WO2014073947A1 - Système d'ultrafiltration pour la concentration de réseaux - Google Patents

Système d'ultrafiltration pour la concentration de réseaux Download PDF

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Publication number
WO2014073947A1
WO2014073947A1 PCT/MY2013/000163 MY2013000163W WO2014073947A1 WO 2014073947 A1 WO2014073947 A1 WO 2014073947A1 MY 2013000163 W MY2013000163 W MY 2013000163W WO 2014073947 A1 WO2014073947 A1 WO 2014073947A1
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WIPO (PCT)
Prior art keywords
membrane
ultrafiltration
cleaning
feedstock
latex
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PCT/MY2013/000163
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English (en)
Inventor
Veerasamy DEVARAJ
Mohd Nor ZAIROSSANI
Subhramaniyun PRETIBAA
Izyana Ismail Aimi
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Lembaga Getah Malaysia
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Publication of WO2014073947A1 publication Critical patent/WO2014073947A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/145—Ultrafiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/22—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
    • C08C1/00—Treatment of rubber latex
    • C08C1/02—Chemical or physical treatment of rubber latex before or during concentration
    • C08C1/075—Concentrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/04—Specific process operations in the feed stream; Feed pretreatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/08—Specific process operations in the concentrate stream
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/10—Temperature control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/14—Pressure control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/18—Details relating to membrane separation process operations and control pH control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/25—Recirculation, recycling or bypass, e.g. recirculation of concentrate into the feed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/25—Recirculation, recycling or bypass, e.g. recirculation of concentrate into the feed
    • B01D2311/252—Recirculation of concentrate
    • B01D2311/2523—Recirculation of concentrate to feed side
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/26—Further operations combined with membrane separation processes
    • B01D2311/2611—Irradiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2315/00—Details relating to the membrane module operation
    • B01D2315/10—Cross-flow filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/16—Use of chemical agents
    • B01D2321/164—Use of bases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/16—Use of chemical agents
    • B01D2321/168—Use of other chemical agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
    • B01D2321/20—By influencing the flow
    • B01D2321/2066—Pulsated flow
    • B01D2321/2075—Ultrasonic treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/02—Details relating to pores or porosity of the membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/02—Details relating to pores or porosity of the membranes
    • B01D2325/0283—Pore size
    • B01D2325/02831—Pore size less than 1 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/06—Tubular membrane modules
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/24—Rubbers

Definitions

  • This invention relates to an ultrafiltration system and a process utilizing the system for concentrating latices.
  • the ultrafiltration system and process of this invention relates to carrying out latices concentration, recovery of waste latex, and latex product isolation.
  • Natural rubber latex as an industrial raw material is supplied as concentrated latex. It serves as the main raw material for natural rubber latex product manufacturing factories.
  • Known methods of concentrating latices are by way of centrifugation, creaming, and evaporation.
  • Latex concentration by centrifugation involves the separation of preserved natural rubber field latex into two fractions. One fraction contains concentrated latex having high dry rubber content while the other having low dry rubber content. The latter fraction is also known as skim latex. Skim latex is generally recovered by coagulation with sulphuric acid. Once skim latex is recovered, there exists an effluent which consists of sulphuric acid-contaminated serum with a high biological oxygen demand value. This effluent is then discharged into effluent ponds (anaerobic ponds).
  • H 2 S hydrogen sulphide
  • Recent improvements to the above method include the development and utilization of membrane separation technology for the concentration of natural rubber field latex, in particular membrane ultrafiltration.
  • Ultrafiltration is an environmentally friendly process and economically viable. It is possible to achieve 'zero discharge' with ultrafiltration as all the products from the concentration process have commercial value.
  • Malaysian patent application PI 20071273 discloses an ultrafiltration process for natural rubber latex concentration.
  • the apparatus used to carry out the process is one or more membrane modules having a plurality of tubular membranes. The process is carried out by pumping latex through the membrane modules.
  • an ultrafiltration system having tubular filtration membranes separates natural rubber latex into two fractions i.e. permeate and retentate, by filtering the latex through the tubular filtration membranes.
  • the resultants are concentrated natural rubber latex and a latex free natural rubber serum.
  • the ultrafiltration system may also be used to concentrate skim latex (produced from centrifugation process) to produce latex- free serum and skim latex concentrate.
  • skim latex produced from centrifugation process
  • the membrane modules can only be used in a serial arrangement, which results in a system having a relatively large footprint. The system was also observed to take a substantially long time to stabilize i.e. 20 minutes before the concentration process can begin.
  • the main disadvantage of this system is that the ultrasonic transducers are placed beneath the tank only. As ultrasonic waves are concentrated at the bottom of the tank, the intensity of the ultrasonic waves are not uniformly distributed throughout the membrane area. The bottom portion of the tubular membranes receive a higher intensity of ultrasonic waves, as opposed to the top portion of the tubular membranes which is further away from the ultrasonic transducers. As the membrane modules are immersed in an ultrasonic bath, the number of membrane modules the system can have depends on the size of the ultrasonic bath used. As with the prior ultrafiltration system of PI 20071273, the membrane modules can only be used in a serial arrangement, which results in a system having a relatively large footprint.
