CA2058440C - Use of mixed hydroxy ethers as aids for drying solids materials - Google Patents

Use of mixed hydroxy ethers as aids for drying solids materials Download PDF

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Publication number
CA2058440C
CA2058440C CA002058440A CA2058440A CA2058440C CA 2058440 C CA2058440 C CA 2058440C CA 002058440 A CA002058440 A CA 002058440A CA 2058440 A CA2058440 A CA 2058440A CA 2058440 C CA2058440 C CA 2058440C
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Prior art keywords
solids
water
carbon atoms
surfactant
alkyl group
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Expired - Fee Related
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CA002058440A
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French (fr)
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CA2058440A1 (en
Inventor
Rita Koester
Maria Liphard
Gilbert Schenker
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00Drying solid materials or objects by processes not involving the application of heat
    • F26B5/005Drying solid materials or objects by processes not involving the application of heat by dipping them into or mixing them with a chemical liquid, e.g. organic; chemical, e.g. organic, dewatering aids

Abstract

The use of mixed hydroxyethers of the general formula I
R10-(CH2CH20)x-CH2-CH(OH)R2 (I) in which R1 denotes an alkyl group having 1 to 10 carbon atoms, R2 denotes an alkyl group having 8 to 20 carbon atoms, and x denotes a number in range from 1 to 20, as auxiliaries for the dehydration of water-containing finely divided solids, gives solids having a low water content without foaming in the water separated therefrom.

Description

a os ~ ~~yo Use of mixed hydroxyethers as auxiliaries for the dehydration of solids The invention relates to the use of mixed hydroxyethers of the general formula I
R10-(CH2CH20)x-CH2-CH(OH)R2 (I) in which R1 denotes an alkyl group having 1 to 10 carbon atoms, R2 denotes an alkyl group having 8 to 20 carbon atoms and x denotes a number in the range from 1 to 20 as auxilaries for the dehydration of water-containing finely divided solids.
In many branches of industry, e.g. in mining or in sewage treatment plants, large amounts of finely divided solids having high water contents, which have to be dehydrated before further processing of the solids or their disposal, are formed. Thus, for example, the dehydration of water-containing coal or coke is a central process in the processing of fuels based on coal.
The maximum allowable values for the water content of these materials demanded by the market can often be adhered to only with difficulty, since, for example, the coal supplied is produced in very fine particles due to the extensive mechanization of the underground coal mining. Currently, about 38% of the run-of-mine coal is fines having a particle diameter in the range from 0.5 to lOmm; a further 14% is duff having a particle diameter below that.

-z- ~o~~y~a It is known to use surfactants as dehydration auxiliaries for the dehydration of water-containing finely divided solids, in particular coals, which make it possible to reduce the residual moisture of fines and duff. This is explained by the property of the surfactant to reduce the surface tension and the capillary pressure of water in the material to be extracted. At the same time, this reduces the adhesive energy which must be supplied to remove the surface water. This leads to improved dehydration, when surfactants are used, while the amount of energy remains unchanged.
Dialkyl sulfosuccinates (USD- 2,266,954) and nonionic surfactants of the type of alkylphenol polyglycol ethers [Erzmetall 30, 292 (1977)] have been described as surfactant-based dehydrating auxiliaries of the above mentioned types. However, these surfactants have the disadvantage of showing excessive foaming, which leads to considerable problems in the processing plants, in particular in the recirculation of the water which is usually employed.
The invention is based on the finding that nonionic surfactants of the general formula I increase the dehydration rate without foaming and reduce the residual moisture of the dehydrated solids when employed in water/solid systems.
The group R1 of the mixed hydroxyethers to be used according to the invention of the general formula I is a straight-chain or branched or cyclic alkyl group having 1 to 10 carbon atoms, for example a methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl or decyl group. Alkyl groups of the above list having 1 to 4 carbon atoms are preferred. The group RZ in the general formula I is an alkyl group having 8 to 20 carbon atoms, for example an octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, nonadecyl or eicosyl group, in particular an :~ ;.

