CA1104593A - Coherent rigid solid material - Google Patents
Coherent rigid solid materialInfo
- Publication number
- CA1104593A CA1104593A CA299,891A CA299891A CA1104593A CA 1104593 A CA1104593 A CA 1104593A CA 299891 A CA299891 A CA 299891A CA 1104593 A CA1104593 A CA 1104593A
- Authority
- CA
- Canada
- Prior art keywords
- parts
- mixture
- water
- sodium silicate
- silicate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L59/00—Thermal insulation in general
- F16L59/02—Shape or form of insulating materials, with or without coverings integral with the insulating materials
- F16L59/021—Shape or form of insulating materials, with or without coverings integral with the insulating materials comprising a single piece or sleeve, e.g. split sleeve, two half sleeves
- F16L59/024—Shape or form of insulating materials, with or without coverings integral with the insulating materials comprising a single piece or sleeve, e.g. split sleeve, two half sleeves composed of two half sleeves
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Thermal Insulation (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
Abstract
?-781-1 COHERENT RIGID SOLID MATERIAL
Abstract of Disclosure An especially high strength, high temperature, economical material useful for insulation is preferably made by making up a mix having the following proportions in parts by weight: 20-50 parts expanded perlite; .5-4 parts sodium fluosilicate; .2-5 parts fiber material; a water solution having 9.5-19 parts total of solids content of sodium or potassium silicate; 2-9 parts zinc oxide; and water which, along with the water in the sodium silicate solution totals 21.5-67 parts; thereafter storing the mix under cover for less than 2 1/2 hours, compressing the mix to a desired form, and curing and drying it by heating.
Abstract of Disclosure An especially high strength, high temperature, economical material useful for insulation is preferably made by making up a mix having the following proportions in parts by weight: 20-50 parts expanded perlite; .5-4 parts sodium fluosilicate; .2-5 parts fiber material; a water solution having 9.5-19 parts total of solids content of sodium or potassium silicate; 2-9 parts zinc oxide; and water which, along with the water in the sodium silicate solution totals 21.5-67 parts; thereafter storing the mix under cover for less than 2 1/2 hours, compressing the mix to a desired form, and curing and drying it by heating.
Description
` M-781-1 Ba~kground o~ the Invention This invention relates to a new coherent rigid solid material particularly adapted for use as an insulating material.
Heat insulating materials are known which are prepared from fillers having at least a 75~ reactive expanded perlite con-tent and alkaline ionic silicates~ Such materials are formed -~
and cured so as to enable the perlite fract;on of the filler to react with the silicate to produce a crystalline reaction product.
U.S. patent 3,658,564 discloses such a material and a method of making such a material.
The material of U~S~ patent 3,658,564 is made by using an extended curing period o at least three days and preferably seven to achieve relative water insensitivîty~ Moreover, curiny . . ..
is accomplished under carefully controlled condîtions of humidity and temperature during this period. ThG requîred curing creates some difficulties in the large ~cale production GL the high tem-perature insulating material~
In addition, the material of U~S. patent 3,658,564 must be made with speci~ic ~iO2;K2 and SiO2:Na2 ratios in the alkaline ionic silicates. In particular, water resistive or insensitive products require SiO2:Na2O ratios of 3:1 to 4:1 and SiO2 K2 o~
Heat insulating materials are known which are prepared from fillers having at least a 75~ reactive expanded perlite con-tent and alkaline ionic silicates~ Such materials are formed -~
and cured so as to enable the perlite fract;on of the filler to react with the silicate to produce a crystalline reaction product.
U.S. patent 3,658,564 discloses such a material and a method of making such a material.
The material of U~S~ patent 3,658,564 is made by using an extended curing period o at least three days and preferably seven to achieve relative water insensitivîty~ Moreover, curiny . . ..
is accomplished under carefully controlled condîtions of humidity and temperature during this period. ThG requîred curing creates some difficulties in the large ~cale production GL the high tem-perature insulating material~
In addition, the material of U~S. patent 3,658,564 must be made with speci~ic ~iO2;K2 and SiO2:Na2 ratios in the alkaline ionic silicates. In particular, water resistive or insensitive products require SiO2:Na2O ratios of 3:1 to 4:1 and SiO2 K2 o~
2:1 to 2.6:1 to achieve a water insensitive product. Furthermore, the material of U.S. patent 3,658,564 has a rough surface texture which is undesirable from a cosmetic standpoint~ The roughness is also undesirable because of the inability to provide intricate ~ `
shapes, e.g., mitre joints~
Summary of the Invention It is a purpose of the invention to provide such a ma~erial which is especially useful as heat insulating materiai.
~ further purpose is to provide such a material which is at ;
once practical and reasonably economical and has especially ~ood . .
~4~;;93 strength, low bulk densi-ty, low thermal conduc-tivity, and good dimensional stability.
It is also a purpose to provide a material which has a relatively smooth and cosmetically pleasing texture.
A ~urther purpose is -to provide such a material which has expanded perlite as a major constituent.
A further purpose is to provide such a material which has relatively good water resisti~ity, that is, ability to main-tain shape and weight and reasonable strength in the face of ex-posure to water, and even better resistivity as to oil, has a corrosion inhibition property in the presence of such things as chlorides and chlorine, and resistivity to surface burning.
A Eurther purpose is ~o provide such a material which can be made by a practical, economlcal and effective process.
Thus -this invention provides a coherent rigid solid material made from a mixture subjected to heat so as to reduce the original content of water, said mixture comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts;
sodium fluosilicate 1 through 6 parts; and water, to make a total of water, including any tha-t may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
In a particularly preferred embodiment of the invention utilizing sodium silicate, the mixture comprises 29 through 45 parts expanded perlite with 36 through 42 parts representing an optimum. 11.5 through 18 parts of sodium silicate is present with 14.5 through 16.5 parts representing an optlmum. 3 through ... .
shapes, e.g., mitre joints~
Summary of the Invention It is a purpose of the invention to provide such a ma~erial which is especially useful as heat insulating materiai.
~ further purpose is to provide such a material which is at ;
once practical and reasonably economical and has especially ~ood . .
~4~;;93 strength, low bulk densi-ty, low thermal conduc-tivity, and good dimensional stability.
It is also a purpose to provide a material which has a relatively smooth and cosmetically pleasing texture.
A ~urther purpose is -to provide such a material which has expanded perlite as a major constituent.
A further purpose is to provide such a material which has relatively good water resisti~ity, that is, ability to main-tain shape and weight and reasonable strength in the face of ex-posure to water, and even better resistivity as to oil, has a corrosion inhibition property in the presence of such things as chlorides and chlorine, and resistivity to surface burning.
A Eurther purpose is ~o provide such a material which can be made by a practical, economlcal and effective process.
Thus -this invention provides a coherent rigid solid material made from a mixture subjected to heat so as to reduce the original content of water, said mixture comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts;
sodium fluosilicate 1 through 6 parts; and water, to make a total of water, including any tha-t may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
In a particularly preferred embodiment of the invention utilizing sodium silicate, the mixture comprises 29 through 45 parts expanded perlite with 36 through 42 parts representing an optimum. 11.5 through 18 parts of sodium silicate is present with 14.5 through 16.5 parts representing an optlmum. 3 through ... .
-3-1~45~93 : :
8 parts of zinc oxide is present with 4.5 through 6.8 parts xepre-sentiny an optimum. Water including any which is associated with -the sodium silicate is present as 26.5 through 57 parts with 32.5 through 43.5 parts representing an optimum.
In order to provide green strength, the preferred embodi-ment may comprise organic or inorganic fiber material. The fiber material may be from a class comprising 1 through 5 parts fiber-glass, .2 through 1.5 parts heat resistant nylon, 1 through 5 parts mineral wool and 1 through 5 parts of netting, all by weight as part of the mixture. Where nettlng is used, the fibers of the netting are preferably of a thickness in the range oE .007 to .0125 inches with the openings of the mesh having areas prefer-ably in the range of .06 to 1 square inch and the weight of the ;
netting less than 1 lb. per 1000 sq. ft. Where fiber material other than netting is utilized, an average length of 1/8 through 1 inch is preferred. ~;
Preferably, expanded perlite of the mixture has a dry bulk density of 2 through 8 lbs. per cubic foot and the AFS aver-age screen size for the perlite is in the range of from 70 through 120 and preferably 110.
In the preferred embodiment of the invention, the zinc ;~
oxide has an average fineness not in excess of .5 microns with a fineness of .1 through .2 microns being preferred Preferably, the sodium silicate has a proportion of sili-con dioxide to sodium oxide of 3.1 to 1 through 3.4 to 1. The sodium silicate is introduced into the mixture in a solution having a solids content of 36 through 44~. Where potassium sili~
cate is used, the silicon dioxide to potassium oxide ratio is 2~0 to 1 through 2.7 to 1 with a solids content of 24 to 35~.
