Beruflich Dokumente
Kultur Dokumente
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USOO5179063A
5,179,063
Jan. 12, 1993
106/2868
[75]
lnven10r$=
[73] Assignee:
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[51]
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and 3-6 weight percent of at least one sodium polyphos phate. Preferably, this composition is prepared by a
106/65 process comprising the step of calcining a mixture of a1
528/485
528/485 _ 502/183
585/852
210/682 14 Claims, N0 Drawings
1
HYDROTALCITE COMPOSITION
BACKGROUND OF THE INVENTION
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comprising hydrotalcite and an inorganic binder. In another aspect, this invention pertains to a method of
organic liquids.
SUMMARY OF THE INVENTION It is an object of this invention to provide a composi
514-528, and include sodium tripolyphosphate (Na5P 3010), sodium tetrapolyphosphate (Na6P4O13), sodium
metaphosphates such as Maddrells salt and Kurrols
tametaphosphate, and higher linear sodium metaphos phates having the general formula of (NaPO3)x, with
x=10-2l. Presently preferred is a linear sodium meta
The composition in accordance with this invention compounds from aqueous or organic liquids. Other comprises (preferably consists essentially of) hydrotal objects and advantages will be apparent from the de 30 cite (preferably about 94-97 weight-%) and about 3-6 tailed description of this invention and the appended weight-% sodium polyphosphate. These two compo claims.
In accordance with this invention, a composition comprises at least one hydrotalcite and about 3-6 weight percent of at least one sodium polyphosphate. Also in accordance with this invention, a process for
nents can be combined in any suitable manner, such as
by dry-blending in a suitable, conventional mixer. After the above-described components have been mixed
is in the range of about 0.4:1 to about 0.6:1. After the DETAILED DESCRIPTION OF THE 45 pasty mixture (containing hydrotalcite, sodium poly INVENTION phosphate and water has been shaped, it is substantially dried (preferably at a temperature of about 100-l50 C. Any hydrotalcite material can be used as the principal
for about 1-60 hours), and then calcined (preferably in air) for about 10-20 hours at about 370480 C., prefer ably for about 14-18 hours at 390-460 C., more prefer
ably for about 15-17 hours at about 400-450 C.
are the hydrotalcite materials described in US. Pat. Nos. 4,347,353 and 4,284,762. The presently more pre ferred hydrotalcite has a chemical formula of Mg4_5A12
(OH)13CO3.3.5H3O. This preferred hydrotalcite mate rial is manufactured by Kyowa Chemical Industry Company, Ltd., Osaka, Japan, and is marketed by Mit sui and Company, Ltd., Osaka, Japan, and by Mitsui and Company (USA), Inc., Houston, Tex., under the prod
uct designations of DHT-4 and DI-IT-4A. The preferred hydrotalcite is a basic aluminum hy
sured by N; adsorption in accordance with the BET method) of 5-15 mZ/g, a density of about 2.1 g/cc, and
a Mohs hardness of 22.5. This hydrotalcite has a lay
a manufacturing process for producing poly(phenylene sul?de) in the presence of N-methyl-Z-pyrrolidone (NMP). NMP is generally recovered from a produced
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slurry of the phenylene sul?de polymer in an aqueous brine by liquid-liquid extraction with n-hexanol. The formed n-hexanol/NMP extract contains undesirably
high amounts of NaCl, which must be removed from the extract before any further separation (e.g., by frac tional distillation). The composition of this invention is
drotalcite/Na-metaphosphate particles of this invention for removing chloride ions from liquids. Blends of DHT-4 hydrotalcite (described above) and
various amounts of Na metaphosphate binder (de
scribed above) were mixed with enough water to pre
15 pare a paste which was dried at room temperature for
about 16 hours and then at 125 C. for about 16 hours. The dried material was ground and sieved. A 20-40 mesh fraction of each test batch was calcined for 16 particles comprising hydrotalcite and sodium meta phosphate binder. hours at various temperatures. 3.0 grams of a particular 80 grams of Dl-lT-4 hydrotalcite (provided by Mitsui 20 calcined blend was then stirred at 65 C. with 250 mL of and Company, Osaka, Japan) and various amounts of a an aqueous NaCl solution containing about 500 ppm sodium metaphosphate, (NaPO3)13, as binder (provided C1. Test results indicated that after 25-50 minutes of by Fisher scienti?c Company, Pittsburgh, PA) were contact at 65 C., the calcined particles (in accordance
phate binder were chosen so as to provide binder con 25 metaphosphate binder (having been calcined at 450 C.
