CA1338340C - Inorganic fiber composition - Google Patents

Abstract

Inorganic fibers which have a silicon extraction of greater than about 0.02 wt% Si/day in physiological saline solutions. The fiber contains SiO2, MgO, CaO, and at least one of Al2O3, ZrO2, TiO2, B2O3, iron oxides, or mixtures thereof. Also disclosed are inorganic fibers which have diameters of less than 3.5 microns and which pass the ASTM E-119 two hour fire test when processed into a fiber blanket having a bulk density in the range of about 1.5 to 3 pcf.

Description

r ~

INORGANIC FIBER COMPOSITIO~

. Field of the Invention This invention relates to inorganic fiber compositions and more particularly it relates to inorganic fiber compositions which can contain silica, magnesia, calcium oxide, alumina, and other oxides. Some of the inventive fibers have excellent ~ire ratin~s, some have especially low durabilities in physiological saline solutions, and some have combinations of these foregoing properties.
Back~round of the Invention For many years inorganic fibers, generically referred to in the industry as "mineral wool fibers", made from slag, rock, fly ash, and other by-product raw materials have been manufactured.
These fibers have been typically manufactured by melting the sla~, rock, etc., cont~ining such oxides as silica, alumina, iron oxide (ferrous and ferric), calcium oxide, and magnesia; allowing the molten material to be blown by gas or steam or to impinge on rotors at high speeds; and causing the resulting blown or spun fibers to be accumulated on a collecting surface. These fibers are then used in bulk or in the form of mats, blankets, and the like as both low and hi~h temperature insulation. U.S. Patent No. 2,576,312 discloses a conventional mineral wool composition and method for making the same.
In the past, the industry has well recognized the standard ~ _ -2- 1~34~
drawbacks associated with conventional mineral wool fibers.
Conventional mineral wool fibers may have hi~h contents of undesired oxides which often detract from their refractory properties. The conventional mineral wools are coarse, i.e. they have avera~e fiber diameters of 4 to 5 microns (measured microscopically) and have hi~h shot contents in the ran~e of 30 to 50 wei~ht percent. The coarseness of the fiber reduces the insulatin~ value of the fiber and makes conventional mineral wool unpleasant to handle and unfriendly to the touch. For example, because of their coarse fiber diameters, conventional mineral wool blankets must have bulk densities of from 4 to 8 pcf and even hi~her in order to pass the ASTM E-ll9 two hour fire test. On the other hand, fiber ~lass blankets are often made with bulk densities of 2 pcf or lower.
While the fiber ~lass blankets are friendly because of their low bulk densities and relatively fine fiber diameter, they do not have sufficient fire resistance so as to pass even the one hour ASTM
E-ll9 fire test.
Recently, another potential problem with traditional mineral wool and other types of fiber has been reco~nized. It is well known that inhalation of certain types of fiber can lead to elevated incidence of respiratory disease, includin~ cancers of the lun~ and surrounding body tissue. Several occurrences are well-documented in humans for several types of asbestos fiber.
Althou~h for other varieties of natural and manmade mineral fiber Z5 direct and unequivocal evidence for respiratory disease is lackin~, the potential for such occurrence has been inferred from results of tests on laboratory animals. In the absence or insufficiency of direct human epidemiolo~ical data, results from fiber inhalation or implantation studies on ~n~ provides the best "baseline information" from which to extrapolate disease potential.
Chronic toxicolo~ical studies on animals have, however, been able to statistically demonstrate the importance of three key factors that relate directly to the potential for respiratory disease and especially carcinoma: (a) dose of fiber received (includin~ time of exposure); (b) dimension of the inhaled fiber;
and (c) persistence of the fiber within the lun~. The effects of dose and dimension have been well-characterized from such studies -_- -3 1338~4~
~-~ and as a result are fairly well known in regard to human disease potential. The dose is obviously a product of the environment in which the fiber is used and the manner in which it is used. The dimension and persistence of the fiber within the lung, on the other hand, are functions of the manner in which the fiber is formed and of its chemical composition. In general, the smaller the fiber the more likely that it will become embedded in lung tissue when inhaled, thus increasing the danger of respiratory disease.
Although less is known about the link between persistence of the fiber within the lung and respiratory disease, increasing attention is being focused on this aspect of the health issue.
Biological persistence refers to the length of time a fiber endures as an entity within the body. The physiochemical concept that most closely relates to persistence and is perhaps more easily quantified is that of "durability" - specifically, the chemical solubility (or resistance to solubility) of fibers in body fluids and the tendency of such fibers to maintain physical integrity within such an environment. In general, the less durable a fiber is, the less will be the potential health risk associated with the inhalation of that fiber. One method of measuring the chemical durability of a fiber in body fluids is to measure its durability in physiological saline solutions. This can be done by quantifying the rate of extraction of a chemical component of the fiber such as silicon into the physiological saline solution over a certain period of time.
Thus, as can be easily concluded from the foregoing discussion, conventional mineral wool fibers have several serious drawbacks. However, even the alternatives to mineral wools have problems. For example, as mentioned earlier glass fibers have a fire resistance problem and whereas the refractory ceramic fibers have been gainin8 increasing use in recent years as an alternative to mineral wool fibers because of their ultra-high temperature resistance and superior ability to pass all fire rating tests, their use is limited by the fact that they are relatively expensive and have a relatively high chemical durability in physiological saline solutions as well.
In conclusion, there is a great need in the industry for low cost, friendly feeling low bulk density inorganic fibers which _ -4- 1 3 3 ~ ~ q ~

have ~ood fire resistance properties as measured by their ability to pass the ASTM E-ll9 two hour fire test. Additionally, there is a tremendous demand for fibers which have especially low durabilities in physiological saline solutions. What would be particularly advantageous to the industry would be fibers with combinations of the above mentioned sou~ht after properties. Also advantageous would be fibers which also have excellent refractory properties as well, e.g. high continuous service temperatures.
Summary of the Invention In one embodiment of the present invention there are provided inorganic fibers having a silicon extraction of ~reater than about O.OZ wt% Si/day in physiolo~ical saline solutions and a composition consistin~ essentially of about 0-10 wt% of either Al203~ zro2~ TiO2, B2o3~ iron oxides, or mixtures thereof; 35-70 wt% SiO2; 0-50 wt% MgO; and CaO.
In another embodiment of the present invention, there are provided inor~anic fibers which have a 5 hour silicon extraction in physiological saline solutions of at least about 10 ppm. These fibers can broadly have compositions consistin~ essentially of the 20 following ingredients at the indicated weight percenta~e levels:
0-1.5 wt% of eitherA1203- ZrO2- Ti2' B203' iron oxides, or mixtures thereof; 40-70 wt70 SiO2; 0-50 wt% MgO;
and CaO
1.5-3 wt% of eitherA1203, ZrO2,TiO2, B203, iron oxides, or mixtures thereof; 40-66 wt% SiO2; 0-50 wt% MgO;
and CaO
3-4 wt% of eitherA1203~ zro2~ Ti 2~ 2 3 iron oxides, or mixtures thereof; 40-63 wt% SiO2; 0-50 wt% M~O;
and CaO
4-6 wt70 of eitherA1203~ ~ro2~ Ti 2~ 2 3 iron oxides, or mixtures thereof; 40-59 wt% SiO2; 0-25 wt% MgO;
and CaO
6-8 wt% of eitherA1203~ zro2~ TiO2, 2 3 iron oxides, or mixtures thereof; 35-54 wt70 SiO2; 0-25 wt% ~gO;
and CaO
8-10 wt70 of eitherA1203. ZrO2.Ti2' B203' iron oxides, or mixtures thereof; 35-45 wt% SiO2; 0-20 wt% MgO;

