THE APPLICATION OF PROCESS MASS SPECTROMETRY TO FUMED SILICA PRODUCTION

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1 JPACSM 5 Process Analytical Chemistry THE APPLICATION OF PROCESS MASS SPECTROMETRY TO FUMED SILICA PRODUCTION Peter Traynor and Steven Trimuar Thermo Electron Corporation Houston, TX Robert G. Wright Thermo Electron Corporation Winsford, Cheshire, UK KEYWORDS: PROCESS MASS SPECTROMETRY, FUMED SILICA PRODUCTION, EMISSIONS MONITORING, COMBUSTION CONTROL ABSTRACT This paper describes the application of process mass spectrometry to the production of fumed silica (amorphous silicon dioxide, widely used for improving the mechanical properties of many materials, such as paint and food products). In this process, gaseous silicon tetrachloride is hydrolyzed at high-temperature to silicon dioxide in an oxygen-hydrogen flame. Product particle size distribution, surface area, and surface properties are controlled by precise regulation of the combustion conditions by mass spectrometric on-line monitoring of oxygen and carbon dioxide concentrations. Emissions of various chlorine containing species are continuously monitored by mass spectrometry as well. These include hydrogen chloride (HCl), chlorine (Cl 2 ), chloromethane (CH 3 Cl), methylene chloride (CH 2 Cl 2 ), chloroform (CHCl 3 ), and carbon tetrachloride (CCl 4 ). These chlorine containing species are monitored in order to minimize their release into the atmosphere. This paper describes how all these measurements are performed rapidly and precisely by a process mass spectrometer. INTRODUCTION Fumed silica, or colloidal silica, is a ubiquitous, through little known, compound existing as an amorphous glass. Due to its high surface area, it makes an excellent dispersant. It is used in products such as paints, adhesives, and sealants to hold these heterogeneous mixtures in suspension. Similarly, a food-grade product is produced which is used in the same capacity in products such as sauces, dressings, and toothpaste. It is also used in aggregates and powders such as fine chemicals, cereal grains, and spices to promote free-flow and inhibit clumping. In the semiconductor industry, with wafer diameter increasing and mask thickness decreasing, it is increasingly used as an ultra-fine abrasive. Current global production is in excess of 200 million pounds annually. The raw material typically used for the industrial production of fumed-silica is silicon tetrachloride (SiCl 4 ), which is a common by-product generated in the production of silicone products. Liquid silicon tetrachloride is first vaporized and then injected into a hydrogen flame inside a furnace to produce the final product, silicon dioxide (SiO 2 ), with hydrogen chloride (HCl) as the primary by-product. The process can be summarized as follows: SiCl 4 + 2H 2 + O 2 SiO 2 + 4HCl Product particle size distribution, surface area and surface properties are controlled by precise regulation of the combustion conditions in order to meet the needs of particular applications and customers 1. Typically, the temperature of the hydrogen flame is in the range of C, depending on the ratio of air, hydrogen, and silicon tetrachloride. When the temperature is at the lower end of the range, the product has a smaller particle size and greater surface area better for use as thickening agent. At higher temperature, the product has a larger particle size and lower surface area better suited as a thixotropic agent. Carbon dioxide is generated due to the introduction of methyltrichlorosilane along with the SiCl 4 feed. The mass spectrometer measures oxygen and carbon dioxide in the furnace exhaust. These are used as control inputs for the air-to-fuel ratio of the gas burner. The analysis of oxygen (O 2 ) and carbon dioxide (CO 2 ) could alternatively be performed using less complex and expensive instrumentation than a mass spectrometer (MS), but the MS is also used to measure chlorine containing species in the exhaust. The main by-product of the process is hydrogen chloride (HCl), much of which is recovered and sold. The process also produces chlorine (Cl 2 ), chloromethane (CH 3 Cl), methylene chloride (CH 2 Cl 2 ), chloroform (CHCl 3 ), and carbon tetrachloride (CCl 4 ).

