GB2085044A - Method for producing asbestos free machinable calcium silicate high heat-resistant material - Google Patents
Method for producing asbestos free machinable calcium silicate high heat-resistant material Download PDFInfo
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- GB2085044A GB2085044A GB8031176A GB8031176A GB2085044A GB 2085044 A GB2085044 A GB 2085044A GB 8031176 A GB8031176 A GB 8031176A GB 8031176 A GB8031176 A GB 8031176A GB 2085044 A GB2085044 A GB 2085044A
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- parts
- weight
- lime
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- xonotlite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/18—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
- C04B28/186—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type containing formed Ca-silicates before the final hardening step
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
A composition for producing a calcium silicate heat-resistant material, comprises: (A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6-1.2; (B) 20-170 parts by weight of xonotlite obtained by hydrothermal synthesis; (C) 15-150 parts by weight of fibrous wollastonite; and (D) water in an amount of 2-8 times as much as that of the total solid contents. A method for producing a calcium silicate heat-resistant material, comprises the steps of: i) molding a slurry of the above composition; ii) curing said molded body in an atmosphere of steam under a pressure not less than 6 kg/cm<2> to react the siliceous material with the lime; and iii) treating to remove water at a temperature not lower than 100 DEG C under atmospheric pressure. p
Description
SPECIFICATION
Method for producing asbestos free machinable calcium silicate high heat-resistant material
This invention relates to a method for producing an asbestos calcium silicate high heat-resisitance material which can be machined into any shape or size required.
Calcium silicate heat-resistant materials having machinability are well known, and are used for
manufacturing items such as conduits, troughs, pouring boxes and the like which are used to transport, hold
and supply molten metals such as molten aluminum. These heat-resistant board materials are used as they are or fabricated into various shapes according to their intended use. For this purpose, the calcium silicate board has various good properties such as low density, low thermal conductivity; it is not wetted with molten metals; and it does not stain molten metals. In addition to these properties, other properties such as high mechanical strength, accurate machinability and endurability, when the hot molten metals come in contact, are further required. Therefore, ordinary calcium silicate thermal insulation composed of tobermorite or xonotlite cannot be used, for the above purpose.A typical example of a commercially available material conventionally used has been prepared by a special process comprising molding a body made of amosite asbestos and diatomaceous earth with the addition of an inorganic binder, curing the molded body in an atmosphere of steam under high pressure, and heat treating the cured body.
Not only the above example but also other conventional materials contained a large amount of asbestos. Asbestos has many outstanding advantages; it provides not only high mechanical strength to the final product but also provides green strength to the molded body prior to its being cured by steam induration and to provide stress distribution during curing and heat treating. However, since it is indicated that asbestos fiber hazard human health, it is preferable not to use it.
Under these circumstances, the development of a heat-resistant material free from asbestos is demanded. However, an alternative reinforcing fiber which has satisfactory properties comparable to those of asbestos and which can replace asbestos could not be developed heretofore.
With this background, we have studied to develop a method for producing a calcium silicate heat
resistant material free from asbestos, which can be used for conveying molten metals, and have achieved the present invention as fully mentioned below.
The invention provides a composition for producing a calcium silicate heat-resistant material, which comprises;
(A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6-1.2; (B) 20-1 70, preferably 30-100 parts by weight of xonotlite obtained by hydrothermal synthesis;
(C) 1 5-1 50, preferably 50-100 parts by weight of fibrous wollastonite; and
(D) water in an amount of 2-8 times as much as that of the total solid contents.
Another object of this invention is to provide a method for producing a calcium silicate heatresistant material, which comprises the steps of:
(i) molding a slurry of a uniform mixture of:
(A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6-1.2; (B) 20-1 70, preferably 30-100, parts by weight of xonotlite obtained by hydrothermal synthesis;
(C) 1 5-1 50, preferably 50-1 00, parts by weight of fibrous wollastonite; and
(D) water in an amount of 2-8 times as much as that of the total solid contents;
(ii) curing said molded body in an atmosphere of steam under a pressure of not less than 6 kg/cm2 to react the siliceous material with the lime; and
(iii) heating said cured body to remove water therefrom at a temperature of not lower than 1 000C, preferably 330-1 0000 C, under atmospheric pressure.
A method of this invention is further described hereinafter.
Siliceous material and lime used as the component (A) in this invention are not specially limited, but any material used for preparing an ordinary calcium silicate type product are available. Preferable examples of the siliceous material include diatomaceous earth, siliceous sand, ferrosilicon dust, siliceous sinter and the like. Preferable examples of the lime include slaked lime, quick lime, carbide residue and the like. These two materials are mixed in such a ratio as to give a CaO/SiO2 mole ratio of 0.6-1.2, preferably 0.7-1.0.