~058'1%D
alkyl group form the above list having 12 to 16 carbon atoms, straight-chain R2 radicals being particularly preferred. x in the general formula I is a number in the range form 1 to 20, the range from 2 to 15 being preferred.
In accordance with their use according to the invention, the mixed hydroxyethers of the general formula I have to be water-soluble. It may occur that the water solubility is not quite sufficient, if the mixed hydroxyethers of the general formula I have low values of x and long-chain radicals R1 and/or R2 where the chain lengths are within the abovementioned limits; however, the required water solubility can be obtained by increasing the value for x within the abovementioned range.
The mixed hydroxyethers of the general formula I are described in DE-A 3,723,323; they can be obtained by reacting,ethoxylated alcohols of the general formula II
R10(CH2CH20)x-OH (II) with epoxides of alpha-olefins of the formula III
R2 - CH - CH (III) ~ 2 ~O
in the presence of catalysts, in which Rl, R2 and x are as defined above.
In accordance with their preparation and the starting materials used, which are in most cases employed in the form of technical grade mixtures, the mixed hydroxyethers to be used according to the invention of the general formula I can also be present as technical grade mixtures.
In accordance with an advantageous embodiment of the invention, the mixed hydroxyethers of the general formula I are used in an amount of 0.5 to 10, in particular 3 to 8, kg per m3 of the water to be removed from the finely t .~., ~~~~44~

divided solids.
As mentioned at the beginning, the mixed hydroxyethers of the general formula I are suitable in particular for the dehydration of water-containing finely divided coal or coke; however, they can also be used in the dehydration of other water/solid systems, for example for beneficiated ores or gangue materials in ore mining, sewage sludges and the like. In this respect, a further advantage of the surfactants to be used according to the invention of the general formula I is that they are compatible with surfactants of different composition, which may be present, for example with dialkyl sulfo-succinates such as di-noctyl sulfosuccinates or polyacry-lamides, which were added to the solids to be dehydrated in previous processing steps.
The invention is illustrated in more detail below by way of preferred embodiments.
In the examples, washed fines having the following analytical data were used:
6.8 % by weight of water 3.7 % by weight of ash (wf; calculated with respect to water-free coal) 27.2 % of volatile components (waf; calculated with respect to water- and ash-free coal) Screen analysis of the fines gave the following values:
- 0.5 mm 1.5 %
0.5 - 2.0 mm 23.1 %
2.0 - 6.3 mm 51.5 %
+ 6.3 mm 23.9 %.
The efficiency of the mixed hydroxyethers of the general formula I in the dehydration was determined by treating the fines with aqueous solutions of the mixed hydroxy-- ~0~~~~~
ethers of defined concentration and dehydrating them under defined conditions; the residual moisture obtained with and without the addition of surfactant was determined according to DIN 51718 by drying at 106°C and weighing.
The present examples are laboratory tests in which the amounts of surfactants used in kg are based on 1000 kg each of the solids to be dehydrated (calculated as water-free solids). In practice, the necessary amounts of surfactants will be less than the ones used in the examples; moreover, the necessary amounts of surfactants used depend on the amount of the water to be removed from the solids, when the solids are dehydrated in practice.
The structure of the mixed hydroxyethers tested of the general formula I and their abbreviations used below can be seen from Table 1.
The term "surfactant" used here and hereinafter refers to the mixed hydroxyethers of the general formula I.
Table 1 Mixed hydroxyethers of the formula I
R10- ( CHZCHzO ) =-CHz-CH ( OH )-Rz Surfactant Rl Rz x CH3 n-ClzHzs 2 B CH3 n-ClzHzs 4 C n-C~H9 n-ClzHzs 2 D n-C4H9 n-C16H33 2 Example 1 Dehydration in a pressure filter 50 g of coal were added to 400 ml of distilled water or surfactant solutions in distilled water and were filtered after being exposed for 60 seconds. This was done by using a pressure filter which consisted of a sealed neutral filter which was filled with the material to be dehydrated. The dehydration was carried out by subjecting the filter to a pressure of 3 bar. The dehydration time was 30 seconds. The filter material used was a filter fabric having a mesh size of 0.2 mm.
The surfactants tested, the surfactant concentration of the solution with which the coal was treated, the amount of surfactant calculated per 1000 kg of coal and the residual moisture determined are summarized in Table 2.
Table 2 Pressure filter test Surfactant Surfactant Amount of sur- Residual concentra- factant (kg) moisture tion per 1000 kg (% by wt.) (g/1) of coal A 1.0 g g,g 8 1.0 g g,5 C 1.0 g ~,2 D 1.0 g g,9 without the addition of surf actant - - 11. 6 As can be seen from Table 2, the residual moisture of the dehydrated coal is substantially reduced, when the surfactants to be used according to the invention are used compared with that without the addition of surfactant.
Example 2 Dehydration in a centrifuge In this example, a bucket-type centrifuge was used with which at revolutions of 300 to 3,400 per minute - ' - Q~~4~
centrifugal characteristic values of 15 to 2000 can be obtained. Perforated plates having sieve openings of 0.4 x 4.0 mm were used as sieve plate for the centrifuge. The surfactants used as filtering aids (mixed hydroxyethers of the general formula I) were dissolved in distilled water in concentrations of 0.1 g/1 and 1.0 g/1. To carry out the tests, 400 ml each of the surfactant-containing solutions were poured into a glass vessel. 25 g of coal were dipped into each of these solutions. The wetting time was in each case 60 seconds. This was followed by predehydration of the samples at a constant dripping time of 180 seconds. The values obtained in the predehydration of the samples, the surfactant concentration and the amount of surfactant calculated per 1000 kg of coal are summarized in Table 3.
To dehydrate the predehydrated samples in the bucket-type centrifuge, centrifugal characteristic values of 43.2, 111 and 389 (corresponding to revolutions of 500, 800 and 1500 per minute) were established. The dehydration time was 30 seconds. The results obtained are summarized in Table 4.
In a second test series, a surfactant concentration of 1.0 g/1 at a centrifugal characteristic value of 111 (corresponding to revolutions of 800 per minute) was tested at dehydration times of 5, 10 and 30 seconds. The results obtained are summarized in Table 5.
As can be seen from Tables 3 to 5, all surfactants tested have a very good effect on the dehydration. Even in the predehydration (Table 3), the efficiency of the surfactants compared with a sample without the addition of surfactant became obvious. While the untreated sample had a residual moisture of 43.6 % after a dripping time of 180 seconds, this value could be reduced down to 26.5 % by means of the surfactants used according to the invention. This corresponds to a relative reduction in residual moisture by 39 %.

