WO2010119484A1 - Procédé de récupération de cristaux à partir d'une bouillie de cristallisation - Google Patents

Procédé de récupération de cristaux à partir d'une bouillie de cristallisation Download PDF

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WO2010119484A1
WO2010119484A1 PCT/JP2009/001763 JP2009001763W WO2010119484A1 WO 2010119484 A1 WO2010119484 A1 WO 2010119484A1 JP 2009001763 W JP2009001763 W JP 2009001763W WO 2010119484 A1 WO2010119484 A1 WO 2010119484A1
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pressure
filtration
crystals
slurry
washing
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PCT/JP2009/001763
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English (en)
Japanese (ja)
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原徳明
豊嶋弘幸
山▲崎▼初太郎
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株式会社日立プラントテクノロジー
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Priority to CN2009801587091A priority Critical patent/CN102395553A/zh
Priority to PCT/JP2009/001763 priority patent/WO2010119484A1/fr
Priority to MX2011010502A priority patent/MX2011010502A/es
Publication of WO2010119484A1 publication Critical patent/WO2010119484A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • B01D9/0045—Washing of crystals, e.g. in wash columns
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

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  • the present invention relates to a crystal recovery method for improving the purity of recovered crystals when recovering the crystals by continuous filtration in which the steps of filtration, washing, liquid removal and peeling are repeatedly performed under pressure from the crystal precipitation slurry.
  • Crude terephthalic acid is dissolved in high-temperature water, hydrotreated in the presence of a reduction catalyst, 4-CBA (4-carboxybenzaldehyde) contained in the crude terephthalic acid is reduced to p-toluic acid,
  • 4-CBA 4-carboxybenzaldehyde
  • p-toluic acid Widely commercialized is a method for producing purified high-purity terephthalic acid by collecting crystals by solid-liquid separation from a crystallization slurry produced by reducing the pressure stepwise through a plurality of crystallization tanks connected in series. Has been done.
  • p-toluic acid contained in the purified aqueous solution of terephthalic acid has higher solubility and molecular weight than p-toluic acid in the process of precipitation of terephthalic acid crystals and separation and recovery of the precipitated crystals. This is because it is easily separated from the terephthalic acid crystal because of its crystal structure. For this reason, a purification method has been adopted in which 4-CBA is hydroreduced into p-toluic acid with good separability and then terephthalic acid is crystallized and recovered.
  • Patent Documents 1, 2, and 3 Japanese Patent Publication Nos. 47-49049 and 53-24057
  • Patent Documents 4 and 5 Japanese Patent Application Laid-Open No. 11-228492
  • Patent Documents 4 and 5 Specific Tables
  • the separation property of p-toluic acid in the recovery step is that terephthalic acid crystals are separated at high temperature from the difference in solubility between terephthalic acid and p-toluic acid (Table 1 of Patent Document 1 is shown in FIG. 5). Since the separability from p-toluic acid is better, the temperature and pressure of the crystallization slurry in the final crystallization tank are maintained high, and the crystallization slurry is reduced without lowering the temperature (pressure). The terephthalic acid crystals are recovered by solid-liquid separation.
  • the filtration system recovery system
  • the filter cake is put into a high-pressure filter cell-type filtration zone in which the filter cake is formed by forming a water reservoir layer that covers the filter cake in the filter cell with wash water at a temperature of about 38 to 205 ° C.
  • the pressure on the low pressure side of the filtration surface is filtered and separated and washed under a high pressure (pressure on the filtration surface side) so that the pressure on the low pressure side of the crystallization slurry is not substantially lower than the generation pressure of the crystallization slurry.
  • a method for producing terephthalic acid has been proposed, but the final crystallization stage pressure is crystallized at 1.5 to 15 bar, and the pressure on the filtration side is preferably 2 to 15 bar, ie high temperature filtration. Has proposed.