  • Prior ultrafiltration systems have been unable to provide uniform distribution of the ultrasonic waves throughout the membranes for preventing premature membrane fouling as well as to provide for effective cleaning of the membranes.
  • This invention thus aims to alleviate some or all of the problems of the prior art.
  • an ultrafiltration system for the concentration of latices.
  • the system comprises a first tank for storing the latex feedstock, a second tank for storing cleaning solution used in the cleaning of the system, a pump for pressurized circulation of the feedstock and cleaning solution through the system, and at least one vertically disposed ultrafiltration membrane module.
  • Each module is provided with a plurality of vertically disposed tubular membranes for filtering the feedstock, and with a plurality of ultrasonic transducers to generate ultrasonic waves for enhancement of membrane permeation flux.
  • the transducers are arranged in vertically spaced apart pairs so as to span the height of the module, with each pair of transducers arranged to also enable generation of ultrasonic waves across the width of the module.
  • the feedstock exits the first tank and is pumped through the membrane module for ultrafiltration, where lower molecular portions of the feedstock pass through the tubular membranes as permeate and higher molecular portions of the feedstock are retained as retentate.
  • the resulting retentate is recycled back to the first tank and ultrafiltration is repeated until the desired latex concentration is reached.
  • the cleaning solution exits the second tank and is pumped through the membrane module for cleaning of the membranes.
  • the arrangement of the ultrasonic transducers enables the generation of ultrasonic waves across the width and along the height of the module for effective enhancement of membrane permeation flux during both the ultrafiltration and cleaning cycles.
  • the first tank may further comprise a temperature sensing means to detect temperature variation of the feedstock.
  • the first tank may further comprise a pH sensing means for reading the pH level of the feedstock.
  • the first tank may further comprise a separating means for allowing only liquid portions of the retentate back into the first tank.
  • the system may further comprise a pressure indicator means to detect pressure variation of the feedstock entering the membrane module and pressure variation of the retentate leaving the membrane module.
  • each of the membrane modules may have from seven to thirty- seven cross-flow tubular membranes for filtering the feedstock.
  • each of the membrane modules may have seven tubular membranes for filtering the feedstock.
  • the tubular membranes may have a pore size ranging from about 0.1 to about 0.2pm.
  • the tubular membranes may be ceramic cross-flow tubular membranes.
  • the membrane module may be of a substantially cuboidal shape.
  • the membrane module may be provided with a compartment for holding the ultrasonic transducers on either side of the membrane module.
  • ultrasonic transducers may further comprise a time regulator means to enable continuous or intermittent operation of the transducers.
  • the ultrasonic transducers used may have a drive frequency of 25 kHz.
  • Each membrane module may be provided with twenty four units of ultrasonic transducers having a drive frequency of 25 kHz.
  • the ultrasonic transducers used may have a drive frequency of 40 kHz.
  • Each membrane module may be provided with thirty six units of ultrasonic transducers having a drive frequency of 40 kHz.
  • each membrane module may be provided with ultrasonic transducers having a drive frequency of 25 kHz and 40 kHz.
  • system may further comprise a plurality of valves for controlling the flow of the feedstock or cleaning solution entering each membrane module or, retentate or cleaning solution exiting each membrane module.
  • the membrane module may be operated in a serial arrangement or a parallel arrangement by opening or closing selected valves.
  • the system may further comprise a thermal cleaning device for cleaning of said tubular membranes. In use, the membranes are removed from the membrane modules and are subject to thermal cleaning with the device upon reaching membrane permeation flux of 50%.
  • the system may be particularly suitable for recovering natural rubber skim latex, concentrating epoxidised natural rubber, and recovering waste nitrile latex.
  • an ultrafiltration process for concentration of latices utilizing the system of this invention.
  • the process comprises the steps of:
  • step (i) continuously during which higher molecular portions of the feedstock is removed from the membrane module as retentate for recirculation to the first tank;
  • ultrasonic transducers are operated either continuously or intermittently throughout steps (i) to (v) for effective cleaning and enhancement of membrane permeation flux.
  • a predetermined amount of deionized water is fed into the membrane modules.
  • the tubular membranes may be operated at a pH range of 0 to 14.
  • tubular membranes may be operated at a breaking pressure of not more than 9 MPa (90 bar).
  • tubular membranes may be operated at a running pressure of not more than 1 MPa (10 bar).
  • tubular membranes may be operated at a temperature below 400°C.
  • the cleaning cycle may comprise the step of cleaning the tubular membranes with deionized water. In a further embodiment, the cleaning cycle may comprise the step of cleaning the tubular membranes with 1% NaOH solution.
  • the cleaning cycle may comprise the step of cleaning said tubular membranes with a solution of 1% NaOH and 0.025% NaOCI.
  • each cleaning cycle may be carried out for 30 minutes at a temperature of 50°C.
  • the cleaning cycle may be conducted at a transmembrane pressure of 50 kPa (0.5 bar).
  • the process may further comprise the step of:
  • the membrane modules may be heated at a temperature ranging from about 250°C to about 300°C.
  • the process may be particularly suitable for recovering natural rubber skim latex, for concentrating epoxidised natural rubber, and for recovering waste nitrite latex.
  • the present invention seeks to overcome the problems of the prior art, and to provide an ultrafiltration system and process utilizing the system for the concentration of latices.
