AU2005244022B2 - Molasses treatment for the "molassperse" surfactant production for concrete plasticizers (water reducing admixtures) and cement clinker grinding additives applications - Google Patents
Molasses treatment for the "molassperse" surfactant production for concrete plasticizers (water reducing admixtures) and cement clinker grinding additives applications Download PDFInfo
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- AU2005244022B2 AU2005244022B2 AU2005244022A AU2005244022A AU2005244022B2 AU 2005244022 B2 AU2005244022 B2 AU 2005244022B2 AU 2005244022 A AU2005244022 A AU 2005244022A AU 2005244022 A AU2005244022 A AU 2005244022A AU 2005244022 B2 AU2005244022 B2 AU 2005244022B2
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Description
01/12 2008 MON 15:22 FAX Snmoorenburg Plnl -44 IP AUSTRALIA Q006/032 00 o MOLASSES TREATMENT FOR THE "MOLASSPERSE"
SURFACTANT
N PRODUCTION FOR CONCRETE PLASTICIZERS (WATER REDUCING ADMIXTURES) AND CEMENT CLINKER GRINDING ADDITIVES 0
APPLICATION
1. Background The present invention relates to a method of treating molasses to provide a csurfactant. The treated molasses of the method of the present invention is osuitable for use as an additive to plasticise concrete and as a cement clinker grinding additive.
In this specification where a document, act or item of knowledge is referred o to or discussed, this reference or discussion is not an admission that the document, act or item of knowledge or any combination thereof was at the priority date publicly available, known to the public, part of the common general knowledge or known to be relevant to an attempt to solve any problem with which this specification is concerned.
1.1. Concrete admixtures Molasses (see molasses typical analysis in Table 1) is traditionally used as a retarding agent in concrete admixtures 11,4]. it allows increased setting times and as a result slightly reduced water consumption in concrete mixes.
Chinese patent CN1067231A titled: "PROCESS FOR PREPARING SETTING RETARDANT TYPE-HIGH- EARLY STRENGTH
WATER-REDUCING
AGENT AND PRODUCTS THEREOF" describes a typical concrete admixture of the prior art that includes molasses. As noted in the English language abstract for CNI 067231; This invented setting-retardant type high-early strength water reducing agent is prepared as follows: after molasses is diluted to 1.22-1.25 Baum'e degrees and heated to 70-80 0 C, lime of 1-2 wt. of that of diluted molasses is added for reaction to make a portion of sugar react with calcium oxide to form soluble calcium sugar which can produce optimum effect of water reduction. The result is that the product after reaction still retains a portion of sugar component so that the said product not only possesses the effect of water reduction, but also that of setting retarding, meanwhile, the addition of anhydrous sodium sulphate in a certain proportion makes it have the effect of high-early strength.
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:23 FAX Smoorenburg Pinl IP AUSTRALIA Q007/032 00 2
C
It is known that sugar (molasses sugar) added to the concrete mix Simmediately reacts with calcium oxide (which is produced in the process of cement hydration) and forms "soluble calcium sugar".
The principal difference between the method taught in CN1067231, and the traditional use of molasses by direct addition to a concrete mix, is that a ¢C relatively small proportion of the molasses sugar is converted to "calcium sugar".
SThe disadvantages of the method of CN1067231 are: from a position of molasses modification: the ingredients of concrete mn mix are practically unchanged; just the process of formation of a small quantity of "calcium sugar" is slightly intensified "calcium sugar" starts to precipitate at temperatures lower than 0 C misbalancing the hardening of concrete sodium sulfate is used for reduction of the typically strong molasses sugar retardation effect.
Another relevant publication in the field of this invention is Korean patent KR3037597A titled: CONCRETE ADMIXTURES CONTAINING MOLASSES FERMENTATION BYPRODUCTS which discloses a traditional method used in the Soviet Union "Molasses fermentation byproducts" are essentially spent waste liquor created by fermentation of molasses sugars and extraction of fermentation products (mainly alcohol and yeast) from the "mother liquor".
This molasses spent waste liquor in comparison with original molasses contains a relatively small quantity of the byproducts from the sugar fermentation process, mainly in the form of different organic acids. These acids slightly increase the surfactant properties of molasses spent waste liquor in comparison with original molasses. The main disadvantage (problem) of the "molasses fermentation byproducts" (molasses spent waste liquor) is their still lower surfactant properties in comparison with traditional water reducing agents such as lignosulphonates. Also the composition of "molasses fermentation byproducts" is too variables. Therefore these byproducts are seldom used in concrete admixtures application.