-As can be seen from Tables 4 and 5, the residual moisture could be reduced not only by increasing the centrifugal characteristic value but also by adding the surfactants to be used according to the invention.
A surfactant solution of 0.1 g/1 made it possible to reduce the residual moisture to 4.0 % by weight at a centrifugal characteristic value of 111. A surfactant solution of 1.0 g/1 decreased the residual moisture down to 3.0 %. These values can also be reached with short dehydration times.
Table 3 Centrifuge test Results of the predehydration Surfactant Surfactant Amount of Residual concentra- surfactant moisture tion (g/1) (kg) per (% by wt.) 1000 kg of coal A 10 16 26.5 H 1.0 16 30.3 C 10 16 30.1 1.0 16 34.8 without surfactant - - 43.6 A 0.1 1.6 37.5 0.1 1.6 31.9 _ g _ Table 4 Centr ifugal dehydration Revolutions per minute 500 800 1500 500 800 1500 S Centrifugal characteristic value 43.2 111 389 43.2 111 389 Surfactant concentra-IO tion (g/1) 0.1 0.1 0.1 1.0 1.0 1.0 Surfactant Residual moisture A 5.7 5.3 3.5 3.6 3.1 2.6 B 4.5 4.0 3.7 3.? 3.0 2.5 C 5.8 4.7 3.1 6.0 4.8 3.3 15 D 6.9 5.9 4.1 7.0 5.2 3.7 without addit-ion of surfac taut 7.8 6.1 3.9 7.8 6.1 3.9 Table 5 20 Results at a centrifugal racteristic value 111 cha of Dehydration times) 5 10 30 Surfactant Residual moisture (% by wt.) 25 A 3.6 3.2 3.1 3.8 3.5 3.0 C 5.5 5.1 4.8 D 5.7 5.5 5.2 without surfactant 6.8 6.7 6.1 ~

Claims (13)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE PROPERTY
OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. The process of dehydrating water-containing finely divided solids, comprising contacting said solids with a mixed hydroxyether of formula I
R10-(CH2CH20)x-CH2-CH(OH)R2 (I) wherein R1 represents an alkyl group having 1 to 10 carbon atoms R2 represents an alkyl group having 8 to 20 carbon atoms, and x represents a number from about 1 to about 20.
2. The process as in claim 1 wherein R1 represents an alkyl group having 1 to 4 carbon atoms.
3. The process as in claim 1 wherein R2 represents an alkyl group having 12 to 16 carbon atoms.
4. The process as in claim 1 wherein x represents a number from about 2 to about 15.
5. The process as in claim 1 wherein said mixed hydroxyether is present in an amount of from about 0.5 to about 10 kg per m3 of the water to be removed from said solids.
6. The process as in claim 1 wherein said mixed hydroxyether is present in an amount of from about 3 to about 8 kg per m3 of the water to be removed from said solids.
7. The process as in claim 1 wherein said solids are selected from the group consisting of finely divided coal and coke.
8. The process as in claim 1 wherein said solids are selected from the group consisting of beneficiated ores and gangue materials.
9. The process as in claim 1 wherein said solids are selected from the group consisting of sewage sludges.
10. The process as in claim 1 wherein said mixed hydroxyether is present in an aqueous system.
11. The process as in claim 1 including filtering said solids after contacting said solids with said mixed hydroxyether.
12. The process as in claim 11 wherein said filtering step is conducted under pressure.
13. The process as in claim 1 including centrifuging said solids after contacting said solids with said mixed hydroxyether.
CA002058440A 1989-06-05 1990-05-28 Use of mixed hydroxy ethers as aids for drying solids materials Expired - Fee Related CA2058440C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DEP3918274.6 1989-06-05
DE3918274A DE3918274A1 (en) 1989-06-05 1989-06-05 USE OF HYDROXYMISCHETHERS AS A SOLVENT FOR SOLIDS HEATING
PCT/EP1990/000851 WO1990015295A1 (en) 1989-06-05 1990-05-28 Used of mixed hydroxy ethers as aids for drying solids materials