  • the cleaning solution used to remove the p-toluic acid-containing filtrate remaining in the terephthalic acid crystal filter cake should avoid the problem of flushing or cooling, which can cause the risk of precipitation impurities. And are introduced at substantially the same temperature.
  • none of the above proposals proposes filtration separation of the crystallization slurry at high temperature and high pressure in order to recover the crystals of purified terephthalic acid. The actual situation is that cleaning is performed using this cleaning solution.
  • the temperature and pressure of the crystallization final tank are maintained and the crystals are separated by centrifugal sedimentation (centrifugal settling method without using a filter medium).
  • the separated crystals (wet cake) are reslurried with a washing solution (water), and then centrifuged again (sedimentation).
  • the first-stage separated crystals are replaced by washing by slurrying and terephthalic acid by a two-stage centrifuge method. Crystals are also collected (Patent Document 1).
  • Japanese Patent Publication No.47-49049 Japanese Patent Publication No.53-24057 JP 11-228492 A JP-T 6-506461 JP 7-507291 JP Japanese Unexamined Patent Publication No. 1-299618
  • the separation method of filtration with reduced p-toluic acid content in recovered terephthalic acid with improved separation of p-toluic acid In general, a separation method of high temperature and high pressure (pressurization) is adopted. Therefore, in the recovery of purified terephthalic acid crystals, it is preferable from the separation of p-toluic acid that the final crystallization tank slurry is separated as high as possible (up to 205 ° C) and at a high pressure. High-cost and high-pressure equipment has been required as a centrifuge) and its system (such as separation wet cake take-out, separation liquid / wash liquid receiving tank and pressurized circulation gas system).
  • the two-stage separation method by centrifugation has problems such as requiring a large amount of washing water to reslurry with 3 to 5 times the water of the separated crystals (Japanese Patent Publication No. 47-49049).
  • the present invention is based on the above-mentioned actual situation of the production technology of high-purity terephthalic acid.
  • a relatively low-pressure filtration system is used to recover impurities contained in a normal amount of washing liquid.
  • the present invention provides a filtration and washing method in which separability of (p-toluic acid) becomes better.
  • the maximum (operation) pressure of the filtration system (filter) is 6 kg / cm 2 G
  • the terephthalic acid crystallization slurry has a relatively low loss of terephthalic acid to the filtrate, 160 ° C (water vapor pressure: 5.3 kg)
  • the purpose of the present invention was to improve the separability of p-toluic acid by using a filter and a system for the temperature below / cm 2 G).
  • the high-temperature and high-pressure filtration system is a conventional vacuum rotary cylinder filter (rotary vacuum filter) and a vacuum belt filter type filter with a pressure of 6 kg / cm 2 G (withstand pressure 9 kg / cm 2 G). It is designed to be installed in a casing (high pressure vessel) and can be filtered. Withstand pressure devices with a maximum working pressure of 6 kg / cm 2 G for relatively low pressure specifications, even for incidental equipment and accessories accompanying filtration. The equipment cost is suppressed by using the
  • terephthalic acid loss (0.33gr / 100grH2O) due to dissolution in the filtrate during filtration separation is about 1 of the recovered terephthalic acid crystal amount. Since the amount was less than% by weight, crystals were recovered from the terephthalic acid crystallization slurry in which the maximum operation temperature of the final crystallization tank was set to 160 ° C.
  • the differential pressure between the high pressure side and low pressure side of the filtration surface in the filter is usually 0.2 to 0.9 kg / cm 2 (about 0.5 kg / cm 2 ), the maximum is 160 ° C (water vapor pressure: 5.3 kg /
  • a pressure filtration system with an operating pressure of up to 6 kg / cm 2 G can be carried out on the crystallization slurry of cm 2 G), which is a preferred method for continuous filtration with reduced clogging of the filter medium (filter cloth).
  • the filtration separation temperature does not decrease from the separability of p-toluic acid, but in the method of the present invention, at least the solubility ratio (p-toluic acid / terephthalic acid) in FIG. It was intended to perform filtration separation at a temperature of 30 or higher (130 ° C. or higher).