- ~ - s -1~3~340 and CaO
In a preferred embodiment, inventive fibers with 5 hour silicon extractions of greater than about 20 ppm and most preferably greater than about 50 ppm are provided.
In another embodiment of the present invention there are provided inorganic fibers having a diameter of less than 3.5 microns and which pass the ASTM E-119 two hour fire test when processed into a fiber blanket having a bulk density in the range of about 1. 5 to 3 pcf and having a composition consistin~ essentially of about: 0-10 wt70 of either A1203, ZrO2, TiO2, B203, iron oxides, or mixtures thereof; 58-70 wt% SiO2; 0-21 wt70 MgO; 0-2 wt70 alkali metal oxides; and CaO and wherein the amount of alumina + zirconia is less than 6 wt% and the amount of iron oxides or alumina + iron oxides is less than 2 wt%. Preferably, the inventive fibers in this embodiment may have compositions consisting essentially of about:
0-1.5 wt% Of either A1203, ZrO2, TiO2~ B203 ~
iron oxides, or mixtures thereof; 58.5-70 wt% SiO2; 0-21 wth MgO;
0-2 wt% alkali metal oxides; and CaO
greater than 1.5 wt% up to and including 3 wt70 of èither A1203~ zro2~ TiO2, B203, iron oxides, or mixtures thereof; 58.5-66 wtZ SiO2; 0-21 wt% MgO; 0-2 wt70 alkali metal oxides; and CaO
greater than 3 wt% up to and including 4 wt% of either A1203, ZrO2, TiO2, B2o3~ iron oxides or mixtures thereof; 58-63 wt70 SiO2 ; 0-8 wt% MgO; 0-2 wt70 alkali metal oxides;
and CaO
greater than 4 wt% up to and including 6 wt% of either A1203~ zro2~ TiO2, B2o3~ iron oxides, or mixtures thereof; 58-59 wt70 SiO2; 0-7 wt% MgO; 0-2 wt70 alkali metal oxides;
and CaO.
As discussed herein earlier, there has been a demand in the industry for inorganic fibers with an excellent fire rating at low bulk densities and fibers with especially low chemical durabilities in physiological saline solutions. Therefore, each category of 35 inventive fibers should fulfill a real need in the industry and should be available for applications where heretofore low cost, mineral wool type fibers have not been available. What is 13383~0 particularly advantageous about the present invention is the fact that fibers are provided where a special demand exists, i.e.
applications in the industry where fibers with both an excellent fire rating and an especially low durability in physiological saline solutions are in demand.
In its method aspect, the invention relates to a process for decomposing a silica-containing fiber comprising the steps of:
(1) providing an inorganic fiber prepared from a composition consisting essentially of: (a) if present, in an amount up to 6 wt%
Al2O3; (b) 50-70 wt% SiO2; (c) if present, in an amount up to 30 wt%
MgO; and (d) the remainder consisting essentially of CaO, the total being 100% by weight; (2) subjecting the silica-containing fiber to a physiological saline fluid; and (3) extracting the silica at a rate of at least 5 parts per million (ppm) of silicon in 5 hours, thereby decomposing the silica-containing fiber.
In its composition aspect, the invention relates to a refractory inorganic fiber composition consisting essentially of approximately: (a) 58.5-68.9 wt% SiO2; (b) 18.1-40.5 wt% CaO; (c) 0.11-16.4 wt% MgO; (d) if present, in an amount up to 1.5 wt% Al203;
(e) if present, in an amount up to 4.5 wt% ZrO2; (f) if present, in an amount up to 8.41 wt% B2O3; (g) if present, in an amount up to 2.9 wt% Fe203; (h) if present, in an amount up to 2.6 wt% Na2O; and (i) if present, in an amount up to 10 wt% Tio2; wherein the total quantity of Al2O3, ZrO2, Tio2~ B2O3 and iron oxides does not exceed 10 wt%; and wherein the inorganic fiber composition is capable of withstanding the rising temperatures of a simulated fire reaching 1,010C in two hours and is soluble in physiological saline solution.

rn/sg P~

1~3~3~
-6a-Other features and aspects, as well as the various benefits and advantages, of the present invention will be made clear in the more detailed description which follows.
Detailed ~escription of the Invention The inventive fiber compositions of the present invention can be made from either pure metal oxides or less pure raw materials which contain the desired metal oxides. Table I herein ~ives an analysis of some of the various raw materials which can be used to make inventive fiber compositions. Physical variables of the raw materials such as particle size may be chosen on the basis of cost, handleability, and similar considerations.
Except for meltin~, the inventive fibers are formed in conventional inor~anic fiber forming equipment and by usin~ standard inor~anic fiber formin~ techniques as known to those skilled in the art. Preferably, production will entail electric furnace melting rather than cupola meltin~ since electric melting keeps molten oxides of either pure or less pure raw materials more fully oxidized thereby producin~ longer fibers and stron~er products. The various pure oxides or less pure raw materials are ~ranulated to a size commonly used for electric melting or they may be purchased already so ~ranulated.
The ~ranulated raw materials are then mixed to~ether and fed to an electric furnace where they are melted by electric resistance meltin~ with electrodes preferably positioned according to the teachin~s of U.S. Patent No. 4,351,054. Melt formation can be either continuous or batchwise althou~h the former is preferred.
The molten mixture of oxides is then fiberized as disclosed in U.S.
Patent No. 4,238,213.
While the fiberization techniques tau~ht in U.~. 4,238,213 are preferred for makin~ the inventive fibers, other conventional methods may be employed such as sol-~el processes and extrusion throu~h holes in precious metal alloy baskets.

~ ~ -7~ 1338340 The fibers so formed will have lengths in the range of from about 0.5 to 20 cm and diameters in the range of from about 0.05 to 10 microns with the average fiber diameter being in the range of about 1.5 to 3.5 microns. Table 2 shows the average fiber diameter (measured microscopically) and the unfiberized shot content of various inventive fibers. As may be seen, the avera~e microscopic fiber diameter was 2.3 microns and the average unfiberized shot content was 277..
For purposes of comparison, conventional mineral wool fibers were also tested with the results being given in Table 2 as numbers 226 to 22~. These conventional fibers averaged 4.7 microns (measured microscopically) in diameter and had an average 40 wt70 shot content. The continuous service temperature ranged from 1370F
to 1490F, averaging 1420F.
Table 3 contains an extensive chemical analysis of a number of inventive fibers. Because of the large number of fiber samples containing alumina additives made to the base calcium oxide/magnesia/silica system, only the average analysis of the minor constituent- of these fibers are given in Table 3. The silica, alumina, magnesia, and calcium oxide contents for these fibers are given in Table 4.
As used herein, the "service temperature" of an inorganic fiber is determined by two parameters. The first is the obvious condition that the fiber must not soften or sinter at the temperature specified. It is this criterion which precludes the use of ~lass fibers at temperatures above about 800F to 1000F (425 to 540C). Additionally, a felt or blanket made from the fibers must not have excessive shrinkage when soaking at its service temperature. "Excess shrinkage" is usually defined to be a maximum of 5~ linear or bulk shrinkage after prolonged exposure (usually for 24 hours) at the service temperature. Shrinkage of mats or blankets used as furnace liners and the like is of course a critical feature, for when the mats or blankets shrink they open fissures between them through which the heat can flow, thus defeatin~ the purpose of the insulation. Thus, a fiber rated as a "1500F (815C) fiber" would be defined as one which does not soften or sinter and which has acceptable shrinka~e at that temperature, but which begins to suffer 13~8~0 in one or more of the standard parameters at temperatures above 1500~ ~815C).
The service temperatures for a representative number of fibers in the inventive compositional range are listed in Table 2.
The continuous service temperature for constant silica/magnesiatcàlcium oxide ratios are given in Table 6. As may be seen in all cases, the lower the alumina content of the fiber, the higher the service temperature will be, with the highest service temperature being at zero percent alumina for alumina contents less than 307.. Thus to attain the most desired properties of the inventive fiber it is not possible to accept any of the alumina contents resulting from melting the traditional mineral wool raw materials. Rather, various amounts of sufficiently pure oxides will be required to dilute the alumina ,contents to the desired low levels. To attain fibers of the highest service temperatures, only pure raw materials with essentially no significant amounts of . ~ lt~m; n~ must be used.
A series of inventive fibers were also tested for their silicon extraction in a saline solution according to the following procedure:
A buffered model physiological saline solution was prepared by adding to 6 liters of distilled water the following ingredients at the indicated concentrations:
In~redient Concentration, ~/l g 2 2 0.160 NaCl 6.171 KCl 0.311 Na2HP04 0.149 Na2S4 0 079 CaC122H2 0.060 NaHC03 1.942 NaC2H302 1.066 Before testing, this solution was buffered to a pH of 7.6 35by bubbling with a 'gaseous mixture of 5% C02/95%N2.
One half (1/2) gram of each sample of fiber listed in Table III was then placed into separate closed, plastic bottles along with -9- 13~

50 cc of the prepared physiolo~ical saline solution and put into an ultrasonic bath for 5 hours. The ultrasonic vibration application was adjusted to ~ive a temperature of 104F at the end of the 5 hour period. At the end of the test period, the saline solution was filtered and the solution chemically analyzed for silicon content.
The silicon concentration in the saline solution was taken to be a measure of the amount of fiber which solubilized durin~ the S
hour test period. The CaO and N~0 contents of the fiber were similarly solubilized.
One of the inventive fibers was tested for silicon extraction in a physiolo~ical saline solution for periods of up to 6 months. Results were as follows:

Steady State Tolal Conunents on Sili(o~ lico~ xtraction Amphoteric Fiber Residue Fiber F.xtractioll Rate For 0.20 m /g Oxides in After 6 Number in 6 Holltlls Surface Areal% Si/day Fiber Months 29 (inventive) 9670 0.16% 1.07O carbonate hy(iroxyl apatite fiber, disintegrated into small particles 137 (non- 37O 0.013% 8.9% sligh~ fine graine~
inventive) ~ibers with uni~o~n corrosion 235 (non- 47O 0.012% 25.670 no fiber inventive) corrosion;
some sur~ace deposition ,.