  • the system and process of this invention enables enhancement of membrane permeation flux and provides for an effective cleaning of the ultrafiltration membranes.
  • the arrangement of the ultrasonic transducers enables the generation of ultrasonic waves across the width and along the height of the membrane modules, i.e. allows the ultrasonic waves to be distributed in uniform intensity over the entire membrane area of the tubular membranes. This greatly enhances membrane permeation flux and aids in preventing premature membrane fouling leading to an increase in the economic life of the membranes.
  • the generation of ultrasonic waves across the width and along the height of the membrane modules can be applied for all type of membrane separation processes such as microfiltration, nanofiltration, reverse osmosis, electrolysis, and dialysis.
  • the additional cost for an ultrafiltration system to have ultrasonic application is only 5% more than that of an ultrafiltration system without ultrasonic application.
  • the vertical arrangement of the membrane modules within the system also allows for easy incorporation of additional membrane modules when needed, as well as to allow for convenient drainage of the concentrated latex before the cleaning cycle is carried out.
  • the system and process of the present invention also produces concentrated latex that has superior film qualities when compared to the film properties of centrifuged latex concentrate.
  • FIG. 1 is a schematic diagram of the ultrafiltration system according to an embodiment of this invention.
  • FIG. 2 is a cross-sectional view of the membrane module having ultrasonic transducers used in the system of Figure 1.
  • Figure 3 is a cross-sectional view of a tubular membrane housed in the membrane module of Figure 2.
  • Figure 4 shows a membrane module for use with the system of Figure 1, having thirty six units of ultrasonic transducers with a drive frequency of 40 kHz.
  • Figure 5 shows a membrane module for use with the system of Figure 1, having twenty four units of ultrasonic transducers with a drive frequency 25 kHz.
  • Figure 6 shows a thermal cleaning device for use with the embodiment of Figure 1.
  • Figure 7 is a graph showing membrane permeation flux during the concentration of natural rubber field latex with and without ultrasonic application as explained in Example 2.
  • Figure 9 is a graph showing membrane permeation flux during the concentration of epoxidised natural rubber (ENR25) latex as explained in Example 3.
  • the invention is an ultrafiltration system and process having ultrasonic transducers for enhancement of membrane flux and cleaning capabilities, developed to enable environmentally friendly latices concentration.
  • the system and process of this invention may be used for the concentration of various types of industrial liquids, for example natural rubber latex, epoxidised natural rubber latex (ENRL), nitrile butadiene rubber latex (NBRL), styrene butadiene rubber latex (SBRL) and polyvinyl chloride latex (PVCL).
  • natural rubber latex epoxidised natural rubber latex
  • NBRL nitrile butadiene rubber latex
  • SBRL styrene butadiene rubber latex
  • PVCL polyvinyl chloride latex
  • the invention may be used for the concentration of natural rubber field latex (NRFL) and natural rubber skim latex (NRSL), where natural rubber serum and natural rubber skim serum, respectively, are produced as useful environmentally friendly by-products.
  • NRFL natural rubber field latex
  • NRSL natural rubber skim latex
  • Natural rubber field latex Concentration of natural rubber field latex by centrifugation typically requires the latex to be preserved before the centrifugation process can be carried out.
  • natural rubber field latex is preserved with ammonia, but may also be preserved with various other preservatives in addition to ammonia.
  • the natural rubber field latex can be concentrated with lower concentrations of preservation chemicals beforehand. This reduces costs as less preservation chemicals are required.
  • the invention may also be used for recovery of waste nitrile latex, which is a scheduled waste of nitrile latex glove manufacturing.
  • waste nitrile latex is disposed by way of incineration at high disposal costs.
  • the system and process of this invention enables recovery of waste nitrile latex such that the concentrated nitrile latex may be reused in the processing of new batches of nitrile latex.
  • Epoxidised natural rubber (ENR) latex is a structurally modified natural rubber field latex. Structure modification is done to incorporate superior properties of synthetic rubber, such as resistance to oil and chemicals. Concentration of epoxidised natural rubber latex by centrifugation is not feasible. This is because the difference of specific gravity between epoxidised natural rubber latex and water is too small for any meaningful separation to occur during centrifugation. Epoxidised natural rubber latex can only be can only be concentrated by the process of this invention. The system
  • the ultrafiltration system of this invention mainly comprises a first tank 1 (feed tank) for storing the latex feedstock, a second tank 2 (washing tank) for storing cleaning solution used in the cleaning of the system, a pump 3 for pressurized circulation of the feedstock and cleaning solution throughout the system, and at least one vertically disposed ultrafiltration membrane module 4 provided with a plurality of ultrasonic transducers 9.
  • the feed tank 1 can be made of any suitable material such as stainless steel and can be of any suitable shape and configuration. In the embodiment of Figure 1, the tank is vertically disposed and is substantially of a cylindrical shape with a tapered bottom.
  • the feed tank 1 can be of any suitable size depending on the processing capacity of the system. For example, the feed tank in Figure 1 has a capacity of 1250 L. If necessary, the size of this tank may be increased depending on the amount of feedstock to be processed.
  • the feed tank 1 has an inlet located at the top of the tank for receiving feedstock as well as incompletely filtered latices (retentate) and an outlet located at the bottom of the tank for the egress of feedstock.