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:23 FAX Smoorenburg Pinl 44 IP AUSTRALIA Q008/032 00 3 1.2. Cement clinker grinding additives
U
STraditionally molasses is not used as a grinding additive because of its low dispersant properties (low surfactant properties). However Chinese patent CN1089245A titled: METHOD FOR USING TALC MOLASSES AS CEMENT GRINDING AID suggests the use of molasses for this application in combination with talc in approximate proportions, 1:10. It seems that in this composition molasses is used as a well known adhesive agent. In the process of grinding, talc is a much softer material than cement clinker and gets ground significantly thinner than clinker. The very fine particles of talc in combination with molasses (as adhesive agent) hypothetically can envelope cement particles averting them from (against) aggregation.
This method is not widely used because of its low effectiveness. The main disadvantage of this method is that molasses is not used as a surfactantdispersant.
2. Idea of the Suggested Molasses Treatment Accordingly, there is a need for deep modification of the molasses ingredients, converting them to the effective surfactants with improved plasticizer (water reducing) and dispersant properties.
3. Description of the Treatment (Invention) 3.1 Essence of the treatment The present invention relates to the treatment of molasses in and acid environment, and subsequently in an alkali environment at temperatures higher than ambient.
This means the ingredients of the molasses are exposed to acid and alkali hydrolysis.
3.2 Regimes and parameters of the treatment 3.2.1 Inorganic and organic acids can be used for acidification of molasses up to pH 0.8.
3.2.2 Inorganic and organic alkalis can be used for alkalization of molasses up to 3.2.3 The temperature of the acid and alkali treatments can be 50-200°C at ambient, positive and negative pressure.
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:23 FAX Smoorenburg Pini IP AUSTRALIA 1009/032 00 0 4
O
c 3.2.4 Catalysts of acid and alkali hydrolysis (oxidation) can be used for the U treatment.
3.2.5 Solids content of molasses can be 5.0-90.0%.
3.2.6 Typically, the time of the treatment is as follows: acid treatment 10min-24 hours C alkali treatment 10min-24 hours S3.2.7 After both the acid and alkali treatment, the pH of the molasses can be adjusted to the required levels.
S4. Treatment effect on molasses properties Without wishing to be bound by theory it is believe that the present invention provides the following chemical transformations.
4.1 Acid treatment according to the present invention provides: conversion of polysaccharides to monosaccharides (reducing sugars); conversion of the part of monosaccharides to aldonic acids; and decomposition of proteins to aminocarbonic acids with a relatively high quantity of carboxyl and amino groups.
4.2. Alkali treatment according to the present invention provides: conversion of monosaccharides (reducing sugars) to saccharinic acids and their salts; conversion of aldonic acids to their salts; decomposition of the residuary proteins to aminocarbonic acids; converting of aminocarbonic acids to their salts; and converting (saponification) of wax ethers to the soluble soaps.
5. Properties of the components of the treated molasses 5.1 The salts of saccharinic and aldonic acids are quite strong anionic surfactants with high dispersion properties.
The salts of aminocarbonic acids and wax soaps are effective wetting agents and detergents 5.2 The method of the present invention will produce a complex mixture of surfactants in which there is; domination by saccharinic and aldonic acids salts, and COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:23 FAX Smoorenburg Pini 4 IP AUSTRALIA Q010/032 00 a small proportion of aminocarbonic acids salts and wax soaps 5.3 The complex mixture of surfactants provides a relatively high effectiveness of the treated molasses as a concrete plasticizer (water reducing admixtures) and O clinker grinding additive.
6. Application tests of the treated molasses 6.1 The modified molasses was tested as a plasicizer in cement mortars in 0 comparison with the best general European softwood Na and Ca lignosulphonates.
In The test results are shown in Example 2.
6.2 The modified molasses was also tested as a clinker grinding additive.
The test results are shown in Example 3.
7. Conclusion The results of the tests show that the molasses modified according to the method of the present invention can be effectively used as concrete plasticizers (water reducing admixtures) and cement clinker grinding additives.
