CA2383440C - High temperature resistant saline soluble fibres - Google Patents

High temperature resistant saline soluble fibres Download PDF

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Publication number
CA2383440C
CA2383440C CA002383440A CA2383440A CA2383440C CA 2383440 C CA2383440 C CA 2383440C CA 002383440 A CA002383440 A CA 002383440A CA 2383440 A CA2383440 A CA 2383440A CA 2383440 C CA2383440 C CA 2383440C
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CA
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Prior art keywords
fibres
fibre
mgo
cao
high temperature
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Expired - Fee Related
Application number
CA002383440A
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French (fr)
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CA2383440A1 (en
Inventor
Gary Anthony Jubb
Jean-Louis Martin
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MORGAN ADVANCED MATERIALS PLC
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Morgan Crucible Co PLC
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Filing date
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Priority claimed from GBGB9921504.8A external-priority patent/GB9921504D0/en
Application filed by Morgan Crucible Co PLC filed Critical Morgan Crucible Co PLC
Publication of CA2383440A1 publication Critical patent/CA2383440A1/en
Application granted granted Critical
Publication of CA2383440C publication Critical patent/CA2383440C/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00—Fibre or filament compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2213/00—Glass fibres or filaments
    • C03C2213/02—Biodegradable glass fibres

Abstract

A fibre is disclosed having a maximum use temperature of 1200 °C or more which comprises: SiO2 > 64.25 wt% CaO > 18 wt % MgO < 17 wt% and in which the amount of MgO in mol % is greater than the amount of CaO in mol %. Such fibres have high solubility and low dustiness.

Description

HIGH TEtdEERATURE RESISTANT SALINE OLtI3LE FIBRES

This invention relates to high temperature resistant saline soluble fibres and particularly relates to calcium-magnesium-silicate fibres.

Calcium-magnesium-silicate fibres are known for example from W089/12032, W093/15028 and W094/15883.

W089/12032 first disclosed a broad class of fire-resistant saline soluble fibres.
W093/15028 showed that a class of the fibres of W089/12032 were usable at temperatures up to 1000 C or more.

W094/15883 showed that some of the fibres of W093/15028 had higher use temperatures still, of up to 1260 C or more, and indicated that such fibres needed a Si02 excess (defined as the amount of Si02 remaining after crystallisation of CaO, MgO and any Zr02 as silicates) of greater than 21.8mol%.

W097/16386 while falling in the general class of calcium-magnesium-silicate fibres looked to low calcium fibres to show use temperatures of 1260 C or more.

It is apparent that there are regions of the CaO-MgO-SiO2 and CaO-MgO-Si02-Zr02 composition fields within which high temperature performance fibres can be made and other regions where they cannot.

The applicants have now found a new and narrow range of compositions that are usable at temperatures of 1200 C or more and even 1250 C or 1260 C or more, and yet fall outside the scope of W094/15883 and W097/16386. These compositions preferably have little or no zirconia.

Accordingly the present invention provides a fibre having a maximum use temperatare of 1200 C or more in which the amount of MgO in mol% is greater than the amount of CaO
in mol % and which comprises:-Si02 >64.25 wt%
CaO > 18 wt%
MgO < 17 wt%.
However, no claim is made to fibres having a Si02 excess as specified of greater than 21.8mol%.

Further features of the invention are apparent from the appended claims.

The excess Si02 figure is calculated by treating all of the CaO as being bound as CaO.MgO.2SiO2; all of the Zr02 as being bound as ZrO2.SiO2; and the remaining MgO
as being bound as MgO.Si02. The applicants also assume that any A1203 crystallises as A1203.SiO2. Any remaining Si02 is called the excess Si02.

The invention is illustrated by way of example in the following description with reference to the drawings in which Fig 1 is a graph showing linear shrinkage with temperature for blankets comprising the fibres A4-2 and A4-3 of Table 1 below.

Fig. 2 is a graph showing shrinkage through the height of blankets comprising the fibres A4-2 and A4-3 of Table 1 below.

Fig. 3 is a graph showing shrinkage of preforms produced from fibres A4-1, A4-2 and A4-3 of Table 1 below.

