systems based on thermal precipitation and ultrafiltration both operate at lower costs than a conventional desizing system not involving size reclamation. A desize and reclamation system using HPC operates at a maximum water temperature of about 50°C whereas a system using PVA operates at a temperature of about 95°C. The result is an energy savings of about 0.655 x 106 Btu per 100 Ib. of fabric desized. Recommendations Size reclamation is an economical approach to chemical and water con- servation and will reduce the pollution load from most woven fabrics finishing plants. The size reclamation technique that is most applicable to a particular mill must be selected based on factors peculiar to that mill. A critical compari- son of all size reclamation techniques is not presently available, but such a comparison would be useful for decision makers in the textile industry. Size reclamation using thermal pre- cipitation appears to be technically and economically feasible at present only for selected types of plants. Those plants weaving cotton or polyester/cotton on narrow looms can probably use hydrox- ypropylcellulose as the warp size. This size can be recovered by thermal precip- itation and reused for sizing. HPC may also be useful in shuttleless weaving. The possibility of using HPC as a size in be useful in shuttleless weaving. The possibility of using HPC as a size in machines using projectile, rapier and air jet filling insertion mechanisms should be investigated. HPC is not recommend- ed for weaving of 50-inch wide fabrics at a speed of 215 picks per minute using shuttle looms at the current stage in its development as a warp size. The greatest deficiency of HPC as a warp size is insufficient hardness. The possibility of chemical modification of the material to make this property suitable for warp sizing purposes should be investigated. This work would best be done by a chemical company experi- enced in evaluation of polymers for warp sizing. HPC accumulates on the shuttle during the weaving of 50-inch wide fabrics if the shuttle is made of wood or of laminated cotton fabric composite materials. Shuttles made of other mate- rials should be tested to determine if the accumulation of HPC occurs. Hot melt sizmg is a developing tech- nology for the textile industry. The process applies a molten size to the yarn and uses no water. The first production model hot melt sizing machine will be available in the near future. Since HPC is a thermoplastic material its applica- bility as a hot melt size should be inves- tigated. Conventional recoverable size materials such as PVA and CMC are not applicable bythe hot melttechnique and * U.8. OOVEBHMEHIPRIKTIHO OFFICE «61 -757-012/72Z8 ------- size materials which have been developed especially for hot melt sizing are not recoverable. Therefore, the availability of the recoverable hot melt size would be highly desirable. Warren S. Perkins. Robert P. Walker, and Leo J. Hirth are with Auburn University, Auburn, AL 36830. Max Samfield is the EPA Project Officer (see below). The complete report, entitled "Textile Warp Size Reclamation Using Thermal Precipitation," (Order No. PB 81-129 041; Cost: $8.00, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Industrial Environmental Research Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 f United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Postage and Fees Paid Environmental Protection Agency EPA 335 Official Business Penalty for Private Use $300 U S £MVIR PROTECTION REGION 5 LIBRARY 230 S DEARBORN STREET CHICAGO IT, 60604 ------- |