Zirconium -acetate

Note Both above specifications give 370.2 as the factor, which seems to be an error e) Acetate Resin. Subtract from 100% the sum of percentages of diatomaceous earth, ferric oxide and zirconium Method No 214. Ig niter Composition Type II of Delay Charge Compositions Z-2A or Z-2B. Its composition Barium Chromate, Zirconium Acetate Resin and procedures... 

Zinc Sulfate Heptahydrate Zinc Sulfocarbolate Zinc Sulfophenate Zinc Vitriol Zinc Yellow Zirconium Acetate Zirconium Acetate Solution Zirconium Nitrate Zirconium Nitrate Pentahydrate... 

In the case of organic derivatives such as zirconium acetate, direct bonding of the carboxyiate to the zirconium is found. Similar structures are also found in solvent-soluble, water-insoluble carboxylates such as zirconium propionate. Zirconium alkoxide derivatives tend to be monomeric in solvent-based systems but hydrolyse rapidly with ambient water to give polymeric species. 

The aqueous chemistry of zirconium is complex and dominated by hydrolysis. One aspect is that polymerization takes place when salt solutions are diluted. The polymeric species can be cationic, anionic, or neutral. Polymers that are formed include ammonium zirconium carbonate, zirconium acetate, and zirconium oxychloride. 

The zirconium salts of organic acids are widely applied in industry. Carboxylatozirconylic acids are used in treating dermatitis and in making textiles water repellent, while zirconium acetate, Zr(OAc)4, and the trilactozirconate Na2H[Zr(0H)(MeC(0H)C02)3] are components of body deodorants, and the 2-ethylhexanoate and naphthenate are used as siccatives. 

Non-aggressive way using zirconium acetate for preparation of zirconium pillared clay developing high sulfur thermal stability over 830 °C... 

In this work, zirconium acetate solution was used in order to increase the pH of the pillaring solution and the content of sulfate ions introduced. Different preparation parameters and their effect on the structural and textural properties have been investigated. The resulting materials present a best zirconium-sulfate intercalation with higher sulfate rate and develop very high thermal stability of sulfur even at about 830 °C. 

The present study deals with the incorporation of zirconium sulfate hydroxyl complex in Na-montmorillonite using zirconium acetate as a precursor. The effect of the preparation parameters on the textural and structural properties of the resulting materials will be discussed. 

Catalysts preparation. Intercalation solutions were prepared by addition of an ammonium sulfate solution to a fresh zirconium acetate one. The mixture was adjusted to the desired pH using a HCl solution. In another beaker, Na-montmorillonite suspension was adjusted at the same pH than the intercalation solution. 

It is known that a zirconyl chloride solution is not stable [11]. The pH of a fresh 0.1 mol/L ZrOCl2 solution decreases from 2.1 to 1.9 after 10 minutes. To study the stability of the zirconium acetate solution, the pH was measured periodically. It was found to be equal to 3.76 and a very weak decrease was observed after two days. These properties could give, besides the non aggressive medium for clay layers, a better reproducibility than the zirconyl chloride solution. The effect of the addition of 2 mol/L ammonium sulfate to the 0.1 mol/L zirconyl chloride solution or to the 0.1 mol/L zirconium acetate solutions on the pH values is plotted in Fig. 1. 

This plot shows two important results. The first one is the absence of precipitation occurring for high SOaiZr ratios for the acetate solution. The second one is the increase of pH of the zirconium acetate solution when the sulfate quantity increases. This increase of pH is probably due to the release of acetate groups in solution substituted by sulfate ions, which is more important than the weak acidity of the ammonium ion. 

The diffraction patterns of dried zirconium sulfate pillared clay obtained after different intercalation times are presented in Fig. 2. These samples were prepared using a 0.1 mol/L zirconium acetate solution with an S04 Zr ratio = 0.5. The clay concentration was 10 g/L, with Clay Zr =10 g/mol, at pH = 4.00. The intercalation was performed at 15 °C. 

Fig. 1. Variation of pH as a function of sulfate to zirconium ratio for 0.1 mol/L zirconyl chloride and zirconium acetate solution at 20 °C.

Thus, the increase of the pH does not seem very important when the zirconium acetate is used. It is not the case for zirconyl chloride where a change of the pH induces a very important change of the texture of the obtained solids [12]. 