  • the pressure in the filtration system is about 2.5 to 6 kg / cm 2 G (withstand pressure 9 kg / cm 2 G).
  • a purified terephthalic acid crystallization slurry of about 130-160 ° C. can be obtained as an effect of separating impurities, which becomes a higher temperature recovery step.
  • the present invention relates to a method for recovering crystals by continuous filtration in which a slurry consisting of a solvent and precipitated crystals is repeatedly filtered, washed, and peeled in order.
  • the filtration of the slurry is performed by pressurizing the high pressure side of the filtration surface (slurry side) using the circulating solvent vapor-containing gas
  • the crystal separated by filtration is washed with a washing liquid accompanied by vapor generation using a washing liquid heated to a vapor pressure exceeding the pressure on the high pressure side of the filtration surface.
  • the present invention provides the crystal recovery method described above, wherein in the filtration step, a terephthalic acid aqueous solution in which crude terephthalic acid is dissolved in high-temperature and high-pressure water is reduced with hydrogen in the presence of a reduction catalyst.
  • the cleaning liquid (water) heated to a vapor pressure exceeding the pressure on the high pressure side of the filtration surface is supplied, and the crystals separated by filtration with the washing liquid accompanied by the generation of vapor are washed.
  • cleaning water heated to a vapor pressure of about 2.7-7Kg / cm 2 G (about 140-170 ° C) or higher, which exceeds the high-pressure side pressure, is supplied and separated by washing water with steam generation. The crystal is washed.
  • the present invention also provides cleaning water heated to a vapor pressure of about 7 Kg / cm 2 G (about 170 ° C.) or higher in the recovery of crystals at about 151 ° C. (about 4 Kg / cm 2 G) of the described crystallization slurry.
  • a vapor pressure of about 7 Kg / cm 2 G (about 170 ° C.) or higher in the recovery of crystals at about 151 ° C. (about 4 Kg / cm 2 G) of the described crystallization slurry.
  • the rate of steam generation from the superheated washing water corresponds to about 2% or more, more preferably about 4% or more.
  • the steam pressure of the superheated washing water is about 16.5Kg / cm 2 G (about 205 ° C, steam generation rate 9.6%) or more, the reduction effect of contained impurities (p-toluic acid) tends not to change. A high-pressure equipment burden is required.
  • an overheated washing liquid that has a vapor pressure exceeding the high pressure on the filtration surface is supplied, and about The filter-separated crystals are washed with a washing liquid with 2 to 10% vapor generation.
  • the present invention provides a crystallization slurry obtained by a crystallization method in which the pressure of the purified terephthalic acid aqueous solution is gradually reduced and simultaneously the temperature is lowered, and the temperature in the final crystallization tank (about 130 to 160 ° C) is increased.
  • a method of maintaining and supplying this crystallization slurry to a continuous filter of a filtration system pressurized to about 2.5 to 6 kg / cm 2 G and recovering purified terephthalic acid crystals by filtration separation A cleaning liquid (water) heated to a vapor pressure exceeding the pressure is supplied to a filter washing zone, and the cake separated by filtration is washed while at least generating steam.
  • the content of p-toluic acid in the recovered terephthalic acid crystal can be improved.
  • the p-toluic acid-containing liquid remaining in the cake after filtration is thoroughly replaced with a washing solution and washed with washing water at a temperature substantially equal to or lower than that of the separation cake.
  • Patent Document 1 which has been considered preferable, there are impurities (p-toluic acid) that remain due to the physical and chemical affinity of the crystal, such as adhesion and adsorption of the cake layer to the crystal surface, and are eliminated only by substitution washing. There seems to be a limit amount that cannot be obtained. The present inventors have intensively studied to further reduce these limit amounts, and as a result have reached the present invention.
