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A kind of preparation method of zirconia trifluoromethanesulfonate

A technology of trifluoromethanesulfonic acid and zirconia, applied in directions such as zirconia, can solve the problems of high cost and limited economy, and achieve the effects of low cost, easy availability of raw materials and simple operation

Active Publication Date: 2022-03-15
SUZHOU XIANGYUAN SPEICAL FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Majid Moghadam et al. (Majid Moghadam, Shahram Tangestaninejad, ValiollahMirkhani, et al. Journal of Organometallic Chemistry, 2008, 693(11): 2041-2046.) reported a method using ZrOCl 2 •8H 2 O and AgCF 3 SO 3 A method for preparing zirconia trifluoromethanesulfonate, however, the preparation method uses relatively expensive silver salts, which limits the economics of the method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A method of preparing zirconia triflate: Example 1

[0017] Weighing zirconium oxychloride (of ZrOCl 2 • 8H 2 O) 5.14g, was dissolved in 80mL of deionized water, under agitation in a solution of 25 ~ 28wt% of concentrated aqueous ammonia, to a pH of 10, to stop the dropwise addition, stirring was continued for 10min; aging for 30 min at room temperature; deionized the precipitate was washed repeatedly with water to pH 6 ~ 7, no chlorine ions residue with 0.1mol / L silver nitrate solution was detected, most of the water was removed by filtration; the resulting wet precipitate of zirconium hydroxide was added all at a concentration of 80mL 0.4mol / L aqueous solution of triflic acid and stirred IH; filtered; and the filtrate was distilled to remove the solvent to give triflate, zirconium oxide, 41% yield.

Embodiment 2

[0018] Example 2: Method for preparing triflate zirconia

[0019] Weighing zirconium oxychloride (of ZrOCl 2 • 8H 2 O) 4.0g, was dissolved in 42mL of deionized water, under agitation in a solution of 25 ~ 28wt% of concentrated aqueous ammonia, to a pH value of 8 to 10, the dropwise addition, stirring was continued for 15min; aging for 30 min at room temperature; with the precipitate is repeatedly washed with deionized water to a pH of 6-7, no chlorine ion was detected residue with 0.1mol / L silver nitrate, most of the water was removed by filtration; 6mL the aqueous solution of 3.73g of triflic acid added to the resulting wet precipitate zirconium hydroxide, stirred for IH; 115mL deionized water added; filtered; and the filtrate was distilled to remove the solvent to give triflate, zirconium oxide, 76% yield.

Embodiment 3

[0020] Example 3: one kind of zirconium triflate preparation

[0021] Weighing zirconium oxychloride (of ZrOCl 2 • 8H 2 O) 2.0g, was dissolved in 30mL of deionized water, under agitation in a solution of 25 ~ 28wt% of concentrated aqueous ammonia, to a pH value of 8 to 10, the dropwise addition, stirring was continued for 20min; RT 60min aging; with the precipitate is repeatedly washed with deionised water to a pH of 6-7, no chlorine ions residue with 0.1mol / L silver nitrate solution was detected, most of the water was removed by filtration; the resulting precipitated zirconium hydroxide was added all wet 12mL solution of 1.86 g of an aqueous solution of triflic acid, stirred for IH; 50mL deionized water was added; filtered; and the filtrate was distilled to remove the solvent to give triflate, zirconium oxide, 63% yield.

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Abstract

A preparation method of zirconia trifluoromethanesulfonate. The method comprises the following steps: preparing a certain concentration of zirconium oxychloride aqueous solution, adjusting the pH value to 8-10 with concentrated ammonia water, obtaining zirconium hydroxide precipitate, washing repeatedly until no chloride ion is detected, filtering, and trifluoromethanesulfonic acid The aqueous solution and the obtained zirconium hydroxide precipitate are mixed, stirred, an appropriate amount of water is added, and filtered, and the solvent in the filtrate evaporates to obtain zirconium oxide trifluoromethanesulfonate. Zirconia trifluoromethanesulfonate has excellent catalytic performance in chemical synthesis such as silyl etherification of alcohols and ring opening of epoxy compounds.

Description

Technical field [0001] The present invention belongs to the technical field of zirconium preparing of chemical raw materials, method for making a triflate zirconia. Background technique [0002] Zirconium salts, for example sulfated zirconia, etc. can be efficiently catalytic isomerization, alkylation, acylation, cyclization and other types of reactions. Metal triflate as the Lewis acid catalyst is often used in many reactions, such as alcohols, phenols, amine acylation. Zirconium triflate, the formula ZrO (CF 3 SO 3 ) 2 , Trifluoromethanesulfonic acid or said zirconium oxide, zirconium triflate, the silyl ether alcohols, ring-opening reaction of the epoxy compound and the like (Majid Moghadam, ShahramTangestaninejad, Valiollah Mirkhani, et al. Synthetic Communications , 2009,39 (3): 552-561) demonstrated a high yield, short reaction time, high selectivity excellent catalytic performance. [0003] Majid Moghadam et al (Majid Moghadam, Shahram Tangestaninejad, ValiollahMirkhani, e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02
CPCC01G25/02
Inventor 庄海玉周建
Owner SUZHOU XIANGYUAN SPEICAL FINE CHEM
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