  • the feed tank 1 may preferably be provided with a separation means 14 for allowing only liquid portions of the retentate back into the feed tank 1 for recirculation and further ultrafiltration.
  • the separation means 14 may be a sieve having a suitable pore size, for example a 40 mm mesh sieve. To avoid high turbulence in the feed tank 1 during processing, the feed tank 1 may also additionally be provided with the appropriate conventional fittings such as baffles and the like.
  • the feed tank 1 may have a temperature sensing means 6 connected to an electrical control panel 10 positioned near the tapered bottom of the tank such as a stainless steel thermocouple type K temperature probe.
  • a pH sensing means 5 such as a panel mounted pH meter may also be provided for detecting the pH of the contents of the feed tank 1, and may be located adjacent the temperature sensing means 6.
  • the washing tank 2 can be made of any suitable material such as stainless steel and can be of any suitable shape or configuration.
  • the tank is vertically disposed and is substantially of a cylindrical shape with a tapered bottom.
  • the washing tank 2 can be of any suitable size depending on the cleaning solution to be used in the cleaning cycle and the desired capacity of the system. For example, in the embodiment of Figure 1, the washing tank has a capacity of 300 L. If necessary, the size of this tank may be increased.
  • the feed pump 3 can be any type of pump of a suitable capacity for providing pressurized circulation of the contents of the feed tank 1 and washing tank 2 throughout the system and may be provided with industry-standard components such as an air regulator, air muffler and/or a non-stalling air valve.
  • the pump may be a compressed air powered double-diaphragm pump having a capacity of 10 hp.
  • At least one membrane module 4 is provided with the system of this invention.
  • the module may be of any suitable shape and configuration.
  • four vertically disposed membrane modules is provided, each module being of a substantially cuboidal shape and having an inlet for receiving feedstock, a primary outlet for outflow of retentate (incompletely filtered latices) and a secondary outlet for outflow of permeate (lower molecular weight).
  • the primary outlets of all four modules are operatively connected to a common retentate line that removes the retentate for recirculation back to the feed tank for further processing.
  • the secondary outlets of all four modules are operatively connected to a common permeate line for removing permeates of the feedstock at predetermined intervals.
  • Each membrane module 4 houses a plurality of cross-flow tubular membranes 13 of a suitable type.
  • the membranes used should be able to withstand a pH range of 0 to 14, a breaking pressure of not more than 9 MPa (90 bar), a running pressure of not more than 1 MPa (10 bar) and temperatures of not more than 400°C. Ceramic tubular membranes may be used.
  • the number of tubular membranes provided per module and the total membrane area per module is dependant on the feedstock to be concentrated and the desired capacity of the system.
  • the tubular membrane used may have any suitable number of channels and may be made of any suitable material.
  • a ceramic tubular membrane is used.
  • the ceramic membrane is made of Zr0 2 - Ti0 2 , has eight channels with each channel having a hydraulic diameter of 6 mm, a pore size of 0.14 microns, a length of 1178 mm and has a total membrane area of 0.2 m 2 .
  • the total membrane area per module is 1.125 m 2 and the total membrane area of the system is 4.5 m 2 .
  • the tubular membranes used may have a pore size ranging from about 0.1 ⁇ to about 0.2 pm.
  • the pore size is dependent on the type of feedstock to be concentrated. For example, for natural rubber field latex concentration, recovery of skim latex, and recovery of waste nitrile latex the tubular membrane pore size should be in the range of from about 0.1 pm to 0.2 pm. For epoxidised natural rubber latex concentration, the tubular membrane pore size should be in the range of from about 0.14 pm to 0.16 pm.
  • Each membrane module 4 is provided with a plurality of ultrasonic transducers 9 to generate ultrasonic waves for enhancement of membrane permeation flux and to enhance cleaning of the membranes during a cleaning cycle.
  • the transducers are arranged in vertically spaced apart pairs so as to span the height of the module.
  • Each pair of transducers are arranged to also enable generation of ultrasonic waves across the width of the module, for example by placing each transducer of a pair of transducers on either side of the module.
  • the transducers are fixedly attached to each module, either directly on the module wall or housed in a separate holding compartment 11.
  • each membrane module is provided with a compartment 11 for holding the transducers on either side of the module.
  • any suitable type of ultrasonic transducers may be used in the system of this invention.
  • transducers having a drive frequency of 25 kHz or 40 kHz may be used.
  • All of the membrane modules in the system may be provided with transducers of identical or different drive frequencies, for example, in a system having four modules, two of the modules may be fitted with transducers having a drive frequency of 40 kHz and the remaining two modules fitted with transducers having a drive frequency of 25 kHz.
  • each of the membrane modules in the system may be provided with ultrasonic transducers of different frequencies.
  • each membrane module may be provided with transducers having a drive frequency of 25 kHz and 40 kHz.
  • the number of ultrasonic transducers provided per module is dependent on the drive frequency of the transducers used.
  • each module is provided with thirty six units (eighteen pairs) of transducers having a drive frequency of 40 kHz.
  • each module is provided with twenty four units (twelve pairs) of transducers having a drive frequency of 25 kHz.