:
M-781-1 .
Preferably, the mixture is formed ~y bringing together a dry powder material including the perlite and the slurry includ~
ing the sodium silicate, zinc oxide and water and mixing the powder and the slurry at least to the time the mix appears damp and dust-free and short of the time the mix begins shrinking substantiall.
in volume. After the mixing of the mixture is completed the mix-ture is held in storage for a period not exceed;ng 2 l/Z hours so as to permit the material to ~e Eormed into s~ape under compression.
Compression to achieve the desired shape may be achieved prior to heating by vibration ox a plurali.ty of compression steps.
The shaping may al~o be accompli.shed by blowing the material into shape.
Heating of the mixture may ~e accomplished by heating in an oven at a tempera~ure of 93 through 99C for four hours for each inch of minimum dimension of ~hape~ In the alternative, the material may b~ subjected to he~t by micro~ave energy.
The material is characterized ~y a bulk density of 13.0 to 14.0 lbs. per cubic foot ~hen subjected to ASTM test C-303 ~.nd preferably 13. a to 13.5. The material is also characterized by less than 1% linear change and less than 4% weight loss when sub-jected to ASTM test C-356.
The flexural strength of the material i5 in excess of 45 lbs. per square inch for a bulk densit~ of less than 13.5 lbs.
per cubic foot when tested in accordance with ASTM test C-203.
The thermal conductiviti.es of the material is less than O53, .6S and .78 Btu's per inch of thickness per square foot per degree F. per hour at 50QF, 700F and 900F respectively when tested in accordance with ASTM test C-777.
- 5 ~
The material is characterized ~y a surface which is smoother than SIS-3 on the oficial alloy casting Institute Surface Indicator Scale and preferably as smooth as or smoother than SIS-2 on that scale.
In accordance with another important as.pect of the in-vention, the material may be formed into shaped bodies. Preferably, the material is formed into a hollow tubular confi.guration comprising a plurality of separable segments where the segments include mating tongues and grooves or mitre ioints, The segments may be separable along surfaces extending substantially parallel to the axis of the tubular configuration with the tongues and grooves being formed in the suraces.
'' ' ' - 6 ~
~ .
~~7~
.. . .
S~3 Brief Description of the Draw gs ~ ig. 1 i9 a diagram illustratiny t~e thermal conductivity of the material of the invention;
Fig. 2 is an exploded perspective view of the material of 5 this invention formed into hollow tubula;r configuration;
Fig. 3 is a sectional view of the tongue and grooving in another embodiment of the invention;
Fig. 4 is another sectional view of the tongue and groov-ing in yet another embodiment of the invention; and Fig. 5 is a sectional view of a tongue and grooving of still another embodiment of the invention.
Detailed Description o Preferred Embodiments The material o~ the present invention starts out ultimately on a basis o approximately lQ0 parts by weigh.t as a mix of the lS following:
expanded perlite 2Q through 50 parts, preferably 29 through 45 parts, with 36 through 42 representing an optimum:
sodium fluosili.cate .5 throu~h 4 parts, preferably 1 through 3.5 parts, with. 2 through 3 preferred;
fiber material ~2 through 5 parts, pre~era~ly l through S parts;
sodium silicate or potassium silicate including 9~5 through l9 parts, preferably 11.5 thxough 18 parts, solids content of sodium silicate itself, with 14.5 through 16~5 representing the optimum;
zinc oxide 2 through ~ parts, preferably 3 through 8 p~rts, with ~.5 through 6.8 representing the optimum;
water, to mak.e a total of water, including any that may be associated with the sodium silicate, of 21~5 through 67 parts, preferably 26.5 through 57, with 32~5 through 43.5 xepresenting the optimum.
It is ~rought to this state by mixing the expanded perlite, the sodium fluosilicate and the fiber material together in powder form and separately mixing the sodium silicate in a solution of preferably 36 thxough 44% solids, with 38% preferred or potassium silicate in a solution of preferably 24 to 35~, zinc oxide and water together to form a slurry which is in turn mixed in with the powder. The mixing is then continued up at least to the time the mix appears damp and dust-free, but not up to the time the mix starts to shrink substantially.
Various mixing devices, such as a planetary batch mixer~
or a co~tinuous screw feed mixer, are suitable for tne mixing, a pug mill batch mixer also being suitable.
The material may be passed through a screen, which will preferably have half inch openings~ after the mixing.
The material is then preferably held in storage under covex up to two and one half hours. T~îs step has ~een observed to have the effect of markedl~ increasing the strength of the final product~
~ The material i5 then compressed, ~y a ram or vibration, into the shape in which it ~i~l ultimately be wanted. Another less preferred way of bringing it into shape is to put part of it into a mold or the like that may be used and compress that part and then put in part or all of the additional and compress it, and so on.
The material is then heated to cure it, this being pre-2S ferably done in a micro~ave oven. If in a conventional oven uti-lizing hot air then it should preferably be done in the temperature range from 93C through 99C and preferably from approximately two through approximately four hours per inch of the smallest dimension of the shape t and most preferably at 96C for four hours for each inch of the smallest dimension of the shape~
r r-The fiber material may comprise a class of organic or inorganic materials including 1 through 5 parts fi~erglass or a heat resistant nylon-type fibrous material, such as poly (1, 3-~J phenylene isophthalamide~, sold commercicllly under the -~Eaæ~
S Nomex, can be used less preferably instead of the fiberglass, in which case the amount will be ~2 through l~S parts by weight and preferably .5 parts hy weight~ Another less prefera~le possibility for this is mineral wool, such as rockwool in the amount of l through 5 parts or preferably l part. Cotton or wood fibers may also be used.
The fiberglass or other fibrous material i5 in the form of a floc - that is, a set o~ fibers in short lengths~ averaging pre~erably 1/8 through l/4 inch long and most prefera~ly in fibers averaging 1/4 inch long.
The class of fiber material aIso inc7udes l through 5 parts of netting which may be organic or inorganic materials in-cluding polypropylene, polyester, nylon or Dacron~ The netting comprises fibers of a thickness in the range of .Q07 to .125 inches, openings having areas in the range of ~06 to 1 square inch and weight of less than 2 lbs. per thousand square feet~ The netting s~rength should exceed 4 grams per denier when suhjected to an Instron tester at 65~ relative humidity. The openings in the netting may take on a variety of shapes including squares, rectan-gles, circles or ovals~
All fiber materials must be stable at temperatures in excess of 250F., i.e., there is no substantial softening below these temperatures.
The expanded perlite should have a dry bulk density of 2 through 8 lbs. per cubic foot, and preferably 2 through 3 1/2 lbs.
per cubic foot. The perlite is a complex sodium potassium aluminum ~ e /~
_ g _ silicate volcanic granular glass~ Its scre~n sizing should be AFS
(~merican Foundry Society) average screen size designation of 70 through 120 and preferably 110. A perlite with 25% maximum con-taminants including no more than ~5% each of Fe o Ca and no more than .1~ of each of arsenic, barium, beryllium, boron, chlorlne, chxomium, copper, gallium, lead, manganese, molybdenum, nickel, sulphur, titanium, yttrium and zirconium i5 suitable~ Expanded perlite includes all perlite made from naturally occurring perllte sand which is expanded by heat. The fusion temperature is in ex-cess of 2300F and has a solubility of less than 1% in water, less than 10% in lNONaO~ and less than 3% in mineral acids, The sodium silicate should become part Gf the mix in theform of a water solution capable of being handled in a practical manner. Any commercially available solution will suffice but it is preferred that its ratio of silicon dioxide to sodium oxide should preferably be in the range of 3~1 to 1 through 3.4 to 1, and most preferably 3.22 to 1, and it should have a solids content preferably~
in the range of 36 through 44%~ and most preferably 38~. An e~-ample~
of a suitable sodium silicate grade to use is the N grade of Phila-delphia Quartz. Where potassium silicate is used, the ratio ofsilicon dioxide to potassiNm oxide shauld preferably be in the range of 2.0 to 1 through 2~7 to 1 with a solids content of 24 to 35~.
For good results, it i5 important that the zinc oxide should be finely divided and fairly clean, e.g~, the type that is produced by the so-called French process. Use of the zinc oxide in finely divided form has been found to quite substantially in-crease the strength and the water resistivity. A zinc oxide havlng an average fineness o no more than .50 mi rons is suitable, .10 to .20 preferred, and 1.7 most preferred; 9~ to 99% purity or more particularly reagent grade is suitable from the standpoint of purity.
~4593 Instead of including the sodium fluosilicate as a solid-iying agent to add green strength, a less preferred alternative which'nevertheless has special advantages is to pass carbon dioxide gas under pressure into or through the material after it has been S compressed into shape.
