CA1142419A - Process and apparatus for removing sludge from salt baths - Google Patents

Process and apparatus for removing sludge from salt baths

Info

Publication number
CA1142419A
CA1142419A CA000347843A CA347843A CA1142419A CA 1142419 A CA1142419 A CA 1142419A CA 000347843 A CA000347843 A CA 000347843A CA 347843 A CA347843 A CA 347843A CA 1142419 A CA1142419 A CA 1142419A
Authority
CA
Canada
Prior art keywords
bath
sludge
salt
filter
melt
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.)
Expired
Application number
CA000347843A
Other languages
French (fr)
Inventor
Christian Scondo
Egon Weinhold
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.)
Evonik Operations GmbH
Original Assignee
Degussa GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Degussa GmbH filed Critical Degussa GmbH
Application granted granted Critical
Publication of CA1142419A publication Critical patent/CA1142419A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/34Methods of heating
    • C21D1/44Methods of heating in heat-treatment baths
    • C21D1/46Salt baths
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/0012Settling tanks making use of filters, e.g. by floating layers of particulate material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/003Sedimentation tanks provided with a plurality of compartments separated by a partition wall
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/24Feed or discharge mechanisms for settling tanks
    • B01D21/245Discharge mechanisms for the sediments
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/11Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
    • B01D29/13Supported filter elements
    • B01D29/23Supported filter elements arranged for outward flow filtration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/60Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor integrally combined with devices for controlling the filtration
    • B01D29/605Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor integrally combined with devices for controlling the filtration by level measuring
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D35/00Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/26Filters with built-in pumps filters provided with a pump mounted in or on the casing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D35/00Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/30Filter housing constructions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Filtering Materials (AREA)
  • Treatment Of Sludge (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

ABSTRACT OF THE DISCLOSURE
The removal of sludge from polluted salt baths, parti-cularly nitride salt baths, has been very time-consuming hereto-fore and resulted in interruptions of the operation and in varying qualities of the treat material. These disadvantages are removed by continuously purifying the salt melt during the operation of the baths in that the melt is continuously passed over a filter. The apparatus preferably comprises an air compressor immersed in the melt and a filter disposed above and outside the bath.

Description

1~2~9 The present invention relates to a process and an apparatus for removing sludge from polluted salt melts such as those used, for example, for nitriding metals, preferably iron containing metals. These salt baths are used on a large scale and consist primarily of carbonates and cyanates of alkali metals. Some of these baths also contain alkali metal cyanides.
These salt melts are normally operated at an operating temperature of 560 to 600C.
During the treatment of structural members of an iron material these baths become clogged with sludge to a varying degree, i.e., in that adhering steel particles, as for example, turnings or grindings, accumulate on the bottom of the treatment vessel or remain in a finely dlvided form in a state of suspension.
Likewise the treatment of scaled or unmachined surfaces (casting or forging skin) result in the pollution of the bath. Further-more the slude component is also formed in that nitride particles scale off from the charaing aids, such as baskets or racks, after repeated treatment and remain in the bath. The "sludge" thus formed consists chiefly of iron nitride and iron oxide.
Other salt baths, as for example, cooling baths based on hydroxide, become increasingly thick liquids due to the formation of insoluble carbonates so that the melting point of the baths increases and the cooling effect decreases. Therefore, this kind of salt bath must be purified.
Since the sludge content of the nitride bath greatly influences the reproducibility of the expected nitriding result a continuous purification of the bath is very important. There-fore, various devices for removing the sludge are used in practice. However, the fact that the operation must be interrupted in order to remove the sludge, i.e., the removal of the sludge must be carried out on the non-charged bath, has ! ~
2~
been a common factor in all the systems used heretofore.
Furthermore in all the systems used heretofore the removal of the sludge is carried out with perforated plates, wire mesh screens or even with mineral wool, or glass wool which are housed in a suitable device. In many cases said device consists of one or several superposed basket-like structures of perforated plate, which are adapted to the shape of the crucible and, when required, thev are covered with a wire mesh screen. Even simple, disc-shaped devices with an added rim of perforated plate are used. For the xemoval of the sludge the device is placed into the non-charged salt bath and after a settling andquiescent phase it is withdrawn. The major portion of the sludge particles present in the bath settle on the wire mesh screen or on the glass wool. A cylindrical vessel having a hinged bottom of perforated plate is also disclosed in German Offenlegungsschrift No~ 2,645,669. Said vessel is placed with its opened bottom into the bath, whereupon the bottom is closed and the entire device is again withdrawn. Filtration of the bath is thus attained. In order to attain a complete removal of the sludge from the salt melts, the procedure must be repeated several times in all the conventional sludge removing processes and devices~
In all the conventional procedures the continuous interruptions of the operation, which is required for the purification of salt baths and can be substantial when re~uire-ments of purity of the bath are high, is a disadvantage. In many cases the removal of the fine suspended particles is insufficient.
Moreover in the case of sensitive structural membexs the results of the treatment vary since the sludge content of the bath increases between two removals of sludge and the results of the treatment thus deteriorate. However, in the case of sensitive structural members the way out, namely to remove the sludge z~