  • the configuration and arrangement of the ultrasonic transducers and the type of transducers used is chosen so as to enable propagation of the ultrasonic waves throughout each membrane module.
  • a suitable generator may be provided with the system of this invention for generating power for the ultrasonic transducers.
  • a suitable time regular means may also be provided for optional selection of continuous or intermittent operation of the transducers.
  • a suitable pressure meter for measuring the pressure of the feedstock entering the membrane module 4 and retentate exiting the membrane module 4 may be provided with this system.
  • the pressure meter may have a pressure range of from 0 to 700 kPa (7 bar).
  • the system of this invention may be further provided with suitable valves, pipes and fittings for operation and control of the system.
  • Selected valves can be opened or closed for operation of the membrane modules either in a parallel or a serial arrangement.
  • the valves can also be used for controlling the desired trans-membrane pressure for driving the feedstock through each membrane module 4.
  • a suitable main structure frame is provided to support all the apparatus of the system such as the feed tank 1, washing tank 2 and membrane modules 4.
  • the main structure frame can be made of any suitable material such as SUS304 stainless steel.
  • the system may have an electrical control panel 10 that may be mounted onto the main structure frame or separately provided.
  • the electrical control panel 10 consolidates all the signals of the pH meter, temperature meter, and pressure meters.
  • the system may further comprise a thermal cleaning device 12 such as a muffle furnace ( Figure 6) for receiving and cleaning the tubular membranes.
  • the thermal cleaning device 12 can be of any suitable shape or size. The size of the device is dependent on the desired number of tubular membranes to be cleaned at any one time. For example, in the embodiment of Figure 6, the length of the device is 1400 mm so as to be able to accommodate fourteen tubular membranes of 1020 mm length. The device is able to generate heat of up to about 500°C.
  • the ultrafiltration process for concentration of latices utilizing the system of this invention mainly comprises the following steps: i. pumping feedstock from the feed tank to the membrane module to commence ultrafiltration;
  • step (i) continuously during which higher molecular portions of the feedstock is removed from the membrane module as retentate for recirculation to the first tank;
  • serial or parallel arrangement of the membrane module 4 is selected by opening and closing the appropriate valves.
  • deionized water is fed into the membrane modules 4 prior to commencing an ultrafiltration run. This is done to surround the tubular membrane with a medium for transmitting the ultrasonic waves. Preferably, deionized water is fed into the membrane module until it reaches the permeate line.
  • the pump is then turned on to commence ultrafiltration where feedstock from the feed tank 1 is circulated to the membrane modules 4.
  • Trans-membrane pressure is set by adjusting the pressure adjustment means 8 after the system has stabilized.
  • the system is usually stable after 10 minutes from the commencing of the circulation.
  • feedstock is pumped from a first membrane module to the last membrane module in sequence.
  • the feedstock is pumped through more than one membrane module simultaneously.
  • permeate is removed from the membrane modules 4 through the permeate line, while the retentate is removed through the retentate line.
  • Retentate is recirculated via the retentate line to the feed tank 1 for further ultrafiltration, until the desired latex concentration is reached.
  • the pH and temperature of the feedstock is monitored.
  • the temperature of the feedstock should not exceed 55°C when the feedstock is natural rubber field latex.
  • Pressure of feedstock entering the membrane module 4 and retentate exiting the membrane module 4 should also be monitored periodically.
  • the ultrafiltration cycle continues until the required concentration is reached.
  • the required concentration of the product is calculated using the initial concentration of the feed and the volume of permeate produced during an ultrafiltration run.
  • the ultrafiltration process Upon reaching the required concentration, the ultrafiltration process is stopped. Retentate is isolated in the feed tank 1 by opening and closing the appropriate valves. The resulting retentate is the fully concentrated latex which is removed from the system by draining it from the feed tank 1. The cleaning cycle is then commenced. Cleaning solution from the washing tank 2 is pumped through the membrane module 4 until the appearance of the cleaning solution leaving the membrane module is clear. Throughout the ultrafiltration and cleaning cycles, the ultrasonic transducers are turned on either continuously or intermittently.
  • Cycle 1 The preferred cleaning cycles of the process of this invention are set out below. Cycle 1
  • Clean water is circulated from the washing tank 2 to the membrane modules 4.
  • the circulation of clean water is carried out until the milky appearance of the rinsed water disappears. During this cleaning cycle, no trans-membrane pressure is set. After the milky appearance of the rinsed water disappears, a final rinsing is done. This final rinsing is done by circulating deionized water having a temperature of 50°C and at a transmembrane pressure of 50 kPa (0.5 bar).
  • cycle 1 After cycle 1 is completed, a 1% NaOH solution having a temperature of 50°C is circulated from the washing tank to the membrane modules 4. This cleaning cycle is carried out for thirty minutes at a trans-membrane pressure of 50 kPa (0.5 bar). The system is then packed with the 1% NaoH solution and left idle overnight. The next day, the 1% NaoH is discharged and deionized water is circulated through the system. Cycle 3
  • a 1% NaOH and 0.025% NaOCI solution having a temperature of 50°C is circulated from the washing tank to the membrane module 4. This cleaning cycle is carried out for thirty minutes. The system is then packed with the 1% NaOH and 0.025% NaOCI solution and left idle overnight. The next day, the 1% NaOH and 0.025% NaOCI is discharged and deionized water is circulated through the system.
