Note: Descriptions are shown in the official language in which they were submitted.
r ~
1338340
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.
-13- 13383 10
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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
-15-
~ ~ 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
4 - - 1410
- 28
12 - - 1380
16 - 26 1400
17 1.9 - 1420
19 - - 1430
2.3 22 1440
22 2.9 - 1350
23 - 34 1390
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
- 33 1460
43 1.9 32 1460
2.3 - 1500
58 - - 1490
2.0 25 1420
81 - - 1500
82 - - 1370
83 - - 1390
-16-
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
107 - - 1420
3 To 4% A~hoteric Okides
110 - - 1320
111 - 23 1440
114 - - 1380
117 - - 1450
120 - - 1440
4 To 6% A~hoteric Oxides
122 3 3 1410
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
131 - 25
133 - - 1420
--17--
` 133~340
Average
Fiber Shot Service
Diameter Content Temperature
Test No. Microns % F
108 To 10~ A~u?hoteric O~cides
134 - - 1380
135 2.9 _ 1410
137 3.1 - 1370
138 1.8 - 1450
139 1.8 - 1370
140 - - 1400
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
-18-
13383~0
Average
Fiber Shot Service
Diameter Content Temperature
Test No. Micro~s % F
O~ide Additions other than Alu~in~
167 2.5
173 - - 1800
174 3.1 25 1600
176 2.1
178 1.41
179 o.g
182 30
183 1.7 26
186 - 25 1500
189 - 26
192 1.8
200 2.0 36
211 - - 1400
216 1480
No. of Measurements: 42 22 56
Average Value: 2.3 27
Conventional Mi~eral Wood Fibers
226 4.3 33 1370
227 4 7 48 1350
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
241 3 0
Average: 2.9 31
- -20- ~3~3~0
TABLE 3
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
163
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
--21--
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
--22--
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~
--23--
"~ m ~
- '~ 1 1 I I 1 1 I I I I I I I I I I
Z 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
a~ ~ ~ ~ o r` t~ O ~ o ~ ~o ~ o o ~ ~ r~
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1 1 I I I I I I 1 1 I I I I I I I I I I
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
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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
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O o I I I I I I I I I I I I I I o. o I I I I .o 8
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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
1338340
--24--
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
242 -- 28 -- 28 19 50 3 72
243 -- 64.5 -- 64.5 -- 27.4 27.
X
1338340
-24a-
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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
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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
... ... .... .. ....
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. TABLE 6
CONTINUOUS SERVICE TEMPERATURE
FOR CONSTANT SiO2/CaO/MgO RATIOS
0 5 10 20 30
SiO2/CaO/MgO Ratio Continuous Service TemPerature for max 5% shrinkaae
F
50/50/0 1480 1480 1470 1420 1550
50/40/10 1440 1430 1420 1400 1520
50/30/10 1400 1380 1370 1350 1480
60/40/0 1500 1460 1460 1460 1600
60/30/10 1430 1420 1400 1410 1520
60/20/20 1380 1370 1360 1350 1500
-40- ~
1338340
_ 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.
