Title of Invention

GROWTH HORMONE SECRETAGOGUES

Abstract APPARATUS AND METHOD OF CONDITIONING SCALE ON A METAL SURFACE ABSTRACT OF THE DISCLOSURE A composition and apparatus and method of using the composition for aqueous spray descaling or conditioning of scale or oxide on metal surfaces, especially stainless steel strip or the like, in one embodiment, although it can be used to descale or condition oxide or scale on other work pieces such as metal bar, or even discrete objects. An aqueous solution having a base composition of an alkali metal hydroxide, such as sodium hydroxide, potassium hydroxide, or a mixture of alkali metal hydroxides such as sodium hydroxide and potassium hydroxide is used. The aqueous solution may contain certain additives to improve the descaling performance of the salt. In one embodiment, the solution is used to condition the scale or surface oxide on a strip of stainless steel. The strip of steel is at a temperature between the melting point of the alkali metal hydroxide in anhydrous form and a temperature at which the Leidenfrost effect appears. One or more nozzles is provided to spray the solution, and the heated strip is passed by the nozzle or nozzles where the solution is sprayed on the surface or surfaces of the strip that have the scale or oxide. The invention also includes the apparatus and control thereof for the spraying of the solution.
Full Text
FORM 2
The Patents Act, 1970 (39 of 1970)
1. "APPARATUS AND METHOD OF CONDITIONING SCALE ON A METAL SURFACE"
2(a) KOLENE CORPORATION
(b) 12890 Westwood Avenue, Detroit, Michigan 48223, United States of America
(c) United States of America
The following specification describes the nature of this invention.and the manner
in which it is to be performed








nozzles, one of which is shown at 2i, to spray the top surface of the a strip l3. and a set of lower nozzles, one of which if shown at 30, to spray the lower surface of the strip 13. A second or backup set of spray nozzles including upper nozzles, one of which is shown at 34, and lower nozzles, one of which is shown at 36, may optionally be added to insure coverage if necessary, as will be described presently. (Of course, only one set of nozzles may be needed in some cases, or more than two sets of nozzles may be required in some cases, depending on the speed and width of the strip 13 and other factors.) The nozzles 28,30,34, and 36* are of a type that can receive liquid and spray the liquid as very fine atomized droplets onto (he strip of steel 13. The nozzles can be Air Atomizing type VAU as supplied by Spraying Systems Co. While an air atomizing nozzle is described, other spray forming techniques that provide adequate atomizau'on / small droplet size, such as high pressure hydraulic nozzles, may also be used effectively. Specialized techniques such as electrostatic deposition may be used to enhance transfer efficiency. A rinse section 38, shown in dotted outline, is provided adjacent the spray section 24. This rinse can optionally be either of the spray type or immersion type. In the immersion type, rinse is carried out by passing the strip under a rubber immersion roll submerged in a water rinsing tank, and in the spray type, rinsing is carried but by the strip passing through an array of water spray nozzles being supplied with fresh water, or by a pump from a collection sump located below the spray area. A surface analyzer 42 is optionally provided adjacent the nozzles 28 that will monitor the surfaces of the strip to detect lack of conditioning. This analyzer 42 may be an infrared linescan system or other machine vision system. One suitable infrared system is Landscan supplied by Lan Instruments International Inc. The analyzer provides input to the line dynamics operating system that will be described presently.
Following the rinse section, the strip is guided by a set of conventional tracking and bridle roils 44. This set of rolls 44 will keep the strip on track and maintain proper tension in the strip. The strip of steel 13 typically then goes to an acid pickling section. Acid pickling usually includes one or more acid tanks, although acid spray could be used. Multiple acid pickles may be required on some grades of stainless steel, as illustrated at 48,50 and 52. Rinse tanks 49,51 and 53 are provided following pickle tanks 48,50 and 52, respectively. Typically, the tank 48 contains sulfuric acid, tanks 50 and 52 contain either a mixture of nitric acid and hydrofluoric acid or nitric acid. One or more of these may be used on any given strip 13 of stainless steel depending on many factors, including the composition of the steel, the thickness of the oxide, and other factors known in the art In addition, other acids and mixtures of acids may be used, which also is well known in the art
Following emergence of the strip 13 from the acid pickle and rinse, the strip is recoiled on recoiler 54. At this point, all of the scale conditioning and pickling has been completed



