EP3829761A1 - Verfahren zur herstellung eines adsorbens für phosphat in wässrigem medium - Google Patents

Verfahren zur herstellung eines adsorbens für phosphat in wässrigem medium

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Publication number
EP3829761A1
EP3829761A1 EP19742785.9A EP19742785A EP3829761A1 EP 3829761 A1 EP3829761 A1 EP 3829761A1 EP 19742785 A EP19742785 A EP 19742785A EP 3829761 A1 EP3829761 A1 EP 3829761A1
Authority
EP
European Patent Office
Prior art keywords
suspension
iron
oxy
hydroxide
process according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP19742785.9A
Other languages
English (en)
French (fr)
Inventor
Josep SALAET FERRÉ
Marta Pomares Marco
Francisco De Asís MARQUILLAS OLONDRIZ
Berta GIRBAU CAPELLA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Interquim SA
Original Assignee
Interquim SA
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Filing date
Publication date
Application filed by Interquim SA filed Critical Interquim SA
Publication of EP3829761A1 publication Critical patent/EP3829761A1/de
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01D61/16—Feed pretreatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • B01D2311/18—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
    • B01D2311/24—Quality control
    • B01D2311/243—Electrical conductivity 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
    • 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
    • B01D2315/00—Details relating to the membrane module operation
    • B01D2315/16—Diafiltration

Definitions

  • This invention relates to a process for preparing an adsorbent for phosphate comprising stabilized iron oxy-hydroxide in aqueous medium at industrial scale.
  • WO9201458A1 discloses a method of controlling serum phosphate levels in patients by use of phosphate adsorbers based on iron oxy-hydroxides which bind to ingested phosphate.
  • Sucroferric oxy-hydroxide (INN; trade name Velphoro, by Vifor Fresenius Medical Care Renal Pharma) is a non-calcium, iron-based phosphate binder used for the control of serum phosphorus levels in adult patients with chronic kidney disease on haemodialysis or peritoneal dialysis.
  • Sucroferric oxy-hydroxide is a complex which consist of polynuclear iron (III) oxy-hydroxide (pn-FeOOH), sucrose, and starch.
  • the pn-FeOOH moiety is chemically not stable and cannot be isolated and stored as an active pharmaceutical ingredient.
  • the sucrose and the starch are also necessary for the processability of the active substance during the manufacturing process of the finished product (cf. Chemical review for Velphoro of the FDA, page 8 or Assessment Report of the EMA, page 12).
  • Sucroferric oxy-hydroxide was first described in the patent family of US6174442B1 (EP0868125B1 ).
  • This patent describes polynuclear beta-iron hydroxide stabilized by carbohydrates and/or humic acid.
  • the product was prepared by reacting, in a first step, an aqueous solution of iron (III) chloride with an aqueous solution of a base which produced a suspension of polynuclear iron (III) oxy-hydroxide (pn-FeOOH).
  • the resulting suspension was washed with water to remove interfering anions, such as chloride ions.
  • the carbohydrate or humic acid was added to the suspension before the resulting beta-iron oxy-hydroxide ages.
  • W02009/062993A1 relates to pharmaceutical compositions comprising stabilized iron (III) oxy-hydroxide compounds.
  • Example 1 a premixture of the stabilized iron (III) oxy- hydroxide was obtained by mixing amounts/ratios of an iron oxy-hydroxide suspension prepared according to EP0868125B1 with several excipients. The suspension was subjected to spray drying at 135-200 °C to obtain a flowable powder.
  • W02008/071747A1 discloses a process for preparing iron (lll)-based phosphate adsorbent comprising iron (III) oxy-hydroxide, insoluble carbohydrate, such as starch; and soluble carbohydrate, such as sucrose.
  • the reaction between an aqueous solution of iron (III) salt and an aqueous base is performed in the presence of starch.
