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WO2006011690A1 - Exfoliation - Google Patents

Exfoliation Download PDF

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Publication number
WO2006011690A1
WO2006011690A1 PCT/KE2005/000013 KE2005000013W WO2006011690A1 WO 2006011690 A1 WO2006011690 A1 WO 2006011690A1 KE 2005000013 W KE2005000013 W KE 2005000013W WO 2006011690 A1 WO2006011690 A1 WO 2006011690A1
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WO
WIPO (PCT)
Prior art keywords
cement composition
weight
cement
raw material
range
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.)
Ceased
Application number
PCT/KE2005/000013
Other languages
French (fr)
Inventor
A. Shariff Mehboob
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
REGIONAL MINING Ltd
Original Assignee
REGIONAL MINING Ltd
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Filing date
Publication date
Application filed by REGIONAL MINING Ltd filed Critical REGIONAL MINING Ltd
Publication of WO2006011690A1 publication Critical patent/WO2006011690A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/14Compositions 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 calcium sulfate cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/28Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • C04B2111/285Intumescent materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/52Sound-insulating materials

Definitions

  • Differential thermal analysis curves of vermiculite generally show three principal endothermic peaks, corresponding to the expulsion of inter-layer water and a further two peaks due to the disruption of the structure by loss of hydroxyl ions.
  • the above results of exfoliation can also be achieved by treating the mineral with hydrogen peroxide.
  • the cement when the mineral is combined with Portland cement in specific volumetric ratios, the cement can acquire Fire resistance, Light weightedness, Insulation capabilities and Sound deadening attributes.
  • This type of cement tends to have two main constituent. These are
  • This type of cement tends to have three main constituent. These are
  • the magnesium-oxide level was detected to be higher than the standard of 5%. Normally any value above the standard, should cause an expansivity of 10mm in a bath of water at 100 0 C for a period of 1 hr, but despite volume of magnesium being above 5% standard, the vermicuiite cement exhibited no significant expansivity (if any, it was within the stipulated standard of below 10mm). As shown in Table C (see appendix), we draw to the tentative conclusion that the magnesium did not participate in any reaction.
  • vermiculite or mica was the main cause of resistance in the cement to higher temperatures affecting the structure since it was the only additive used in the test. Hence the attribute of fire resistance was proved.
  • the mineral has a refractive index of 1.6, giving the final product a pearly lustre and goldish brown hue, instead of a dull grayish coloration consistent with all Portland cement.
  • a Block of 9 inch width mortars were made, one control and two with
  • the golden colour was generally visible in the cement constituting

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

Admixtures are materials added to cement during its manufacture; for example, Gypsum is used as a retardant, Pulverized fuel ash and silica fumes are added in significant amount >10% of cement content. Today in most industrialised countries admixture usage accounts for 50% of the concrete. Hence the additive used in set proportions gave the cement various attributes of: - (1) Fire proofing; - (2) Sound deadening; - (3) Insulation; - (4) Colour; - (5) Non-toxicity.