The liquid scale conditioning solution sprayed on the strip 13 by the nozzles 21,30,34, end 36 is supplied thereto from one or more liquid product storage vessels 56,58, and 60 having temperature sensors 57,59 and 61, respectively. The reason for several vessels is to store different solutions that may be required or desirable for different grades of steel and/or storing additives to the base solution that can be mixed in-line to provide the desired composition, all as will be described presently. The vessels 56,58, and 60 are provided with discharge pumps 62,64, and 66, respectively, to pump liquid from their respective storage vessel. At the output side of the pumps 62,64, and 66 are flow controllers 68,70 and 72, respectively. (It is to be understood that it is possible to use metering-type variable flow pumps 62,64, and 66 and thus combine the metering and flow regulating functions in a single unit, eliminating the need for flow controllers, although flow meters may be desired.) From the flow controllers 68,70, and 71, the liquid is delivered to nozzle supply line 74 which contains an in-line mixer 76 to assure complete mixing of product delivered from two or more storage vessels 56,58, and 60. Lines 80,82,84 and 86 supply the nozzles 28,30, 34 and 36, respectively, with the liquid product that is to be sprayed, on the strip 13, and flow sensors 87,88,89 and 90 and metering valves 92,94, % and 98 are provided in the lines 80,82,84 and 86, respectively, to monitor and control the flow to each spray nozzle 28,30,34 and 36, respectively. Another way of utilizing multiple storage vessels is to use one vessel with a concentrated feedstock that might not allow some additives to be in solution with it, and a second vessel containing the additive(s). The first vessel would feed a first array of nozzles, and the second vessel would feed a second, downstream array of nozzles. This would be used where in-line mixing would not be feasible or desirable because of solubility limitations, ion-exchange, precipitation, or other untoward results of in-line mixing of concentrated solutions, eg, nozzle blockages, filter blinding, etc.
The system controls include a line dynamics operating system 112 which receives operating line system inputs, and outputs line variables 114 to operate the annealing line, as' will be'described presently. There is also provided a scale conditioning process control system 120 which receives as control variables outputs from the line dynamics operating system 112.
Before describing the operation of the line in detail, a description of the method of the present invention will be given. According to one embodiment of this invention, an aqueous solution containing an alkali metal hydroxide is sprayed In the form of droplets onto a strip of stainless steel or other metal, with the strip being held at a temperature above the melting point of the essentially anhydrous form of the material in solution and below that at which the Leidenfrost effect appears. As used herein, the term "essentially anhydrous form of the material" means after the water of solution is evaporated, even though there may be some water of hydration still present



in the material. As used herein, the term "Leidenfrost effect on the strip" is a mottled or speckled surface appearance of the strip, which reveals patches, or spots of incomplete scale conditioning. This is believed to be due to the Lidcafrost effect on the aqueous solution of chemicals if the strip is above what is known as the Leidenfrost temperature or Leidenfrost point of the solution being sprayed. When the strip is above the Leidenfrost temperature of the solution being sprayed, a thin film of the sprayed liquid is converted to a vapor phase barrier between die metal surface and the droplet, preventing the droplet from contacting the surface of the strip and depositing the chemicals on the metal surface upon evaporation of the liquid. The Leidenfrost effect is well known and described in many publications. Two such publications are; "Disk Model of the Dynamic Leidenfrost Phenomenon" (Martin Rein at DFD96 meeting of American Physical Society) and "Miracle Mongers and Their Methods" (pages 122-124 by Harry Houdini, published 1920 by E. P. Dutton).
Figure 2 is a photograph of the surface of a type 304 stainless steel sample that does not show the Leidenfrost effect after a treatment according to this invention, which treatment will be described presently; Figures 3-5 are photographs of the surfaces of type 304 stainless steel samples that show the Leidenfrost effect to various degrees after scale conditioning (Figure S being the worst) outside the scope of the present invention and pickling, also as will be described presently. It should be noted that with respect to Figures 3-5, there are areas where the scale conditioning is complete, i.e. the white or gray areas, as well as areas where there is incomplete scale conditioning, i.e. the dark areas. This indicates that some of the droplets exhibited die Leidenfrost effect, i.e. where the dark spots appear, and some of the drops of solution either did not experience or overcame the Leidenfrost effect and, thus, were effective for scale conditioning, i.e. the white or bright areas. Thus, as used herein, the term "a temperature below which the Leidenfrost effect appears" refers to a temperature at which no appreciable scale in the form of dark spots exists after scale conditioning according to this invention and subsequent picklingThe surface as shown in Figure 2 is an example" of a temperature at which no Liedenfrost effect is present, and Figures 3-5 are examples of temperatures at which the Leidenfrost effect is present
The samples of Figures 2-5 as well as other samples were prepared and treated as follows: The samples were 4 inch x 6 inch panels of 0.025 inch gage type 304 stainless steel. Each sample was heated to a temperature of about 1950 °F in air and then removed and clamped in a test fixture The samples were cooled to a predetermined temperature as measured by a contact thermocouple. The samples were then sprayed with an aqueous alkali hydroxide-containing solution, rinsed with water and then acid pickled. Table 1 below sets out the values for the variables used for the different samples and the descaling results.