  • a precipitate containing iron (III) oxy-hydroxide and starch is isolated and washed three times with water using a decanter centrifuge
  • the resulting iron oxy-hydroxide may be stabilized by adding the soluble carbohydrate to the precipitate before the iron hydroxide ages.
  • the inventors have found a dynamic process based on the use of tangential-flow filtration to desalinate and concentrate the suspension of precipitated polynuclear iron (III) oxy- hydroxide, that allows reducing considerably the production times, avoids product loss, and maintain the stability and the phosphate binding capacity of the polynuclear iron (III)- oxy-hydroxide when the product is produced at industrial scale.
  • the most common uses of tangential-flow filtration are water treatments and purifications of biomolecules where the permeate is of most value.
  • tubular filtration membranes can be effectively used to desalinate the suspension of polynuclear iron (III) oxy-hydroxide by tangential-flow filtration is unexpected since one skilled in the art would have expected that the fine particles of the precipitated polynuclear iron (III) oxy-hydroxide had settled out in the membrane. He would have also expected that the use of a dynamic system that requires a huge amount of energy had produced the degradation of the polynuclear iron (III) oxy-hydroxide.
  • the process of the present invention is easy to set up and can be easily scaled-up, it is economical since the membranes can be reused, and allows achieving high concentrations in the suspension in less time than when centrifugal devices or static decantation systems are used, without degradation of the product.
  • an aspect of the present invention relates to a process for producing an adsorbent for phosphate from aqueous medium comprising polynuclear iron oxy- hydroxide stabilized by at least one constituent that inhibits ageing of the iron oxy- hydroxide, the process comprising the following steps:
  • step b) submitting the suspension of precipitated iron (III) oxy-hydroxide of step a) to a desalinization process through tangential-flow filtration which comprises the steps of: b1 ) pumping the suspension to a tubular filtration membrane which is connected to the feed reservoir to flow parallel to the membrane face, thereby interfering ions are removed from the suspension with the permeate;
  • step b) contacting the resulting aqueous suspension of step b) with at least one constituent that inhibits ageing of the iron oxy-hydroxide selected from the group consisting of one or more carbohydrates and/or humic acid; and
  • interfering ions refers to the chloride ions which are the anions of the trivalent iron compound used as starting material.
  • cross-flow filtration or “tangential-flow filtration” are used interchangeably herein to refer to a separation process that uses a tubular filtration membrane to separate the salts in a liquid on the basis of size and that it is characterized for operation in a recirculation mode where the retentate is returned to the system as feed. It is
  • the permeate is recovered from the system in a container and the retentate is recirculated to the feed tank. Recirculation of the retentate improves salt separation effectiveness.
  • feed or “feed flow” or “feed stream” refer to the suspension comprising polynuclear iron oxy-hydroxide that is delivered to the tubular filtration membrane.
  • permeate refers to the portion of the feed that has permeated through the membrane.
  • retentate refers to the suspension that has been retained by the membrane and is enriched in a retained species.
  • microfiltration membrane is used herein to refer to a membrane that has average diameter pore size in the range of about 0.1 pm to 0.65 pm.
  • pressure inlet is used here to refer to the feed pressure on inlet side of membrane.
  • Pressure outlet is the feed pressure on outlet side of membrane.
  • Permeate pressure is the permeate pressure on outlet side of membrane.
  • the process according to the invention allows producing an adsorbent for adsorbing phosphate from aqueous medium comprising polynuclear iron (III) oxy-hydroxide stabilized by at least one constituent that inhibits ageing of the iron oxy-hydroxide. It comprises several steps disclosed in detail below.
  • the polynuclear iron oxy-hydroxide is polynuclear beta-iron oxy-hydroxide.
  • the process comprises reacting in a feed reservoir a base, which is an alkali metal compound, with iron (III) chloride in water to yield a suspension of a pH of at least 3 of precipitated iron (III) oxy-hydroxide comprising from 50 to 120 L of water per Kg of Fe (FeC ).