Particle size and degree of purity of the lime and siliceous components will be substantially the same as those lime and siliceous components used in the past for asbestos reinforced calcium silicate materials.
Hydrothermal synthesis to obtain xonotlite satisfactorily usable as the component (B) in this invention can be carried out in a usual manner. For example, the xonotlite preferably used in an this invention can be obtained by adding water to a mixture of siliceous material and lime in an amount of
10-30 times as much as that of the mixture and hydrothermally reacting the mixture under a steam pressure of 14-20 kg/cm for 2-8 hours stirring.
The xonotlite thus prepared adsorbs the powdery siliceous material and lime well, thus preventing the loss of these powdery materials in filtered water during the molding step. Asbestos fiber also adsorbs powdery material, but wollastonite fiber does not have this adsorption property. Therefore, the property of xonotlite in the moulding step is very important.
Xonotlite also gives various other contributions to providing "green strength" to the molded body before curing and improving heat-resistance and strength of the final product.
However, an amount of xonotlite should be in the above mentioned range. If the amount of xonotlite is less than the above range, satisfactory effects can not be obtained. On the other hand, if the amount of xonotlite is larger than the above range, molding requires extraordinary high pressrure and a final product which is obtained by usual molding pressure has an unsatisfactory low density and poor strength.
With regard to fibrous wollastonite, a commercially available product such as "NYARD-G" sold by
Interpace Co. in U.S.A. can be used. It is known to use fibrous wollastonite in the production of a calcium silicate heat-resistant material, but it is impossible to replace asbestos by fibrous wollastonite as a reinforcing material since the fiber of wollastonite is much shorter than asbestos fiber and furthermore the specific surface area of fibrous wollastonite is smaller. The reason for using fibrous wollastonite is not that one can expect any reinforcing effect, but to prevent cracking of the molded product during the heat treating and to improve the machinability of the product.
Another advantage of using fibrous wollastonite is that the heat treating time can be shorter than in the case of asbestos fiber having crystal water since fibrous wollastonite does not contain crystal water.
But the use of fibrous wollastonite in an excess amount should be avoided since the strength of the final product is lowered.
In this invention, if necessary, a small amount of inorganic fibers such as alkali-resistant glass fiber, rock wool and the like may be used for reinforcement. Also, if desired, organic fibers such as rayon, pulp and the like may be used in order to improve filterability during molding and strength of the molded product before heat treating.
The materials for conveying molten metals should bot contain combustible materials so organic fiber contained in a molded body must be burnt off thoroughly. If the molded body contains a large amount of organic fiber, the strength of the product after heat treating is much lowered.
According to this invention, the starting materials as mentioned above are uniformly mixed to prepare a slurry, and the slurry is molded to the desired shape, and enough water is expressed from the slurry to leave a shape retaining molded body having a density of 0.5-0.9 g/cm2. Typically such a shape is a flat board.
Generally, if the density of the product is higher, the strength also becomes higher. However, if the density is too high, machinability becomes poor and thermal conductivity becomes high.
The steam curing step of the molded body is carried out to react a siliceous material and a lime material and, possibly, to react these materials with the surface of xonotlite particles, thereby producing a matrix comprising calcium silicates. The steam curing is conducted in an autoclave under a vapor pressure of 6-20 kg/cm3 until tobermorite or xonotlite is formed from the silicic acid material and lime material. There is no problem even if small part of the cured body may form a mixed crystal of calcium silicate hydrate-l (CSH-I) and calcium silicate hydrate-ll (CSH-II).
The steam cured product is then dried and heat treated at a temperature of at least 1 000C, preferably 330-1 0000C, more preferably 330-6000C under air-flow.
The heat treating at a temperature 100--3000C removes only adsorption water and the dehydration of crystal water does not occur in this temperature range. Therefore most remained crystal water is removed when in contact with hot molten metals. This is undesirable for some special uses such as metal supply nozzles of the Hunter Engineering continuous sheet casting machine and the like.
On the other hand the heat treating at a temperature 600-1 0000C gives the final product a slightly large thermal expansion coefficient when reheated. It is unnecessary to heat treat the cured body at a temperature higher than the melting point of aluminium (6600 C) which is the highest among those of corresponding metals. Also, the heat treating at a too high temperature is a waste of energy.
However, the heat treating at a temperature 600-1 0000C does not do a lot of damage to the final product.