The word 'comprising' and forms of the word 'comprising' as used in this description and in the claims does not limit the invention claimed to exclude any variants or additions.
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:23 FAX Smoorenburg Pini IP AUSTRALIA @011/032 Table 1: Mill Solids by Drying Total Sugar Sucrose Reducing Sugars Unfermentable Sugars Crude Protein Ash Major Elements: Potassium 3.5-5.5 Calcium 0.5-1.2 Sodium 0.05-0.10 Trace Elements: Iron ppm Max Copper ppm Max Zinc ppm Max Lead ppm Max Arsenic less than ppm Cadmium less than ppm Molasses Typical Analysis 70-80 40-65 30-40 (Jackson Gillis method) 10-20 (Lane Eynon method) 2-5 (Kjeldalh N) 10-15 (double sulphation) 250 0.02 COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:23 FAX Smoorenburg Plni 4- IP AUSTRALIA @012/032 00 7 Examples SThe invention will be further described with reference to the following nonlimiting examples: O Example 1: Description of the concrete plasticizers and grinding additives production Five samples of molasses labelled Molassperse P-1, Molassperse P-2, SMolassperse P-3, Molassperse G-1 and Molassperse G-2 were modified by the application of an acid environment, and subsequently, an alkali Senvironment. The parameters for treatment according to step and step are set out in Tables 2 and 3.
Production of concrete plasticizers: Molassperse P-1, Molassperse P-2 and Molassperse P-3 Table 2: Parameters for Concrete Plasticizers Production Product Acid treatment Alkali treatment name Molassperse P-1 pH Temp Solids Time pH Temp Solids Time 0.8 500 62% 24 hrs 14 50° 62% 24 hrs Molassperse 4.1 2000 54% 10min 12 2000 56% P-2 s Molassperse 2.9 900 58% 7 hrs 13 900 61% 7 hrs P-3 Plasticizer Molassperse P-3 has shown better results than Molassperse P- 1 and Molassperse P-3 for concrete application (See Example 2).
Production of cement grinding additives: Molassperse G-1 and Molassperse G-2 Table 3: Parameters for Cement Grinding Additives Production Product Acid treatment Alkali treatment name pH Temp Solids Time pH Temp Solids Time Molassperse 2.1 850 69% 8 hrs 13 850 71% 24 hrs G-1 Molassperse 3.5 950 71% 7 hrs 12 950 75% 9 hrs G-2 Cement Grinding Additive Molassperse G-2 has shown better results than Molassperse G-1 for cement grinding application (See Example 3).
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:24 FAX Smoorenburg Pini IP AUSTRALIA @013/032 00 0 8
O
C Example 2: Investigations of "Molassperse" Modified Molasses for Concrete SApplications Modifications Molassperse P-1, Molassperse P-2 and Molassperse P-3 were tested to investigate their performance as concrete plasticisers.
C Testing in cement mortars O The best general European softwood Na and Ca lignosulphonates were used as control samples.
IConsumption of the Molassperse P-I, Molassperse P-2 and Molassperse P-3 and lignosulphonates were 0.1, 0.2 and 0.3% of cement mass.
Blue Circle Southern Cement was used for making the cement mortars.
Two river sands (coarse and fine) were used in the tests (ratio 1:1).
Water/Cement ratio for all cement mortars was constant 0.55.
Ratio Cement: Sand Water was 1 3: 0.55.
Fluidity of cement mortars was determined with Flow Table.
Air entrainment was determined by a volumetric method.
Cement mortar ISO prisms 40x40x160mm were made for compressive strength determination.
The results of the tests have shown in Table 4.
Discussion NA and CA Lignosulphonates (control) are typical middle range water reducers and retarders.
Cement mortars with Molassperse P-l, Molassperse P-2 and Molassperse P-3 in comparison with NA Lignosulphonate and CA Lignosulphonate have a higher fluidity at low consumption 0.1%.
At the middle consumption 0,2% and high consumption the mortar fluidity is similar for the molasses modifications and lignosulphonates.
Compressive strength of all cement mortars with the molasses modifications is a slightly higher in comparison with the mortars with lignosulphonates. This can be explained by a higher air entrainment of lignosulphonates.