after each charge, is very cumbersone and time-consuming.
Therefore, the present invention provides a process and apparatus for removing sludge from polluted salt baths, particularly nitride salt baths, which operate with as little as possible an interruption of the operation and also assure complete removal of the sludge. They also are suitable for any bath size and are simple and uncomplicated to handle.
According to the present invention there is provided a process for removing sludge from a polluted salt bath in which during the operation of the bath a por~ion of the salt melt is continuously purified.
Thus in accordance with the present invention during the operation some of the salt melt is continuously purified.
This purification is carried out in that a portion of the salt melt is continuously passed over a filter to remove the sludge and that the purified melt is returned to the bath. The portion of the melt which is passed over the filter is preferably such that the total volume of the salt bath is purified once within a period of one to five hours.
The present invention also provides an apparatus for removing sludge from polluted salt bath including a filter for removing the sludge and a pump immersed in the salt adapted to continuously recirculate a portion of the salt melt from the bath through said filter.
The apparatus according to the invention thus includes a pump immersed into the salt bath and a filter into which a portion of the melt is continuously fed.
The filter is disposed above and outside the bath.
Continuous removal of sludge from the bath is thus possible.
This has the advantage of a higher productivity of the bath since it is no longer necessary to interrupt the operation.

~ 2~1~

A further advantage lies in that the state of the bath is continuously the same with respect to the sludge content i.e., the minimal sludge content of the bath does not vary over a lengthy period of time. Complete uniformity of the treatment results is thus attained.
The present invention will be further illustrated by way of the accompanying drawings in which:
Fig. 1 is a schematic of an apparatus for effecting the process according to the embodiment of the present invention;
Fig. 2 is a detail of the filter system of Fig. 1 and;
Fig. 3 is a detail of an alternate filter system of Fig. 1.
Referring to Figs. 1 and 2, the salt melt (1) is in a titanium crucible (2). An air compressor (3), for example, an air lift pump with the compressed air contact (4) and the ascending pipe (5) is dipped into the salt melt (1). The salt flow conveyed by the air lift pump (3) passes into the filter system (6) and leaves this system through the discharge pipe (7).
The filter system (6) comprises, for example, a double-walled sheet-iron jacket (8 and 9). The intermediate space is insulated with glass, slag or mineral wool (10) to avoid heat losses and the recrystallization of bath components associated therewith.
A pot of perforated plate (11), into which a sheeth of fine-meshed wire net is inserted (12), is disposed within said insulating jacket.
The liquid salt is pumped into the filter sheeth, which is open at the top. The sludge particles are retained on passing this filter. The purified salt melt leaves the filter system through the discharge system (7). In order to assure that in the case of an obstructed filter, complications due to overflowing of the pot are avoided, an overflow (13) is provided. Filter _~