Table 1 shows compositions extracted from W089/12032, W093/15028, W094/15883, and W097/16386 together with A4, a target composition fibre having the composition:-SiOZ 65 wt%
CaO 19.5 wt%
MgO 15.5 wt%

and A4-1, A4-2, and A4-3, which are analysed fibre samples.

The fibres extracted from the data of W089/12032 (referred to as Manville fibres), W093/15028, W094/15883, and W097/16386 (referred to as Unifrax fibres) are those for which the Si02 excess as specified is less than than 21.8mol% and for which the amount of MgO in mol% is geater than the amount of CaO in mol%.

A4-1 was produced as bulk fibre; A4-2 was produced as needled blanket having a density of approximately 96 kg.m 3; and A4-3 was produced as needled blanket having a density of approximately 128 kg.m 3.

In Table I shrinkages are indicated from the documents concerned or, for A4-1, A4-2, and A4-3, from measuring the shrinkage of vacuum formed preforms of the fibres concemed.
y 00 N 00 M M ON \~O C\ 'IT
~O N ~D ~
N ~D O~ ~O r= 00 N N
N O q,,:O M ~O
O 00 ~O 00 [-r c~ .-M-i '--~ .=-~ o6 .-r--~ t N ~ ~
.--+
.,.., C/] (~
"O O vl v) -t -zt o0 O =-+ ~ M M
N 00 ,1: M O O 0~ O~ 00 --~ oo N N M ~O 00 0 [- o0 Q\ o0 a, o0 o0 O\ \D vi vi c1 o0 cV l~ O o0 o0 tn W1 t!1 W1 kn W) t!1 Vl V') N N W1 V1 N N \-O W) tn O O O
O O
M a1 v'~ oo N
~n ~ '-, ~ .-= ' = O d 00 0o O~ '-+ rt ~ O =- N
Q '-+ O O O O O O O O ~+ O O O O O O O O
N O O v1 O O O C) O O O tn O d N M M N O

o N o 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 ~t Cn 00 C) N M ~ O cl, O~ ~ W, 14D l-0 l- 00 O =-+ ~ r+ N V [~ [~ '7 N [-to O O v1 ~. N N N N N N N N N N N N N N N N N N
-+ a\ ~D 00 N [- C) 1~0 ~~ N \O O 00 l- C\
O a1 ~ [- M 00 U U O~ O O~ O O~ O~ O~ (7N =-= O ~ [~ t~ M o0 v) --~ N '-+ N r. - =--~ =-+ N N N -- --~ N ~ r, r, r.
~
(U ~ O O O O O C) -s O O O O O O O O

N C) O O O O O O C) O tn O O N C) C) \,O 00 N M [~ N 'O ~O W) l~ O oo M o0 - 1: oo O O v~ ~O
0 vi O a1 Oy ~h ~ \%D M "O M M
t/1 ~O ~O v1 ~O ~D ~O ~D

o O
0 ~' l- O O O \0 O o0 O O O M O d' O O en ~n -4 N N N M
N N o0 M vl oo N [~ N r+ MI:
- N =-+ O O O O O 0 M =--+ =-, O C) O O O O
~
0 ry~ O 00 .-~~ O O O O O O
U O O O O O O O O O O
O O N O O O O O O vl O O \,O O C) C) O -+
W~ N ,--~ N kn W) ~O v1 d vl \O M .-+ M rn =~ O N
tn tn t/'i Wi Wi Vl W'i t!i N N %O [- [- l- 00 00 00 r + .==+ -4 .-.+ ~ .--4 .-4 .--~ .--i r~ .-+ .-+ r. '~ .~ .-+ .--~ .-.
00 O O N O O O O O O O O O N O O v~ \O
~ l- ~n 01 O~ N N N ~n ~ l- ~-- ON
00 .- i In O
cd ON O ON O O O (=> 0\ --~ O --+ l- 00 M 00 W) \O %O
U --~ N ~ N N N N -- Cl N N - N - - - -c~ O 00 N ~ O C~ cl~
o ~ r+ O K1 N \0 N ~
~
~
GC ~