This example illustrates the effects of binder content and calcination conditions on the crush strength of
tents in the blend ranging from 1.5 to 6 weight-% so dium phosphate. Water was mixed with the dry blend of hydrotalcite and sodium metaphosphate (generally at a
waterzsolids weight ratio of about 0.5:1) so as to make a sodium metaphosphate binder (also having been cal 30 paste, which was then extruded through a 1/32 inch die. cined at 450 C. for 16 hours) had removed only about The extrudates were dried at room temperature and 18% Cl and respectively, from the aqueous NaCl
various periods of time. 35 10-20 mesh hydrotalcite/Na-metaphosphate particles The calcined extrudate pieces of a particular hy were treated at 65 C. under a N2 atmosphere with 250 drotalcite/Na-metaphosphate blend were then sub mL of the liquid described in Example I, which con merged in a liquid mixture (obtained from a polyphenyl tained 73.0 weight-% n-hexanol, 14.4 weight-% NMP. ene sul?de pilot plant) containing 73 weight-% n-hex 12.6 weight-% H30 and 152 ppm NaCl (equivalent to anol, 12.6 weight-% water, 14.4 weight-72 N-methyl-2 40 92 ppm Cl). Test results indicat that the materials in pyrrolidone (NMP) and 152 ppm NaCl (i.e., 152 parts of accordance with this invention. which contained 3-6 NaCl by weight per million parts by weight of the total weight-% sodium metaphosphate binder and had been mixture). The extrudate pieces were stirred for 50 min calcined for about 16 hours at 450 C., had removed utes in above-described liquid mixture at a temperature about 50-70% of Cl from the liquid n-hexanol/NMP/ of 65 C. Thereafter, the slurry was ?ltered. and the 45 H3O mixture within a period of time of 5-50 minutes. extrudates were dried at 120 C. for about 16 hours. Reasonable variations. modi?cations and adaptations
the scope of the disclosure and the appended claims, without departing from the scope of this invention. plates of? inch diameter and a 0-30 lb. force gauge. The 50 That which is claimed is: force required to crush an extrudate particle placed 1. A process for preparing a composition of matter between the two plates was recorded. Average crush consisting essentially of about 94-97 weight-% of at strengths of 15 extrudate pieces of each of the various least one hydrotalcite and about 3-6 weight-% of at calcined hydrotalcite/Na-metaphosphate blends are least one sodium polyphosphate comprising the steps of summarized in Table I. 55 mixing said at least one hydrotalcite and said at least one sodium polyphosphate, and calcining the obtained mix TABLE I
About 15 dried extrudate pieces from each test batch were tested in a conventional laboratory pistol grip
for various usages and conditions can be made within
Calcination
Calcination
Crush Strength
Wt-% Binder
1.5 3.0 3.0 6.0 6.0 6.0 60 6.0 6.0 60
Temp. (C.)
450 450 450 300
Time (Hrs)
16 16 16 16 16 1 16 50 16 16
(lb)
l 12.3 12.5 ]
400 450
450 450 525 900
20.0 El 11.5 21 S1 S1
5 P0913
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8. A process in accordance with claim 1, wherein said calcining is carried out for about l4~18 hours at about 390-_460 C. 9. A process in accordance with claim 8, wherein said calcining is carried out for about 15-17 hours at about 400-450 C.
10. A composition of claim 1. 11. A composition 10 of claim 2. range of about 0.4:1 to about 0.611. 12. A composition 6. A process in accordance with claim 4 further com of claim 3. prising the steps of extruding said pasty mixture and 13. A composition drying the obtained extrudates before said calcining. of claim 6. 7. A process in accordance with claim 6, wherein said 14. A composition drying is carried out for about 1-60 hours at about of claim 8. 100-l50 C., and said calcining is carried out for about
5. A process in accordance with claim 4, wherein the weight ratio of added water to said dry mixture is in the
14-48 hours at about 390~460 C.
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