  • the amount of impurities adhering to and adsorbing on the cake layer crystal surface in accordance with the concentration of the filtrate impurity (p-toluic acid) in the filtration separation is at least from the temperature at the time of filtration separation by the introduced superheated water. It is cleaned with a steam-liquid mixed phase cleaning liquid with high temperature steam. In this cleaning, the flow rate of the cleaning solution is increased by steam, the crystal surface is activated by high temperature, and the desorption and desorption of impurities are promoted to dissolve and eliminate, thus reducing p-toluic acid. Appears. As a result, detachment was promoted even in the water content of the recovered recovered terephthalic acid crystal cake, and the wet rate tended to decrease.
  • a pressure filtration system capable of pressurization to 2.5 to 6 kg / cm 2 G can be used, and the cleaning liquid heated to a vapor pressure that exceeds the system pressure is supplied. This is achieved by using equipment that can be used to supply at least a cleaning liquid with steam generation to the cleaning zone of the filter.
  • the cleaning solution that has been heated to a vapor generation rate exceeding about 2%, preferably about 4% or more, the effect of reducing contained impurities (p-toluic acid) is more prominent. Become.
  • the improvement in the separation property of p-toluic acid due to the improvement to the superheated cleaning liquid accompanied by the generation of steam can achieve the same effect as the filtration / separation effect at higher pressure (high temperature) in the conventional method,
  • the pressure strengthening measures of the filtration system equipment for p-toluic acid content could be suppressed.
  • stepwise flash crystallization proposed in Patent Document 2 (Japanese Patent Publication No. 53-24057), Japanese Patent Application Laid-Open No. 2006-96710, etc.
  • a crystallization slurry is produced by the method, and in the crystal recovery step, pressure filtration according to proposals of Patent Document 6 (Japanese Patent Laid-Open No. 1-299618), Patent Document 5 (Special Table of Hei 7-507291), etc.
  • the method of the present invention is not limited to the production of high-purity terephthalic acid.
  • recrystallization from the crystallization slurry by recrystallization which is expected to reduce the impurity content by crystallization, is also proposed. It can be applied to filtration and washing for collecting crystals, and a favorable effect can be expected.
  • the separability of impurities is achieved. Can be improved, and high-purity crystals can be recovered, contributing to the improvement of product value.
  • the improvement of the purity of high-purity terephthalic acid (purified terephthalic acid) reduces the burden on the production of crude terephthalic acid.
  • the effect of reducing the content of p-toluic acid (impurities) in high-purity terephthalic acid can be converted into an allowable amount for increasing the 4-CBA content of crude terephthalic acid. It will also contribute to mitigation.
  • the flowchart of the filtration system of this invention Example.
  • the schematic diagram of the section of a pressurization type rotary cylindrical filter similarly.
  • the characteristic diagram showing the relationship between the wet rate (wt%) of the terephthalic acid discharge cake and the p-toluic acid content (ppm) with respect to the washing water temperature.
  • a table showing the relationship between the wet rate (wt%) of the terephthalic acid discharge cake and the p-toluic acid content (ppm) with respect to the washing water temperature.
  • FIGS. 1 and 2 Schematic diagrams of an example of a filtration system and a filter for carrying out the method of the present invention are shown in FIGS. 1 and 2, respectively.
  • the inside of the casing is pressurized to about 2.5 to 6 kg / cm 2 G using a pressurized circulating gas (containing steam) of an inert gas.
  • a cylindrical rotary filter 11 is rotatably installed inside the casing, and is filtered in turn while rotating clockwise from the filtration area 13 at the bottom to the upper cleaning / drainage area 14 and then the peeling area 15. -Collect the filter cake through each step of washing and peeling.
  • the crystallization slurry is supplied from the slurry supply tank 1 to the bottom 12 of the casing of the filter 2 by a pressure pump or the like, and is added in the filtration zone 13 at the bottom of the rotary filter 11 where the liquid level of the crystallization slurry is maintained. Filtered by pressure and suction. The surplus slurry for this filtration is discharged from the filter 2 through the overflow pipe and returned to the slurry supply tank 1 or the like, but is discharged to a lower pressure than the casing internal pressure, so that the casing internal pressure and the slurry temperature are maintained.