Description

DESCRIPTION
EXFOLIAΗON
When vermiculite is heated suddenly to temperatures ranging from 300° C to 8000C a rapid generation of steam is released and separation of the structural layers occurs in the direction perpendicular to the cleavage plane.
Differential thermal analysis curves of vermiculite generally show three principal endothermic peaks, corresponding to the expulsion of inter-layer water and a further two peaks due to the disruption of the structure by loss of hydroxyl ions. The above results of exfoliation can also be achieved by treating the mineral with hydrogen peroxide.
After the exfoliation there is generally an increase in the bulk volume, eight to twelve times its original. The mineral generally attains certain attributes that when combined with other products, the attributes are accentuated. Hence the attributes are due to;-
(1) Unreactivity (2) Sintering temperatures of 1150° - 125O0C
(3) Cation exchange capacity : 50 - 150 m/100g
(4) Specific heat : 0.20 - 0.26 Kcal/Kgk
Thus when the mineral is combined with Portland cement in specific volumetric ratios, the cement can acquire Fire resistance, Light weightedness, Insulation capabilities and Sound deadening attributes. PORTLAND CEMENT
There are two types of cement products manufactured based on the type of constituents used which are:-
1) Ordinary Portland cement (OPC)
2) Pozzolanic Portland cement (PPC)
1. Ordinary Portland Cement (OPC)
This type of cement tends to have two main constituent. These are
a) Gypsum - 5% by weight b) Clinker - ranging from 95% to 75% by weight.
„ By virtue of its strength, the cement is used in building of bridges and buildings that require high strengths.
Pozzolanic Portland Cement (PPC)
This type of cement tends to have three main constituent. These are
a) Gypsum - 5%by weight - b) Clinker - minimum of 60% by weight c) Pozzolanic - maximum of 35% by weight The constituents :-
a) Gypsum
This is a naturally occurring mineral which is used as a retardant in cement manufacture. It generally slows the pace of reaction when the cement is 5 combined with water.
b) Pozzolanic
This is also a natural occurring mineral which is used as an additive in cement. Manufactured according to internally set standards, it should not exceed 35% by weight. It reduces the quantity of alkaline elements and -|_Q heat generation during combination of cement with water. Hence reducing the occurrence of cracks and breakages during cement setting; internally averting weakness in the cement.
c) Clinker
This is an admixture of various minerals formed under intense temperature 15 and pressure and is the main constituent that gives the cement its strength, considering it has binding abilities.
In order for us to prove the fire resistance abilities in cement, we had to conduct experiments by mixing various proportions of vermiculite to 0 pozzolanic, maintaining set proportions of Gypsum and Clinker, in order to maintain the strength and conditions set for cement manufacture. As per the results in table A (see appendix) the higher the percentage of Mica used (above 30%), the greater the strength of the cement is reduced. Hence after increasing the surface area of the proportions mixed to a range of 4500 - 5300 units and also increasing the proportion of Clinker between 70% - 85%, the desired results of strength were achieved within a stipulated 2 day and 7 day period.
In table B (see appendix), the level of alkali metals were analysed and an inverse relationship was observed between the percentile increase of Mica to the prescence of detectable alkali metals. Hence the less the alkali metal available, the less likelihood of salt formation thus reducing the formation of any cracks and weakening of the concrete strength.
The magnesium-oxide level was detected to be higher than the standard of 5%. Normally any value above the standard, should cause an expansivity of 10mm in a bath of water at 1000C for a period of 1 hr, but despite volume of magnesium being above 5% standard, the vermicuiite cement exhibited no significant expansivity (if any, it was within the stipulated standard of below 10mm). As shown in Table C (see appendix), we draw to the tentative conclusion that the magnesium did not participate in any reaction.
FIRE RESISTANCE
Various ratios of vermiculite and modules made were added in the standard cement of Pozzolana Portland cement (PPC). These modules were subjected to temperatures of 9000C and HOO0C for a period of 4 hours and observations were made after every one hour. Thus within a period of two hours, the vermiculite cement exhibited discontinued cracks and change of coloration to a lighter goldish-brown hue. Though feasibility was evident, compaction of the modules were also evident.
But the control module of PPC after a period two hours exhibited cracks and disjointment, both cross sectionally and longitudinally.
Under HOO0C the results were markedly identical to those at 9000C, only that the cross section of the control exhibited continous cracks and total deformity
Hence we can tentatively conclude that vermiculite or mica was the main cause of resistance in the cement to higher temperatures affecting the structure since it was the only additive used in the test. Hence the attribute of fire resistance was proved.
Figure imgf000006_0001
The mineral has a refractive index of 1.6, giving the final product a pearly lustre and goldish brown hue, instead of a dull grayish coloration consistent with all Portland cement. A Block of 9 inch width mortars were made, one control and two with
vermiculite of 10% to 15% in proportion. Heat was then subject to one
face of the block. For a period of lhour, the blocks constituting
vermiculite, the opposite face did not show any rise in temperature, but
5 the Normal Portland -pozzolana cement block the temperature- rose
steadily. Hence indicating transmission of the heat in the p.p.c .
The golden colour was generally visible in the cement constituting
vermiculate by virtue of the golden colour of the vermiculate, which was
/ o determined by the temperature range during its beneficiation