All samples were prepared using 0.1 mol/L zirconium acetate solution at 15 °C with 42 hours intercalation reaction. The clay suspension pH was fixed at the same value as that of the intercalation solution. The X-ray diffraction patterns of zirconium sulfate pillared clays prepared with different sulfate to zirconium ratios are shown in Fig. 4. This figure shows a shoulder at about 19.5 A for the sample prepared using a S04 Zr ratio equal to 0.125. The 19.5 A spacing corresponds to the intercalation of non sulfated zirconium polycations [13]. Non-drastic loss in surface area is observed when the sulfate to zirconium ratio increases. But the use of zirconyl chloride solution shows a drastic loss of surface area when the SOarZr ratio increases (more than 50 %) [13]. 

The XRD patterns of zirconium sulfate pillared clays obtained after 90 hours of intercalation with different zirconium acetate concentrations using 0.5 as sulfate to Zr ratio and the same clay concentration as used earlier are presented in Fig. 5. The diffraction data show the appearance of two first order reflections. The first one is at 23.4 A for the lowest zirconium concentration and appears as a shoulder at the same distance for 0.05 mol/L concentration. The second reflection is observed at approximately 12.3 A for the lowest concentration and at 13.7 A for 0.1 mol/L zirconium acetate. The first one results from the intercalation of sulfated zirconium species. Those species are more voluminous than the non sulfated one which gives a distance spacing at only 19.6 A. The better intercalation of sulfated zirconium species at low Zr concentration is probably due to the slow progress of polycondensation reactions. This process reduces the number of different zirconium species and gives a better cristallinity of the solid. Table 2 summarizes the textural properties of samples prepared with different zirconium concentrations. The decrease of the surface area with the decrease of the Zr concentration is probably due to the increase of the sodium clay layers by comparison with the intercalated layers. The microporous volume increases when the Zr concentration decreases. The higher microporosity is due to the important basal distance of this sample. 

Zirconium-sulfate pillared clay prepared with reaction time of 140 hours and using 0.1 mol /L zirconium acetate solution has been analyzed with mass spectrometry. When the sample was heated in air, masses of 17, 18, 44, 48, 64 and 80 were recorded, corresponding, respectively, to OH+, H2O+, COz, SO+, S02" and SO3+. Figs. 7, 8 and 9 show the variation of the different masses with heating temperature. 

Fig. 10 displays the SO2 weight loss evolution (mass 64) as a function of temperature for different Zr concentrations and S04 Zr ratio = 0.5. This figure shows that the SO2 peak shifts to higher temperature when the Zr concentration decreases. In the case of 0.025 molZr/L, the major sulfate loss occurs at 830 °C. This indicates that the sulfates linked to the pillars which give a dooi at 23.4 A develop the best thermal stability. However, for samples prepared with higher zirconium acetate concentration, the departure of sulfur occurs at lower temperatures. As those samples contain a polymeric phase, this Zr-SOa phase probably gives a less stable sulfate. 

However, the decrease of surface area is very important in the samples prepared with high concentrations of zirconium acetate (from 195 at 120 °C to 140 m /g at 400 °C). The presence of amorphous phase exerts a great effect on the thermal stability of the solids. The dehydroxylation of the zirconium complex seems not to be the only factor responsible for the loss of surface area, as reported by Figueras et al. [16]. 

Zirconium acetate seems to be a very interesting zirconium precursor for the preparation of zirconium sulfate pillared clay because of its high and stable pH level and its low sensitivity to the precipitation when the sulfate was added. Nevertheless, the progress of the polymerization reaction is very rapid at high Zr concentrations, even at reduced intercalation temperature (15 °C). 

Non-aggressive way for preparation of zirconium sulfate pillared clay using zirconium acetate developing high sulfur thermal stability over 830°C... 

Zirconium Acetate Rubber gloves, chemical goggles or face shield. Flush with water. Flush with water for at least 15 minutes. 

Zirconium Acetate 5 mg/m- Data not available 0.5-5 Data not available... 

Zirconium Acetate Not flammable Not flammable Not flammable Not flammable Not pertinent Not pertinent Not pertinent Not pertinent No ... 

Chemical Designations- nonymr Zirconium acetate solution Chemical Formula ... 

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