The curing or drying step, can well take place in an oven, for example in an electric or other con~entional oven with air circulati~g around within it, and in such a case the piece of material being subjected to the heating should be so supported that the maximum area of the piece will have direct access to the air in the oven. For example,, a piece with.relatively l~nger and shorter dimensions should be supported with.its longest dime.nsion in the vertical direction~ whi.ch will achieve this result and also - tend to prevent warping~ Dehydrating and oth.erwise curing the . material can also be accomplished by the use of microwave energy in heating devices such as ovens, which have a capability of securing the result in a much shorter time, for example for some time such as 5 minutes to the inch.of minimum dimension. Vse o~ :
this has been found on the average to enhance the strength more than 20% as compared to using a conventional oven.
To further illustrate the invention, the ollowing ex- .
amples are illustrative of suitably carrying out of the invention.
. EXAMPLE 1 This example involves the making of a block 12 inches by 8 inches by 2 inches, for the purpose of which 200 cubic inches of material is made in order to have enough. to make the block to-gether with a small excess to accommodate ha,ndling lossesr .. : .
. ~ .,, l:~V~S~3 The following materials are secured:
1. PFF 10 perlite ~powder) 352 g ~29%~
. Sodium ~luosilicate ~powder) 24 g ~2%) 3. Fiberglass ~1/8" fibers) 12 g (1~)
8 parts of zinc oxide is present with 4.5 through 6.8 parts xepre-sentiny an optimum. Water including any which is associated with -the sodium silicate is present as 26.5 through 57 parts with 32.5 through 43.5 parts representing an optimum.
In order to provide green strength, the preferred embodi-ment may comprise organic or inorganic fiber material. The fiber material may be from a class comprising 1 through 5 parts fiber-glass, .2 through 1.5 parts heat resistant nylon, 1 through 5 parts mineral wool and 1 through 5 parts of netting, all by weight as part of the mixture. Where nettlng is used, the fibers of the netting are preferably of a thickness in the range oE .007 to .0125 inches with the openings of the mesh having areas prefer-ably in the range of .06 to 1 square inch and the weight of the ;
netting less than 1 lb. per 1000 sq. ft. Where fiber material other than netting is utilized, an average length of 1/8 through 1 inch is preferred. ~;
Preferably, expanded perlite of the mixture has a dry bulk density of 2 through 8 lbs. per cubic foot and the AFS aver-age screen size for the perlite is in the range of from 70 through 120 and preferably 110.
In the preferred embodiment of the invention, the zinc ;~
oxide has an average fineness not in excess of .5 microns with a fineness of .1 through .2 microns being preferred Preferably, the sodium silicate has a proportion of sili-con dioxide to sodium oxide of 3.1 to 1 through 3.4 to 1. The sodium silicate is introduced into the mixture in a solution having a solids content of 36 through 44~. Where potassium sili~
cate is used, the silicon dioxide to potassium oxide ratio is 2~0 to 1 through 2.7 to 1 with a solids content of 24 to 35~.
:
M-781-1 .
Preferably, the mixture is formed ~y bringing together a dry powder material including the perlite and the slurry includ~
ing the sodium silicate, zinc oxide and water and mixing the powder and the slurry at least to the time the mix appears damp and dust-free and short of the time the mix begins shrinking substantiall.
in volume. After the mixing of the mixture is completed the mix-ture is held in storage for a period not exceed;ng 2 l/Z hours so as to permit the material to ~e Eormed into s~ape under compression.
Compression to achieve the desired shape may be achieved prior to heating by vibration ox a plurali.ty of compression steps.
The shaping may al~o be accompli.shed by blowing the material into shape.
Heating of the mixture may ~e accomplished by heating in an oven at a tempera~ure of 93 through 99C for four hours for each inch of minimum dimension of ~hape~ In the alternative, the material may b~ subjected to he~t by micro~ave energy.
The material is characterized ~y a bulk density of 13.0 to 14.0 lbs. per cubic foot ~hen subjected to ASTM test C-303 ~.nd preferably 13. a to 13.5. The material is also characterized by less than 1% linear change and less than 4% weight loss when sub-jected to ASTM test C-356.
The flexural strength of the material i5 in excess of 45 lbs. per square inch for a bulk densit~ of less than 13.5 lbs.
per cubic foot when tested in accordance with ASTM test C-203.
The thermal conductiviti.es of the material is less than O53, .6S and .78 Btu's per inch of thickness per square foot per degree F. per hour at 50QF, 700F and 900F respectively when tested in accordance with ASTM test C-777.
- 5 ~
The material is characterized ~y a surface which is smoother than SIS-3 on the oficial alloy casting Institute Surface Indicator Scale and preferably as smooth as or smoother than SIS-2 on that scale.
In accordance with another important as.pect of the in-vention, the material may be formed into shaped bodies. Preferably, the material is formed into a hollow tubular confi.guration comprising a plurality of separable segments where the segments include mating tongues and grooves or mitre ioints, The segments may be separable along surfaces extending substantially parallel to the axis of the tubular configuration with the tongues and grooves being formed in the suraces.
'' ' ' - 6 ~
~ .
~~7~
.. . .
S~3 Brief Description of the Draw gs ~ ig. 1 i9 a diagram illustratiny t~e thermal conductivity of the material of the invention;
Fig. 2 is an exploded perspective view of the material of 5 this invention formed into hollow tubula;r configuration;
Fig. 3 is a sectional view of the tongue and grooving in another embodiment of the invention;
Fig. 4 is another sectional view of the tongue and groov-ing in yet another embodiment of the invention; and Fig. 5 is a sectional view of a tongue and grooving of still another embodiment of the invention.
Detailed Description o Preferred Embodiments The material o~ the present invention starts out ultimately on a basis o approximately lQ0 parts by weigh.t as a mix of the lS following:
expanded perlite 2Q through 50 parts, preferably 29 through 45 parts, with 36 through 42 representing an optimum:
sodium fluosili.cate .5 throu~h 4 parts, preferably 1 through 3.5 parts, with. 2 through 3 preferred;
fiber material ~2 through 5 parts, pre~era~ly l through S parts;
sodium silicate or potassium silicate including 9~5 through l9 parts, preferably 11.5 thxough 18 parts, solids content of sodium silicate itself, with 14.5 through 16~5 representing the optimum;
zinc oxide 2 through ~ parts, preferably 3 through 8 p~rts, with ~.5 through 6.8 representing the optimum;
water, to mak.e a total of water, including any that may be associated with the sodium silicate, of 21~5 through 67 parts, preferably 26.5 through 57, with 32~5 through 43.5 xepresenting the optimum.
It is ~rought to this state by mixing the expanded perlite, the sodium fluosilicate and the fiber material together in powder form and separately mixing the sodium silicate in a solution of preferably 36 thxough 44% solids, with 38% preferred or potassium silicate in a solution of preferably 24 to 35~, zinc oxide and water together to form a slurry which is in turn mixed in with the powder. The mixing is then continued up at least to the time the mix appears damp and dust-free, but not up to the time the mix starts to shrink substantially.
Various mixing devices, such as a planetary batch mixer~
or a co~tinuous screw feed mixer, are suitable for tne mixing, a pug mill batch mixer also being suitable.
The material may be passed through a screen, which will preferably have half inch openings~ after the mixing.
The material is then preferably held in storage under covex up to two and one half hours. T~îs step has ~een observed to have the effect of markedl~ increasing the strength of the final product~
~ The material i5 then compressed, ~y a ram or vibration, into the shape in which it ~i~l ultimately be wanted. Another less preferred way of bringing it into shape is to put part of it into a mold or the like that may be used and compress that part and then put in part or all of the additional and compress it, and so on.
The material is then heated to cure it, this being pre-2S ferably done in a micro~ave oven. If in a conventional oven uti-lizing hot air then it should preferably be done in the temperature range from 93C through 99C and preferably from approximately two through approximately four hours per inch of the smallest dimension of the shape t and most preferably at 96C for four hours for each inch of the smallest dimension of the shape~
r r-The fiber material may comprise a class of organic or inorganic materials including 1 through 5 parts fi~erglass or a heat resistant nylon-type fibrous material, such as poly (1, 3-~J phenylene isophthalamide~, sold commercicllly under the -~Eaæ~
S Nomex, can be used less preferably instead of the fiberglass, in which case the amount will be ~2 through l~S parts by weight and preferably .5 parts hy weight~ Another less prefera~le possibility for this is mineral wool, such as rockwool in the amount of l through 5 parts or preferably l part. Cotton or wood fibers may also be used.
The fiberglass or other fibrous material i5 in the form of a floc - that is, a set o~ fibers in short lengths~ averaging pre~erably 1/8 through l/4 inch long and most prefera~ly in fibers averaging 1/4 inch long.