Claims

WHAT IS CLAIMED 1) The cement composition of A + B + C + D = 100% by weight Where; A = Clinker B = Gypsum C = Pozzolana D= Vermiculite 2) A cement composition according to claim (1) wherein; a) D is a percentage range increase of 5% - 30% by weight b) C is a percentage range decrease of 5% - 30% by weight in relation to D c) A is not less than 65% nor more than 80% by weight 3) The cement composition of; A + B + D = 100% Where; A = Clinker B = Gypsum D = Vermiculite 4) A cement composition according to claim (3) Wherein; A = is not less 65% by weight nor more than 90% by weight D = is in the range of 5% to 30% by weight 5) Cement composition as in any one of claims 1 to 4 for use in fire resistance 6) Cement composition as in any one of claims 1 to 4 for use in insulation 7) Cement composition as in any one of claims 1 to 4 for use in sound deadening 8) Cement composition as in any one of claims 1 to 4 for its goldish-brown hue. 9) Cement composition as in any one of claims 1 to 4 for its non-reactivity 10) Cement composition as in any one of claims 1 to 4 for use as a light weight plaster. 11) The process of making the cement composition of any of the preceding claims comprising the following steps: - a) Mixing A, B, C and D in ratios by weight b) Grinding the admixture to attain an SSA range of 4300 to 5300 <* /, units. 12)The process for preparing D for use in making cement composition of any of the preceding claims 1 to 10 comprises of the following steps :- STEPS: a) Extracting the raw material from a suitable explored area using basic mining methods. b) Grinding the raw material to reduce the size (surface Q area) to a range from 16mm to 0.5mm. c) Emplacing the crushed raw material in a furnace and subjecting it to a range of temperatures from 9000C to 2000C. d) The crushed raw material shall exfoliate 8 to 12 times its 5 volume in the process of releasing water as a by-product. e) The crushed raw material can also be exfoliated by subjecting it to a hydrogen peroxide chemical. f) The exfoliation material attains:-
(1) Fireproofing abilities Q
(2) Sound deadening abilities
(3) Non-reactivity
(4) Insulation
(5) Light gold-brownish hue
APENDIX TABLE A.
STRENGTH Isoluble. Residue 2days 7 days S.S.A SETTING TIME
INITIAL FINAL < 35% 10 N/mα 24 Nlrn > 4500 40m 600m MICA Pozzo lana Clinker
23.51 10.68 21.11 4867 210 345 10% 10% 75%
H 15.2 17.73 27.58 45.67 248 318 5% 10% 80%
10.69 16.7 30.48 4506 220 290 10% 5% 80%
12.84 11.72 24.6 4504 257 332 15% 5% 75%
NB. GYPSUM HAS A 5% PROPORTION IN SETS G. H. I. J.
APPENDIX
TABLE B
SET Ha,fi% Mg 0% Aψ3% Si 0χ% Si O3 % K1O % Ca 0 % Fo2O5 % TOTAL Loi
G 1.09 6.7 7.95 31.47 2.54 0.77 42.45 4.52 97 0
H 0.78 5.62 6.45 28.04 3.24 0.68 50.1 3.78 99 0
I 0.5 8.06 5.91 25.39 3.71 0.62 51.1 3.76 99 0
J 0.46 9.49 6.11 26.22 3.01 0.62 50.07 3.97 100 0
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PCT/KE2005/000013 2004-07-27 2005-06-14 Exfoliation Ceased WO2006011690A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KE42204 2004-07-27
KEKE/P/04/00422 2004-07-27

Publications (1)

Publication Number Publication Date
WO2006011690A1 true WO2006011690A1 (en) 2006-02-02

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Application Number Title Priority Date Filing Date
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6309740B1 (en) * 1999-07-20 2001-10-30 W. R. Grace & Co.-Conn. High temperature heat transfer barrier and vapor barrier and methods
AU752467B2 (en) * 1996-04-26 2002-09-19 Building Technologies Australia Pty Limited Improved lightweight prefabricated construction element
RU2197450C1 (en) * 2001-08-01 2003-01-27 Владимиров Владимир Сергеевич Method of porous refractory material production

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU752467B2 (en) * 1996-04-26 2002-09-19 Building Technologies Australia Pty Limited Improved lightweight prefabricated construction element
US6309740B1 (en) * 1999-07-20 2001-10-30 W. R. Grace & Co.-Conn. High temperature heat transfer barrier and vapor barrier and methods
RU2197450C1 (en) * 2001-08-01 2003-01-27 Владимиров Владимир Сергеевич Method of porous refractory material production

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