Method for measuring content of iron carbonyl in synthesis gas
A measurement method and synthesis gas technology, applied in the direction of measuring devices, preparation of test samples, color/spectral characteristic measurement, etc., can solve problems such as poisoning reaction, high operation level, methanol synthesis catalyst deactivation, etc., and achieve equipment cost and The effect of reduced operating requirements
Inactive Publication Date: 2016-07-13
TIANJIN BOHUA YONGLI CHEM IND
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Problems solved by technology
[0002] Due to pipeline corrosion and other reasons, there may be traces of carbonyl iron in the synthesis gas, which can cause irreversible poisoning reaction to the methanol synthesis catalyst, leading to the deactivation of the methanol synthesis catalyst
[0003] At present, there is no national standard method for the analysis of carbonyl iron content in gas samples. Graphite furnace atomic absorption method is mostly used in the production process. The detection limit of this method is about 10ppb, but the equipment cost is high and requires a high level of operation.
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[0028] Connect eight 125ml absorption bottles in series in front of the flowmeter, add 70mL of pre-prepared washing liquid to the first six absorption bottles, add 70mL of water to the seventh bottle, and feed synthesis gas into the eighth bottle without liquid. Transfer the solution from the first 6 bottles to a 1000 mL beaker, rinse each bottle and connecting tubing with the water from the 7th bottle, and add the rinse to the aforementioned beaker. Measure 420mL of blank washing solution and pour it into another 1000mL beaker. Evaporate the liquids in the two beakers to complete dryness respectively, add 15mL of high-grade pure concentrated nitric acid to each of the two beakers, and evaporate again to complete dryness, then add 10mL of high-grade pure concentrated hydrochloric acid to each of the two beakers, and use Cover the mouth of the beaker with a watch glass, heat until the precipitates at the bottom of the beaker are completely dissolved, and flush the condensed wat...
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The invention discloses a method for measuring the content of iron carbonyl in synthesis gas.The method includes the steps that the synthesis gas is introduced into an absorption bottle filled with washing liquid, an absorption bottle filled with water and an empty absorption bottle, wherein the bottles are sequentially connected in series; all the washing liquid is poured to one beaker, all the absorption bottles and connecting tubes are washed with the water in the absorption bottle, cleaning liquid is also poured to the beaker, and a washing solution is obtained; the other beaker is taken and filled with the blank washing liquid, the beaker filled with the blank washing liquid and the other beaker are heated and evaporated to be dry; concentrated nitric acid is added to the two beakers, evaporation to dryness is conducted, concentrated hydrochloric acid is added to the two beakers, heating is conducted till precipitates at the bottoms of the beakers are dissolved; the liquid in the two beakers are diluted with distilled water, one kind of liquid absorbing the synthesis gas serves as a sample solution, and the other kind of liquid is a blank solution; a spectrophotometer is utilized for measuring the content of iron in the synthesis gas, and then the content of iron carbonyl in the synthesis gas is calculated.Iron carbonyl in the synthesis gas is completely absorbed.
Description
technical field [0001] The present invention relates to a kind of measuring method, more specifically, relate to a kind of measuring method of hydroxyl iron content in syngas. Background technique [0002] Due to pipeline corrosion and other reasons, the synthesis gas may contain trace amounts of carbonyl iron, which can cause irreversible poisoning reaction to the methanol synthesis catalyst, leading to the deactivation of the methanol synthesis catalyst. [0003] At present, there is no national standard method for the analysis of carbonyl iron content in gas samples. Graphite furnace atomic absorption method is mostly used in the production process. The detection limit of this method is about 10ppb, but the equipment cost is high and requires a high level of operation. Contents of the invention [0004] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for measuring the content of iron hydroxy in synthesis gas, wh...
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IPC IPC(8): G01N21/31G01N1/38
CPCG01N1/38G01N21/3103
Inventor 郎云涛李树杰蒋云龙邓建悦史静
Owner TIANJIN BOHUA YONGLI CHEM IND