The class of fiber material aIso inc7udes l through 5 parts of netting which may be organic or inorganic materials in-cluding polypropylene, polyester, nylon or Dacron~ The netting comprises fibers of a thickness in the range of .Q07 to .125 inches, openings having areas in the range of ~06 to 1 square inch and weight of less than 2 lbs. per thousand square feet~ The netting s~rength should exceed 4 grams per denier when suhjected to an Instron tester at 65~ relative humidity. The openings in the netting may take on a variety of shapes including squares, rectan-gles, circles or ovals~
All fiber materials must be stable at temperatures in excess of 250F., i.e., there is no substantial softening below these temperatures.
The expanded perlite should have a dry bulk density of 2 through 8 lbs. per cubic foot, and preferably 2 through 3 1/2 lbs.
per cubic foot. The perlite is a complex sodium potassium aluminum ~ e /~
_ g _ silicate volcanic granular glass~ Its scre~n sizing should be AFS
(~merican Foundry Society) average screen size designation of 70 through 120 and preferably 110. A perlite with 25% maximum con-taminants including no more than ~5% each of Fe o Ca and no more than .1~ of each of arsenic, barium, beryllium, boron, chlorlne, chxomium, copper, gallium, lead, manganese, molybdenum, nickel, sulphur, titanium, yttrium and zirconium i5 suitable~ Expanded perlite includes all perlite made from naturally occurring perllte sand which is expanded by heat. The fusion temperature is in ex-cess of 2300F and has a solubility of less than 1% in water, less than 10% in lNONaO~ and less than 3% in mineral acids, The sodium silicate should become part Gf the mix in theform of a water solution capable of being handled in a practical manner. Any commercially available solution will suffice but it is preferred that its ratio of silicon dioxide to sodium oxide should preferably be in the range of 3~1 to 1 through 3.4 to 1, and most preferably 3.22 to 1, and it should have a solids content preferably~
in the range of 36 through 44%~ and most preferably 38~. An e~-ample~
of a suitable sodium silicate grade to use is the N grade of Phila-delphia Quartz. Where potassium silicate is used, the ratio ofsilicon dioxide to potassiNm oxide shauld preferably be in the range of 2.0 to 1 through 2~7 to 1 with a solids content of 24 to 35~.
For good results, it i5 important that the zinc oxide should be finely divided and fairly clean, e.g~, the type that is produced by the so-called French process. Use of the zinc oxide in finely divided form has been found to quite substantially in-crease the strength and the water resistivity. A zinc oxide havlng an average fineness o no more than .50 mi rons is suitable, .10 to .20 preferred, and 1.7 most preferred; 9~ to 99% purity or more particularly reagent grade is suitable from the standpoint of purity.
~4593 Instead of including the sodium fluosilicate as a solid-iying agent to add green strength, a less preferred alternative which'nevertheless has special advantages is to pass carbon dioxide gas under pressure into or through the material after it has been S compressed into shape.
The curing or drying step, can well take place in an oven, for example in an electric or other con~entional oven with air circulati~g around within it, and in such a case the piece of material being subjected to the heating should be so supported that the maximum area of the piece will have direct access to the air in the oven. For example,, a piece with.relatively l~nger and shorter dimensions should be supported with.its longest dime.nsion in the vertical direction~ whi.ch will achieve this result and also - tend to prevent warping~ Dehydrating and oth.erwise curing the . material can also be accomplished by the use of microwave energy in heating devices such as ovens, which have a capability of securing the result in a much shorter time, for example for some time such as 5 minutes to the inch.of minimum dimension. Vse o~ :
this has been found on the average to enhance the strength more than 20% as compared to using a conventional oven.
To further illustrate the invention, the ollowing ex- .
amples are illustrative of suitably carrying out of the invention.
. EXAMPLE 1 This example involves the making of a block 12 inches by 8 inches by 2 inches, for the purpose of which 200 cubic inches of material is made in order to have enough. to make the block to-gether with a small excess to accommodate ha,ndling lossesr .. : .
. ~ .,, l:~V~S~3 The following materials are secured:
1. PFF 10 perlite ~powder) 352 g ~29%~
. Sodium ~luosilicate ~powder) 24 g ~2%) 3. Fiberglass ~1/8" fibers) 12 g (1~)
4. Water 290 g (24%)
5. Sodium silica-te ~3.22:1) 473 g ~39~) ~liquid)
6. Zinc oxide (powder, rubber pigment type) 61 g (5 1212 g (100~) lQ Items 1, 2 and 3 are added to a ten gallon bowl capacity Hobart mixer. Items 4~ 5 and 6 are pr~-mixed ln a slurry. The mixer is turned on and the slurry is poured into bowl in a way that the stream will meet the path of the impelle~u It is impor-tant in this par~icular case that the mixing does not~exceed 35 seconds nor be less than 20 seconds, ., The material may be passed through: a 1/2 inch opening screen. The material is then held in storage 90 minutes~under cover. At thi. time, the material is added to the mold~box. About one third is added and spread evenly across the bottom of the box.
This is gently and carefully rammed, after which the remaining portion is added. The box which is designed to receive about 2~3 pounds of the damp mix is then positioned under a hydrauliG;press head. A close-~itting, smooth, wooden block is then inserted into the loaded mold box. ~
~5 This block being high enough will act as a piston and will dr1ve the mixture downwardr compressing it into the proper 5i zed block. ~ 3 The mold box is 50 constructed that it is more than deep enough to receive the batch as given and rammed according to the instructions given above.
,.
M-781-1 .
The box surface~ should have three coats of pattern lacquer, rubbed smooth~ and paste wax applied giving it a final shiny, good-releasing surface~
The box is constructed in a way that the corners can be loosen~d after block forming, thus~ allowing easy, scuf-free re-moval o~ the molded piece, At this point, t~e driving piston block can be used to eject the formed piece, for its subsequent transfer to a dryer plate The oven drying then takes place as ollows:
Measuring the total thickness a~ 2 inches, eight hours at 96C eliminates sufficient free water and apparen~ly properly accomplishes the formation of willemite which is believed to be important for securing the best results wi~h suc~ a block~ This lnvolves four hours of such heat for each inch o~ minimum dimen-sion, in an ordinary air heat oven~
At this time, if the particular material in question was being produced for commercial use, the block could ~e stored, packed or shipped.
Where sodium fluosilicate is used, it should be of pharma~
ceutical grade finely powdered with an analysis purity of in excess of 23% Na2SiF6 and a fineness of 95% through a 20Q mesh screen.
Where carbon dioxide gas is used, it should be at more than 9~%
purity, and can be applied under 15 lbs. gauge pressure for four to five seconds per inch of thickness of matrix, i.e,, inside dimension to outside dimension.
Where sodium fluosilicate is used, it should be of pharma-ceutical grade finely powdered, Where carbon dioxide gas is used, it should be a~ more than 99% purity, and can be applied under 15 lbs.
gauge pressure ~or four seconds per inch of thickness of matrix.
In the forming stept a compressive action by the moving ~ 13 ~
head of 30 to 100 lbs. per square inch i.s sui.table and of course the mold should have a strength to withstand this. The compacting step with vibration should take no longer than ten seconds per cubic foot of material. Vibration can suitably be at a rate of ~.
300 or 1000 pulses per minute., for example~
The matexial can instead ~e formed ~y ~lo~ing it into a suitable cavity, in a mold to make a pre~shaped piece, in the manner of core blowing in foundry practice~ Suitahly screened vents permit the escape of the air whic~ is carrying the material, ;
while keeping the materi.al in the cavity t in a shape formed under pressure of the blowing.
In the mold used in the forming step, a coating of Teflon or epoxy with h.igh. glo~s. can take the place of the pattern , lacquer used in the example~
So likewise the hox construction ~;th pro~ision for ` loosening the corners found in th.e example can ~e~made unnecessary by securing a good straigh.t travel in ejection~
EX~MPLE 2 Th.e following mixture is prepared;
1. PFF 10 perlite ~powder~ 164 g ~39~00.%~
2. Sodium ~luos.ilicate (powderl 10 g ~2.40%) 3. ~ater ~ 45 g (10~70%) 4. Zinc oxide 27 g (6.50%) 5. Sodium sili.cate solution 174 g (41.40%) as Items 1 and 2 are dry mixed in a ~obart mixer for 10 ; seconds at which time the slurry made by separately mixing 3, 4~and 5 is added to the running mixer and s~ch mixing is continued until the mixture appears dust free ~uk short of a time when it starts to shrink in volume.
.
~ . .. . .
After 30 minute storag~ under a plastic sheet cover, a 50 gram portion is lightly tamped into a ~pecial Dietert transverse metal mold box with split corners. A drop weight rammer is actuated 8 to 12 times making an exact 1 x 1 x 8 inch bar of compressed material whose d~nsity will be 13.5 to 14.~ lbs~ per cubic foot after the bar has been dried by microwave energy for 4 to 6 minutes.