WE CLAIM:
1. An apparatus for conditioning scale on the surface of a metal object, wherein a
mechanism moves the metal object first past a cooling mechanism and then past at least one nozzle adapted to spray droplets of an aqueous caustic solution contained in at least one reservoir, wherein the improvement is characterised by:
a temperature-sensing device positioned adjacent said cooling mechanism to sense the temperature of the surface of said metal object prior to the metal object passing said at least one nozzle; and
a control mechanism to control said cooling mechanism responsive to the sensed temperature of the surface of said metal object, said control mechanism configured to control the cooling device to cool the surface of the metal object to a temperature above the melting point of the composition contained in the aqueous solution and below the temperature at which the Leidenfrost effect appears.
2. The apparatus as defined in claim 1 wherein there is at least a second reservoir for a fluid
communicating with said at least one nozzle and with said control mechanism.
3. The apparatus as defined in claim 1 wherein there is at least a second nozzle adapted to spray droplets of a solution communicating with said reservoir, and with said control mechanism.
4. The apparatus as defined in claim 1 wherein the control mechanism includes flow control devices to control the flow individually from each reservoir to said nozzle.
5. The apparatus as defined in claim I wherein the mechanism for moving the metal object
is configured to move a metal strip, and said metal object is a metal strip.
6. The apparatus as defined in claim 5 wherein there is at least one nozzle disposed on each
side of said strip.
7. The apparatus as defined in claim 1 further comprising an acid pickling station, and
wherein the mechanism for moving the metal object is configured to the move the object through
the acid pickling station after moving the object past the at least one nozzle.


The apparatus as defined in claim 5 further characterized by a surface coverage analyzer adjacent said at least one nozzle.
The apparatus as defined in claim 1 wherein there is a speed sensing device to sense the speed of said metal object, and said control device is configured to vary the flow of said aqueous caustic solution responsive to the sensed speed of the metal object.. The apparatus of claim 4 wherein:
a) the metal object has a composition and dimensions; and -
b) the control mechanism flow control devices control said flow responsive to at
least one of the group consisting of the composition and the dimensions of said
metal object
1. The apparatus of claim 9, wherein:
-a)—the metal object has a composition and dimensions; and
b) the control mechanism flow control devices control said flow responsive to at least one of the group consisting of the composition and the dimensions of said metal object.

12. The apparatus of claim 5 further comprising a surface condition analyzer in communication with said control mechanism and positioned to measure a degree of surface conditioning of said metal strip after said strip has been engaged by the spray droplets, wherein the control mechanism is further configured to control a flow rate of said aqueous caustic solution through said at least one nozzle responsive to the degree of surface conditioning measured by the surface analyzer.
13. The apparatus of Claim 1 further comprising a heating mechanism disposed to heat the surface of the metal object prior to the metal object passing said temperature-sensing device to a temperature above the melting point of the composition contained in the aqueous solution.
14. A method of treating scale on the surface of a metal object with an aqueous solution comprised of an alkali metal hydroxide or mixture of alkali metal hydroxides, wherein the improvement is characterised by the steps of:

a) controlling the temperature of the surface of the metal object to a temperature above the melting point of the alkali metal hydroxide or hydroxides in anhydrous form and where conditioning occurs, and below the temperature at which the Leidenfrost effect appears; and
b) thereafter spraying said solution on the surface of the metal object.