  • the membrane flux of the tubular membranes is expected to deteriorate due to accumulated foulants consisting of rubber particles and scales of latex proteins plugging the membrane pores.
  • a thermal cleaning cycle is carried out.
  • the tubular membranes are removed from the membrane module 4 and are subsequently placed in the thermal cleaning device 12.
  • the device 12 is turned on to generate heat at a preferred temperature of about 250°C to about 300°C.
  • the membranes are heated in the device 12 for a predetermined amount of time.
  • This thermal cleaning cycle further cleans the fouled membranes by ashing out rubber particles and scales of latex proteins that are plugging the membrane pores.
  • the thermally cleaned tubular membranes are then ready for reuse in new ultrafiltration runs.
  • Example 1 The effect of different cleaning solutions on membrane permeation flux during the cleaning cycle A study was carried out with the system and process of this invention to determine the effects of different cleaning solutions on membrane permeation flux. In this study, two membrane modules connected in parallel, each module having fourteen tubular membranes were used, with each membrane module having ultrasonic transducers with a drive frequency of 40 kHz.
  • Cycle 1 of membrane cleaning is carried out by rinsing the tubular membranes with clean water with the ultrasonic transducers turned on, without trans-membrane pressure to remove remnants of latex from the system, until milky appearance of rinsed water disappears.
  • a final rinse is done with deionized water (DIW) at a temperature of 50°C with the ultrasonic transducers turned on and a trans-membrane pressure (TMP) of 50 kPa (0.5 bar).
  • DIW deionized water
  • TMP trans-membrane pressure
  • Cycle 2 of membrane cleaning is carried out after cycle 1 has been completed by circulating the system with 1% NaOH solution at a temperature of 50°C with the ultrasonic transducers turned on at a trans-membrane pressure of 50 kPa (0.5 bar) for thirty minutes and packing the system with the cleaning solution overnight and rinsing with deionized water the next day.
  • Cycle 3 of membrane cleaning is carried out after cycle 2 has been completed by circulating the system with 1% NaOH and 0.025% NaOCI solution at a temperature of 50°C with the ultrasonic turned on for thirty minutes and packing the system with the cleaning solution overnight and rinsing with deionized water the next day.
  • Membrane flux recovery is calculated as shown in Equation (1).
  • Membrane flux recovery £ — (1) permeate of deionized water when the membrane was unused
  • Example 2 A comparison between natural rubber field latex concentrated using ultrafiltration with ultrasonic application and natural rubber field latex concentrated using ultrafiltration without ultrasonic application
  • Natural rubber field latex concentrated using ultrafiltration with and without ultrasonic application are compared to show the extent of flux enhancement obtained using ultrasonic transducers.
  • FIG 7 compares the flux values against processing time with and without ultrasonic application.
  • the flux profiles and other readings obtained are shown in Table 1 and Table 2.
  • Total solid contents (TSC) can also be indirectly calculated from the volume of permeate collected.
  • Table 3 gives the total solid content values of the feed, calculated from the volume of permeate collected at hourly intervals. The initial and the final total solid content were accurately calculated by in-house accredited laboratory.
  • Table 3 Hourly increase of tota solid content values wit 1 and without ultrasonic application Without ultrasonic application, the concentration polarizations caused the sudden drop of flux by 0.55 Liters/M 2 /Hr after one hour of processing. The drop in flux continued, all the way until the ninth hour of concentration. After concentration was concluded, the total solid content attained was only 46% for ultrafiltration without ultrasonic application compared to 65% for ultrafiltration with ultrasonic application. With ultrasonic application the required total solid content of 50% was attained after three and a half hours of concentration compared to more than nine hours without ultrasonic application.
  • filtration resistances are sub-classified into five types and each one impact the filtration process at different stages.
  • J v is flux through the membrane (cm/s)
  • ⁇ is trans-membrane pressure (Pa)
  • ⁇ is dynamic viscosity (Pa.s or gscm -1 ).
  • the resistances are as given below (all resistances are in cm -1 ): r m is membrane hydraulic resistance, r c is concentration polarization resistance, r g is gel layer resistance, r ai is weak adsorption resistance and r a2 is strong adsorption resistance.
  • r m which remains constant, is the intrinsic membrane resistance, but r c increases with an increase of total solid content.
  • concentration polarization, gel layer, and weak adsorption resistances may be considered to be reversible by clean water and NaOH extraction, while strong adsorption resistance is not.
  • Ultrasonic application during ultrafiltration creates micro-streaming which disrupts the formation of concentration polarization. Subsequently gel layer formation would be delayed. Concentration polarizations would eventually occur even with ultrasonic application, but only at a higher total solid content value.
  • the target total solid content is 60%.
  • Latex and film properties of latex concentrated using ultrafiltration are superior to that of latex concentrated using centrifugation as shown in Table 4 below:
  • the film prepared from latex concentrated using ultrafiltration has a higher tear resistance and is stiffer compared to latex concentrated using centrifugation. Higher tear resistance is an advantage but a stiffer glove is not comfortable to the user.
  • the throughput of an ultrafiltration system could match that of centrifugation, by scaling accordingly (such increasing its membrane area and pump capacity etc.).