2 JPACSM 6 The discharge from the furnace is passed through an agglomerator system and cyclone separator and bag filter to collect the silica product. Although the gas stream from the silica collecting system is treated with cooling, absorbing, and scrubbing systems, inevitably significant levels of chlorine containing species can remain in the stack gases released to atmosphere. The level of Cl 2 is minimized by injecting natural gas and hydrogen at 800 C to convert the Cl 2 into HCl. This process generates CO, which also requires monitoring. In most countries, the release of CO and the various chlorine compounds are strictly regulated; some form of periodic monitoring is beneficial for optimizing the gas treatment processes. In this regard, the mass spectrometer comes into its own as the instrument of choice since it performs the analysis of all of the compounds of interest both accurately and rapidly. The only exception is CO, the analysis of which by process MS is somewhat limited in this application. IMPLEMENTATION OF PROCESS MS This paper describes the application of a Thermo ONIX VG Prima process MS to fumed silica process gas. This instrument has been described in previous publications 2-5. The process gas contains high levels of water and is dried using Naflon drying tubes. It is also filtered before being sampled by a rapid multi-stream sampling (RMS) valve of the process MS which directs the sampled stream into a capillary inlet. This continuously consumes about 15 ml/minute of sample gas, most of which is bypassed to a rotary pump with just a very small proportion, less than 0.1%, flowing through a molecular leak into the MS itself. The reason for drying the sample gas is to minimize the possible corrosive effect of the water, hydrogen chloride, chlorine combination. Table I Analysis Setup for Fumed Silica Process Gas Analysis The components measured in the analysis include He, H 2 O, CO, N 2, O 2, HCl, Ar, CO 2, CH 3 Cl, Cl 2, CH 2 Cl 2, CHCl 3, and CCl 4. Water is included in the analysis in order to check the efficiency of the drying process. Helium is included for leak checking purposes. The use of the RMS valve allows the analysis of various sample points in the process with one instrument. In this way, both combustion data and emission control data are provided simultaneously. It should be mentioned that the RMS valve for this application is made from Hastelloy alloy C-276 rather than the standard material 316 stainless steel. Hastelloy C- 276 is a nickel-chromium-molybdenum alloy which provides excellent corrosion resistance. The vacuum system is protected from corrosion by using perfluoropolyether fluid in the rotary pump and a nitrogen purge for the turbomolecular pump bearings. The typical mass peaks used for analysis are shown in Table I. It is seen that CO is included in the analysis, but since it is present at only a low level (typically 0.1 mol %), it is only analyzed at mass 12, not at its molecular ion peak mass 28. This is because at mass 28 there is very severe interference from N 2 which is usually present at about 80 mol %. There is interference however from CO 2 at mass 12 and this, combined with the relatively weak signal at mass 12 (100 times smaller than the molecular ion peak), limits its detection. The measurement of HCl suffers from interference from Cl 2 and the argon isotope peak 36 Ar; this is why Ar is included in the analysis. The interference from Cl 2 is unexpected because the atomic masses of the isotopes are 35 and 37 and the resolution of the instrument is such that there should be negligible intensity at mass 36. However, it is seen in the spectrum of Cl 2 that there is a definite peak at mass 36. It is assumed that this is a result of the Cl 2 reacting with surface adsorbed water and generating some HCl. The existence of a peak also at mass 38 in the expected isotope ratio of 1:3 relative to the mass 36 peak supports this explanation. Cracking Patterns Component Detector Relative Sensitivity He SEM H 2O Faraday CO Faraday N 2 Faraday O 2 Faraday HCl Faraday Ar Faraday CO 2 Faraday CH 3Cl SEM Cl 2 Faraday CH 2Cl 2 SEM CHCl 3 SEM CCl 4 SEM