15. The method as defined in claim 14 wherein the solution contains sodium hydroxide or potassium hydroxide or a mixture thereof.
16. The method as defined in claim 14, further comprising the step of acid pickling the metal object after spraying the metal object with said solution.

17. The method of claim 14 wherein the concentration of the solution is between about 15% and 65% solids by weight.
18. The method as defined in claimH wherein the solution concentration is between about 35% and 45% solids by weight.
19. The method as defined is claim 14 wherein the concentration of the solution is about 40% solids by weight.
20. The method as defined in claim 14 wherein the temperature of the surface of the metal object is at least about 232 °C (450°F), and does not exceed about 371 °C (700°F), as measured by a contact thermocouple.
21. The method as defined in claim 17 wherein the temperature of the surface of the metal object is at least about 232 °C (450°F) and does not exceed about 316 °C (600°F), as measured by a contact thermocouple.
22. The method as defined in claim 14 wherein the metal object is stainless steel strip.
23. The method of claim 14 wherein the solution contains an effective amount of an additive selected from the group of alkali metal carbonates, alkali metal chlorates, alkali metal nitrates, alkali metal permanganates, and mixtures thereof.

24.

The method of claim 23 wherein the additive is an alkali metal permanganate.

25. The method of claim 15 wherein aqueous solution is comprised of a eutectic mixture of sodium hydroxide and potassium hydroxide.
26. The method of claim 14 wherein the step of spraying said solution on the surface of the metal object is performed in an oxidizing atmosphere.
27. The method of claim 14, further comprising the steps of:

a) providing a composition and dimensions for the metal object; and
b) controlling the amount of the solution sprayed on the surface of the metal object; wherein the step of controlling the amount of the solution sprayed is responsive to at least one of the composition and the dimensions of the metal object.
28. The method of claim 27, further comprising the step of analyzing the sprayed metal
object surface to measure the degree of surface scale conditioning; and wherein the step of
controlling the amount of the solution sprayed is further responsive to the step of analyzing said
sprayed metal object surface.
29. An apparatus for conditioning scale on the surface of a metal object having a surface
temperature, wherein a driving mechanism moves the metal object first past a heating
mechanism and a cooling mechanism and then past at least one nozzle adapted to spray
droplets of an aqueous caustic solution comprising at least one salt having a melting point
and contained in at least one first reservoir, wherein the improvement is characterised by:
a second reservoir containing a second liquid solution and communicating with said at least one nozzle, wherein the at least one nozzle is adapted to spray an atomized mist of a treatment mixture of said aqueous caustic solution and said second liquid solution and thereby cause the treatment mixture to engage the surface of the metal object, said treatment mixture having a concentration of the aqueous caustic solution and a concentration of the second liquid solution;
a control mechanism in communication with said at least one nozzle, the control mechanism configured to control the flow rate of said treatment mixture through said at least one nozzle as an atomized mist engaging said metal object surface; and

a temperature-sensing device in communication with said control mechanism and positioned to sense the surface temperature of said metal object prior to the metal object passing said at least one nozzle;
wherein the control mechanism is configured to direct the cooling mechanism responsive to the temperature-sensing device to decrease the surfece temperature of said metal object prior to the metal object surfece engaging said atomized treatment mist to a temperature above said salt melting point and below the temperature at which the Leidenfrost effect appears on said metal object surface.
30. The apparatus of claim 29 wherein the atomized treatment mixture mist engages the surface of the metal object in an oxidizing atmosphere.
31. The apparatus of claim 30, further comprising a surface analyzer in communication with said control mechanism and positioned to measure a degree of surface conditioning of said metal object surface after said surface has been engaged by said atomized treatment mist, wherein the control mechanism is further configured to control the flow rate of said treatment mixture through said at least one nozzle responsive to the degree of surface conditioning measured by the surface analyzer.
32. The apparatus of claim 31, further comprising a speed sensing device in communication with said control mechanism and positioned to measure the rate at which said metal object surface passes said at least one nozzle, wherein the control mechanism is further configured to control the flow rate of said treatment mixture through said at least one nozzle responsive to the speed sensing device.
33. The apparatus of claim 29, further comprising:
a flow monitor in series with the at least one nozzle configured to monitor the flow of the treatment mixture through said nozzle, said monitor communicating with the control mechanism; and
at least a second nozzle in communication with said control mechanism and said first and second reservoirs and adapted to spray an atomized mist of a treatment mixture of said aqueous caustic solution and said second liquid solution and thereby cause the treatment mixture to engage the surface of the metal object;