  • the pressure shut-off and slurry discharge control are performed with the discharge valve.
  • the filter cake peeled by the inert gas pulse supply in the peeling zone 15 of the rotary filter material 11 is maintained in the pressure buffer zone M ⁇ such as a two-stage valve (slide valve) or a rotary valve in order to maintain the casing internal pressure. 2 is discharged and collected.
  • the pressure buffer zone M ⁇ such as a two-stage valve (slide valve) or a rotary valve in order to maintain the casing internal pressure. 2 is discharged and collected.
  • the rotating cylindrical filter medium 11 sucks the filtrate (differential pressure 0.2 to 0.9 kg / cm) while rotating the attached cake filtered by pressurizing (about 2.5 to 6 kg / cm 2 G) in the filtration region 13 at the bottom. 2 ) Eliminate and move to cleaning / dehydration zone 14.
  • cleaning liquid (water) 17a heated to a vapor pressure exceeding the casing internal pressure is introduced through the flash valve 17, and the introduced cleaning liquid 17a is subjected to pressurization of the circulating gas (about 2.5 to At 6 kg / cm 2 G), at least with the generation of steam, it is sucked out together with the residual filtrate inside the cake.
  • the effect As for the generation ratio of the cleaning liquid vapor, the effect (cleaning effect, cake wetting rate) appears by supplying the cleaning liquid that has been heated to a temperature accompanied by the generation of steam exceeding about 2% of the supplied cleaning liquid volume. The effect becomes favorable by the cleaning liquid having a temperature of the steam generation exceeding.
  • the steam generation effect tends to be small in the overheated cleaning liquid at a temperature where the steam generation amount exceeds 10%. Therefore, it is effective to perform cleaning with a cleaning liquid that has been heated to a temperature at which 2 to 10% of the cleaning liquid generates steam.
  • the cleaning liquid superheated through the heater E-2 to the liquid temperature having a vapor pressure exceeding the casing internal pressure on the flash valve 17 controlled to a constant pressure exceeding the casing internal pressure is in the casing at a pressure exceeding the flash valve control pressure. And supplied to the cake in the washing zone 14 while flushing through the flush valve 17.
  • the rotating filter material 11 rotates and the adhering cake moves to the peeling zone 15, and a pulsed gas is sprayed from the back side of the filtration surface to a gas pressure higher than the casing internal pressure (+0.1 to 0.5 kg / cm 2 ). Removes the filter cake.
  • the exfoliated filter cake is transferred to a dryer which is usually under atmospheric pressure through a special valve that suppresses fluctuations in the casing internal pressure, and is discharged and produced as a dried product (terephthalic acid) powder.
  • the filtrate and washing drained liquid withdrawn by suction are individually supplied to the filtrate receiving tank 4 and the washing drain receiving tank (not shown) together with the suction vapor, or to the same filtrate / washing drain receiving tank 4.
  • the filtrate and washing drained liquid withdrawn by suction are individually supplied to the filtrate receiving tank 4 and the washing drain receiving tank (not shown) together with the suction vapor, or to the same filtrate / washing drain receiving tank 4.
  • it is temporarily retained and transferred to each processing step.
  • the vapor mixed gas (non-condensed gas) separated in the receiving tank 4 is slightly cooled by the cooler E-3 for temperature stabilization, and the condensed liquid is recovered in the receiving tank 4 by the gas-liquid separation tank 5.
  • the vapor mixture gas component that could not be condensed is supplied to the suction side of the compressor M-4, and the pressure regulator PIC-2 for the discharge pressure of the compressor M-4 is used to supply the excess (inert gas) and the excess. It discharges and is supplied to the filter 2 as circulating gas.