~ O
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...
w SUBSTITUTE SHEET (RULE 26) rn rn v r-~o ~n ~ r = v, .-~ c~ =~ ~n cV ~ O Z~ 4 00 tn v~ O t~ ~ V N N ~ Izi: Izf Q W ~ p 6 ~ 00 ~ O
.-+ en N ~ N M
O vl l~ N O\ t- ~ N 0~0 ~ N l~ r+ r+ 01 N N
V 1 O" 00 .-- ~!1 00 O\ 1~0 M [- 01 OO M OO O
U) 'zt N tn In tn vl 141 tn tn tn tP1 W) W) "n ~~O
O O O o 1- O O O o '~ %O --~ QN 00 IT [~ "Kt =-+ 00 "t v1 O N M ~ N
0 N N -- "O .-~ r+ O --4 Wl ~ O - "t M M
o O O O C O --~ O O O O O O O O O

--~ o v'~ 00 O N
o o O O O O O O O O ~ N O M O\ o N
o N o 0 0 000 o 0 0 0~ o 0 0~ o 0 [~ 00 ~t ~ ON W) ~O d' 00 l~ O r+ N 00 N
00 M =-+ [- O~ 00 \O =-+ M 00 O 00 ~O 41 to l- 00 O O - N M cM d tn \~O [- 00 N N N N en M M en en M en M M en M
O _ d N V'~ ~ N 00 N v~=~ O c~*M opo ~ 00 Q N
U U 00 00 c~ 00 c) 0 00 \O \O o M O

O oo ~O O oo O O \O O N O N O M
N N ~O =-~ ~t M .-~ N M a\ r+ ~ oo [~ =-+ ~O
=--~ O O Nt 00 ~t \D v i [- N vi ~O o0 Uj \O vl tn \O "If \~O \-O ~O ~D W) tn E p N

O 00 O 't ~t t~ =~ ~n N cM O O~ cM \~O Ol\ N
~t N M O~ M .-+ O M ~ N N [~ v1 ~O
O O O O O O O N O O O O O O O O
N Q

~ ry N O O en ~ 00 [~ ~ [- O ~ 00 Q p p O O p d oo ~n U N o 0 0 o M o o N o o 00 "0 "r 00 0 o 0 00 0 00 0 0 0 0 W) Q c ~ ~o c ~ rn rn ~.~ o .~ r,~ oo n cy n ~ r,:
~ oo a; o~ o~ ~O v Nt~ d~ NO ~.O tn oo ON

v~1 O ~t ":T ~ ~ ~ 0 ~ 0 0 00 0 ~ en ~ O M
p O w w ,M, a\ 00 ~ O o0 ,O ~O O 4 O
cd O d0 O p U c= i cn vi p =-- N N N
00 ~
O o N
M D\ '- ~ ~ ~
M CV .-~r .~+ N ~i M ~r M X l!1 ~
~
.. r, , dtl ~D
'a ~D :D

SUBSTITUTE SHEET (RULE 26) m 100 tn tn 00 tn N0 O~ d ,t N ~
0 0 tn oo 00 00 v~ W
~ 01 M M M ~f N l~ N N N --+ o 0 r- ON [- [~ ON C7~ O
o 0 o O
O o 0 0 0 ~ O O O O

o 09 r- 00 ~ O o O o O o O O O o o v) o Q o O O o o N o o N o 0 0 0 0 0 0 0 Q O~ O N N a1 N
=" 00 01 01 Qs O1 C\ t!1 M M M M M M ~h c~ N
U N -- N N O O M
.s~
O

O tn oo tn tn r- r- r-tn ~

H p N

o I' O l~'~ --1 rl O~
.--~ N
O

o 0 U N o 0 0 ~ o 0 0 0~o t- r-[~ =-~ =-= ~ N ~n o rn o 0 0w, M M M M M M
Q ~ ~ N N ~
cd N -- M M O o M

cd U l- N
N

O O '-~ ~p ~ [- o 00 r- r- d' V
~N '~~ a: =-~
> > > ~
y ~ g c~d c~d ~ ~D

SUBSTITUTE SHEET (RULE 26) It can be seen that the fibres according to the present invention show lower shrinkage at 1260 C than do the extracted fibres other than fibre Uniffiax 42 which has a radically different composition.

In Figs. 1-3, graphs show the shrinkage characteristics of the fibres A4-1, A4-2, and A4-3 after 24 hours exposure to the indicated temperatures. it can be seen that the fibres are readily usable at temperatures of 1200 C or more.