-11- 13~3~1~
Cate~orization of oxides melts accordin~ to scales of acidity or basicity has been well known for many years. (See "A
Scale of Acidity and Bascity in Glass", Glass Industry, February 1948, pp 73-74) We have now found that by strictly controllin~ the compositions of the oxide melts accordin~ to the acidic or basicity behavior of the respective oxides, fibers can be made which are surprisin~ly soluble in saline solutions. Increasin~ the content of silica, alumina, and the amphoteric oxides in the fiber increases the acid ratio of the fiber composition. This tends to stabilize the system a~ainst silicon extraction by weak solutions as a result of relative chan~es in the interatomic bondin~ forces and extension of the silica network. Other amphoteric oxides besides alumina will have an alumina equivalency with respect to extraction by saline solutions. The amphoteric oxides zirconia and titania appear to`
have an alumina equivalency of close to 1 to l. We have found that in ~eneral for desired hi~h saline solubility the amount of total amphoteric oxides must be kept below about 1070 dependin~ upon the amount of silica present. On the other hand, with the exception of iron and man~anese oxides, the basic oxides can vary widely since their alumina equivalency is small. However, while iron and man~anese oxides are ~enerally considered to be basic in nature, their behavior with respect to saline solubility more closely relate to the amphoteric oxides, thus the amounts of iron and man~anese oxides must be similarly limited.
~any of the fibers were tested for their fire resistance accordin~ to the followin~ simulated fire ratin~ test procedure:
For screenin~ test purposes, a small furnace was constructed usin~ an electrically heated flat-plate element at the back of the heat source. A 6 inch x 6 inch x 2 inch thick sample of l 3/4 to 6 1~2 pcf density of each formulated fiber was mounted parallel with the element and 1 inch from it. Thermocouples were then positioned at the center of the fiber sample surfaces. A
computer was used to control power via a simple on-off relay system to the heating element. The position of the relay was based on the reading of the thermocouple on the sample surface nearest the element and the pro~rammed fire test heat-up schedule.
The furnace was heated so as to follow a standard ASTN

- 133~3~0 ~_ -12-E-119 timettemperature curve for the 2-hour test period. In the test utilized herein, failure of the fiber is considered to occur when the furnace is unable to maintain the standard temperature per ASTM E-ll9 because the fiber insulation has sintered sufficiently to allow heat to escape through the fiber layer.
The results of the testing of the fibers for saline solubility and the two hour ASTM E-ll9 f ire test are given in Table 4 for the fibers made with alumina addition and in Table 5 for the re~-;n;ng fibers to which other oxidic constituents were added.
These additions included: B2o3~ P205, TiO2, ZrO2, 2 3 ' 2 3' 2 3' Na20. For glass fibers within the scope of the invention to function in an ASTM E-119 fire test, i.e. to withstand the rising temperatures of a simulated fire which can reach 1850F in two hours, it is necessary that they convert from an amorphous condition to a beneficial psuedo crystalline state during heat-up. The inventive fibers do this but can be assisted in this function by the inclusion of suitable crystal nucleating agents. Such agents may include TiO2, ZrO2, platinum, Cr203, P2 5~ others. Such additions are within the scope of this invention.

: t) ~
~ ~ 3 ~ ~ I o o ~ ~ I I I ~

..

3 ~ b~ o r~ ~ ~ o o~
O r~ ~; O ,~ O ~ o!

~
d, ~ ~ o o o o o -- ~ _ -- r~ I ~ O O O
~ O o~ O

8 ~ _ o ~ o ~o , '~ O I ~ O r~ O
O 0 O~ 0 1 ~ 0 ~ 0 1 1 1 0 3 ~ ~
O O v) _ ~n ''? ~ "? ~ I , ~ ~ ~ ~ o O a O O I ~ ~ O ~ I I ~ C
_.

o ~ r~ o o1~ ~
O ~ O O I O ~- O O I I I O
C''~ CJ~ V~
~d ~ O O ~ ~ ~ O
U r~ O ~ ~ O O O r~
z c; o o o o c~ o u O n U ~3 U

O O

e - ~ ~ e ¢ ~ ~
X

Silica Sand: Ottawa Silica - Sil-co-Sil Grade 295 Quick Limc: Mississippi Lime - Pulverized Quick Lime 5 Calcined Dolomite: Ollio Lime NO. 16 Burnt Dolomitic l.ime Aluminum Oxide: Reynolds Calcined Alumina, RC-23 Magnesium Oxide: Baymag 56 Feed Grade 0 Kaolin: American Cyanamide Andersonville Kaolin Blast Furnace Slag: Calumite Morrisville Slag Nepheline Syenite: Indusmin Grad A400 ~5 Talc: Pfizer Grade MP4426 '0 Additives:

Soda Ash: 58.3% Na20 Boric Ac id: 55.5% B203 Magnetite Iron Concentrates: 98.5% Iron Oxides Zircon: 66.2% ZrO2 l0 Manganese Oxide: 99% MnO2 Titanium Dioxide: 99% TiO2 ~3 ~5 Chromium Oxide: 99.5% Cr203 ~3 I,anthanum Carl>onate: ~Soly Corp. C~3 o ~ ~ TABLE 2 FIBER DIAMETER, SHOT CONTENT, AND
SERVICE TEMPERATURE OF TEST FIBERS

1 33~ 0 Average Fiber Shot Service Diameter Content Temperature Test No. Microns ~ F

O - 1 1/2~ A~ho teric 0~ ides 17 1.9 - 1420 2.3 22 1440 22 2.9 - 1350 24 2.8 33 1400 2.9 - 1440 29 1.6 - 1450 1.5 - 1450 32 1.5 23 1450 34 _ - 1400 1.7 - 1450 37 2.4 22 1450 39 1.9 - 1450 43 1.9 32 1460 2.3 - 1500 2.0 25 1420 13383~0 Average Fiber Shot Service Diameter Content Temperature Test No. Microns Z F

1 1/2 To 3Z A~hnteric O~ides 87 1.9 24 1410 2.0 - 1430 2.1 - 1440 97 _ 24 3 To 4% A~hoteric Okides 4 To 6% A~hoteric Oxides 6 To 8% A~hoteric O~ides 126 1.8 26 1470 127 2.2 - 1370 128 3.3 - 1380 4~ 129 3.4 - 1430 ` 133~340 Average Fiber Shot Service Diameter Content Temperature Test No. Microns % F

108 To 10~ A~u?hoteric O~cides 135 2.9 _ 1410 137 3.1 - 1370 138 1.8 - 1450 139 1.8 - 1370 10 To 12% A"~;photeric O~ides 141 1.9 - 1460 141 2.0 - 1460 143 2.6 - 1360 144 3.0 - 1360 3512 To 20% A~hoteric O~ides 146 2.0 - 1460 20 - 30ZA~Dhoteric 02tides 150 2.5 - 1460 152 3.4 - 1520 153 3.8 32 13383~0 Average Fiber Shot Service Diameter Content Temperature Test No. Micro~s % F

O~ide Additions other than Alu~in~

167 2.5 174 3.1 25 1600 176 2.1 178 1.41 179 o.g 183 1.7 26 192 1.8 200 2.0 36 No. of Measurements: 42 22 56 Average Value: 2.3 27 Conventional Mi~eral Wood Fibers 226 4.3 33 1370 228 5.4 45 1450 229 4.4 35 1490 Avera~e 4.7 40 1420 _lg_ 1~3~311~