  • Circulating gas from the compressor M-4 is adjusted to the system pressure by the pressure controller PIC-2 for pressurization of the filtration system, and sent to the internal pressure of the filter 2 and the pressure buffer area for discharging the peeled cake. . Meanwhile, the circulating gas is adjusted to a temperature equal to or higher than the supply slurry temperature (TIC-2) by the heater E-4.
  • the supply of the circulating gas to the filter 2 is preferably blown into the area before the cleaning area 14 in order to suppress the evaporation of the filtrate.
  • the above method not only recovers crystals from purified terephthalic acid crystal slurry in the production of high-purity terephthalic acid, but also recovers crude terephthalic acid crystals from crystallization slurry obtained by oxidation reaction. It can be applied for reduction.
  • the present invention can be applied to the reduction of impurities contained in the recovery of crystals from a crystallization slurry by a crystal generated by crystallization and a solvent.
  • the system pressure of the pressure filtration system used for those methods becomes the pressure which does not exceed 6 kg / cm ⁇ 2 > G, and the method implemented under comparatively low pressure is taken.
  • Crystallized terephthalic acid slurry is a high-purity terephthalic acid production plant by hydrorefining crude terephthalic acid.
  • a high temperature crystallization terephthalic acid slurry from the slurry supply tank 1 was supplied to a pressure filtration system, and the crystal recovery method was performed by filtering and separating the crystallization slurry under pressure.
  • the pressure filtration system uses a rotary cylindrical filter 2 with a filtration area of 0.2 m 2 mounted in a pressure-resistant 7 kg / cm 2 G casing, a cake receiving tank 3, a filtration mother liquor / washing drainage / receiving tank 4, 1 is a flow system within a dotted line in FIG. 1 including a gas-liquid separation tank 5, a compressor M-4, a cleaning liquid heater E-2, and the like.
  • the terephthalic acid crystallization slurry from the slurry supply tank 1 (final crystallization tank) is supplied to the bottom of the filter 2 pressurized to 5.3 kg / cm 2 G (steam-containing N 2 gas) by the compressor M-4.
  • pressure (suction) filtration is performed at the immersion part (bottom part 12 in FIG. 2) of the cylindrical rotary filter material 11.
  • the rotary filter medium 11 rotates clockwise at a speed of 2 RPM, and the filter cake adhering to the slurry immersion part is washed with a washing liquid 17a introduced from the upper part of the rotary filter medium 11 while sucking and draining the filtered mother liquor.
  • the filter cake is peeled off by pulse pressure (5.5 kg / cm 2 G) from the inside of the filter medium by the gas supply pulser M-1.
  • the peeled filter cake is discharged to the cake receiving tank 3 under normal pressure by adjusting the pressure with a pressure buffer valve M-2 blocked by two slide valves.
  • Wash water is supplied under pressure through a flush valve 17 set to about 20 kg / cm 2 G and injected into the washing zone of the filter 2.
  • the heater E-2 is heated (TIC-1) to each cleaning water set temperature shown in FIG. 4, and the washing liquid 17a is flushed (released) in the washing zone 14 to wash the filter cake.
  • Washing water whose washing water temperature exceeds 160 ° C. water vapor pressure 5.3 kg / cm 2 G will wash the filter cake as washing water accompanied by at least the generation of water vapor at the same time as flushing.
  • the filtered (mother) liquid sucked and filtered in the filtration area 13 at the bottom of the rotary filter 11 and the washed waste liquid sucked and washed in the upper washing / drainage area 14 are simultaneously filtered mother liquor / washing waste liquid / receiving tank 4. And is discharged from the lower portion of the receiving tank 4 as a mixed solution.
  • the suction gas containing the vapor separated from the filtered mother liquor / cleaning drainage / reception tank 4 is cooled to about 145 ° C. from the top through the cooler (condenser) E-3, and the condensate is cooled in the gas-liquid separation tank 5. Collected.
  • the vapor / gas component which has not been condensed is supplied as a circulating gas to the suction of the compressor M-4. Circulating gas from compressor M-4 is circulated after adjusting to 5.3 kg / cm 2 G with pressure controller PIC-2 and 151 ° C with temperature controller TIC-2 to pressurize the filtration system. .