The sodium fluosilicate. o Example 2 is eliminted and .
the procedure to make and tesk bars as set forth in Example 2 is`
otherwise followed. After the compressed ~ars are formed, they are treated by passing carbon dioxide gas through them at a pres-~. :
sure of 15 lbs. per square inch. for 5 seconds~
The follo~ing mixture is prepared using the method of 15Example 2:
1. PFF 10 perlite tpowder)168 g (40%) 2. Sodium fluosilica*e (powder] lZ.5 g (3%) 3. ~ater 12~5 g (3~
4. ~inc oxide 25 g (6%) 5. Sodium silicate solution202 g (48%) The following mixture is prepared using the method of Example 2: ~
1. PFF 10 perli.te ~powder~151 g (36%3 2. Sodium fluosilicate (powder~ 14.5 g (3.5%~
3. ~ater 89.5 g (21.5%)~ .
4. Zinc oxide :33 g ~8~) 5. Sodium silicate 130 g (31~) M-781~ g S ~ 3 The following mixture is prepared using the method of Example 2:
1. PFF 10 perlite (powder) 168 g (40%) 2. Sodium fluosilicate (powder) 12.5 g (3%) 3. Water 12~5 g (3~) ~. Zinc oxide 25 g (6%) 5. Potassium sili.cate 202 g (48%) The following mixture is prepared using the method of Example 2: .
1. PFF 10. perlite (powder) 151 g (36~) 2. Sodium fluosilicate (powder) 14~5 g (3.5%) 3~ Water 89~5 g (21,5%) 4. ~inc oxide 33 g ~8~) 5~ Potassi~um silicate 130 g (31%) ~he procedure of Example 2 i~ utilized with. the mixture o Example 6 except the sodium fluosilicate is eliminated.
The material o~ each. example is parti.cularly resistant to boiling water. For example~ the material of Example 2 retained its exact shape when subjected to boiling water for 5 hQurs and only suffered a weight loss of lQ~a%~ Similarly, the material of~
Example 3, when subjected to 5 hours of boiling water retained its exact shape and only suffered a weight loss of 11~5%, In contrast, the samples similar to Example 2 but without the sodium fIuosilicate . or the carbon dioxide of Examples 3 and ~ completely lost their shape and disintegrated into fine particles within 5 minutes of the time it was introduced into boiling water. In the absence of zinc .
.
~/
. ' r~ !
oxide in ~xample 2, the material completely disintegrated within 30 minutes after being introduced into the boiling water.
The properties of the material made in accordance with this invention make the material particularly well suited for use as a high temperature insulation.
When the material was tested or bulk density in accor-dance with ASTM standard test C-303, it was found that the material had a bulk density ranging from 13.0 to 14.0 lbs~ per cubic foot, .
more than satisying the ASTM requirement of 13,5 throu~h 14.0 lbs~
per cubic foot.
The material of Example 2, when tested in accordance with ASTM standard test C-356 demonstrated a percent linear change of less than 1% at 12Q0F and a percent weight loss of less than 4% at 1200F as contrasted with the standard of less than 2% linear change and less than 5% weight loss at 120QF~
The flexural strength of the material made in accordance with this invention and tested pursuant to ASTM standard test~C-610 produced a flexural strength in excess of 45 lbs~ per sq. inch for bulk densities of less than 13.5 lbs, per cubic foot. The flexural ~0 strength of bars made in accordance with Examples 4 and 5 is 66 and 55 lbs. per square inch respectively~
The material also passed the ASTM standard test C-421 for mechanical stability, test C-165 for compressive strength, test C-411 for hot surface per~ormance and test E-84 for surface burn chaxacteristics. The ASTM standard test C-692 for chlorine cor-rosion and the DANA stress corrosion test on stainless ste 1 per military specification I-24-244 were also passed.
Reference will now be made to Fi~, 1 for an illustration of the thermal insulating properties of the material, The curve as shown in Fig. 1 represents the results of ASTM standard test C-177 ~ 17 -which measures the thermal conductivity K in Btu's per inch thick-ness per square foot per degree F per hour~ As s~own in Fig. 1, the K factor is found on the ordinant and the temperature is found on the abscissa. It will be observed that a K factor of the material of this invention is sub~tantially lower or ~etter than the K fact~r of the ASTM standard. For example~ the K factor of the material of this invention i~ .42 at 300 as compared with. the ASTM test standard of less than .5Q. The K factor at 50~F or the material of this invention is less than .53 and typically ~44 whereas the ASTM stand-lQ ard is less than .6Q. At 7Q0.F, thd ASTM standard is less than .71whereas the material of thi.s invention has a K actor of less than .65 and typically ~55~ At ~QQF~ the K factor o~ this învention is :
less than .78 and typically less than .72~
The ASTM tests. referred to in th.e foregoing are described in detail in ths ASTM 1975 Annual Standards Part 18 which is incor- -porated herein by reference.
The material has a cosmetically pleasing appearance due ~ :
in large measure to the smoothness of the material~ In this re-gard, the surface which is smoother than SIS~3 on official alloy Casting Institute Surface Indicator Scale and preferably as smooth as or smoother than 5IS-2 on that scale~
The material will provide solid rigid shapes suitable for enclosing and insulating hot pipes, furnace outer walls, oven walls, cold pipe and walls, and fittings and valves, :
The ability of the material to hold solid rigid shape and the smoothness of the material allows the matexial to be formed for making a tongue and groove or mitred ~oints such as that shown in Figs. 2-5. As shown in thes.e Figures, the tongues 10 (a-d) and the grooves 12(a-d) in surfaces 14 may take on various shapes, some of which are fairly intricate. However~ due to the ability of the :. . , . r material to hold its shape and the relative smoothness of the sur-~aces, appropriate mating of the tongues and grooves is assured.
As shown in Fig. 2(.a-c), the material comprises a hollow tubular configuration having a plurality of two or more segments 16 which include the tongue~ and grooves lO~a-d) and 12(a-d).in the surface 14 which extend parallel to the axis of the tubular config-uration. However, it will be appreciated that the tongues and grooves may be utilized in planar sheets and other configurations such as might be required to accommodate the configurations of furnaces, fittings, valves. and ov~n walls, etc~ It will be noted thak the dove-tail tongues and grooves of Fig~ 5 permit the two segments to be joined without benefit of straps.
As already largely indicated, the material of the inven-tion forms heat insulation of special strength and good heat re~
sistance and water resi.stivi.t~ made in a very practical, economical way.
It is thought that the particular componenks o the present inven'.ion work together in a very special way to give a high quality product. For example~ it is ~elieved that the sodium :.
silicate, watex and zinc oxide when dealt with in *he way indicated herein as part o~ the present overall material react together to form willemite in large part, which is a complex material which is mainly a form of zinc s.ilicate (Zn2SiO4) plus some basic zinc : 25 ~ilicate plus some zinc sodium sillcate (Zn2Na2SiO4H2O) and is believed to contribute greatly to the strength and water resistivity : o~ the material. It is also believed that potassium silicate, water and zinc oxide will react to produce an analogous complex material.
The sodium fluosilicate as applied in this particular setting is beli.eved to help secure dimensional stability while the material is undergoing dehydration, and also help pxevent dis-- , .
- 19 ~
~ 3 integration of the other components as a result of the presence of water. The fiber material is believed to help increase the final strength and also reduce any tendency toward fracture of the structure by impact.
In view of our invention and disclosure, variations and modifications to meet indiYidual whim or particular need will doubt-less become evident to others skilled in the art to obtain all or part cf the benefits of our invention without copying the process and product shown, and we, therefore r claim all such insofar as they fall within the reasonable spirit and scope o~ our claims.
.
-- ?O --
This is gently and carefully rammed, after which the remaining portion is added. The box which is designed to receive about 2~3 pounds of the damp mix is then positioned under a hydrauliG;press head. A close-~itting, smooth, wooden block is then inserted into the loaded mold box. ~
~5 This block being high enough will act as a piston and will dr1ve the mixture downwardr compressing it into the proper 5i zed block. ~ 3 The mold box is 50 constructed that it is more than deep enough to receive the batch as given and rammed according to the instructions given above.
,.
M-781-1 .
The box surface~ should have three coats of pattern lacquer, rubbed smooth~ and paste wax applied giving it a final shiny, good-releasing surface~
The box is constructed in a way that the corners can be loosen~d after block forming, thus~ allowing easy, scuf-free re-moval o~ the molded piece, At this point, t~e driving piston block can be used to eject the formed piece, for its subsequent transfer to a dryer plate The oven drying then takes place as ollows:
Measuring the total thickness a~ 2 inches, eight hours at 96C eliminates sufficient free water and apparen~ly properly accomplishes the formation of willemite which is believed to be important for securing the best results wi~h suc~ a block~ This lnvolves four hours of such heat for each inch o~ minimum dimen-sion, in an ordinary air heat oven~
At this time, if the particular material in question was being produced for commercial use, the block could ~e stored, packed or shipped.