Average Fiber Shot Service Diameter Content Temperature Test No. Micro~s ~ F

Refractorv Fiber 233 3.0 38 1600 234 2.9 37 2400 235 3.3 44 1600 236 2.4 37 2300 237 2.8 29 2300 238 3.0 28 2400 239 3.0 27 2400 240 3.0 20 2450 Average: 2.9 31 - -20- ~3~3~0 COMPOSITION OF FIBERS
ACIDIC OXIDES _ AMPHOTER~C OXIDES
TEST SUB SUB
NO. BiO3 SiO2 P2O~ TOTAL TiO2 Al2O3 ZrO2 TOTAL
Co..1posilion o~Pibers wit Al2O3 additions (minor cons~ituents only) 1 10 0.00 _ 0.00 -- 0.01 -- 0.01 0.02 Comp~sition of Fibers with ~323 additions ~64 0.32 64.8 -- 65.12 -- 0.06 -- 0.06 165 0.52 63.9 -- 64.42 -- 1.20 -- 1.20 l66 0.64 64.6 -- 65.24 -- ~.U6 -- 0.~6 167 0.8~ 64.5 -- 65.32 -- 0.06 -- 0.06 168 1.33 64.1 -- 65.43 -- 0.06 -- 0.06 1 6g 1.37 64. 1 -- 65.47 -- 0.06 -- 0.06 170 2.22 ~3.6 -- 65.82 -- 0.06 -- 0.06 171 8.41 ~9.6 -- 68.01 -- 0.06 -- 0.06 Composition of Fibers with P2OS additions 172 -- 4g.6 6.05 55.65 0.06 0.38 0.04 0.48 Composition Or Fibers with TiO2 additions 173 -- 4~.6 -- 48.6 10.0 41.4 -- 51.4 Composition of Fibers with ZrO2 additions 174 -- 63.5 -- 63.S .~1 0.~8 0.2l 1.10 175 -- 59.2 -- 59.2 -- 0.33 0.40 0.73 176 -- 59.5 -- 59.5 -- D.31 0.42 0.73 177 -- 59.7 -- 59.7 -- û.34 0.S~ 0.84 178 -- 60.0 -- 60.0 -- 0.36 0.S4 0.g0 179 -- 59.2 -- 59.2 -- 0.35 0.58 0.93 180 -- 54.3 -- 54.3 .01 1.29 0.58 1.88 181 -- 59.2 -- 59.2 -- û.32 0.83 l.l5 1 82 -- 46.85 -- 46.85 .02 2.03 0.84 2.89 1 82(a) -- S9.4 -- 59.4 -- 0.38 2.31 2.69 1 83 -- S9.~5 -- 59.05 -- 0.30 2.65 2.9S
184 -- ~7.g6 -- 57.96 -- 0.42 3.1~ 3.53 ~ 85 -- 57.8 -- 57.80 -- 0.56 3.12 3.68 1 86 -- 59.05 -- 59.05 -- 0.38 3.27 3.~5 187 ~ 56.88 -- S6.88 -- 0.32 3.3~ 3.62 1 88 -- 57.7 -- 57.7 -- 0.20 3.30 3.50 189 -- 58.19 -- 58.19 -- 0.39 3.36 3.75 IgO S7.86 -- 57.86 -- 0.36 3.37 3.73 191 -- 58.6 -- 58.6 -- 0.5B 3.67 4.25 192 -- S8.4 -- 58.4 -- 0.65 3.69 4.34 193 -- ~6.6S -- S6.6S .0~ 3.35 4.S0 7.87 ' ~

- -13383~0 V ~ o ~ I I I I I I I I O I I I I I I I O I O I O I I I I I I I I I O

-. ~ I IIIIIIII I IIII111~1~IIIIIII11 rr v~ O

-I IIIIIIII ~ I IIIII~11IIIIIII11 ~ ~ I I I I I I I I I I I I I I IC' 1 1 111111111 m, ~o I I I I I I 1 1 1 8 1 1 _ ,~, O

~ ~`"'OI.OCIIIIIIII 0.1IIIIIIIIIIIIIIIIIIIII

o ~ I O co 00 x oo oo ~o co ~ O -- O~ I O O ~ O cj O O O ~ o ~ ~ ~ ~ r.
"~ rl p~ ~ N
7 v ~- 1 3 1 1 1 1 1 1 1 1 ~ 0,3 I s3 1 1 1 1 1 1 1 1 1 1 o I I I I I I I r.~
~ ~ 3 ~ r ~ 3 1 ~ I I I I I I I I o I o o v r !O I I I I I I I I I 8 .- I . I I I I I I o I o 1 8. 1 1 1 1 1 1 1 1 I g ~ " 1~ I I I I 1 1 1 1 1 1 1 1 ! I I 1 1 133~0 TABLE 3-continued COMPOSITION OF FIBERS
AClDIC OXIDES AMPHOTERIC OXlDES
T~ST S~B SUB
2~0. B203 SiO2 P2OS TOT~L TiO2 Al2O3 ZrO2 T{)TAL
Composition of Fibers with FcO3 ~nd ~nO additions 194 -- 64.9 -- 64.9 -- 0.06 -- 0.06 1g5 -- 49.8 -- 49.~ .0l 18.0 .01 18.02 196 ~ ~0.4 -- 50.4 .03 7.45 .01 7.49 197 -- 64.34 -- 64.34 -- 0.06 -- 0.~6 l98 -- 63.70 ~ 63.70 -- 1.20 -- 1.2~
199 -- ~3.54 - 63.54 -- 1.20 -- 1.20 38 9 -- 38.9 .01 ~.7~ .01 6.72 201 -- 6i.3 -- 64.3 -- 0.06 -- 0.06 ~02 _ 44.6 -- 44.6 .01 0.9~ .01 0.94 203 -- 63.3 -- 63.3 ~ -- 1.1S
2~4 -- 63.6 -- 63.6 _ 0.06 -- 0.06 20S -- 43.8 -- 4~.8 .a~ 15.~6 .01 ~S.28 206 -- 6~3 -- 62.3 -- 1.20 -- . 1.~
207 -- 63.3 -- 63.3 -- 0.06 -- 0.06 208 -- 43.~ -- 4~.9 .~1 14.3 .~)1 14.3 209 -- 62.0 -- 62.0 -- 0.06 -- 0.06 210 -- 60.0 -- 60.0 -- 2.~ -- 2.0 21 1 -- 60.0 -- 60.0 -- -- --Compositi~n o~ Pibers with La203 addltions 2t2 -- S8. 1 -- S8.1 -- 0.Q6 -- 0.06 213 -- S7.8 -- 57.8 -- 0.06 -- 0.06 ~14 -- 57 5 -- 57.5 -- 0.06 -- 0.06 21S _ ~6.9 ~ S6.9 -- û.06 -- 0.06 Composition of Fibers wlth Cr203 additions ~16 -- 62.6 -- 62.6 0.01 0.49 0.~)1 0.51 ~r 1338~

"~ m ~

- '~ 1 1 I I 1 1 I I I I I I I I I I

a~ ~ ~ ~ o r` t~ O ~ o ~ ~o ~ o o ~ ~ r~
~ O

o I I ~. I I I I I I I 1- 1 1 1 1 1 1 1 1 1 1 o m I I I I I I I I I I I I I I I I I I I I 1 8 O 1~ o o ~ ~ ~ ~ ~ O
Q V ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~
~ C
o ~ O I I I I I I I I I I I I I I I I I 1~ 1 1 1 I,a l ~ ~ O ~ ~ ~ 00 ~ ~ ~ o o ~ o o o ~ ~ ~ ~n ~ ~
~ T ~ o ao O ~ O ~ W ~ W 00 ~ W O O O ~ ~~ o ~
r O I I I I I I I I I I I ~ I I I I I I .~ I I 1 1 ~3 o n n ~'~3 1 1 1 1 1 1 ¦ ¦ ¦ ~ L c:i o o o L

O o I I I I I I I I I I I I I I o. o I I I I .o 8 ~ ~ _ ~ o v~ ~ o ~ ~ ~o ~ ~ ~ E 00 rn ~o ~ 00 0 c~ ~ O ~ O `O ~ O~ O ~ ~ 00 0 _ _. _ _ o o O c~ O . . . . . . ~ I ~ O d c~ O U o E

~ O~ o o c~ o o o o o o O _ ~ _ _ _ _ "X

TABLE 3-continued COMPOSlTION OF PIBERS
ACIDIC OXID~S AMPHOTE~RIC OXIDES
T~ST SUB SUB
NO. B203 SiO2 P20S TOTAL r~ol Al2C)3 ZrO2 TOTAL
Con~position of Fibers with Ns2O additions 217 -- 64.7 -- 64.7 -- 0.06 -- 0.06 218 ~ 64.~ -- 64.5 -- 0.06 -- 0.06 21~ -- 64.4 -- 64.4 -- 0.06 -- 0.06 220 -- 63.~ -- 63.5 -- 1.20 -- 1.20 22 1 -- 64.3 -- 64.3 -- 0.~)6 -- 0.06 222 -- 64.2 -- 64.2 -- 0.06 -- 0.06 223 -- 64.0 -- 64.0 -- 0.06 -- 0.06 224 -- 63.0 -- 63.0 -- 0.06 -- 0.06 225 -- 60.3 -- 60.3 -- 0.06 -- 0.06 Composition of Convcntional Mine~al Wools 226 -- 40.0 -- 40.0 0.37 9.~ 0.03 g.50 227 -- 39.9 0.02 39.92 1.1 l l2.85 0.03 13.99 228 -- 37.65 0.B4 38.49 2.3S 9.85 0.04 12.24 229 -- 41.7S 0.~2 4l.87 1.07 16.0 0.03 17.10 Compo~i~ion of Ref~actory Pibers (~ibcrs with le~s than 25% nasic Oxides) 23 1 ~ 3 l .0 -- 3 1.0 -- 47.5 0.0~ 47.S2 ~32 -- 37. 1 -- 3'1. 1 -- S9.2 ~ 59.2 233 -- 50.0 -- S0.0 -- 40.0 ~ 40.0 234 -- S4.0 -- 54.0 -- 46.~) -- 46.0 235 -- S8.47 1.15 59.62 0.98 24.54 0.03 2S.~S
236 -- S2.1 -- S2.1 1.76 44.4 .~3 46.39 237 52.0 -- 52.0 1.71 42.2 2.93 46.84 238 49.8 -- 49.8 1.60 38.3 9.32 49.22 ~39 -- 48.6 -- 48.6 l.SS 36.2 12.~ ~0.~S
240 -- 4t.8 -- 47.8 1.50 34.4 I 5.1 51.00 241 -- 46.2 -- 46.2 1.40 31.0 20.7 53. 10 243 -- 64.5 -- 64.5 -- 27.4 27.
X