  • the cake in the cake receiving tank 3 was obtained by discharging the terephthalic acid cake under atmospheric pressure using a screw type discharge machine M-3 attached to the lower part. A sample of the discharged cake was collected, and the wet rate and the amount of p-toluic acid containing terephthalic acid crystals were measured.
  • FIG. 3 is a characteristic diagram showing the relationship between the wet rate (wt%) of the terephthalic acid discharge cake and the p-toluic acid content (ppm) with respect to the temperature, pressure, and evaporation rate of the washing water in each example shown in FIG. is there.
  • the p-toluic acid content of 150 ppm or less which is the production standard for the production of high-purity terephthalic acid, can be achieved at the washing water temperature of Example 2 (washing water temperature 180 ° C., evaporation rate 4.2%) or more. I understood.

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Abstract

Dans une récupération classique de cristaux d'acide téréphtalique pur, une séparation tout en maintenant la bouillie du réservoir de cristallisation final à la température la plus élevée possible (maximum 205°C) et à une pression élevée est préférée du point de vue de la facilité de séparation de l'acide p-toluylique, et une installation haute température haute pression coûteuse est nécessaire pour le séparateur (filtre, centrifuge) et le système associé (retrait du gâteau de séparation humide, réservoirs de réception du liquide de séparation/liquide de lavage et un système de gaz de circulation pressurisé, etc.). L'invention porte sur un procédé efficace pour la filtration et le lavage, qui est un procédé pour récupérer des cristaux à partir d'une bouillie de cristallisation comprenant un solvant et des cristaux précipités par filtration sous pression, dans lequel la teneur des impuretés dans les cristaux récupérés est diminuée par l'emploi d'un système de filtre utilisant une pression relativement faible. Dans la filtration sous pression à pas plus d'environ 6 kg/cm2 au manomètre, le gâteau de filtration est lavé par l'emploi d'une solution de lavage surchauffée jusqu'à ce que la pression de vapeur de celle-ci dépasse la pression du système filtrant, la solution étant fournie au moins comme solution de lavage avec traitement à la vapeur. On effectue le lavage en adressant une solution de lavage surchauffée jusqu'à ce que la proportion de vapeur produite dépasse environ 2 %, et de préférence une solution de lavage surchauffée jusqu'à ce que cette proportion soit d'au moins environ 4 %.
PCT/JP2009/001763 2009-04-16 2009-04-16 Procédé de récupération de cristaux à partir d'une bouillie de cristallisation WO2010119484A1 (fr)

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CN2009801587091A CN102395553A (zh) 2009-04-16 2009-04-16 由晶析浆液回收结晶的方法
PCT/JP2009/001763 WO2010119484A1 (fr) 2009-04-16 2009-04-16 Procédé de récupération de cristaux à partir d'une bouillie de cristallisation
MX2011010502A MX2011010502A (es) 2009-04-16 2009-04-16 Metodo para recuperar cristales de una suspension cristalizada.

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WO2014049793A1 (fr) * 2012-09-27 2014-04-03 三菱化工機株式会社 Procédé de fonctionnement d'un dispositif de filtration rotatif à chambre unique mis sous pression
JP2017502966A (ja) * 2013-12-31 2017-01-26 ビーピー・コーポレーション・ノース・アメリカ・インコーポレーテッド 非乾燥ロータリープレッシャーフィルターを用いる固液分離
WO2020006446A1 (fr) * 2018-06-29 2020-01-02 Bp Corporation North America Inc. Processus de séparation solide-liquide utilisant un filtre à larges pores
CN114990645A (zh) * 2022-06-30 2022-09-02 深圳惠科新材料有限公司 硫酸铜晶体回收装置及方法

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CN102847338B (zh) * 2012-09-13 2014-05-14 宁波明欣化工机械有限责任公司 一种酸吸收结晶装置及其工艺流程
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