wherein said control mechanism operates said second nozzle responsive to said flow monitor.
34. The apparatus of claim 33 wherein the control mechanism is furthered configured to operate said second nozzle responsive to the degree of surface conditioning measured by the surface analyzer.
35. The apparatus of claim 29, wherein the metal object has a composition, and wherein the control mechanism is further configured to vary the concentration of said first aqueous caustic solution and vary the concentration of the second liquid solution within said treatment mixture responsive to the composition of said metal object.
36 The apparatus of claim 31, wherein the metal object has a composition and dimensions, and wherein the control mechanism is further configured to vary the concentration of said first aqueous caustic solution and vary the concentration of the second liquid solution within said treatment mixture responsive to at least one of the group consisting of the composition of said metal object, the dimensions of said metal object, and the degree of surface conditioning measured by the surface analyzer.



Documents:

in-pct-2002-01550-mum-cancelled pages(05-11-2001).pdf

in-pct-2002-01550-mum-claims(granted)-(05-11-2001).doc

in-pct-2002-01550-mum-claims(granted)-(05-11-2001).pdf

in-pct-2002-01550-mum-correspondence(27-09-2007).pdf

in-pct-2002-01550-mum-correspondence(ipo)-(16-10-2008).pdf

in-pct-2002-01550-mum-form 13(04-08-2005).pdf

in-pct-2002-01550-mum-form 13(27-05-2003).pdf

in-pct-2002-01550-mum-form 13(29-03-2006).pdf

in-pct-2002-01550-mum-form 18(28-12-2005).pdf

in-pct-2002-01550-mum-form 1a(05-11-2002).pdf

in-pct-2002-01550-mum-form 2(granted)-(05-11-2001).doc

in-pct-2002-01550-mum-form 2(granted)-(05-11-2001).pdf

in-pct-2002-01550-mum-form 3(05-11-2002).pdf

in-pct-2002-01550-mum-form 3(20-09-2007).pdf

in-pct-2002-01550-mum-form 3(23-01-2007).pdf

in-pct-2002-01550-mum-form 3(28-08-2007).pdf

in-pct-2002-01550-mum-form 5(05-11-2002).pdf

in-pct-2002-01550-mum-form-pct-ipea-409(06-11-2001).pdf

in-pct-2002-01550-mum-form-pct-isa-210(06-11-2001).pdf

in-pct-2002-01550-mum-petition under rule 137(23-01-2007).pdf

in-pct-2002-01550-mum-power of authority(21-01-2003).pdf

in-pct-2002-01550-mum-power of authority(23-01-2007).pdf


Patent Number 224552
Indian Patent Application Number IN/PCT/2002/01550/MUM
PG Journal Number 02/2009
Publication Date 09-Jan-2009
Grant Date 16-Oct-2008
Date of Filing 05-Nov-2002
Name of Patentee ZENTARIS AG
Applicant Address WEISSMULLERSTRASSE 45, 60314 FRANKFURT/MAIN. GERMANY.
Inventors:
# Inventor's Name Inventor's Address
1 JEAN MARTINEZ CHEMIN DES ROMAINS, F-34570 SAUSSAN. FRANCE.
2 JEAN-ALAIN FEHRENTZ RUE DES SALADELLES, F-34400 ST. NAZAIRE DE PEZAN. FRANCE
3 VINCENT GUERLAVAIS 58, RUE DES GABARES BAT. B, F-34000 MONTPELLIER. FRANCE.
PCT International Classification Number C07D209/20,C07D401/1
PCT International Application Number PCT/EP01/06717
PCT International Filing date 2001-06-13
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/234,928 2000-09-26 U.S.A.
2 60/211,326 2000-06-13 U.S.A.