-24a-I I I I I I I I oo o~
z O ~ O ~ I I I I o I I I I I ~ I I

5~ 11lIIIIII ~o~o IIIloIIIIIIII

o ~ ~ ~ O ~ ~ ~ ~ ~n ~ ~ I ~ ~ ~i ~ 8 ~ a~ I

~ ~--O ~ J 00 ~
O I I I I I I I I ~ o o o o a o w n _ I~ ~ _ o o ~ ~ r~--~ '.~ ~ u~ ~ ~ ~ 4~ ~
2 ~ ~ ~ ~ o~ o ~ ~ ~ ~ ~r, ~--~, v~ o c~ o ~ o o, ~IS O C O C~ O----~ ~ o o ~ ~

m I I I I I I I I I O c, O ' I I I I o I

o fi I I I I I I I I I ~ d ' o ~ o ~ oo V
O e~ d o o c~ o o O ~'~IIIIIIIII,ooooo:~IIIIoI
Z; V ~
m o ~ o o O
V I I I I I I I I I o o o o ~ ~O r~ ~ ~ O co 1 3 ~
C~
I cl-, ~ 4 ~
- Q O O o ~, *~IIC`lI~C~IIIICII

O -~ C
O _ ,~ ~ E o ~ o _ `D 1~ ~D o U\ _ Z
O
,_ ¢
C
z ~ o ~ r~ I~ r~ ~ r~ r~ ~ o y ~ _ o o ~ ~D ~ ~ ~ u~ ~ _ u~
C~,. .. . ...........
JJ ~ o o C~ o o o _ _ _ _ o o _ o o o o --O--' OOCJ~OOOOOOOOOOOOOOOO~
¢ E~- __ ____.___~________ ¢9 ¢
C ~ . . ....
c E~ ~o ~D ~ ~ ~ ~
_, r 0 ~
Z ~1 Irl _ ~ ~D _ _ ~D U--1 O t~ t~) O 1~ 0 0 t~ r/
~ ~ ~ I~ ~ ~ CD t~J CO t~ Cl~ ~ 0 ~4 E~ 0 11 U~ r-U
~ U~ O ~ ~ ~ O ~ 0~ ~ O ~ O 1~ X 1~ CO ~O 0 E-l ~ol 0 E-~ 3 11 z O ~C
~ 1 C u~ 1~ ~ ~ ~ ~J 0 CO ~ cr~ C~J C`~ 1~ 1/~ ~D O
~ o ...... ...................... ~...... -Oc~E~ oOooooooooooooooooo ~ G
a ;!Ç rc O t~~r O ~ X ~ U~ O O o c~l ~D 'D ~ I~ O O U~ ~ ~ X
<5~ t.lOOOOOOOOOOOOOOOOOOO
. r~
' r-~
o~ D
~ W
. r~ 0, C`~ E3 r~rt rC ~ O ~ ~ O~ U~ ~D ~ C~J O 1~ _ C`~
c~ x ta ~ c~ _ _ t~ ~ Ir~ ~D 00 r-- co oO cr~ O~ O O -- _ O Z
~ o _ ~ ~
O _ _ _ _ _ _ _ _r~ _ Z O

-26- 13~8~0 _.

aY o 1~ --C
~. C o~
.~ o ooo oooooooooo C . . . . `

o .
~ C J
o ...
= _ 5 E
W .~ C
c l ,~ ~ a:) o-- c~ o ~ ~o o ~D ~ o a~ _ ~t 0 ~ ~o w _ .,~
Q ~ O 1` 1` 0 ` Cr` I` o o ~D u~ ~ ~ _ ~ ~ c~ ~ c~
o_~ ...................
E~ ~ o o c~ o c~ o~ o o o~ oct~ o q o o o~ O~ o ~ o~ o o ~ cr~ oc~ o c6 61 ,_ -w o ~ -- y~ -- o ~ ~ ~
-- O ~D ~O ~ ~ ~ ~ ~ ~ _ _ _ _ O _ _ O O O _ ~
~1 Q
51 x u~u~ ~ O ~1 ~t ~D c~ o~ ~ u~ I~ ~ ~ ~ ~ ~D ~ 11 l -- ~O O ~O r`~ 1-- 1~ ~ ~ ~o ~ ~ O ~ O u~
C -- ~ ~ -- _ ~
E~ o O
3 ~ o V , U~
o o ~ _ U~ o ~ ~ ~ 0 C~ o Z:~LO .................
O ~; U~ o U~ U~ o ~ U~

r~

O _ ~ ~`I ~ O _ O~ l~ O _ O t~ _ O U~ ~
oo--Ioooo__ooo_oooooo V~

v~
r~ .. 5 X
.O ~ , o ~ ~ O O x o o _ ~ ~ ~ u~ ~ o~ ~ I~ ~ u~ a~ _ ~ O ~ ~ o o ~ ~ Cr~ o o ~ r~ o o o ~ o o _~ ... ~.............. .
C~OO_OOOo__ooO_oooooo 5~ 5 ~ _.
o ~::
u~ Q ~ N
._~ 5~ ~ E. u~
o ¢ c~ a~ o ~ ~ o o ~~ ~ C~ C~
Y U~ o ~ X C~ C~ C~ oo ,~
-J
o z o ~ O _ ~ ~ ~ U~ ~D r~ c~ ~ O _ c~ ~ c~ 11 Z O ic 9 ~ _ , ~

EXPE~IMENTAL DATA

COMPOSITION, WT% 5 llour Acidic Amphoteric Saline E-ll9 Fire T
Oxides O~ides Basic Oxides Total Extraction Tl~ickne3s NO. SiO2 A1203 ~al CaO M~O TotalAnalytical ppm. Si Density 0 to 1 1/2% A~hoteric O~ides 39 5~.9 0.08 0.10 34.2 6.10 40.4 99.45 67 2.0/1.86 59.0 0.24 0.26 35.9 3.8 39.9 99.21 49 2.0/1.97 41 59.1 0.09 0.11 40.3 0.43 40.83100.09 68 2.0/1.90 42 59.2 0.24 0.26 4.7 36.8 41.60101.11 47 2.5/1.4 43 59.15 0.32 0.34 35.55 4.75 40.4099.94 60 2.0/1.95 44 59.4 0.04 0.06 29.8 10.7 40.60100.11 61 2.0/1.92 59.5 0.02 0.04 34.2 5.98 40.2899.87 77 2.0/1.90 ~6 59.5 0.02 0.04 32.1 8.16 40.3699.95 73 2.0/1.89 47 59.6 1.43 1.45 22.5 16.8 39.6 100.8 51 2.0/1.88 48 59.6 0.03 0.05 28.7 11.4 40.2 99.9 70 2.0/1.91 59.8 0.28 0.30 40.5 0.11 40.71100.86 30 2.0/2.01 51 59.9 1.48 1.50 25.8 12.9 39.0100.55 47 2.0/1.98 52 59.9 1.31 1.33 28.1 11.0 39.4100.78 45 2.0/1.95 ~
53 60.0 1.41 1.43 22.3 16.4 39.0100.58 41 2.0/1.91 C~3 54 60.3 0.17 0.19 32.3 6.36 38.7699.30 59 2.0/1.89 o 60.4 ' 1.05 1.07 28.5 9.85 38.4599.97 45 2.0/1.95 56 60.5 1.11 1.13 27.9 10.7 38.9100.68 36 2.0/1.94 57 60.7 0.93 0.95 28.7 9.47 38.2799.97 51 2.0/1.93 58 60.8 0.2 0.22 36. 3. 39.10100.17 56 * = Not Fiberizable ** P = Poor, F = Failed -28- - 1 ~383~0 _ E-~
h ,t .

0 c~ _ x o 1~ _ ~o _______C~_____~I___ ~ S: _ _ _ _ _ .~. OOOOOOOOOOOOOO OOO
C~
C

O '-i ~1 aJ ~1 Cll ~ C ~_I
O ~
_- ~ e C.