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CA2058440A1 CA2058440A1 (en) 1990-12-06
CA2058440C true CA2058440C (en) 2001-03-27

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EP (1) EP0475969B1 (en)
AU (1) AU631647B2 (en)
BR (1) BR9007418A (en)
CA (1) CA2058440C (en)
DE (2) DE3918274A1 (en)
NO (1) NO178838C (en)
PT (1) PT94261A (en)
TR (1) TR24599A (en)
WO (1) WO1990015295A1 (en)
ZA (1) ZA904275B (en)

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DE4019174A1 (en) * 1990-06-15 1992-01-02 Henkel Kgaa EXTRACTS FOR FILTRATION AND / OR DEHUMIDIFICATION OF MINERAL AND CARBON SUSPENSIONS
DE4218050A1 (en) * 1992-06-01 1993-12-02 Henkel Kgaa Process for dewatering fine particulate suspensions
DE4218074A1 (en) * 1992-06-01 1993-12-02 Henkel Kgaa Process for dewatering fine particulate suspensions
US5670056A (en) * 1995-04-17 1997-09-23 Virginia Tech Intellectual Properties, Inc. Chemical-mechanical dewatering process
US6526675B1 (en) 1999-06-07 2003-03-04 Roe-Hoan Yoon Methods of using natural products as dewatering aids for fine particles
US6855260B1 (en) 1999-06-07 2005-02-15 Roe-Hoan Yoon Methods of enhancing fine particle dewatering
US6375853B1 (en) * 2000-03-17 2002-04-23 Roe-Hoan Yoon Methods of using modified natural products as dewatering aids for fine particles
US6799682B1 (en) 2000-05-16 2004-10-05 Roe-Hoan Yoon Method of increasing flotation rate
AU2000277395B2 (en) 2000-09-28 2005-11-10 Roe-Hoan Yoon Methods of using natural products as dewatering aids for fine particles
JP4022595B2 (en) * 2004-10-26 2007-12-19 コニカミノルタオプト株式会社 Imaging device
AP2447A (en) * 2005-02-04 2012-08-31 Mineral And Coal Technologies Inc Improving the seperation of diamond from gangue minerals

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US2266954A (en) * 1939-08-26 1941-12-23 American Cyanamid Co Wetting agent in settling of oe pulps
US2975123A (en) * 1957-11-04 1961-03-14 Int Nickel Co Dewatering metal ore concentrates
US3194758A (en) * 1961-05-24 1965-07-13 Petrolite Corp Method of agglomerating finely divided solids in an aqueous medium
US3327402A (en) * 1964-12-28 1967-06-27 Shell Oil Co Solvent drying of coal fines
LU47975A1 (en) * 1965-02-12 1966-08-12
US4014104A (en) * 1975-06-23 1977-03-29 Continental Oil Company Drying of lignite using nonaqueous solvents
JPS5613099A (en) * 1979-07-10 1981-02-07 Nichireki Chem Ind Co Ltd Treating method of sludge
JPS5784708A (en) * 1980-11-18 1982-05-27 Kao Corp Improving agent for filtration/dehydration property of metal hydroxide slurry
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DE3723323C2 (en) * 1987-07-15 1998-03-12 Henkel Kgaa Hydroxy mixed ethers, processes for their preparation and their use
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US4990264A (en) * 1989-10-13 1991-02-05 Sherex Chemical Company, Inc. Ore dewatering process and compositions therefor

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TR24599A (en) 1992-01-01
EP0475969B1 (en) 1994-04-27
US5215669A (en) 1993-06-01
ZA904275B (en) 1991-02-27
DE59005545D1 (en) 1994-06-01
WO1990015295A1 (en) 1990-12-13
NO914001D0 (en) 1991-10-11
AU631647B2 (en) 1992-12-03
AU5668590A (en) 1991-01-07
PT94261A (en) 1991-02-08
BR9007418A (en) 1992-06-16
CA2058440A1 (en) 1990-12-06
EP0475969A1 (en) 1992-03-25
NO178838C (en) 1996-06-12
NO914001L (en) 1991-10-11
NO178838B (en) 1996-03-04
DE3918274A1 (en) 1990-12-06

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