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:24 FAX Snoorenburg Pint -444- IP AUSTRALIA lQj014/032 9 Conclusions Molassperse P-1, Molassperse P-2 and Molassperse P-3 are compatible with the best general European softwood Na and Ca lignosulphonates Molassperse P-1, Molassperse P-2 and Molassperse P-3 can be characterized as middle range water reducers with a low air entrainment.
Table 4: Comparison tests of molasses modifications Molassperse P-1, Molassperse P-2 and Molassperse P-3 with NA and CA Lignosuiphonates N Name of Fluidity of Air Compressive strength admixture cement paste, entertainment MPa mm% 60 1Iday 7 2 mn j___days days 1 Plain molasses 155 150 2 21.4 31.7 40.9 (consumption 0.2% __of cement mass) Admixture consumption of cement mass 0. 1 2 Molassperse P- T8-2 158 1 2 20.3 32.1 43.3 3 MolassperseP-2 182 160 2 21.3 33.2 44.1 4 Molassperse P-3 1831K 2 21.4 33.5 44.4 NA 178 148 1 3 21.5 29.4 40.4 Li 6a CA o lh 179 162 3 20.5 [30.1 4.
Admixture cosum tion of cement mass 0.2% Molassi erse Pi 181 162 2 20.2 33.9 45.0 7 Molassperse P-2 186 163 2 20.6 34.3 45.1 8 _Molassperse P-3 188 169 2 20.9 34.7 45.3 1 A-8-6 164 4 20.3 32.6 43.2 1 CA188 168 4 19.6 r32. 43.9 Admixture consumption of cement mass 0.3% 11 .Molassperse P-i 193 162 3 20.3 34.1 44.9 12 Molassperse P-2 190 160 3 20.1 33.1 43.5 13 Molassperse P-3 198 168 3 20.5 33.6 43.9 1 NA200 170 7 19.5 31.2 41.4 -Lignosulphonate 1 CA[-1 95- 168 7 19.3 31.5 41.9 Lignosulphonate COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:24 FAX Smoorenburg Pini IP AUSTRALIA I015/032 00 CN Example 3: Investigations of "Molassperse" Modified Molasses for Cement SClinker Grinding Applications Modifications Molassperse G-1 and Molassperse G-2 were tested for their suitability as clinker grinding additives.
C-i Testing in laboratory cement grinding mill O Laboratory grinding mill with 2700 revolutions per hour and standard equipment were used.
ICement clinker was ground with gypsum at a ratio of 95:5.
The results of the tests are shown in Table Table 5: Clinker grinding tests of molasses modifications Molassperse G-1, and Molassperse G-2 Grinding additive name Dosage range, of clinker Output at same cement mass (solid/solid) fineness Blank 100 Molassperse G-1 0.02-0.04 106-111 0.06-0.08 109-116 Molassperse G-2 0.02-0.04 108-114 0.06-0.08 112-121 Conclusion Both Molassperse G-l and Molassperse G-2 can be used as effective cement clinker grinding additives.
COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:24 FAX Smoorenburg Plni IP AUSTRALIA 1016/032 00 l Reference Literature 1. B.J.Addis, D.E.Davis Q FULTON'S CONCRETE TECHNOLOGY Portland Cement Institute Midrand, South Africa, 1986 2. WANG RUBIN. QU ZHENBIN PROCESS FOR PREPARING SETTING RETARDANT TYPE-HIGH- EARLY STRENGTH WATER-REDUCING AGENT AND PRODUCTS THEREOF INST. OF LOW-TEMP. ARCHITECTURAL SCIENCE, HEILONGJIANG PROV. China C1 Patent: CN 1067231 A 3. Schoenrock, Karlheinz W. Ogden, UT Hsieh, Chia-Lung; Ogden, UT Rounds, Hugh Ogden, UT Continuous process for the recovery of sugar from molasses Patent: US3997357 4. Admixtures for Concrete Soviet Union's State Standard; 24211-91 Moscow, 1991 5. KIM SEUNG JIN, PARK JEE WON; Republic of Korea CONCRETE ADMIXTURES CONTAINING MOLASSES FERMENTATION
BYPRODUCTS
Patent: KR3037597A 6. BAI XIANMING, SHAO ZHONGJUN; China METHOD FOR USING TALK MOLASSES AS CEMENT GRINDIG AID Patent: CN 1089245A 7. A.M.Schwartz, J.W.Perry SURFACE ACTIVE AGENTS THEIR CHEMISTRY AND TECHNOLOGY New York London 1949, 545 p COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01
Claims (8)
1. A method of treating molasses to provide a surfactant suitable for use as a water reducing admixture to plasticize concrete and as a cement clinker grinding additive, the method comprising the steps of treating the molasses, S(a) in an acid environment, Sand subsequently in an alkali environment, I wherein both steps are carried out at a temperature higher than ambient.