In case of the heat treating at a temperature higher than 10000 C, an extreme shrinkage and cracks appear on the product.
The heat treating at a temperature 330-6000C is most preferable, since it removes crystal water partially and a change of dimension when in contact with hot molten metals.
If organic fiber is used, this heat treatment must be carried out at a temperature of at least 5O00C to burn off the organic fiber.
In this heat treating, the crystal water of CSH--I and CSH--II is removed (the crystal water of tobermorite is also removed thoroughly when the heat treating temperature is about 7000C or higher, and that of xonotlite is removed at about 850"C or higher and subsequently the micro structure of the matrix changes.
The method for producing a heat-resistant material in accordance with this invention has advantages in that the heat treating can be carried out at a relatively low temperature in a short time as mentioned above; that the product does not warp or crack during the heat treating.
The product prepared in accordance with the method of this invention has all the properties necessary for the material used for manufacturing instruments for conveying molten metal as mentioned above, and besides, since it does not contain asbestos, it is satisfactory in view of environmental sanitation, particularly during machining.
The present invention is further illustrated by the following Examples and Comparative Examples.
"Part" in the Examples means part by weight. Xonotlite used in the Examples was prepared by mixing silica sand and slaked lime (obtained by slaking quicklime with 12 times its amount of hot water) in such a manner as to give a CaO/SiO2 mole ratio of 0.98, adding 1 2 times its amount of water to the mixture and reacting the resultant mixture in an atmosphere of steam under a vapor pressure of 16 kg/cm2 for 5 hours while stirring. Wollastonite used in the Examples is "NYARD-G" of Interpace Co. in
U.S.A.
EXAMPLE 1
A mixture of xonotlite 25 parts, wollastonite 30 parts, diatomaceous earth 23 parts, slaked lime 22 parts and water 400 parts was molded into a board of 30 x 300 x 300 mm under a pressure of 1 5 kg/cm2, and the molded body was subjected to steam curing under a vapor pressure of 9 kg/cm2 for 10 hours. By this treatment, the reaction of diatomaceous earth and slaked lime proceeds to produce calcium silicate comprising mainly xonotlite. The molded product was then heat treated for 4 hours at various temperatures as listed in the following Table 1. During heat treating, any warp and crack did not appear on the board, and the appearance of the board did not change.
Various properties of the product are shown in the following Table 1.
EXAMPLE 2
A heat-resistant material was produced by treating a mixture of xonotlite 1 5 parts, wollastonite 40 parts, silica sand 20 parts, slaked lime 21 parts, alkali-resistant glass fiber 4 parts and water 500 parts in the same manner as in Example 1. During heat treating, any warp and crack did not appear on the board, and the appearance of the board did not change.
Various properties of the product are shown in the following Table 2.
EXAMPLE 3
A heat-resistant material was produced by treating a mixture of xonotlite 20 parts, wollastonite 35 parts, silica sand 21 parts, slaked lime 22 parts, puip 2 parts and water 400 parts in the same manner as in Example 1, except that molding was carried out under a pressure of 10 kg/cm2. During heat treating, any warp and crack did not appear on the board, and the appearance of the board did not change.
Various properties of the product are shown in the following Table 3.
EXAMPLE 4
A heat-resistant material was produced by treating a mixture of xonotlite 56 parts, wollastonite 1 9 parts, silica sand 12 parts, slaked lime 13 parts and water 400 parts in the same manner as in Example 1.
Various properties of the product are shown in the following Table 4.
EXAMPLE 5
A heat-resistant material was produced by treating a mixture of xonotlite 8 parts, wollastonite 22 part, silica sand 33 parts, slaked lime 34 parts, alkali-resistant glass fiber 3 parts and water 500 parts in the same manner as in Example 1, except that molding was carried out under a pressure of 5 kg/cm2.
Various properties of the product are shown in the following Table 4.
EXAMPLE 6
A heat-resistant material was produced by treating a mixture of xonotlite 1 2 parts, wollastonite 50 parts, silica sand 19 parts, slaked lime 1 9 parts and water 500 parts in the same manner as in Example 1.
Various properties of the product are shown in the following Table 4.
EXAMPLE 7
A heat-resistant material was produced by treating a mixture of xonotlite 32 parts, wollastonite 6 parts, silica sand 29 parts, slaked lime 30 parts, alkali-resistant glass fiber 3 parts and water 400 parts in the same manner as in Example 1, except that molding was carried out under a pressure of 10 kg/cm2.
Various properties of the product are shown in the following Table 4.