Table 2 below shows the results of solubility tests on the fibres in physiological saline solution indicating that the fibres are soluble in body fluids. (See W094/15883 for a discussion of methods of measuring solubility). Pairs of results are indicated for separate tests on each sample as is a mean total solubility.

Table 2 Fibre type Solubility (ppm CaO MgO Si02 Total Mean Total A typical range of compositions for fibres of the present invention would be Si02 65 ~ 0.5 wt%
Ca0 20 f 0.5 wt%
MgO 15 ~ 0.5 wt%.

Further tests were made on fibres having the inventive composition of Si02 65%, CaO
19.5%, MgO 15.5% in comparison with Superwool 607TM, a fibre having the nominal composition (by weight) of Si02 65%, CaO 29.5%, MgO 5.5%, and A1203 <1% ;
Superwool 612TM, a fibre having the nominal composition (by weight) of Si02 64.5%, CaO 17%, MgO 13.5%, Zr02 5%; and refractory ceramic fibre having the nominal composition Si02 56%, A1203 44%.

The first test was aimed at indicating the amount of dust that might be released on handling. The test comprised the determination of the amount of dust present in a sample of blanket made from the respective fibres. The samples of blanket were vibrated on a Fritsch Analysette type 3010 vibratory sieve shaker, which was set for a frequency of 3000Hz and vertical amplitude of 0.5mm. The apparatus was equipped with a 1.6mm sieve and a pan. In the test method a sample of blanket 135mm x 135mm was placed on the sieve and vibrated for 10 minutes. The material collected in the pan was weighed and expressed as a percentage of the original weight of the sample. The results were as indicated below:-Fibre Material Percent dust released Superwool607TM 0.16%
Inventive material 0.18%
Refractory ceramic fibre 0.25%
Superwoo1612TM 0.36%

From this it can be seen that the inventive fibre is of comparable low dustiness to Superwool 607TM.

The second test made was to look to the shrinkage behaviour of blanket formed from the inventive fibre and the two SuperwoolTM fibres at high temperatures. Samples of blanket were exposed to specified temperatures for 24 hour periods and their linear shrinkage measured. The results are indicated in Table 3 below:-Table 3 Temperature Sample 1050 C 1110 C 1150 C 1200 C 1250 C 1300 C
Inventive fibre 0.8 0.6 1.0 1.0 1.5 4.2 Superwoo1612TM 0.7 1.0 1.1 1.7 1.8 12.1 Superwool607TM 0.4 0.4 0.5 0.6 4.8 7.8 This shows that the inventive fibre is comparable in performance with both SuperwoolTM
fibres up to 1200 C. At 1250 C the Superwool 607TM fibre shows a shrinkage of 4.8%
(which would be considered as too high a shrinkage for most applications). At 1300 C the inventive fibre while still showing a high shrinkage of 4.2% is the best of the three fibres tested.

A further series of tests were made to produce fibres on a production scale and the compositions of fibres obtained were as set out in Table 4 below. All showed low shrinkage at 1250 C (shrinkages were measured by different methods to Table 1 and are not directly comparable). In combination with the results of Table 1, this shows samples of usable characteristics having compositions consisting essentially of (in wt%):-CaO 18.7 to 20.2 MgO 14.47 to 15.9 SiO2 64.5 to 65.1 A1203 0 to 0.56 The fibres of the present invention therefore have a high solubility (desired to permit fibres to be cleared from the body quickly); a low dustiness (desired to reduce the amount of fibre that can be inhaled); and good high temperature characteristics.

N -- M o ED M oo =~ ~n N a o; o~ o; o O
L/~ W
N ~O 01 Vl N
0 W) ~ ~ ~
O
.L..y t+ ~ ~ ~
O N M
N
N O O O O
O O O O
~ N O O O O
~ O O O O O
~ N
N \D 00 M
O N r,: --~
0 =- - O
,+ N N N N
~

o v r, O
O Cd Q'N 00 00 O\
U U ~ ~ ~ ~
~
o O
N Q ~ 00 N
~
L \ N
C 5 O o ~

..~-+ N 0 ~

U N

O o rn pp vi ~, v, O o ~
oo co v~
N .~ .-~ .~

o .r C's =.~ ,L7 ~. ~ C) y ~'' U 00 P. ~ U
O0 l-~D
O M
m cl N~ ~--~
~D ~D
w v~ H U-i EU-~