2. A method as claimed in claim 1 wherein the acid environment comprises inorganic and organic acids for acidification of the molasses up to a pH of about 0.8.
3. A method as claimed in claim 1 or 2 wherein the alkali environment comprises inorganic and organic alkalis for alkalization of the molasses up to a pH of about 14.0.
4. A method as claimed in any one of claims 1 to 3 wherein the temperature of the acid and alkali treatment is about 50 to 200°C at one or a combination of ambient, positive and negative pressure. A method as claimed in any one of claims 1 to 4 wherein catalysts comprising catalysts of acid and alkali hydrolysis are used in the treatment.
6. A method as claimed in any one of claims 1 to 5 wherein a solids content of the molasses comprises about 5.0% to about
7. A method as claimed in any one of claims 1 to 6 further comprising the steps of: performing the treatment in an acid environment for a time period in the range of about 10 minutes to about 24 hours; COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01 01/12 2008 MON 15:24 FAX Smoorenburg Pinl IP AUSTRALIA R018/032 0 13 0 N performing the treatment in a alkali environment for a time period in the U range of about 10 minutes to about 24 hours.
8. A method as claimed in any one of claims 1 to 7 further comprising the step of: C after step adjusting the pH of the molasses to a predetermined value 0using inorganic and organic acids and alkalis. n 9. A surfactant suitable for use as a water reducing admixture to plasticize concrete and as a cement clinker grinding additive produced in accordance with c the method as claimed in any one of claims 1 to 8. A method according to claim 1 and substantially as described herein with reference to the examples.
11. A surfactant according to claim 9 and substantially as described herein with reference to the examples. COMS ID No: ARCS-215416 Received by IP Australia: Time 15:26 Date 2008-12-01
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2005244022A AU2005244022B2 (en) | 2004-05-14 | 2005-04-28 | Molasses treatment for the "molassperse" surfactant production for concrete plasticizers (water reducing admixtures) and cement clinker grinding additives applications |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2004902556 | 2004-05-14 | ||
| AU2004902556A AU2004902556A0 (en) | 2004-05-14 | Molasses treatment for the "Molassperse" surfactant production for concrete plasticizers (water reducing admixtures) and cement clinker grinding additives | |
| PCT/AU2005/000629 WO2005110941A1 (en) | 2004-05-14 | 2005-04-28 | Molasses treatment for the “molassperse” surfactant production for concrete plasticizers (water reducing admixtures) and cement clinker grinding additives applications |
| AU2005244022A AU2005244022B2 (en) | 2004-05-14 | 2005-04-28 | Molasses treatment for the "molassperse" surfactant production for concrete plasticizers (water reducing admixtures) and cement clinker grinding additives applications |
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| AU2007203425 Addition | 2005-04-28 |
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| AU2005244022B2 true AU2005244022B2 (en) | 2009-01-08 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB939545A (en) * | 1960-10-12 | 1963-10-16 | Ile D Etudes Et De Rech S Phar | Process for the preparation of food products from sugar beet vinasses |
| SU983254A1 (en) * | 1981-07-29 | 1982-12-23 | Филиал Северо-Кавказского Государственного Научно-Исследовательского И Проектного Института Нефтяной Промышленности | Composition for cementing high-temperature oil and gas wells |
-
2005
- 2005-04-28 AU AU2005244022A patent/AU2005244022B2/en not_active Ceased
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB939545A (en) * | 1960-10-12 | 1963-10-16 | Ile D Etudes Et De Rech S Phar | Process for the preparation of food products from sugar beet vinasses |
| SU983254A1 (en) * | 1981-07-29 | 1982-12-23 | Филиал Северо-Кавказского Государственного Научно-Исследовательского И Проектного Института Нефтяной Промышленности | Composition for cementing high-temperature oil and gas wells |
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| AU2005244022A1 (en) | 2005-11-24 |
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