CS247333B1 - A method of preparing high purity acetene - Google Patents

Abstract

The solution concerns the preparation of high-purity acetone of MOS Selectipur grade 0 purity for the needs of microelectronics using physicochemical purification methods in equipment made of materials that are resistant to the corrosive effects of acetone. Acetone is distilled continuously or discontinuously under reduced pressure or at atmospheric pressure in stainless steel or glass apparatus without air access. The fraction is taken at a temperature calculated by the relationship: sampling temperature (°C) = = 56.24° — 0.037950 . Δρ (kPa) . The distillate is then passed directly to filtration through a set of Teflon filters of dimensions 1.8 μια, 0.8 μπι, and 0.4 μΐη, respectively.

Description

247333

BACKGROUND OF THE INVENTION The present invention relates to the preparation of high purity acetone purity grade MOS Selectipur class 0 microelectronics through the use of physical-chemical purification methods in a material apparatus that is resistant to the corrosion effects of acetone.

Chemicals used in the manufacture of integrated microelectronic circuits must meet extremely strict purity criteria. For this reason, the purity chemical p. A. Can not be used, but it is necessary to refine it in an apparatus which is suitable for this process and is structurally designed but mainly made of a material which is corrosion-resistant to the respective chemical. The purification must be so constructed that the cleaned chemical does not come into contact with the ambient air after purification and after filtration. Otherwise, the air purifiers would absorb in the cleaned chemical, thereby depleting the chemical.

It is an object of the present invention to provide high purity acetone purity of MOSSelectipur from preformed acetone purity or purity, which acetone is discontinuously or continuously distilled under reduced pressure or at atmospheric pressure in a stainless steel or glass apparatus without air. taking a fraction at the collection temperature (° C) = 56.24 ° - 0.03750. Δ p (kPa), where Δρ (kPa) is the difference in atmospheric pressure and pressure at which distillation is carried out, and the distillation is passed directly to the filtration through 1,2 tzine, 0,8, m, respectively. 0,4 μΐη.

To prepare high purity acetone, MOS Selectipur from acetone technical grade, proceed as follows:

The technical acetone from 50-100 L glass balloons is pumped through a stainless steel pump (stainless 14 or glass (SIMAX glass) reservoir) from a stainless steel or glass vapor pump, distilled continuously or discontinuously at atmospheric pressure or pressure. lowered.

The distillate is collected in a glass preform (SIMAX glass), whereupon the pump is pressed for filtration. The filter device consists of a high-polished stainless steel frame (class 14 stainless steel), two or three Teflon filters with a hole diameter of 1.2 µm, 0.8 µm, and 0.45 µm.

A glass dispensing package is slid onto the outlet of the filter device to prevent air from entering the interior. MOS Selectipur's acetone purity preparation technology also includes the cleaning of shipping packaging. Packaging is glass, glass is the third hydrolytic class. Prior to filling with the purified chemical, the coating must be cleaned first with diluted (1: 1) nitric acid, after rinsing with water, (1: 1) hydrochloric acid and finally with water, first distilled and high purity. water conductivity0.1 / zS. The water must also be free of dust particles on the filter with 0.45mn apertures. Finally, the packaging is dried by the filtered air. Further details on how to prepare purified acetone are given in the Examples. Example 1

Quality Acetone p. A. Is analyzed in addition to the conventional procedures of CSN 686 by differential pulse polarography and atomic absorption spectrometry for chemical impurities and the prescribed micro-scoping method for the content of heterocomponents. Analysis Results: Indicator Spec. wt. g / cm3, 2074 ° C 0.790 water content 0.29% evaporator 0.0008% ash 0.0001% acidity as formic acid 0.00085% Fe 0.18 ppm Cr 0.10 ppm Pb 0.01 ppm Ti 0 01 ppm As 0.17 ppm Zn 0.09 ppm To 0.14 ppm K 0.5 ppm Li 0.01 ppm Cu 0.16 ppm Mg 0.13 ppm

Metals = Cd, Ni, Mn, Bi, Ga, Sn, Cu, Mo, Vsa at a concentration less than Ό, pmppm.

The main component content of the chromatographic analysis is 99.6%.

Heterocast content: 1 to 5, um 223 000 5 to 25 fzm 12 300 over 25 μπ 1 350

The acetone is discontinuously distilled in a glass apparatus (SIMAX glass) at a pressure of 53.3 kPa. A boiling point of boiling point 42 to 43 ° C is removed. The distillate is overpressed by a stainless steel pump through a filter set which consists of Teflon filters with apertures of 0.8 µm and 0.4 µm. The purified acetone was re-analyzed by the same procedures as before. Analysis results:

Claims (2)

247333 5 6 Indicator value and boiling point 55 to 56 ° C, with the spec. weight, g / cm 3, 2074 ° C 0.7885%, i.e. 45 liters. The product and water content of 0.18% are lysed by the same working procedures as the 0.00007% residue in Example 1. Analysis results: less than 1.10% ash 5% acidity as formic acid Fe 0.00076% 0.02 ppm Indicator Value t spec. weight, g / cm3, 2074 ° C Cr 0.01 ppm 0.789 Pb 0.01 ppm water content 0.20% Ti 0.01 ppm evaporator 8.IO-5% As 0.007 ppm ash less than 1.10-5% Zn 0 , 01 ppm acidity as formic acid 8.10-4% Na 0.016 ppm Fe 0.02 ppm K 0.017 ppm Cr 0.01 ppm Li 0.003 ppm Pb 0.01 ppm Ca 0.08 ppm Ti 0.01 ppm Mg 0.012 ppm As 0.008 ppm Zn 0.01 ppm Metals: Cd, Ni, Co, Mn, Bi, Ga, Sn, Cu, Mo, Na 0.013 ppm V are introduced at a concentration of less than K 0.015 ppm 0.01 ppm. Li 0.002 ppm Chromatographic analysis determined Ca 0.05 ppm mainly content of 99.8%. Mg 0.010 ppm Heterocomponent content: Metals: Cd, Ni, Co, Mn, Bi, Ga, Sn, Cu, Mo, 1 to 5 μΐη 12,000 V are applied at less than 5 to 25 μηι 2,100 0.01 ppm. By means of chromatographic analysis the content of the main constituent is determined to be 99,8 ° / o. From the results of the analyzes it can be seen that the concentrations of metal ions have fallen below the prescribed content of heterocastes: the boundaries of u and also the content of 1 to 5 μηι 13,200 particles have also been reduced. 5 to 25 μπι 1 980 over 25 μηι 410 Example 2 Distillation of acetone quality as in Example 1, only at atmospheric pressure of 107.5 kPa. The resultant fraction is taken to show that even at atmospheric pressure distillation is equally effective and distilled at reduced pressure. SUBJECT A method of preparing high purity acetone purity of MOS Selectipur from pre-formed acetone purity by pure or fine distillation, characterized in that the acetone is discontinuously or continuously distilled under reduced pressure or at atmospheric pressure in a stainless or glass-free air apparatus. at a temperature of the invention, the collection temperature [° C] = = 56.24 ° - 0.0337 950. A p, where Aβ (kPa) is the difference in atmospheric pressure and pressure at which distillation is carried out and the distillate is passed directly to the filter through a Teflon filter set of 1.2 μιη, 0.8 μm, or 0.4 μΐη .