  • the reaction product is an iron oxy-hydroxide in colloidal form together with a salt composed of the cation of the base and the anion of the trivalent iron compound.
  • this step is carried out at a temperature comprised from 10 to 25 °C.
  • the process of the present invention is that which comprises mixing an aqueous solution of a base, which is an alkali metal compound, with an aqueous solution of an iron (III) chloride, to form the suspension of precipitated iron (III) oxy-hydroxide.
  • the base is a carbonate or a bicarbonate of an alkali metal such as sodium or potassium.
  • the base is selected from sodium carbonate, and sodium bicarbonate.
  • the base is used in the form of aqueous solution.
  • the pH is comprised from 3 to 10.
  • the pH of the reaction mixture is at least about 6.
  • the pH is 6.5.
  • the amount of base added in step a) is the amount needed to get a pH of at least 3.
  • the suspension in step a) may either be allowed to stand or it can be submitted to intervals of stirring. In a particular embodiment, several cycles of stirring/stop/stirring the suspension of precipitated iron (III) oxy-hydroxide are performed, for instance, five cycles in another particular embodiment, the time of each stirring step and of each stop step is 10-15 minutes.
  • the suspension of precipitated iron oxy-hydroxide is submitted to a desalinization process through tangential-flow filtration to remove interfering ions such as chloride ions.
  • the suspension is maintained under stirring in a feed reservoir at a temperature comprised from 10 to 25 °C to avoid degradation of the product. Preferably, the temperature is from 15 to 25 °C.
  • the concentration of iron in the suspension before the desalinization process is 50-120 L of water per Kg of Fe, which corresponds to around 0.5-2% w/w (g Fe per g of suspension) determined by complexometric titration.
  • the suspension can be submitted directly to the tangential-flow filtration or it can be first diluted and then submitted to the tangential-flow filtration.
  • the concentration of iron in the suspension of step a) is 50 L of water per Kg of Fe (FeC ).
  • an amount from 1 to 70 L of water per Kg of Fe is added before the desalinization step.
  • an amount from 30 to 70 L of water per Kg of Fe is added before the desalinization step.
  • an amount from 50 to 70 L of water per Kg of Fe is added before the desalinization step.
  • the tangential-flow filtration in comparison to the dead-end filtration, allows the solids to be kept in suspension and minimizes the build-up of a filter cake to plug or foul the membrane.
  • filtration tubular membrane refers to a selectively permeable membrane for separating a feed, into a permeate stream and a retentate stream using a tangential flow filtration process.
  • tubular membranes are not self-supporting membranes. They are located on the inside of a tube, made of a special kind of material. This material is the supporting layer for the membrane.
  • the filtration tubular membrane may be a polymeric membrane or a ceramic membrane.
  • the membrane is a polymeric membrane.
  • polymeric membranes are polyvinylidine fluoride (PVDF) and polyether sulfone.
  • PVDF polyvinylidine fluoride
  • the PVDF is commercialized as DuraponeTM.
  • the membrane is a ceramic membrane.
  • the ceramic membrane may either have one canal or a plurality of canals. Ceramic membranes have been known for a considerable number of years.
  • a ceramic membrane comprises a layer of porous ceramic material with a pore diameter of the required size.
  • the average diameter pore is comprised from 0.1 to 0.65 pm. In a particular embodiment the average diameter pore sizes of the membrane is between 0.1 pm and 0.3 pm. In another particular embodiment the average diameter pore is 0.2 pm.
  • the membrane area is comprised from 0.07 m 2 to 1.75 m 2 .
  • the ceramic column has a diameter of 25 mm and a length 1 178 mm. In another particular embodiment, the ceramic column has 23 canals of 3.5 mm of equivalent diameter.
  • the membrane may be supported on a body of coarse pore ceramic material, in particular Zr0 2 -TiC> 2 , and the body and membrane may be sintered together.