U
_ ~ O 1~ C'~ ~ I~ I~ X ~ CO O O

~ cl --c w ~ ~ o ~ ~ u~ o ~`I '` ~ ~ ~ ~ o ~ a~
............. ..

~ r~;
r ~ ~ O 0 0~ 0 ~ 00 0 _ CO GJ
.................. ..
O I u~ u~ ~O I~ u~ O O U~ D O ~ _ I~ O t3 C _ _ _ _ ~ _ ~ 11 - 5 ._i r~ _ ~ O ~ 00 O~ X _ Z~10 .... ........... .
O ~ ~ ~ o a~ _ ~ ~ a~ ~ o oo 1~ ~ 1~ co _ u~
~ O
n o o o o o ~ U~ _ .;, C~ ~ O _ o o o o _ O
o o o o o _ _ _ _ _ _ o _ o o o o G

~ c o o o o o ~ ~ -- ~ ~ ~ o -- o o o o O O O O O ~ _ _ _ _ _ O _ O O O O

_1 . N
~ 3 ro O ~S ~ D X a~

JJ
O
z o ,æl o ~' ~r a 13383 ~ O
~, u~
o~ -~ ~ ~ o o ~ 5 _ a~ o o o ~ c~ ~ ~ ) o I c ~ . . . . .. . .
Y ~J I ~ ~ I~ I I ~ I
.~ oo o o oo oooo o c~
c o _1 ~ c ~
o . ~ v _ ~ E
~ l ~ .
_ o ~ ~ a~ _ o ~ I

o_, ........ .........
E~ ~ ~ o o o O~ o ~ O o o o~ o~ o cr~
q o~ o o o o~ o o~ O o o ~ ~ o a~

C --c æ l ~ ~ I~ ~ ~
. t5 0 0 1~ ~ _ `D ~ O _ ~D O ~ ~ _ ~ _ U~ O
-- o ~ ~ ~ -- O _ O _ co ~ ~ o o~ r~ r~ r-- a Ct I~ u~ O _ O ~ 1~ 0 0 1~ ~D ~ ~ ~ O _ O a~
~ 01 W
~ r C~ ;t O ~ ~ ~1 ~ _ O 1~ ~ I O C~
~ 11 E~

U ~ ~ I~
~1 0 ~ ~D ~D O ~ _ C~ O a~ ~ ~ 0 ~ ~ O
Z~ O ........ .......... .
O ~ ~r ~o CO _ ~ o X r~ U~ ~ o ~ ~ ~ ~ CO U~
~ C~ ct V~

_I _ O ~ O O O ~ 0 0 O C
O O O O O ~ ~`J C~ _ ~ ~ ~ C~ C~l _ Ct~ _~
a ~ u~
V C- a I .,~
.. ~ ~ ~1 O ~ ~ O O O C~ ~ X
< c~J o u~ o ~ o o o ~ x o ~ ~ ~ u~ ~o ~ I . I I . t,` .........
c c~ o o o o ~ c~J ~ ~ ~ ~ o c~
a al ~ a ~ o o ~ ~
C.1 Ul p~ ~ N
~`I 3 ¢ '~
~ -- -- C` ~ ~ o O ~ _ C~ _ ~ O ~ c ~ ~ a~
¢ C ~ ~ ~ o O
~5 o o o _ o ~ ~

EXPERI~E~TAL DATA
f COMPOSITION, WT% 5 I{our AcidicAmphoteric Saline E-ll9 Fire Tes Oxides Oxides Basic Oxides Total Extraction Tl-ickness NO SiO2 A1203 Total _aQ ~Q ~Qal A~alyticalppm. Si Density 1 1 /2~ ~o 3~ A~hoteric Oxides (Cont,) 60.2 2.21 2.23 32.7 4.9 37.7 100.18 50 2.0/2.04 .
96 61.4 2.17 2.19 26.2 10.1 36.4 100.04 18 2.0/1.87 ]
97 61.4 1.66 1.68 29.9 6.9 36.9 100.03 61 2.0/1.91 98 61.8 2.84 2.86 34.0 0.2 34.3 99.01 51 2.0/1.93 99 62.0 2.81 2.83 34.1 0.2 34.4 99.28 55 2.0/1.90 100 62.1 2.75 2.77 33.8 0.2 34.1 99.02 13 2.0/1.91 101 62.7 1.79 1.81 25.6 9.4 35.1 99.66 18 2.0/1.96 102 63^0 2.54 2.56 33.1 0.2 33.4 99.05 37 2.0/1.87 103 63.9 1.84 1.86 30.7 2.5 33.3 99.11 38 2.0/1.94 104 64.1 1.83 1.85 17.7 16.3 34.3 100.4 12 2.0/1.95 105 65.1 2.15 2.17 9.74 23.1 33.15 100.57 17 106 65.6 1.56 1.58 2.7 29.7 32.5 99.73 33 2.0/1.91C~
107 66.7 1.80 1.82 30.7 0.1 30.9 99.47 2 2.0/1.90C~3 3 to 4~ Amphoteric Oxides 108 49.8 3.5 3.52 4.98 40.9 46.18 99.65 33 109 50.3 3.58 3.60 45.0 0.64 45.74 99.69 19 2.0/1.96 110 55.1 3.77 3.79 7.89 33.7 41.89 100.93 33 2.0/2.06 * = Not Fiberizable ** P = Pass, F = Failed ... ... .... .. ....

~ 133~3~0 C~ VJI
oo o ~ ~ o o~ o ~, C _ _ _ . C o o o o o o o o o o o o c ~ C ~
o .,, ~, ; E
-I C
U~ ~ C
I I O~ o _ ~o o ~ (~ ~ I~ r~ ~ e~
_ ~ U~ C~ ~ ~ _ u _ ~ O _ O ~ l-- --o_ E~ _ o o o ~ oo~ C~
R O O O O O0~ oc7~ a~
C Cl C
.
r_ ,L~ ~~
-- G _ O~ O O0 C~ r`I` ~t L.
L~
C ~ o Or~0 ~ ~ ~ U~ ro r ~ 0 ~~O ~ O O OC~ ri -- -- w E~ t~ 11 3 ~
VJ _ U~ ~, ~ O~t _ 0 0 Z ~ 01 O W ~ ~~I~U~ ~ ~O~ ~ O _ 0 ~ 0~ ~~ _ O
O ~ ~ O r~ 0 ~ ~ 1 O ~ t U ~~ _~ ~~ ~ ~~7 ~ ~ ~~ ~U~
~ri ~ V ' Gl C C
O

Ot~ ~O 0 0 < C~ ~C~J~ ~ O ~C`~ O ~ O ~ ~ ~O
~ r O O~-~C~ O ~ ~ ~~)~ ~ ~U~
O O
D

~ ~ W
UVJ Cl U N
ro ~:1 0 ~ ~0 u~ r~1~~ U~ ~ C~l 0 ~ ~1 o r~ X 0 0 1 ~
r~ C~
~ ~O l~ 000 0 '1 ~: ~, ~D O
O ~ O
o~
__________ ~ ____ 3C -o E~
~ 133834U
. .
Gl ~ a~ o -- o~ o o o ~ O
ICl-~
C -- _ _ OOOOO OO O O
--C~ ... .. . .
C

O r~
~1 .~i cn ~ C ~
_ ~ ~ E
~t .. P-J O~ c~l o r`
_ _ _ _ _ _ _ _ t5 o ~ . . . ~ ~ D ~ O O ~ ~
E-~ r ~ o O C~ ~ C 0 /~ ~ O ~ O
a ~ o~ ~ ~ ~ c o c~ ~ o ~ cr~ o o o o ~ __ _ ____I
---......... ......
o c~ D O 1~ X

C~
C`l _ tt ~Cl ..... .
~ o a~ D ~ ~ ~ ~~ ~ O ~ O 0 11 C ~-- --'4 _ _ UJ U~ 0 ~1 ~ 1~ ~
Z~q01 ......... ....... t,~
O ~ ~ ~ U~ ~ O O U~ _ I~ 0 ~ I
n p.
o o _~
CO C`J 0 e~ ~D C`J C~ O C~ ~ 0 O
0 0 ~ 0 O~

~ G~
t . .
U~
Ou O ~D O U~ O ~ ~D 0 ~ ~O 1 ¢ ~ `D 1~ ~O 1~ 1~ ~ ~O ~ ~ o a~ 0 0 0 o~
o t~
~
.r al ,.
~ u~ Cl J N
.,i ~ C~ ~ O O
~ r O O C~ ~ t.~ -~ ~ 0 U~
¢ U'~ <& tTl ~ ~ L~l Ir) U~ U~
C o a ~ Z
u~ a~ ~ o ~ ~ x ~ o 11 C ~ ~ C~ C`~ C~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~
Z ~ ~ _ a~ _ _ r_ _ _ ~ ~ *

_z~ _ ~n o u~ O Ln E~
13383~0 U~
o ~ o ~
O O U~ O O
. ~ . . . . .
~. C
.,~ Co o o o o o , C~

o .
~ C ~
o .,, ~, .
~ C~
C~ 1.
X~o o o o o o o o o C~
w u .,, o , E~ O~ ~c~l _ ~ O~ o o~ o c~
q o~ ~ o o o~ 5~ o ~ ~ C~ o o~
~, ¢
C
, -Z ~ o ~

~ . . . . . . . . . . . .