3 JPACSM 7 There are some other interferences in the analysis: At mass 50 there are interferences with the measurement of CH 3 Cl from CH 37 Cl + ions due to CH 2 Cl 2 and CHCl 3 and at mass 117 there is interference from CHCl 3 on the measurement of CCl 4. Note that CHCl 3 and CCl 4 are measured at their fragment peaks (CHCl + 2 and CCl + 3 respectively) rather than their molecular ion peaks, because the former are significantly more intense. All these interferences are corrected for by the process mass spectrometer software after calibration. The analysis is calibrated using a set of calibration gases as shown in Table II. These gases are chosen to accurately calibrate for all the components relative sensitivities, cracking patterns, and background peak heights. RESULTS The typical analytical performance observed for this application is shown in Table III. This is a 30-second analysis for the measurement of these 13 components. The precision observed is very high, except for CO, which as previously mentioned suffers from significant interference. In practice, a discrete CO infrared (IR) analyser has to be used to give the required precision (±20 ppm). The analog output signal from this device can be read by the process MS as an analog input and incorporated into its results; all these results can be communicated to host control computer using Modbus. Effectively, the VG Prima becomes a hybrid instrument combing both MS and IR analyzers with both analyzers benefiting from the flexibility of the multi-stream selection valve, as shown in Figure 1. Table II Composition (molar) of Gases Used for Calibration Component He 1000 ppm 100% Bal Bal H 2 O CO 0.1% N 2 Bal Bal Bal Bal O 2 18% 21% HCl 200 ppm Ar 1% CO 2 2% 100% CH 3 Cl 10 ppm Cl ppm CH 2 Cl 2 10 ppm 100 ppm CHCl 3 10 ppm 100 ppm CCl 4 10 ppm Table III Analytical Performance by Process MS Component Nominal Range Typical Level Typical Precision (expressed as 3 standard deviations) He mol ppm 5 mol ppm 0.3 mol ppm H 2 O 0 1 mol % 0.2 mol % 0.01 mol % CO mol ppm 1000 mol ppm 400 mol ppm N mol % 80 mol % 0.03 mol % O mol % 15 mol % mol % HCl mol ppm 50 mol ppm 2 mol ppm Ar 0 2 mol % 1 mol % mol % CO mol % 1.5 mol % mol % CH 3 Cl 0 50 mol ppm 5 mol ppm 0.2 mol ppm Cl mol ppm 200 mol ppm 5 mol ppm CH 2 Cl mol ppm 5 mol ppm 0.2 mol ppm CHCl mol ppm 5 mol ppm 0.2 mol ppm CCl mol ppm 5 mol ppm 0.2 mol ppm

4 JPACSM 8 Typical graphical plots are shown in Figure 2 for HCl, Figure 3 for Cl 2, and Figure 4 for the analysis of CH 3 Cl, CH 2 Cl 2, CHCl 3, and CCl 4. These plots show the good reproducibility as exhibited when the calibration gases are analyzed. Long term stability has also been demonstrated to be good. Figure 5 shows actual exhaust gas analysis. Over the past seven years, three VG Prima mass spectrometers have been successfully installed on fumed silica plants. They have enabled optimization of the key process of combustion (gas burner operation) and provided comprehensive emissions control for compliance with environmental regulations. Figure 1. Combination of MS and IR in a single process gas analysis system. Figure 2. Analysis of calibration gas HCl by process MS.

5 JPACSM 9 Figure 3. Analysis of calibration gas Cl 2 by process MS. Figure 4. Analysis of calibration gas CH 3 Cl, CH 2 Cl 2, CHCl 3 and CCl 4 by process MS.

6 JPACSM 10 Figure 5. Analysis of Fumed Silica Plant Exhaust Gases by Process MS. CONCLUSIONS Process MS has been shown to successfully provide comprehensive multi-component gas analysis for fumed silica plant control. Gas analysis is used to control the combustion conditions in order to achieve particular product property requirements. Harmful exhaust gases are monitored to optimize the gas treatment systems. The limited detection of CO by MS due to interference from much higher levels of N 2 and CO 2 has been overcome by the addition of an IR analyzer. The latter can be integrated with the MS into a single analyzer system sharing the same multi-point selection valve. REFERENCES 1. L.J. White and G.L. Duffy, Ind. Eng. Chem., 3, 235, (1959). 2. R.G.Wright, Process Anal. Chem., Vol. IV, (1998). 3. P. Traynor and R.G. Wright, Process Anal. Chem., Vol. VI, (2002). 4. P. Traynor and R.G. Wright, Process Anal. Chem., Vol. VII, (2002). 5. P. Traynor and R.G.Wright, Process Anal. Chem., Vol.VII, (2002).

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