Novel method for preparing hafnium acetylacetonate
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A technology of acetylacetone and hafnium acetone dimer, which is applied in the preparation of aldehyde/ketone chelate, organic chemistry, etc., to achieve high yield, simple operation and high purity
Inactive Publication Date: 2013-04-24
KUNMING INST OF PRECIOUS METALS
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[0004] The preparation method of existing bibliography report hafnium acetylacetonate has following shortcoming and deficiency: the first, all need to strictly control the pH value of solution in two kinds of synthetic methods, operate Difficult, low yield
And method one uses highly toxic substance benzene in the preparation process
The purification process of the second method requires a special area sublimation device, and the product collection is difficult
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[0011] Weigh 40.0g anhydrous HfCl 4 Dissolve in 250ml methanol, transfer to a 1000ml reaction flask, add 74ml Hacac, adjust the pH value between 6-9 with NaOH, if necessary, use Hacac to reverse-adjust, and react at 60℃ for 5h, filter to remove the precipitate, change the reaction solution Concentrate to dryness to obtain hafnium acetylacetonate dimer Hf containing hydroxyl bridge bond 2 (OH) 2 (acac) 6 60.27g, the yield is 98%.
[0012] Hf 2 (OH) 2 (acac) 6 The characteristic structure parameters of the element: (1) Elemental analysis C 36.47% H 4.43% Hf 36.47% is consistent with the theoretical value C 36.51% H 4.46% Hf 36.20%; (2) FAB + -MS m / e=987(C 30 H 44 O 14 Hf·H + , 45%); (3) IR(cm -1 , KBr tablet) 3437 (s, v O-H), 1529 ~ 1595 (s, vC = O), 540 ~ 565 (m, vHf-O); (4) 13 C(dmso, ppm) 188.0, 102.5, 26.7; (5) 1 HNMR(CDCL 3 , Ppm) 5.5 (s, 1H, CH), 4.1 (s, 1H, OH), 1.97 (s, 6H, 2C...
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Abstract
The invention discloses a new technology to prepare (Hf(acac)4), and the technological process is that: anhydrous HfCl4 is dissolved in methanol, and Hacac is added; NaOH is used for adjusting the pH value of the solution; a new intermediate complex Hf2(OH)2(acac)6 is generated after reaction; then Hacac is added for reflux reaction, and the intermediate complex is transferred to the target compound Hf(acac)4. The technology has the advantages that, synthesis technology and purification process are integrated; productivity and purity are high; no special regional sublimation device is required during the purification process; the use of extremely toxic substance benzene is avoided, and scale production can be realized.
Description
technical field [0001] The invention relates to a new process for preparing hafnium acetylacetonate, which belongs to the field of chemical industry. Background technique [0002] Hafnium(IV)acetylacetonate or Hafnium(IV)2,4-pentanedionate), abbreviated as Hf(acac) 4 , its chemical formula is C 20 h 28 o 8 Hf, molecular weight 574.93, white crystalline powder, easily soluble in methanol, ethanol, chloroform, benzene, toluene, ether and other common organic solvents, hydrolyzed in water. Its sublimation temperature is 193°C, and it is MOCVD (metal organic chemical vapor deposition) to prepare HfO 2 An ideal precursor for coatings and thin films, as early as the 1970s M.Balog used Hf(acac) 4 High-purity HfO was prepared for the precursor 2 Thin Films (M. Balog, M. Schieber, Thin Solid Films 1977, 41, 247. M. Balog, M. Schieber, J. Crystal Growth 1972, 17, 298). Take Hf(acac) 4 HfO prepared for the precursor 2 The film has excellent physical and chemical properties su...
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