sheeths filled or obstructed with sludge can be very easily exchanged without having to ~urn off the air lift pump or having to remove it from the bath since the ascending pipe (5) can be rotated about its longitudinal axis towards the bath.
Another feasible embodiment of the sludge removing unit (6) is shown in Figure 3. In this case it consists of a simple box (14), which may also be insùlated to avoid heat losses. Sheet iron barriers (15) of varying heights are disposed in the box (l4). The liquid salt melt conveyed by the air lift pump (3) passes into the first chamber (16) of the sludge-removing unit (6~. When the first chamber (1) is filled the salt melt overflows into the further chambers until it reaches the discharge pipe (7). Since the salt melt must slowly pass through several chambers, it is very quiescent whereby the sludge particles can settle on the bottom. When the chamber is filled with sludge, the viscous sludge can be removed therefrom simply by dumping it out.
The advantages of the process according to the invention are explained in greater detail by means of the Examples hereafter.
Example 1 A crucible furnace with a salt bath crucible of titanium having a diameter of 800 mm and a depth of 1500 mm contains 1100 kg of nitriding salt. At an operating temperature of 580C synchronized bodies of steel C45 having a charge weight of 400 kg are dipped in a rack of 60 kg into the bath as the members to be treated. The time of treatment (residence time in the bath) is one hour, the treatment being performed as a three-shift operation.
In conventional sludge removal the sludge had to be removed four times within the three shifts, i.e., every six hours. Between two sludge removals the content of water-insolu-- ~14~419 ble constituents in the bath varied between 0.017% (immediately after the removal of the sludge) and 0.19% (immediately prior to the next removal of the sludge).
The operation of removing the sludge took 30 minutes in each case, so that within three shifts - taking into account the time required for charging the bath and removing the members - a maximum of 18 charges with 7200 kg could be treated.
When using the process for removing sludge according to the invention and an apparatus according to Figure l and 2, the content of water-insoluble constituents was constant at 0.015%. The filter sheeths could be exchanged during the operation so that a maximum of 20 charges with a total of 8000 kg could be treated.
However, the fact that apart from the increased productivity a distinct improvement of both the quality and the uniformity of the treated material was noticed as a result of the constantly low sludge content is even more important. 540 kg of the bath are passed over the sludge removing unit per hour.
Example 2 A crucible furnace with a salt bath crucible of titanium having a diameter of 600 mm and a depth of 1300 mm contained 550 kg of nitriding salt. The operating temperature was 550C. The members to be treated were crankshafts of steel 42 CrMo 4. The weight of the charge was 240 kg and the weight of the rack 30 kg. The time of treatment (residence time in the bath) was two hours in a two-shift operation.
In this example the sludge was removed after every two charges, requiring 25 minutes. The content of water-insoluble constituents was 0.013% immediately after the removal of the sludge and 0.12~ immediately prior to the next removal of the sludge. When using an apparatus for removing sludge according to the invention corresponding to the Figures 1 and 2, the ~142~19 content of insoluble constituents in the bath could be reduced to a constant value of 0.014% at a throughput of 200 kg of salt melt per hour~ While previously six charges with a total of 1440 kg could be treated within two shifts, seven charges with 1680 kg were treated when applying the continuous sludge removal.
Example 3 A tank furnace having the size of 800 x 600 x 1300 mm was filled with an alkali hydroxide melt as the cooling bath.
The temperature of the bath was 350C.
Members according to Example 2 were dipped into this bath during a treatment time of 10 minutes. By entraining foreign salts and converting the hydroxide the content of insoluble carbonate in`the bath increased, whereby the melting point increased and the cooling effect decreased, resulting in an increase in treatment time.
In conventional sludge removal the bath had to be cooled after some time in two stages and the sludge was removed by means of a screen.
With the apparatus according to the invention, the bath could be kept free from sludge during the entire running time while the entire bath was passed over the sludge removing apparatus once in five hours.

Claims (5)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for removing sludge from a polluted salt bath, in which during the operation of the bath a portion of the salt melt is continuously passed over a filter for purification.
2. A process according to claim 1, in which the total volume of the salt melt is passed over the sludge removing unit during a time period of 1 to 5 hours.
3. A process according to claim 1 or 2, in which the salt bath is a nitriding salt bath.
4. An apparatus for removing sludge from polluted salt bath, including a filter and pump means immersed into the salt adapted to continuously recirculate a portion of salt melt from the bath through said filter, said filter being disposed above and outside the salt bath.
5. An apparatus according to claim 4, in which the pump means includes an air compressor.
CA000347843A 1979-03-22 1980-03-18 Process and apparatus for removing sludge from salt baths Expired CA1142419A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19792911222 DE2911222A1 (en) 1979-03-22 1979-03-22 METHOD AND DEVICE FOR DISCHARGING SALBADES
DEP2911222.9 1979-03-22