Where sodium fluosilicate is used, it should be of pharma~
ceutical grade finely powdered with an analysis purity of in excess of 23% Na2SiF6 and a fineness of 95% through a 20Q mesh screen.
Where carbon dioxide gas is used, it should be at more than 9~%
purity, and can be applied under 15 lbs. gauge pressure for four to five seconds per inch of thickness of matrix, i.e,, inside dimension to outside dimension.
Where sodium fluosilicate is used, it should be of pharma-ceutical grade finely powdered, Where carbon dioxide gas is used, it should be a~ more than 99% purity, and can be applied under 15 lbs.
gauge pressure ~or four seconds per inch of thickness of matrix.
In the forming stept a compressive action by the moving ~ 13 ~
head of 30 to 100 lbs. per square inch i.s sui.table and of course the mold should have a strength to withstand this. The compacting step with vibration should take no longer than ten seconds per cubic foot of material. Vibration can suitably be at a rate of ~.
300 or 1000 pulses per minute., for example~
The matexial can instead ~e formed ~y ~lo~ing it into a suitable cavity, in a mold to make a pre~shaped piece, in the manner of core blowing in foundry practice~ Suitahly screened vents permit the escape of the air whic~ is carrying the material, ;
while keeping the materi.al in the cavity t in a shape formed under pressure of the blowing.
In the mold used in the forming step, a coating of Teflon or epoxy with h.igh. glo~s. can take the place of the pattern , lacquer used in the example~
So likewise the hox construction ~;th pro~ision for ` loosening the corners found in th.e example can ~e~made unnecessary by securing a good straigh.t travel in ejection~
EX~MPLE 2 Th.e following mixture is prepared;
1. PFF 10 perlite ~powder~ 164 g ~39~00.%~
2. Sodium ~luos.ilicate (powderl 10 g ~2.40%) 3. ~ater ~ 45 g (10~70%) 4. Zinc oxide 27 g (6.50%) 5. Sodium sili.cate solution 174 g (41.40%) as Items 1 and 2 are dry mixed in a ~obart mixer for 10 ; seconds at which time the slurry made by separately mixing 3, 4~and 5 is added to the running mixer and s~ch mixing is continued until the mixture appears dust free ~uk short of a time when it starts to shrink in volume.
.
~ . .. . .
After 30 minute storag~ under a plastic sheet cover, a 50 gram portion is lightly tamped into a ~pecial Dietert transverse metal mold box with split corners. A drop weight rammer is actuated 8 to 12 times making an exact 1 x 1 x 8 inch bar of compressed material whose d~nsity will be 13.5 to 14.~ lbs~ per cubic foot after the bar has been dried by microwave energy for 4 to 6 minutes.
The sodium fluosilicate. o Example 2 is eliminted and .
the procedure to make and tesk bars as set forth in Example 2 is`
otherwise followed. After the compressed ~ars are formed, they are treated by passing carbon dioxide gas through them at a pres-~. :
sure of 15 lbs. per square inch. for 5 seconds~
The follo~ing mixture is prepared using the method of 15Example 2:
1. PFF 10 perlite tpowder)168 g (40%) 2. Sodium fluosilica*e (powder] lZ.5 g (3%) 3. ~ater 12~5 g (3~
4. ~inc oxide 25 g (6%) 5. Sodium silicate solution202 g (48%) The following mixture is prepared using the method of Example 2: ~
1. PFF 10 perli.te ~powder~151 g (36%3 2. Sodium fluosilicate (powder~ 14.5 g (3.5%~
3. ~ater 89.5 g (21.5%)~ .
4. Zinc oxide :33 g ~8~) 5. Sodium silicate 130 g (31~) M-781~ g S ~ 3 The following mixture is prepared using the method of Example 2:
1. PFF 10 perlite (powder) 168 g (40%) 2. Sodium fluosilicate (powder) 12.5 g (3%) 3. Water 12~5 g (3~) ~. Zinc oxide 25 g (6%) 5. Potassium sili.cate 202 g (48%) The following mixture is prepared using the method of Example 2: .
1. PFF 10. perlite (powder) 151 g (36~) 2. Sodium fluosilicate (powder) 14~5 g (3.5%) 3~ Water 89~5 g (21,5%) 4. ~inc oxide 33 g ~8~) 5~ Potassi~um silicate 130 g (31%) ~he procedure of Example 2 i~ utilized with. the mixture o Example 6 except the sodium fluosilicate is eliminated.
The material o~ each. example is parti.cularly resistant to boiling water. For example~ the material of Example 2 retained its exact shape when subjected to boiling water for 5 hQurs and only suffered a weight loss of lQ~a%~ Similarly, the material of~
Example 3, when subjected to 5 hours of boiling water retained its exact shape and only suffered a weight loss of 11~5%, In contrast, the samples similar to Example 2 but without the sodium fIuosilicate . or the carbon dioxide of Examples 3 and ~ completely lost their shape and disintegrated into fine particles within 5 minutes of the time it was introduced into boiling water. In the absence of zinc .
.
~/
. ' r~ !
oxide in ~xample 2, the material completely disintegrated within 30 minutes after being introduced into the boiling water.
The properties of the material made in accordance with this invention make the material particularly well suited for use as a high temperature insulation.
When the material was tested or bulk density in accor-dance with ASTM standard test C-303, it was found that the material had a bulk density ranging from 13.0 to 14.0 lbs~ per cubic foot, .
more than satisying the ASTM requirement of 13,5 throu~h 14.0 lbs~
per cubic foot.
The material of Example 2, when tested in accordance with ASTM standard test C-356 demonstrated a percent linear change of less than 1% at 12Q0F and a percent weight loss of less than 4% at 1200F as contrasted with the standard of less than 2% linear change and less than 5% weight loss at 120QF~
The flexural strength of the material made in accordance with this invention and tested pursuant to ASTM standard test~C-610 produced a flexural strength in excess of 45 lbs~ per sq. inch for bulk densities of less than 13.5 lbs, per cubic foot. The flexural ~0 strength of bars made in accordance with Examples 4 and 5 is 66 and 55 lbs. per square inch respectively~
The material also passed the ASTM standard test C-421 for mechanical stability, test C-165 for compressive strength, test C-411 for hot surface per~ormance and test E-84 for surface burn chaxacteristics. The ASTM standard test C-692 for chlorine cor-rosion and the DANA stress corrosion test on stainless ste 1 per military specification I-24-244 were also passed.
Reference will now be made to Fi~, 1 for an illustration of the thermal insulating properties of the material, The curve as shown in Fig. 1 represents the results of ASTM standard test C-177 ~ 17 -which measures the thermal conductivity K in Btu's per inch thick-ness per square foot per degree F per hour~ As s~own in Fig. 1, the K factor is found on the ordinant and the temperature is found on the abscissa. It will be observed that a K factor of the material of this invention is sub~tantially lower or ~etter than the K fact~r of the ASTM standard. For example~ the K factor of the material of this invention i~ .42 at 300 as compared with. the ASTM test standard of less than .5Q. The K factor at 50~F or the material of this invention is less than .53 and typically ~44 whereas the ASTM stand-lQ ard is less than .6Q. At 7Q0.F, thd ASTM standard is less than .71whereas the material of thi.s invention has a K actor of less than .65 and typically ~55~ At ~QQF~ the K factor o~ this învention is :
less than .78 and typically less than .72~
The ASTM tests. referred to in th.e foregoing are described in detail in ths ASTM 1975 Annual Standards Part 18 which is incor- -porated herein by reference.
The material has a cosmetically pleasing appearance due ~ :
in large measure to the smoothness of the material~ In this re-gard, the surface which is smoother than SIS~3 on official alloy Casting Institute Surface Indicator Scale and preferably as smooth as or smoother than 5IS-2 on that scale~
The material will provide solid rigid shapes suitable for enclosing and insulating hot pipes, furnace outer walls, oven walls, cold pipe and walls, and fittings and valves, :
The ability of the material to hold solid rigid shape and the smoothness of the material allows the matexial to be formed for making a tongue and groove or mitred ~oints such as that shown in Figs. 2-5. As shown in thes.e Figures, the tongues 10 (a-d) and the grooves 12(a-d) in surfaces 14 may take on various shapes, some of which are fairly intricate. However~ due to the ability of the :. . , . r material to hold its shape and the relative smoothness of the sur-~aces, appropriate mating of the tongues and grooves is assured.