COMPARATIVE EXAMPLE 1
A comparative material was produced by treating a mixture of wollastonite 35 parts, diatomaceous earth 32 parts, slaked lime 33 parts and water 300 parts, except that molding was carried out under a pressure of 5 kg/cm2. During heat treating, warps and cracks did not appear, but as can be seen from the following Table 5, the strength of the product was low and the heat-resistance was poor.
COMPARATIVE EXAMPLE 2
A comparative material was produced by treating a mixture of xonotlite 20 parts, silica sand 38 parts, slaked lime 38 parts, alkali-resistant glass fiber 4 parts and water 500 parts in the same manner as in Example 1. In this case, hair-like cracks appeared on the product.
Various properties of the product are shown in the following Table 5.
TABLE 1
Example 1
U) (D e v X O heat treating o o o $ (for 4 hours) (00) 100 250 350 450 550 650 750 2) Cq O N O after w O O O 6 of each (o thickness 0.4 .
for 4 hours N O O 4 t O,. & 0.61 O flexural strength (kg/cm2) 80 ~ O U) ~~ O ~ O 10 strength after 52 ~ ~ further heating at 85000 for 3 hours ~~ length 10 (D 0.5 0.5 , 0.2 0.1 after heatIng at 85000 t(DO thickness 1.8 O O Q 0e O r O ~ good good good good good good good v t N (0 s O E O O 0 s ~~ O 00 \ O o0 CQ O r . s s E G) s s E O s s < , ~ ~ ~o mmo > t ~ g ,, ' E c S C s 9 c .~ cs O s c < u s:n ns ffi U @o Ö oC s + c X s E t ~ x x s O sX ~o E TABLE 2
Example 2
uo) ot u) o0 ct lo ot |< heat treating temperature 100 250 350 450 550 650 750 (for 4 hours) (0C) o % after heat length 0.1 0.2 0.2 0.3 0.3 0.4 treating of In o O cc, thickness 0.3 0.5 0.6 0.8 1.0 1.5 for 4 hours CD CO s 0.83 0.82 0.82 09 w .' t n strength (kg/cm2) 130 127 120 115 j'D O 82 m strength after CU heating at 8500C NiDD D 80 78 OCUL 0S O length O O 0.4 itv O' v '.a5 after heating at 8500C for 3 hours thickness 1.6 1.5 1.3 1.2 1.1 0.7 0.4 o' o' o' o ao o' r' fair fair fair fair fair fair fair u > o o cq a) tO S 0 / c; cOo a o O v U a) s X E O s o iv a) s Q L0 @ wsx Eo g , @ E s s U 9 c 2 > Jo gJ,coc C,JO .~ r,@0 Q@;cjo sC S~ S ~ w !J Q ,o Vl X O S C) C O tD n o TABLE 3
Example 3
heat treating temperature (for 4 hours) ( C) 550 650 750 shrinkage % after heat length 0.1 0.3 0.4 treating of each temperature thickness 0.8 1.1 1.6 for 4 hours density (g/cm ) 0.65 0.65 0.65 flexural strength (kg/cm) 82 80 70 flexural strength after further heating at 850 C for 3 hours 60 60 60 shrinkage (%) length 0.3 0.2 0.1 after heating at 850 C for 3 hours thickness 1.2 0.5 0.2 machineability good good good TABLE 4
oinS: O.oL o o' o' o' o cu' m n ExampleS Exarnple6 Example7 heat treating temperature 100 350 (for4hours) (CC) 100 350 100 350 100 350 ~ / ~ after heat length 0.4 0.3 0. 0.3 * oz a cu s o each D 0e O O thickness O O O for 4 hours $E (gim3) 0.42 0.39 0.88 0.81 0.81 7 0.58 0.53 o strength (k/om2) 38 30 125 98 83 o ~ o o strength after iL heating at 85000 C3V)03 21 20 b2 59 58 35 35 o G length 1.1 v Ö t D v G G W after heating at 85000 for 3 hours thickness 2.5 2.0 2.2 1.8 1.0 0.7 2.9 2.3 machineability good good I t D eO eo O X t 0e O' O' O 0e W0 O' C\i 00 X ~7 ~ v O / O eD v C\i L = O N C) = > O E @ s s ~ G 41) S ; = , tD ", E , @ ,m tz ~ U C o > # - @ o < O o sC S '' aC vo Qt V CD S X S J r=J . E TABLE 5
Comparative Comparative Example 1 Example 2 heat treating temperature (for 4 hours) (CC) 350 550 350 550 shrinkage % after heat length 0.6 0.8 0.4 0.5 treating of each temperature thickness 0.9 1,4 0.6 0.8 for 4 hours density (g/m3) 0.64 0.62 0.83 0.81 flexural strength (kg/cm2) 50 43 129 115 flexural strength after further heating at 850"C for 3 hours 30 28 56 54 shrinkage(%) length 2.5 1.9 1.6 1.4 after heating at8500C thickness 15.0 12.2 1.P 1.5 for 3 hours mach Ineabi I i ty good good poor poor
Claims (3)
1. A composition for producing a calcium silicate heat-resistant material, which comprises:
(A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6-1.2; (B) 20-1 70 parts by weight of xonotlite obtained by hydrothermal synthesis;
(C) 1 5-150 parts by weight of fibrous wollastonite; and
(D) water in an amount of 2-8 times as much as that of the total solid contents.