  • the support body may be an elongate element, and may have a plurality of parallel longitudinal channels each lined with a thin membrane layer of the fine-pore ceramic material.
  • the desalinization process through tangential flow filtration comprises a first step b1 ) of pumping the suspension of precipitated iron (III) oxy-hydroxide through a tubular filtration membrane which is connected to the feed reservoir, to flow parallel to the membrane face, thereby interfering ions are removed from the suspension with the permeate which passes through the membrane walls.
  • the remainder suspension is flowed back to the feed reservoir (step b2).
  • the concentration of the iron (III) oxy-hydroxide in the suspension increases when eliminating the permeate through the membrane.
  • fresh deionized water is added to the feed reservoir to continue washing the iron oxy-hydroxide
  • the process of the present invention is that which comprises adding an amount of 230 to 460 L of water per Kg of Fe during the desalinization process.
  • the conductivity of the resulting suspension is equal to or less than 3.5 mS. In a particular embodiment, the conductivity of the resulting suspension is equal to or less than 2 mS.
  • step b4) is recirculated to reduce the volume of the suspension;
  • the process according to the invention further comprises reciculating the retentate obtained in step b4) until reaching a volume of 15 to 25 L per Kg of Fe in the feed reservoir.
  • the tangential-flow filtration process is carried out at a pressure inlet comprised from 100 to 300 KPa (1- 3 bars), preferably 200 KPa (2.0 bar) and a pressure outlet comprised from 50 to 200 KPa (0.5 to 2 bars), preferably, 150 KPa (1.5 bar).
  • the permeate pressure is comprised from 75 to 150 KPa (0.75 to 1.5 bars), preferably 20-30 KPa (0.2-0.3 bars), more preferably, 30 KPa (0.3 bars).
  • the tangential-flow filtration is carried out at a temperature comprised from 15 to 25 °C.
  • the filtration is carried out in discontinuous, the suspension is first diluted and then concentrated back to the starting volume. This process is then repeated until the required concentration of salts remaining in the reservoir is reached.
  • the filtration is a continuous process.
  • the continuous process is advantageous since it requires less filtrate volume to achieve the same degree of salt reduction as discontinuous tangential flow filtration. This represents a substantial saving in time.
  • both the discontinuous and the continuous process of desalinization of the present invention are carried out in a short time at industrial scale (150 Kg), generally it it takes about 24 hours.
  • the iron content of the suspension obtained is up to 6% w/w, preferably 2 to 6% w/w, most preferably, around 2-4% w/w (g Fe per g of suspension). In a particular embodiment, around 5.2% w/w of Fe.
  • the pH of the suspension is generally in the range of approximately 6.5 to 7.5 before further constituents are added.
  • the subsequent step comprises contacting the resulting aqueous suspension of step b) with at least one constituent that inhibits ageing of the iron oxy-hydroxide.
  • the at least one constituent that inhibits ageing of the iron oxy-hydroxide is selected from the group consisting of one or more carbohydrates and/or humic acid.
  • the constituent that inhibits ageing of the iron oxy- hydroxide is a carbohydrate selected from the group consisting of starch, sucrose, and mixtures thereof.
  • the constituent is preferably added in solid form.
  • the amount of carbohydrates or humic acid is preferably selected so that at least 0.5 g carbohydrate or humic acid are added per g of iron (calculated as Fe).
  • the maximum content of carbohydrates and/or humic acid is not subject to any limits.
  • the content of carbohydrates is from 5 to 60% by weight (w/w).
  • Soluble carbohydrates can be used such as sugars, e.g. agarose, dextran, dextrin, dextran derivatives, cellulose and cellulose derivatives, saccharose, maltose, lactose, or mannitol.
  • the carbohydrate is starch, sucrose, dextrin, starch, or mixtures thereof.
  • starch as used herein includes any conventionally used starch products (such as potato starch, corn starch, rice starch, tapioca starch) in native, pregelatinized, degraded, modified and derivatized forms.