As shown in Fig. 2(.a-c), the material comprises a hollow tubular configuration having a plurality of two or more segments 16 which include the tongue~ and grooves lO~a-d) and 12(a-d).in the surface 14 which extend parallel to the axis of the tubular config-uration. However, it will be appreciated that the tongues and grooves may be utilized in planar sheets and other configurations such as might be required to accommodate the configurations of furnaces, fittings, valves. and ov~n walls, etc~ It will be noted thak the dove-tail tongues and grooves of Fig~ 5 permit the two segments to be joined without benefit of straps.
As already largely indicated, the material of the inven-tion forms heat insulation of special strength and good heat re~
sistance and water resi.stivi.t~ made in a very practical, economical way.
It is thought that the particular componenks o the present inven'.ion work together in a very special way to give a high quality product. For example~ it is ~elieved that the sodium :.
silicate, watex and zinc oxide when dealt with in *he way indicated herein as part o~ the present overall material react together to form willemite in large part, which is a complex material which is mainly a form of zinc s.ilicate (Zn2SiO4) plus some basic zinc : 25 ~ilicate plus some zinc sodium sillcate (Zn2Na2SiO4H2O) and is believed to contribute greatly to the strength and water resistivity : o~ the material. It is also believed that potassium silicate, water and zinc oxide will react to produce an analogous complex material.
The sodium fluosilicate as applied in this particular setting is beli.eved to help secure dimensional stability while the material is undergoing dehydration, and also help pxevent dis-- , .
- 19 ~
~ 3 integration of the other components as a result of the presence of water. The fiber material is believed to help increase the final strength and also reduce any tendency toward fracture of the structure by impact.
In view of our invention and disclosure, variations and modifications to meet indiYidual whim or particular need will doubt-less become evident to others skilled in the art to obtain all or part cf the benefits of our invention without copying the process and product shown, and we, therefore r claim all such insofar as they fall within the reasonable spirit and scope o~ our claims.
.
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Claims (67)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A coherent rigid solid material made from a mixture subjected to heat so as to reduce the original content of water, said mixture comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts;
sodium fluosilicate 1 through 6 parts; and water, to make a total of water, including any that may be asso-ciated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts;
sodium fluosilicate 1 through 6 parts; and water, to make a total of water, including any that may be asso-ciated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
2. The material of claim 1 wherein the mixture further comprises an organic or inorganic fiber material.
3. The material of claim 2 wherein the fiber material is from a class comprising 1 through 5 parts fiberglass, 0.2 through 1.5 parts heat resistant nylon, 1 through 5 parts mineral wool and 1 through 5 parts of netting, all by weight as a part of the mixture.
4. The material of claim 3 wherein said netting comprises fibers of a thickness in the ranges of 0.007 to 0.125 inches, openings having areas in the range of 0.06 to 1 square inch and weight of less than 1 pound per square inch.
5. The material of claim 3 wherein said fibers of said class exclu-sive of said netting has an average fiber length of 1/8 through 1 inch.
6. The material of claim 1 wherein the mixture comprises the follow-ing composition by weight:
expanded perlite 29 through 45 parts;
sodium silicate 11.5 -through 18 parts;
zinc oxide 3 through 8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate, of 26.5 through 57 parts.
expanded perlite 29 through 45 parts;
sodium silicate 11.5 -through 18 parts;
zinc oxide 3 through 8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate, of 26.5 through 57 parts.
7. The material of claim 1 wherein the mixture comprises the following composition by weight:
expanded perlite 36 through 42 parts;
sodium silicate 14.5 through 16.5 parts;
zinc oxide 4.5 through 6.8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate, of 32.5 through 43.5 parts.
expanded perlite 36 through 42 parts;
sodium silicate 14.5 through 16.5 parts;
zinc oxide 4.5 through 6.8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate, of 32.5 through 43.5 parts.
8. The material of claim 1 in which the expanded perlite of the mixture has a dry bulk density of 2 through 3 1/2 pounds per cubic foot.
9. The material of claim 1 in which the zinc oxide of the mixture has an average fineness of not over 0.5 microns.
10. The material of claim 1 in which the zinc oxide of the mixture has an average fineness of from 0.1 through 0.2 microns.
11. The material of claim 1 wherein the perlite has an AFS
Fineness No. of 70 through 120.
Fineness No. of 70 through 120.
12. The material of claim 1 in which the sodium silicate has a proportion of silicon dioxide to sodium oxide of 3.1 to 1 to 3.4 to 1.
13. The material of claim 1 in which the potassium silicate has a proportion of silicon dioxide to potassium oxide of 2.0 to 1 to 2.7 to 1.
14. The material of claim 1 in which the sodium silicate is introduced to the mix in a solution having a solids content of 36 to 44 percent.
15. The material to claim 1 in which the potassium silicate is introduced to the mix in a solution having solids content of 24 to 35 percent.
16. The material of claim 1 in which the mixture is formed by bringing together a dry powder material including the perlite and a slurry including the sodium silicate, zinc oxide and water and mixing the powder and the slurry at least to the time the mix appears damp and dustfree, and short of the time the mix begins shrinking substantially in volume, the sodium silicate having a ratio of silicon dioxide to sodium oxide of from 3.1 to 3.4 to 1.
17. The material of claim 1 in which after the mixing of mixture is completed the mixture is held in storage for a period not exceeding 2 1/2 hours so as to permit the material to be formed into shape under compression.
18. The material of claim 1 in which between the time of making up the mixture and the time of the subjecting of the material to heat, the material is compressed under vibration into shape.
19. The material of claim 1 in which between the time of making up the mixture and the time of the subjecting of the mate-rial to heat, the material is compressed into shape in a plurali-ty of separate compression steps.
20. The material of claim 1 in which between the time of making up the mixture and the time of subjecting the material to heat, the material is blown into shape.
21. The material of claim 1 in which the subjection of the material to heat is at 93° through 99°C.
22. The material of claim 1 in which the subjection of the material to heat is in a hot air oven at 93°C through 99°C for four hours for each inch of minimum dimension of the shape.
23. The material of claim 1 in which the material is subjec-ted to heat by microwave energy.
24. The material of claim 1 having a bulk density of 13.0 to 14.0 lb. per cubic foot when subjected to ASTM test C-303.
25. The material of claim 1 characterized by less than 1% linear change when subjected to ASTM test C-356.
26. The material of claim 1 characterized by less than 4% weight loss when subjected to ASTM test C-356.
27. The material of claim 1 characterized by a flexural strength in excess of 45 lb. per square inch for a bulk density of less than 13.5 lb. per cubic foot when tested in accordance with ASTM test C-303.
28. The material of claim 1 characterized by thermal conductivities of less than 0.53, 0.65 and 0.75 Btu's per inch of thickness per square foot per degree F at 500°F, 700°F, and 900°F, respectively when tested in accor-dance with ASTM test C-777.
29. The material of claim 1 characterized by a surface smoother than SIS-3 on the official Alloy Casting Institute Surface Indicator Scale.
30. The material of claim 1 characterized by a surface at least as smooth as or smoother than SIS-2 on the official Alloy Casting Institute Sur-face Indicator Scale.
31. The material of claim 1 comprising a plurality of separable seg-ments, said segments comprising mating tongues and grooves.
32. The material of claim 31 wherein said segments form a hollow tubular configuration having separable surfaces extending substantially par-allel to the axis of the tubular configuration, said tongues and grooves being formed in said surfaces.
33. A coherent rigid solid material made from a mixture subjected to heat so as to reduce the original content of water, said mixture comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate of potassium silicate itself;
zinc oxide 3 through 8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate of potassium silicate itself;
zinc oxide 3 through 8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
34. The material of claim 33 wherein the mixture comprises a solidifying agent.
35. The material of claim 34 wherein the solidifying agent comprises 1 through 6 parts sodium fluosilicate.
36. The material of claim 34 wherein the solidifying agent comprises carbon dioxide.
37. The material of claim 36 in which the zinc oxide of the mixture has an average fineness of not over 0 5 microns
38. The material of claim 36 in which the zinc oxide of the mixture has an average fineness of from 0.1 through .2 microns.
39. A coherent rigid solid material made from a mixture subjected to heat so as to reduce the original content of water, said mixture comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts.
40. A process of making a coherent rigid solid material comprising the steps of mixing materials in the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts;
sodium fluosilicate 1 through 6 parts; and water, to make a total of water, including any that may be asso-ciated with the sodium silicate or the potassium silicate of 21.5 through 67 parts, and thereafter subjecting the mixture to heat as a result of which there is no longer the original content of water.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts;
sodium fluosilicate 1 through 6 parts; and water, to make a total of water, including any that may be asso-ciated with the sodium silicate or the potassium silicate of 21.5 through 67 parts, and thereafter subjecting the mixture to heat as a result of which there is no longer the original content of water.
41. The process of claim 40 including the step of compressing the mixture into shape between mixing and heating.
42. The process of claim 41 in which the compressing is done by vi-bration.
43. The process of claim 41 in which the compressing is done in a plurality of compression steps wherein only part of the mixture is compressed in each of said compression steps.