.i, n~ ~ ~ _ O U~ ~ ~ ~C`~ ~~D O 1 oo~o~ oo~ ooo~
Zl t~ U~
rl ~;;
Z l q O
o ~: xl~ ~ ~ ~ - ~ ~l` - `8 n o O _ C~ r oo~I~ ~ o o ~ ~ U~I~

C o o o o ~ 0 ~ oo _ U~ ~ ~ _ ~rl s U
a, a . .
u u~
a al a O ~ OO~ r~ ~ ~O O ~ ~ ~u~ r~ ~ x ~ ~ O O O O ~~OD ~ ~ 0 _ u~
~: C-- ~ _ _ C_ _ _ C ~C~ ~C`J ~ O ~

s~ ~ ~ r I
al c O Ul 01 0 0 0 N
.~ ~ ~ r r ~r-l O ~ , o~ ~ 1~4 u~ x <J X u~C __CN ~ ~ DO C~ 1 1 U~ D

C~ ~ O
O O O O ~ Z
01 o ~;t~ ~ ~~~~J o~~u ~ o Zl ----_ _-- ___ _ C~__ _ _ _ ~ _ -1 3 ~

, 3i ~ ~ ~ ~ ~ C ~ ~ P~

L ~ 8 ~ I o ~ ~ .
C ., _ _ _ ~ _ ~ ~o _ : oooooooo o o ~3 E C~ ~ c~ c~ ~ c~ ~ ~ ~ C`J

s~ c~ ~
~ - o c ~

~ o -:----- O

a~ ~ o o o o _ _ ~ o l~
;~

o .y ~ ~ x ~ ~ o' ~ `o o x g ~oD O ~o ~0 ~oD o o ~o ........
o ~l o o o o o o o ,~

_ ~~ ~ ~ o O ~

r ., V ' V

3 r 3 ~

E- ~ ~ _ _ _~ _ _ _ _ _ i~ P.... _ ~ E-l --I`

1~-l 0 ~ 11~) 0 13383~0 r ~

~ c o o 8 o r~ o ~o ~ ~3 _ o o 8 8 o ,~ oo'''oooooooo--'o'oooo -. ,~
N
~ ~ ~ 0~ ~ ~ ~ ~o ~o ~ ~ ~ ~ ~
o~o C~ D _ r-~ ~`J ~) ~ ~ ~ `.5 `D
I-- O O O O O O O O O C'J ~-J t'-) t`~ ~ ~ t`-) ~'~ ~) t'~ ~) D _ C~ O ~ O O ~ ~ ~ o . o a~ c~ ~ ~ ~ o~ oo ~ ~ o o ~ c~i o o o o o o c~ r~ c~ o O ~ o O o o o o~
E--~ , . _ _ r_~ _ _ _ _ I I I I O I O O 1 ~ 1 1 1 1 1 1 1 1 O

r~ o~ r ~ o ~ ~ O ~D
æ ~ u~ ~ a~ ~ ~ ~ ~, ,~ O~ ~, 0~ co 0, ,~ O ~ ~

.
O ~ ~ 0 ~ 0 <

~rY ~ ~ O ~ ~t ~ t ~0 æ a~ ~0 3 ~

E-- ~ ~ _ _ _ _ _ _ _ _ _ _ _ _ _ ,~ _ _ _ _ ,, _ _ In ~ S ~ ~ ,_ Ln 13383~0 ~ C~ ~ C~ ~ C~ ~ ~

00 G~ 0 g a~ ~ 8 8 ~ ., _ _ _ ~ _ _ _ _ _ _ ~ ~
_ V o ' ' o o o ' o ' o o ' o o ' o o o CLi E

'CQ u~
,~.,, . ~ o 0 _ ~ U~ I~ ~ C~ ~ _ _ 1~ 0 C~i ~ o o _ _~ u~ _ u~ C`J ~ _ ~ d` -- ~ -- --~C l .a ~,~ _ _ _ _ _ _ .. ~ ~ o o o o o o o o . o _ _ ~ ~ ~ 0 C~

-- ~ ~ ~ ~ ~ ~ _ 0 _ ~ x 8 _ ~D ~ o. ~ . _ o U~ ~ ~ o. o ~ 8 æ 8 ~ 0 a~ 8 8 ~ ~ 8 8 ` 8 ~ 8 8 8 _, _ _ _ _ _ IooIIIoIIII~IIIIII
o o o o ~u~i 0 ~ æ ~ Uo U~ O O
.~ ~ _ ~ ~ ~ ~ ~ V~ O _ 0 ~ ~ ~ ~ ~ U~ ~ ~ $ ~ ~ ~ ~ ~ ~

U~ -CLi U
C ~ ~ ~ ~ O O C~ D X o ~ c~ ~o , o o ~ o ~ I~ o a~ _ o c~ o ~ o o o x r~ o _ _ ~D O O _ O U~ _ O ~ O ~

O 0. ~ ~ Cr~ O. O.
U ~ ~ O ~ ~ ~ 00 ~ ~ t~ ~ ~ ~ Q O
G~ D 0 ~ D ~t ~ W ~

. _ .~ ~ a~ ~ æ ~ 8 -o ~o o ~o o o o O _q~_ ~n ~

- ` 1338340 .
r ~
r;l ~ r c J r r c~i ~D C X O X ~ ; o r 1 ~ ~ o F ~ _ - = c~ _ _ _ _ = _ _ _ r r ~ o o o o o oo o o o o r; r ~

c~ ~ r ~ ~ ~ ~ o r l cr~ O~ ~ 8 8 8 8 a~ 8 8 8 8 ~ IIII I IIIIIIII.1 u~
u~ ~ `J ~ ~ r-l ~

O O O O O O O O _l O O O O O

~r-l ~1 _I X u~ ~ u~ J O O t~
3 ~

.. ...
... ~ ~ .
:~ ~ ~ 3 3 U~ U~ U~
r r r r ~ c~ r ~SI ~ r~ ~ r ~ c~

r-~ / s ~ ~ L~' 3`83~

~ C~
E~
.~ ,. y~ ~ ~ ~3 ~ o o o _ ~ ~ O O O O O O O O O O
C

~ ~ O ~ ~ ~ O ~ ~ ~ ~ ~ u~ ~
3i _ E 1~ _ O _ ~`J O O O O _ O O O O O O O
_~ ~ l ~, . I
~.
-~ o o o _ O~ ~ o o o G~ O~ O a~ ~ o o o E~ oooo ~c~ooo~a~o5~ ooo O O O O ~--, O

~ r~ U~ 0 0 U~-~ C~ ~ ~ O I C~ _ O 0. o o~
C~ _ ~ O ~ _ _ _~ _ O O X
~q G 2 ~

C~
~ o ~ ~ o ~ O
~ ~ ~ u. ~ ~ _ ., u~ ~ o o u~ ~ ~!; ~ o 8 _ ~ O~ o y~ ~ O _ ~ ~ I~
,~
~ ~ ~ o. ~ o. _ o. o. ~. _ o. ~ ~ a~
y ~ 0 ~ ~ ~ $
~ .~

U ~ ~ oJ _ C~

n o Ln o 133~
. TABLE 6 CONTINUOUS SERVICE TEMPERATURE
FOR CONSTANT SiO2/CaO/MgO RATIOS

SiO2/CaO/MgO Ratio Continuous Service TemPerature for max 5% shrinkaae F

-40- ~

_ Reasonable modifications and variations are possible from the foregoin~ disclosure without departin~ from either the spirit or scope of the invention as defined in the claims.

Claims (67)

1. A process for decomposing a silica-containing fiber comprising the steps of:
(1) providing an inorganic fiber prepared from a composition consisting essentially of:
(a) 50-70 wt% SiO2; and (b) the remainder consisting essentially of CaO, the total being 100% by weight;
(2) subjecting the silica-containing fiber to a physiological saline fluid; and (3) extracting the silica at a rate of at least 5 parts per million (ppm) of silicon in 5 hours, thereby decomposing the silica-containing fiber.

2. The process of claim 1 wherein the composition of section (1) further includes Al2O3 in an amount up to 6 wt%.

3. The process of claim 1 or claim 2 wherein the composition of section (1) further includes MgO in an amount up to 30 wt%.