SUBSTITUTE SHEET (RULE 26)

Claims (13)

1. A fibre having a maximum use temperature of 1200°C or more which comprises:-SiO2 > 64.25 wt%
CaO > 18 wt%
MgO < 17 wt%
and in which the amount of MgO in mol% is greater than the amount of CaO in mol% and in which the SiO2 excess as specified is no greater than 21.8mol%.
2. A fibre as claimed in claim 1 and comprising:-CaO < 21 wt%.
3. A fibre as claimed in claim 2 and comprising:-CaO < 20.5 wt%.
4. A fibre as claimed in any one of claims 1 to 3 and comprising:-CaO > 19 wt%.
5. A fibre as claimed in claim 4 and comprising:-CaO > 19.5 wt%.
6. A fibre as claimed in any one of claims 1 to 4 and comprising:-MgO > 14.25 wt%.
7. A fibre as claimed in claim 6 and comprising:-MgO > 14.75 wt%.
8. A fibre as claimed in claim 7 and comprising:-MgO > 15.25 wt %.
9. A fibre as claimed in any one of claims 1 to 8 and comprising:-MgO < 16 wt %.
10. A fibre as claimed in claim 6 and comprising:-SiO2 65 ~ 0.5wt%
CaO 20 ~ 0.5 wt%
MgO 15 ~ 0.5 wt%.
11. A fibre as claimed in any one of claims 1 to 9 and comprising:-SiO2 64.5 - 64.7 wt%
CaO 19.5 - 20.2 wt%
MgO 15.5 - 15.6 wt%.
12. A fibre as claimed in claim 1 and comprising:-SiO2 about 65 wt%
CaO about 19.5 wt%
MgO about 15.5 wt%.
13. A fibre as claimed in claim 1 and consisting essentially of:-CaO 18.7 to 20.2wt%
MgO 14.47 to 15.9wt%
SiO2 64.5 to 65.1wt%
Al2O3 0 to 0.56wt%.
CA002383440A 1999-09-10 2000-08-24 High temperature resistant saline soluble fibres Expired - Fee Related CA2383440C (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
GB9921504.8 1999-09-10
GBGB9921504.8A GB9921504D0 (en) 1999-09-10 1999-09-10 High temperatures resistant saline soluble fibres
GB9924867A GB2348640B (en) 1999-09-10 1999-10-20 High temperature resistant saline soluble fibres
GB9924867.6 1999-10-20
PCT/GB2000/003275 WO2001019744A1 (en) 1999-09-10 2000-08-24 High temperature resistant saline soluble fibres

Publications (2)

Publication Number Publication Date
CA2383440A1 CA2383440A1 (en) 2001-03-22
CA2383440C true CA2383440C (en) 2008-06-17

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US (1) US6861381B1 (en)
EP (1) EP1212265B1 (en)
JP (1) JP4066138B2 (en)
CN (1) CN1373740A (en)
AT (1) ATE243665T1 (en)
AU (1) AU769172B2 (en)
BR (1) BR0013868B1 (en)
CA (1) CA2383440C (en)
CZ (1) CZ296627B6 (en)
DE (1) DE60003569T2 (en)
ES (1) ES2202162T3 (en)
MX (1) MXPA02002380A (en)
PL (1) PL354487A1 (en)
RU (1) RU2247085C2 (en)
WO (1) WO2001019744A1 (en)

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WO2001019744A1 (en) 2001-03-22
BR0013868B1 (en) 2010-01-26
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CZ2002862A3 (en) 2003-12-17
CN1373740A (en) 2002-10-09
AU769172B2 (en) 2004-01-15
EP1212265A1 (en) 2002-06-12
PL354487A1 (en) 2004-01-26
US6861381B1 (en) 2005-03-01
DE60003569T2 (en) 2004-04-29
ATE243665T1 (en) 2003-07-15
DE60003569D1 (en) 2003-07-31
CA2383440A1 (en) 2001-03-22
MXPA02002380A (en) 2002-08-20
AU6713200A (en) 2001-04-17
BR0013868A (en) 2002-05-28
CZ296627B6 (en) 2006-05-17
RU2247085C2 (en) 2005-02-27
EP1212265B1 (en) 2003-06-25
JP2003509320A (en) 2003-03-11

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