  • the process comprises a step d) which comprises drying the suspension thus obtained.
  • the drying can be carried out, for example, by concentration in vacuum or by spray drying.
  • the maximum iron content in the final product is around 40% w/w. In a particular embodiment the iron content is at least 20% w/w.
  • the iron content is given, it has been determined by complexometric titration following the method included in the Examples.
  • the polynuclear beta-iron oxy-hydroxide adsorbent obtained following the process of the present invention shows a good phosphate-binding capacity equal to the adsorbent obtained by the process using static washing instead of tangential-flow filtration at small scale, which evidence that following the process of the present invention, the product does not suffer more degradation when it is prepared at industrial scale.
  • the phosphate binding capacity is determined by spectrophotometric analysis as illustrated in the
  • the phosphate adsorbent of the present invention provides a phosphate binding capacity of at least 0.21 mgP/mgFe.
  • the phosphate binding capacity is equal to or higher than 0.23 mgP/mgFe.
  • the preparation process according to the invention allows obtaining a phosphate adsorbent for adsorbing phosphate from aqueous medium comprising polynuclear beta- iron oxy-hydroxide stabilized by at least one constituent that inhibits ageing of the iron oxy-hydroxide.
  • the adsorbents thus obtained are suitable for the adsorption of phosphates from aqueous solutions, for example, for the adsorption of inorganic phosphate and phosphate bonded to foodstuffs from body fluids, chyme and foodstuffs.
  • Diameter 25” - length 1178 mm.
  • Iron content (complexometric titration): The method is based on USP ⁇ 541 > and Ph. Eur. (2.2.20).
  • Test solution Transfer 1.5 g of the sample, accurately weighed, to a 100 ml. volumetric flask, dissolve with 10 mL of cone. HCI and 10 ml. of water at 45°C, allow the solution to cool at room temperature and dilute to volume with water. Prepare in duplicate.
  • Each mL of 0.1 N CuS0 4 is equivalent to 5.58 mg of Iron.
  • Phosphate adsorption method of analysis (by spectrophotometric analysis): The method is based on USP ⁇ 851 > / Ph. Eur. (2.2.25).
  • Phosphate stock solution Transfer 0.717 g of KhhPCU, accurately weighed, into a 500 mL volumetric flask, dissolve and dilute to volume with water. Transfer 5.0 mL of this solution to a 50 mL volumetric flask and dilute to volume with water.
  • Mix solution mix one part of Solution A and six parts of Solution B. Prepare the solution just before use and maintain the solution in an ice bath during the samples preparation.
  • 0.65 ppm Phosphorous solution Transfer 1.0 mL of the phosphate stock solution to a 50 mL volumetric flask and dilute to volume with water.
  • 1.30 ppm Phosphorous solution Transfer 2.0 ml. of the phosphate stock solution to a 50 ml. volumetric flask and dilute to volume with water.
  • 1.96 ppm Phosphorous solution Transfer 3.0 ml. of the phosphate stock solution to a 50 ml. volumetric flask and dilute to volume with water.
  • Phosphorous solution Transfer 5.0 ml. of the phosphate stock solution to a 50 ml. volumetric flask and dilute to volume with water.
  • 0.16 ppm Phosphorous solution Transfer 5.0 ml. of the 0.65 ppm Phosphorous solution to a 20 mL volumetric flask and dilute to volume with water.
  • 0.065 ppm Phosphorous solution Transfer 5.0 mL of the 0.65 ppm Phosphorous solution to a 50 mL volumetric flask and dilute to volume with water.
  • Phosphorous spiking solution Transfer 20.52 g of Na3P04-12H20, accurately weighed, to a 1 L volumetric flask, dissolve and dilute to volume with water.