4. The process of claim 2 wherein the Al2O3 ranges from 0.06-5 wt%.

5. The process of claim 3 wherein the MgO ranges from 0.25-30 wt%.

6. The process of claim 2 wherein the composition consists essentially of:
(a) 0.06-1.5 wt% Al2O3;

(b) 50-70 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

7. The process of claim 6 wherein the composition further includes MgO in an amount up to 30 wt%.

8. The process of claim 7 wherein the MgO ranges from 0.25-30 wt%.

9. The process of claim 2 wherein the composition consists essentially of:
(a) 1.5-3 wt% Al2O3;
(b) 50-66 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

10. The process of claim 9 wherein the composition further includes MgO in an amount up to 30 wt%.

11. The process of claim 9 wherein the MgO ranges from 0.25-30 wt%.

12. The process of claim 2 wherein the composition consists essentially of:
(a) 3-4 wt% Al2O3;
(b) 50-63 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

13. The process of claim 12 wherein the composition further includes MgO in an amount up to 30 wt%.

14. The process of claim 12 wherein the MgO ranges from 0.25-30 wt%.

15. The process of claim 2 wherein the composition consists essentially of:

(a) 4-6 wt% Al2O3;
(b) 50-60 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

16. The process of claim 15 wherein the composition further includes MgO in an amount up to 25 wt%.

17. The process of claim 16 wherein the MgO ranges from 0.25-25 wt%.

18. The process of claim 1 wherein the fiber has an average diameter of less than 3.5 microns.

19. The process of claim 2 wherein the silicon extraction rate is at least 20 ppm, the Al2O3 content is about 0.06-6 wt%, and the SiO2 content is about 50-66 wt%.

20. The process of claim 2 wherein the silicon extraction rate is at least about 50 ppm, the Al2O3 content is about 0.06-3 wt%, and the SiO2 content is about 50-60 wt%.

21. The process of claim 2 wherein the silicon extraction rate is at least about 50 ppm, the Al2O3 content is about 0.06-0.75 wt%, and the SiO2 content is about 50-60 wt%.

22. A process of protecting a structural member from fire comprising the steps of:

(1) providing a fiber blanket having a bulk density in the range of about 1.5 to about 3 lbs. per cubic foot (pcf); wherein the fiber blanket has the ability to pass ASTM E-119 two-hour fire test; the fibers in the blanket have an average diameter less than about 3.5 microns; and the fiber is an inorganic fiber prepared from a composition consisting essentially of 58-70 wt% SiO2; the remainder consisting essentially of CaO, the total being 100% by weight; and (2) placing the blanket next to the member, and thereby protecting the member from fire.

23. The process of claim 22 wherein the composition of section (1) further includes Al2O3 in an amount up to 10 wt%.

24. The process of claim 22 or claim 23 wherein the composition of section (1) further includes MgO in an amount up to 21 wt%.

25. The process of claim 22 wherein the composition of section (1) further includes alkali metal oxide in an amount up to 2 wt%.

26. The process of claim 23 wherein the Al2O3 ranges from 0.06-7 wt%.

27. The process of claim 24 wherein the MgO ranges from 0.25-21 wt%.

28. The process of claim 22 wherein the composition consists essentially of:
(a) 0.06-3.0 wt% Al2O3;
(b) 58-70 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

29. The process of claim 28 wherein the composition further includes MgO in an amount up to 21 wt%.

30. The process of claim 28 or claim 29 wherein the composition further includes alkali metal oxide up to 2 wt%.

31. The process of claim 29 wherein the MgO ranges from 0.25-21 wt%.

32. The process of claim 23 wherein the composition consists essentially of:
(a) from about 3 wt% up to and including 4 wt% Al2O3;
(b) 58-63 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

33. The process of claim 32 wherein the composition further includes MgO in an amount up to 8 wt%.

34. The process of claim 32 or claim 33 wherein the composition further includes alkali metal oxide up to 2 wt%.

35. The process of claim 33 wherein the MgO ranges from 0.25-8 wt%.

36. The process of claim 23 wherein the composition consists essentially of:
(a) from about 4 wt% up to and including 6 wt% Al2O3;
(b) 58-61 wt% SiO2; and (c) the remainder consisting essentially of CaO, the total being 100% by weight.

37. The process of claim 36 wherein the composition further includes MgO in an amount up to 7 wt%.

38. The process of claim 36 or claim 37 wherein the composition further includes alkali metal oxide up to 2 wt%.

39. The process of claim 37 wherein the MgO ranges from 0.25-7 wt%.

40. The process of claim 1 wherein the SiO2 is made from pure oxidic raw materials.

41. The process of claim 2 wherein the Al2O3 is made from pure oxidic raw materials.

42. The process of claim 3 wherein the MgO is made from pure oxidic raw materials.

43. The process of claim 1 wherein the SiO2 is independently made from raw materials selected from a group consisting of talc, metallurgical slags, siliceous rocks, kaolin, and mixtures thereof.

44. The process of claim 2 wherein the AlO2 is independently made from raw materials selected from a group consisting of talc, metallurgical slags, siliceous rocks, kaolin, and mixtures thereof.

45. The process of claim 3 wherein the MgO is independently made from raw materials selected from a group consisting of talc, metallurgical slags, siliceous rocks, kaolin, and mixtures thereof.

46. The process of any one of claims 1, 2, 4 to 17 or 18 to 21 wherein the composition has added thereto a material selected from the group consisting of ZrO2, TiO2, B2O3, iron oxides and mixtures thereof.

47. The process of any one of claims 22 to 39 wherein the composition has added thereto a material selected from the group consisting of ZrO2, TiO2, B2O3, iron oxides and mixtures thereof.

48. A refractory inorganic fiber composition consisting essentially of approximately:
(a) 58.5-68.9 wt% SiO2;
(b) 18.1-40.5 wt% CaO; and (c) 0.11-16.4 wt% MgO;
wherein the inorganic fiber composition is capable of withstanding the rising temperatures of a simulated fire reaching 1,010°C in two hours and is soluble in physiological saline solution.

49. A refractory inorganic fiber composition as set out in claim 48 further including up to 1.5 wt% Al2O3.

50. A refractory inorganic fiber composition as set out in claim 48 further including up to 4.5 wt% ZrO2.

51. A refractory inorganic fiber composition as set out in claim 48 further including up to 8.41 wt% B2O3.

52. A refractory inorganic fiber composition as set out in claim 48 further including up to 2.9 wt% Fe2O3.

53. A refractory inorganic fiber composition as set out in claim 48 further including up to 2.6 wt% Na2O.

54. A refractory inorganic fiber composition as set out in claim 48 further including up to 10 wt% TiO2.

55. The refractory inorganic fiber composition of claim 48, comprising:
(a) about 64.1 wt% SiO2;
(b) about 30.97 wt% CaO; and (c) about 2.6 wt% MgO.

56. A refractory inorganic fiber composition consisting essentially of approximately:
(a) 58.1-66.7 wt% SiO2;
(b) 2.7-36.6 wt% CaO;
(c) 0.1-36.3 wt% MgO; and (d) 1.5-3 wt% Al2O3;
wherein the inorganic fiber composition is capable of withstanding the rising temperatures of a simulated fire reaching 1,010°C in two hours and is soluble in physiological saline solution.

57. A refractory inorganic fiber composition as set out in claim 56 further including up to 4.5 wt% ZrO2.

58. A refractory inorganic fiber composition as set out in claim 56 further including up to 8.41 wt% B2O3.

59. A refractory inorganic fiber composition as set out in claim 56 further including up to 2.9 wt% Fe2O3.

60. A refractory inorganic fiber composition as set out in claim 56 further including up to 2.6 wt% Na2O.

61. A refractory inorganic fiber composition as set out in claim 56 further including up to 10 wt% TiO2.

62. A refractory inorganic fiber composition consisting essentially of approximately:
(a) 55.1-61.2 wt% SiO2;
(b) 7.89-34.0 wt% CaO;
(c) 0.24-33.7 wt% MgO; and (d) 3-4 wt% Al2O3;
wherein the inorganic fiber composition is capable of withstanding the rising temperature of a simulated fire reaching 1,010°C in two hours and is soluble in physiological saline solution.

63. A refractory inorganic fiber composition as set out in claim 62 further including up to 4.5 wt% ZrO2.

64. A refractory inorganic fiber composition as set out in claim 62 further including up to 8.41 wt% B2O3.

65. A refractory inorganic fiber composition as set out in claim 62 further including up to 2.9 wt% Fe2O3.

66. A refractory inorganic fiber composition as set out in claim 62 further including up to 2.6 wt% Na2O.

67. A refractory inorganic fiber composition as set out in claim 62 further including up to 10 wt% TiO2.