2. A composition according to Claim 1, wherein the amount of xonotlite is 30-1 00 parts by weight and the amount of fibrous wollastonite is 50-100 parts by weight.
3. A method for producing equipment for use in transporting, holding and supplying molten metal, which method comprises the steps of:
i) molding a slurry of a uniform mixture of:
(A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6--1.2; (B) 20-1 70 parts by weight of xonotlite obtained by hydrothermal synthesis;
(C) 15-150 parts by weight of fibrous wollastonite; and
(D) water in an amount of 2---8 times as much as that of the total solid contents;
ii) steam curing said molded body in an atmosphere of steam under a pressure of not less than 6 kg/cm2 to react the siliceous material with the lime; and
iii) treating to remove water at a temperature not lower than 1 00CC under atmospheric pressure.
3. A method for producing a calcium silicate type heat-resistant material, which comprises the steps of:
i) molding a slurry of a uniform mixture of:
(A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6-1.2; (B) 20-1 70 parts by weight of xonotlite obtained by hydrothermal synthesis;
(C) 15-150 parts by weight of fibrous wollastonite; and
(D) water in an amount of 2-8 times as much as that of the total solid contents;
ii) steam curing said molded body in an atmosphere of steam under a pressure of not less than
6 kg/cm2 to react the siliceous material with the lime; and
iii) heat treating said steam cured product to remove water therefrom at a temperature of not
lower than 1 OO"C under atmospheric pressure.
4. A method according to Claim 3, wherein the heat treating of step (iii) is carried out at a
temperature of 330-1 0000C under atmospheric pressure.
New claims or amendments to claims filed on 9 June 81
Superseded claims 1-3
New or amended claims: CLAIMS
1. Equipment for use in transporting, holding and supplying molten metal, the equipment being
made from calcium silicate heat-resistant material prepared by dehydration-moulding
(A) 100 parts by weight of a mixture of lime and siliceous material having a CaO/SiO2 mole ratio of 0.6-1.2;
(B) 20-170 parts by weight of xonotlite obtained by hydrothermal synthesis:
(C) 1 5-1 50 parts by weight of fibrous wollastonite; and
(D) water in an amount of 2-8 times as much as that of the total solid contents.
2. Equipment and heat treating the moulded body at not lower than 1000C according to Claim 1, wherein the amount of xonotlite is 30--1 00 parts by weight and the amount of fibrous wollastonite is 50-100 parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8031176A GB2085044B (en) | 1980-09-26 | 1980-09-26 | Method for producing asbestos free machinable calcium silicate high heatresistant material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8031176A GB2085044B (en) | 1980-09-26 | 1980-09-26 | Method for producing asbestos free machinable calcium silicate high heatresistant material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2085044A true GB2085044A (en) | 1982-04-21 |
| GB2085044B GB2085044B (en) | 1984-07-11 |
Family
ID=10516318
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8031176A Expired GB2085044B (en) | 1980-09-26 | 1980-09-26 | Method for producing asbestos free machinable calcium silicate high heatresistant material |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2085044B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1340729A1 (en) * | 2002-02-28 | 2003-09-03 | E.G.O. ELEKTRO-GERÄTEBAU GmbH | Heat-insulating body |
| WO2024003139A1 (en) | 2022-06-29 | 2024-01-04 | Prtc Nv | Green calcium silicate hydrate boards and process thereof |
-
1980
- 1980-09-26 GB GB8031176A patent/GB2085044B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1340729A1 (en) * | 2002-02-28 | 2003-09-03 | E.G.O. ELEKTRO-GERÄTEBAU GmbH | Heat-insulating body |
| WO2024003139A1 (en) | 2022-06-29 | 2024-01-04 | Prtc Nv | Green calcium silicate hydrate boards and process thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2085044B (en) | 1984-07-11 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PE20 | Patent expired after termination of 20 years |
Effective date: 20000925 |