  • Example 3 Ekoprena 25 (ENR25) latex concentration using ultrafiltration with ultrasonic application at a frequency of 40 kHz
  • Epoxidised natural rubber (ENR) latex is a structurally modified natural rubber latex. Modification is carried out to incorporate superior properties of synthetic rubber, such as resistance to oil and chemicals. Natural rubber latex concentrate undergoes structural modification through chemical reaction/ Upon reaching a total solid content of 32% to 34% it is subsequently processed into epoxidised natural rubber blocks for the manufacture of green tires. Epoxidised natural rubber can be used as raw material for manufacturing niche latex products. For manufacturing latex dipped goods, epoxidised natural rubber latex has to be concentrated from its original total solid content value of 31% to 50%. The concentration of epoxidised natural rubber latex can only be done by membrane separation process. The concentration of epoxidised natural rubber latex by centrifugation is not feasible, because the difference of specific gravity between epoxidised natural rubber latex and water is too small for any meaningful separation to occur.
  • Epoxidised natural rubber latex had to be adequately preserved before concentration process is carried out. Although remnants of preservation chemicals from its production stage is still in the latex, additional preservation chemicals still needs to be added to prevent destabilization of the latex when ultrasound is applied to enhance flux. Even with the additional preservation, , the . behaviour of epoxidised natural rubber latex during ultrafiltration is quite unpredictable at times. If the preservation chemicals used are not suitable, the feed could become destabilized resulting in the coalition of destabilized latex particles which could eventually cause blockages of the piping and plugging of membrane pores.
  • the initial total solid content of 36% is relatively high. As can been seen from Figure 9, there was a gradual increase in flux for about forty five minutes. This was partly due to the ability of ultrasonic waves to destroy any immediate build-up of concentration polarization. Also, time taken by the system to stabilize and to get the full impact of the trans-membrane pressure also causes increase in flux. As the feed concentration increases due to permeation of the aqueous phase, the rate at which the concentration polarization being built is faster than the rate at which it was destroyed by the micro streaming of ultrasonic waves. Permeation has been curtailed considerably causing a reduction in flux as the concentration increased. After the third hour of processing, the permeation still continued but at a reduced rate. This caused a slow increase in feedstock concentration.
  • the application of ultrasound enhances flux at any initial concentration and is capable of diffusing concentration polarizations and gel layer resistances even at high feed concentration.
  • the epoxidised natural rubber latex concentrate at a total solid content of 50% can be obtained by ultrafiltration enhanced by ultrasound within three and a half hours of processing time.
  • Example 4 Enhancing of membrane permeation flux during the concentration of Ekoprena 50 (ENR50) using ultrafiltration with ultrasonic application at frequencies of 25 kHz and 40 kHz
  • ENR50 latex is prone to destabilization.
  • Table 7 shows the flux profiles obtained for the concentration processes carried out using 65 L of feedstock for each concentration process of epoxidised natural rubber latex using ultrasonic application with a 40 kHz frequency, 25 kHz frequency and with no ultrasonic application (control).
  • Table 8 shows the percentage of flux enhancement at every thirty minute intervals as well as the average flux enhancements of 26% and 31% which were obtained for the concentration processes using ultrasonic frequencies of 25 kHz and 40 kHz respectively.
  • 40 kHz frequency enhanced membrane filtration process more effectively compared to 25 kHz.
  • energy absorption is higher and thus greater acoustic streaming occurs which in turn increases the flow rates compared to the lower frequencies for the same power intensity. This mechanism caused the bulk water movement toward and away from the membrane cake layer, with velocity gradients near the cake layer that scoured latex particles from the surface.
  • Example 5 Thermal cleaning of membranes in a thermal cleaning device
  • Ceramic membranes are usually made from thermal and hydrothermal stable material derived from or in combination of ⁇ -alumina, titania and zirconia. At temperatures lower than 900°C (alumina), 600°C (zirconia) and 450°C (titania), these membranes and are stable for phasing and structural transformation. Ceramic membranes which were made from zirconia-titania (Zr0 2 - Ti0 2 ) in combinations were used for this study. This specially designed muffle furnace which measures a length of 1400 mm and could accommodate a total of 14 membranes of 1020 mm length and 20mm of external diameter, arranged systematically. It is also incorporated with a slow heating-cooling facility and can attain a highest temperature of 600°C. It was used to identify an ideal temperature to carry out the thermal cleaning of fouled ceramic membrane. The totally fouled membranes from latex concentration process which is known to be plugged by latex particles and latex proteins and could easily be ashed at temperatures below 300°C.
  • Concentration of natural field rubber latex is greatly enhanced by ultrasonic application. This can be seen in Example 1 where a targeted total solid content of 50% is reached within three and a half hours in an ultrafiltration system with ultrasonic application. In an ultrafiltration system without ultrasonic application, the targeted total solid content of 50% took almost ten hours to reach. This is because ultrasonic waves mitigate or diffuse any increase in concentration polarization and gel layer resistances during ultrafiltration and premature membrane fouling was prevented.