Publications (1)

Publication Number Publication Date
CA1142419A true CA1142419A (en) 1983-03-08

Family

ID=6066098

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000347843A Expired CA1142419A (en) 1979-03-22 1980-03-18 Process and apparatus for removing sludge from salt baths

Country Status (9)

Country Link
JP (1) JPS55161064A (en)
AR (1) AR226055A1 (en)
AT (1) AT367463B (en)
BR (1) BR8001634A (en)
CA (1) CA1142419A (en)
DE (1) DE2911222A1 (en)
FR (1) FR2461018A1 (en)
GB (1) GB2046611A (en)
IT (1) IT7969374A0 (en)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD157966A3 (en) * 1977-08-08 1982-12-22 Siegfried Schelinski METHOD AND DEVICES FOR FASTENING GLASS PRODUCTS BY ION EXTRACTION
EP0089219A3 (en) * 1982-03-15 1984-07-04 Protectaire Systems Company Sludge filtration apparatus
FR2525491B1 (en) * 1982-04-23 1988-04-29 Stephanois Rech Mec FILTER GROUP FOR SALT BATHS
DE3733721C1 (en) * 1987-10-06 1988-04-21 Degussa Device for the continuous desludging of salt baths
DE3836939C1 (en) * 1988-10-29 1989-06-15 Degussa Ag, 6000 Frankfurt, De
JP3280691B2 (en) * 1992-02-18 2002-05-13 パーカー熱処理工業株式会社 Molten salt tank with integrated sludge removal device
ATE149223T1 (en) * 1992-12-30 1997-03-15 Merpro Tortek Ltd WATER HANDLING SYSTEM
ES2138638T3 (en) * 1994-01-13 2000-01-16 Houghton Durferrit Gmbh FILTER UNIT AND DEVICE TO UNSOLLATE SALT BATHS.
JP3187249B2 (en) 1994-05-17 2001-07-11 本田技研工業株式会社 Sludge removal device
CN107875870A (en) * 2016-09-29 2018-04-06 内蒙古乌海化工有限公司 A kind of salt dissolving pond
CN106861582B (en) * 2017-03-07 2019-04-19 上海煜志机电设备有限公司 The purification and hydrodynamics fused salt tank of high-temperature liquid state nitrate
JP2018187555A (en) * 2017-05-01 2018-11-29 パーカー熱処理工業株式会社 Sludge separation apparatus

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE564595C (en) * 1930-11-21 1932-11-21 Frey & Co W Method and device for annealing metal objects in a salt bath
FR938432A (en) * 1945-10-01 1948-09-15 Ajax Electric Company Process and device for the purification of salt baths for heat treatment
GB606734A (en) * 1946-01-17 1948-08-19 Thomas Augustus Goskar Improvements in or relating to the heat treatment of steel
DE866004C (en) * 1950-08-14 1953-02-05 Ernst Matter Apparatus for demonstrating objects, in particular for advertising purposes
DE1198842B (en) * 1958-06-03 1965-08-19 Degussa Method and device for desludging of hot baths in the hardening technique
DE1247361B (en) * 1963-10-02 1967-08-17 Degussa Device for desludging of molten salts, in particular nitriding balls
PL84385B1 (en) * 1973-01-11 1976-03-31 Polotechnika Wroclawska Breslau (Polen)
NO129964B (en) * 1973-03-01 1974-06-17 Hydro N
DE2435830C3 (en) * 1974-07-25 1981-11-05 ARBED-F & G Drahtwerke Köln GmbH, 5000 Köln Method and device for the production of steel wire

Also Published As

Publication number Publication date
JPS55161064A (en) 1980-12-15
GB2046611A (en) 1980-11-19
AR226055A1 (en) 1982-05-31
BR8001634A (en) 1980-11-18
DE2911222A1 (en) 1980-11-06
ATA153880A (en) 1981-11-15
IT7969374A0 (en) 1979-12-11
FR2461018A1 (en) 1981-01-30
AT367463B (en) 1982-07-12

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