44. The process of claim 40 in which a dry material including at least the expanded perlite, and a slurry including the sodium or potassium silicate, zinc oxide, sodium fluosilicate and water, are brought together and mixed at least until the mixture appears damp and dust free but short of the time the mixture starts to shrink substantially.
45. The process of claim 40 in which after the mixing the mixture is held in storage from 1 hour through 2 1/2 hours and then compressed into shape before subjecting to heat.
46. The process of claim 40 in which the subjecting to heat is done in the temperature range from 93°C through 99°C.
47. The process of claim 40 in which the subjecting to heat is done in a hot air oven at approximately 96°C for approximately 4 hours for each inch of minimum dimension of the shape
48. The process of claim 40 in which the mixture is subjected to heat generated by microwave energy.
49. The process of claim 40 including the step of blowing the material into shape between mixing and heating.
50. The process of claim 40 in which an organic or inorganic fiber material is mixed with said materials.
51. The process of claim 50 wherein the fiber material is from a class comprising l through 5 parts fiber-glass, .2 through 1.5 parts heat resistant nylon, 1 through 5 parts mineral wool and 1 through S parts of netting, all by weight as a part of the mixture.
52. The process of claim 40 wherein said materials are mixed by the following parts by weight:
expanded perlite 29 through 45 parts;
sodium silicate 11.5 through 18 parts;
zinc oxide 3 through 8 parts; and water, to make a total of water including any that may be associated with the sodium silicate, of 26.5 through 57 parts.
expanded perlite 29 through 45 parts;
sodium silicate 11.5 through 18 parts;
zinc oxide 3 through 8 parts; and water, to make a total of water including any that may be associated with the sodium silicate, of 26.5 through 57 parts.
53. The process of claim 40 wherein said materials are mixed by the following parts by weight:
expanded perlite 36 through 42 parts, sodium silicate 14.5 through 16.5 parts;
zinc oxide 4.5 through 6.8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate, of 32,5 through 43.5 parts.
expanded perlite 36 through 42 parts, sodium silicate 14.5 through 16.5 parts;
zinc oxide 4.5 through 6.8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate, of 32,5 through 43.5 parts.
54. A process of making a coherent rigid solid material comprising the steps of mixing materials comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 3 through 8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts; and thereafter subjecting the mixture to heat as a result of which there is no longer the original content of water.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 3 through 8 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts; and thereafter subjecting the mixture to heat as a result of which there is no longer the original content of water.
55. The process of claim 54 including the step of compressing the mixture into shape between mixing and subjecting to heat.
56. The process of claim 55 wherein the mixture is compressed into a shape comprising separable segments with mating tongues and grooves.
57. The process of claim 54 including the step of blowing the mixture into shape between mixing and subjecting to heat.
58. The process of claim 57 wherein the mixture is blown into a shape comprising separate segments with mating tongues and grooves.
59. A process of making a coherent rigid solid material comprising the steps of mixing materials comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts; blow molding the mixture to a desired shape; and curing the mix-ture in the blow molded shape by heating such that as a result of said heat-ing there is no longer the original content of water.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts; blow molding the mixture to a desired shape; and curing the mix-ture in the blow molded shape by heating such that as a result of said heat-ing there is no longer the original content of water.
60. The process of claim 59 including the step of solidifying the mixture after blow molding and before curing by exposing the mixture to carbon dioxide gas under pressure.
61. The process of claim 60 wherein the carbon dioxide is under a gauge pressure of 15 pounds per inch of thickness of the molded shape.
62. The process of claim 59 wherein the blow molding forms a tongue in the shape.
63. The process of claim 59 wherein the blow molding forms a groove in the shape.
64. The process of claim 59 wherein the blow molding forms a tongue and groove in the shape.
65. The process of claim 59 wherein the step of curing by heating comprises microwave heating the blow molded shape.
66. The process of making a coherent rigid solid material comprising the steps of mixing materials comprising the following parts by weight:
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts; and thereafter subjecting the mixture to heat as a result of which there is no longer the original content of water.
expanded perlite 20 through 50 parts;
sodium silicate or potassium silicate including 9.5 through 19 parts solids content of sodium silicate or potassium silicate itself;
zinc oxide 2 through 9 parts; and water, to make a total of water, including any that may be associated with the sodium silicate or potassium silicate of 21.5 through 67 parts; and thereafter subjecting the mixture to heat as a result of which there is no longer the original content of water.
67. The material of claim 1 in which the mixture is formed by bringing together a dry powder material including the perlite and a slurry including the potassium silicate, zinc oxide, and water, and mixing the powder and the slurry at least to the time the mix appears damp and dustfree, and short of the time the mix begins shrinking substantially in volume, the potassium silicate having a ratio of silicon dioxide to potassium oxide of from 2.0 to 1 to 2.7 to 1.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US78295077A | 1977-03-30 | 1977-03-30 | |
| US782,950 | 1977-03-30 | ||
| US05/851,407 US4138268A (en) | 1977-03-30 | 1977-11-14 | Coherent rigid solid material |
| US851,407 | 1977-11-14 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1104593A true CA1104593A (en) | 1981-07-07 |
Family
ID=27120077
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA299,891A Expired CA1104593A (en) | 1977-03-30 | 1978-03-29 | Coherent rigid solid material |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JPS5439433A (en) |
| BR (1) | BR7802008A (en) |
| CA (1) | CA1104593A (en) |
| DE (1) | DE2813745A1 (en) |
| FR (1) | FR2385654A1 (en) |
| GB (1) | GB1602403A (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4336068A (en) * | 1978-07-03 | 1982-06-22 | Lebanon Steel Foundry | High strength insulation materials |
| EP0047675A1 (en) * | 1980-09-10 | 1982-03-17 | Lebanon Steel Foundry | A process of making a coherent rigid solid material |
| BG34662A1 (en) * | 1981-07-07 | 1983-11-15 | Popov | Composition of a water-proof insulating material and method of its manufacture |
| DE3131548A1 (en) * | 1981-08-08 | 1983-02-24 | Otavi Minen Ag, 6000 Frankfurt | "LIGHTWEIGHT MATERIAL AND METHOD FOR THE PRODUCTION THEREOF" |
| US4446040A (en) * | 1982-10-01 | 1984-05-01 | General Refractories Company | Strong, heat stable, water repellent, expanded perlite/alkali metal silicate insulation material |
| DE3314033A1 (en) * | 1983-04-18 | 1984-10-18 | Stotmeister GmbH, 7894 Stühlingen | Acoustic coating |
| DE59804312D1 (en) * | 1997-01-25 | 2002-07-11 | Marmorit Gmbh | LIGHT MATERIAL CONTAINING FLOWED PERLITE AND METHOD FOR PRODUCING THE SAME |
| SI22247A (en) * | 2006-04-11 | 2007-10-31 | Trimo D.D. | Inorganic filler for panel core and procedure for its manufacture |
| US10450937B2 (en) * | 2016-12-21 | 2019-10-22 | Tenneco Automotive Operating Company Inc. | Apparatus and method of producing insulation preform with graded porosity |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3658564A (en) * | 1970-06-01 | 1972-04-25 | Du Pont | Water-insensitive bonded perlite structures |
| US3718491A (en) * | 1971-02-19 | 1973-02-27 | Du Pont | Process for silicate-perlite structures |
| US3864137A (en) * | 1971-12-31 | 1975-02-04 | Bayer Ag | Hydrogen peroxide blowing agent for silicate foams |
| US3933514A (en) * | 1973-04-30 | 1976-01-20 | Continental Oil Company | High strength, water resistant silicate foam |
| SU530872A1 (en) * | 1975-03-25 | 1976-10-05 | Ордена Трудового Красного Знамени Академия Коммунального Хозяйства Имени К.Д.Памфилова | Raw mix for the manufacture of insulating material |
-
1978
- 1978-03-29 FR FR7809140A patent/FR2385654A1/en not_active Withdrawn
- 1978-03-29 CA CA299,891A patent/CA1104593A/en not_active Expired
- 1978-03-30 JP JP3740478A patent/JPS5439433A/en active Pending
- 1978-03-30 GB GB1252478A patent/GB1602403A/en not_active Expired
- 1978-03-30 DE DE19782813745 patent/DE2813745A1/en not_active Withdrawn
- 1978-03-30 BR BR7802008A patent/BR7802008A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5439433A (en) | 1979-03-26 |
| BR7802008A (en) | 1979-04-03 |
| FR2385654A1 (en) | 1978-10-27 |
| DE2813745A1 (en) | 1978-10-19 |
| GB1602403A (en) | 1981-11-11 |
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Legal Events
| Date | Code | Title | Description |
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| MKEX | Expiry |