  • Epoxidised natural rubber latex can be only be concentrated using membrane separation. From the results of the tests carried out, it was concluded that concentration of epoxidised natural rubber latex (ENR25) using ultrafiltration is enhanced when a frequency of 40 kHz is applied. The ultrasonic waves destroyed build-up of concentration polarization and gel layer resistances formed on the tubular membranes during the ultrafiltration process.
  • a thermal cleaning device such as a muffle furnace can further improve membrane permeation flux.
  • Tubular membranes are placed in the muffle furnace to undergo ashing.
  • the ashing process removes rubber particles and scales of latex proteins that are plugging membrane pores, and subsequently restores membrane permeation flux.
  • the ideal temperature for thermal cleaning should be around 250°C - 300°C.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un système d'ultrafiltration et un procédé de concentration de réseaux ayant des capacités d'amélioration de flux ultrasonique et de nettoyage de membrane. Le système d'ultrafiltration pour la concentration de réseaux comprend principalement un premier réservoir (1), un second réservoir (2), une pompe (3) et au moins un module de membrane d'ultrafiltration disposé de façon verticale (4). Chaque module est doté d'une pluralité de membranes tubulaires disposées de façon verticale (13) pour filtrer la charge d'alimentation de latex et d'une pluralité de transducteurs ultrasoniques (9) pour générer des ondes ultrasoniques pour l'amélioration du flux de perméation de membrane. Le procédé d'ultrafiltration est effectué par utilisation du système où la charge d'alimentation de latex est pompée à travers le module de membrane pour ultrafiltration, où les parties moléculaires inférieures de la charge d'alimentation passent à travers la membrane tubulaire comme perméat et les parties moléculaires supérieures de la charge d'alimentation sont retenues comme rétentat (concentré de latex). Le procédé est répété jusqu'à ce que la concentration de latex souhaitée soit atteinte.
PCT/MY2013/000163 2012-11-07 2013-09-09 Système d'ultrafiltration pour la concentration de réseaux WO2014073947A1 (fr)

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MYPI2012004868A MY159044A (en) 2012-11-07 2012-11-07 An ultrafiltration system for concentration of latices and a process utilizing the system
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WO2016025590A1 (fr) * 2014-08-12 2016-02-18 Water Planet, Inc. Système de gestion de filtration de fluide intelligent
WO2016204601A1 (fr) 2015-06-18 2016-12-22 Sime Darby Plantation Sdn. Bhd. Procédé et système de concentration de latex d'élastomère-caoutchouc naturel époxydé en un concentré de latex d'élastomère-caoutchouc naturel époxydé
CN106608693A (zh) * 2016-01-08 2017-05-03 约瑟夫·安德鲁·兰德 关闭式节能用管式膜循环系统
CN110152490A (zh) * 2019-06-17 2019-08-23 海南中橡科技有限公司 一种滤膜清洗装置
ES2803954A1 (es) * 2019-07-26 2021-02-01 Izquierdo Juan Carmelo Suarez Sistema de Limpieza Ultrasónica para Contribuir a Procesos de Osmosis, Ultrafiltración y Nanofiltración 100% Libres de Químicos
CN114409829A (zh) * 2022-01-05 2022-04-29 淄博鲁华泓锦新材料集团股份有限公司 一种异戊二烯胶乳浓缩方法
CN115477711A (zh) * 2022-09-13 2022-12-16 中国热带农业科学院农产品加工研究所 一种利用陶瓷膜提高环氧化天然胶乳固含物的方法及装置

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US5632890A (en) * 1991-01-11 1997-05-27 Sugitomo Akitoshi Ceramic filter filtration apparatus for purifying swimming pool water

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016025590A1 (fr) * 2014-08-12 2016-02-18 Water Planet, Inc. Système de gestion de filtration de fluide intelligent
US10562787B2 (en) 2014-08-12 2020-02-18 Water Planet, Inc. Intelligent fluid filtration management system
US11401172B2 (en) 2014-08-12 2022-08-02 Intelliflux Controls Intelligent fluid filtration management system
WO2016204601A1 (fr) 2015-06-18 2016-12-22 Sime Darby Plantation Sdn. Bhd. Procédé et système de concentration de latex d'élastomère-caoutchouc naturel époxydé en un concentré de latex d'élastomère-caoutchouc naturel époxydé
CN106608693A (zh) * 2016-01-08 2017-05-03 约瑟夫·安德鲁·兰德 关闭式节能用管式膜循环系统
CN110152490A (zh) * 2019-06-17 2019-08-23 海南中橡科技有限公司 一种滤膜清洗装置
ES2803954A1 (es) * 2019-07-26 2021-02-01 Izquierdo Juan Carmelo Suarez Sistema de Limpieza Ultrasónica para Contribuir a Procesos de Osmosis, Ultrafiltración y Nanofiltración 100% Libres de Químicos
CN114409829A (zh) * 2022-01-05 2022-04-29 淄博鲁华泓锦新材料集团股份有限公司 一种异戊二烯胶乳浓缩方法
CN115477711A (zh) * 2022-09-13 2022-12-16 中国热带农业科学院农产品加工研究所 一种利用陶瓷膜提高环氧化天然胶乳固含物的方法及装置
CN115477711B (zh) * 2022-09-13 2024-05-14 中国热带农业科学院农产品加工研究所 一种利用陶瓷膜提高环氧化天然胶乳固含物的方法及装置

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