  • Test solution Accurately weigh 250.0 mg of sample into a 50 mL centrifuge tube, Add 10.0 mL of the Phosphorous spiking solution. Adjust the pH to 3.0 with 6N acetic acid and allow the suspension to react for 2 hours at 37 °C. Thereafter, centrifuge the suspension at 4000 rpm during 10 min. Transfer the supernatant liquor to a 25 mL volumetric flask and dilute to volume with water. Transfer 1.0 mL of this solution to a 100 mL volumetric flask and dilute to volume with water. Prepare the sample in duplicate. Apply the molybdenum blue method to Phosphorous standards solutions and Test solutions.
  • the concentration of iron after the reaction and before the desalinization was 1 8%w/w (g Fe per g of suspension determined by complexometric titration).
  • Second decantation The reaction mixture was settled during 12 hours and 400 L of supernatant were being removed. 400 L of deionized water were added to the reactor and the reaction mixture was stirred for 15 minutes at 10-25°C (30 rpm). Then stirring was stopped.
  • Third decantation The reaction mixture was settled during 17 hours and 660 L of supernatant were being removed. 660 L of deionized water were added to the reactor and the reaction mixture was stirred for 15 minutes at 10-25°C (30 rpm). Then stirring was stopped.
  • the process of desalinisation ended after 6 days.
  • To the reaction mixture (632,75 kg, 4.3% of an iron content, determined by complexometric titration) were added 43,6 Kg of potato starch and 43,8 Kg of sucrose.
  • An aliquot of the reaction mixture was concentrated to 35°C in a rotary evaporator and dried at 35°C under high vacuum.23.2 g of powder with iron content 20.94% (determined by complexometric titration) was obtained.
  • Phosphate binding capacity was determined (by spectrophotometric analysis); 0.22 mgP/mgFe.
  • the rest of the batch was dried by spray-drying (146.34 Kg of Sucroferric oxy-hydroxide was obtained).
  • the suspension was concentrated to 35°C in a rotary evaporator and dried at 35°C under high vacuum. 19.48 g of powder with iron content 16.6% (determined by complexometric titration) was obtained. Phosphate binding capacity was determined (by spectrophotometric analysis); 0.19 mgP/mgFe.
  • comparative Example 1 shows that when the process disclosed in the prior art (cf. Example 1 of US6174442B1 ) is carried out at industrial scale (Batch: 150 Kg), a long time is required to carry out the decantations.
  • Comparative Example 2 shows that in conditions of prolonged stirring the product degrades. Therefore, it is unexpected that a dynamic process such as the tangential filtration used in the present invention where the mixture is continuously stirred could work since it would be expected that the product suffered degradation.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
EP19742785.9A 2018-07-30 2019-07-29 Verfahren zur herstellung eines adsorbens für phosphat in wässrigem medium Withdrawn EP3829761A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP18382570 2018-07-30
PCT/EP2019/070384 WO2020025552A1 (en) 2018-07-30 2019-07-29 Process for preparing an adsorbent for phosphate in aqueous medium

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EP3829761A1 true EP3829761A1 (de) 2021-06-09

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3932535A1 (de) 2020-07-01 2022-01-05 Vifor Fresenius Medical Care Renal Pharma, Ltd. Verfahren zur herstellung von durch kohlenhydrate und/oder huminsäure stabilisierten mehrkernigen eisenverbindungen

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Publication number Priority date Publication date Assignee Title
US4970079A (en) 1989-06-05 1990-11-13 Purdue Research Foundation Method and composition of oxy-iron compounds for treatment of hyperphosphatemia
DE19547356A1 (de) 1995-12-19 1997-06-26 Vifor Int Ag Adsorbens für Phosphat aus wäßrigem Medium, dessen Herstellung und Verwendung
ES2526171T3 (es) * 2006-12-14 2015-01-07 Novartis Ag Adsorbente de fosfato a base de hierro (III)-carbohidratos
TWI468167B (zh) 2007-11-16 2015-01-11 威佛（國際）股份有限公司 藥學組成物

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