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Method for analyzing elemental copper in organosilicone slag slurry

An organosilicon slag and element technology, applied in thermal excitation analysis, material excitation analysis, etc., can solve the problems of forming acid mist and gelatinous substances, complex composition of organosilicon slag, and irritating odor, etc. Simple instrument operation, fast and efficient analytical methods, and simple sample processing

Active Publication Date: 2018-12-11
湖北环宇化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the composition of organic silicon slurry is complex, mainly composed of a large amount of liquid high boiling matter, silicon powder and copper powder, with pungent smell, strong corrosiveness, easy to burn and form acid mist and gel when exposed to air Substances, solid and liquid are difficult to separate and cannot be detected by traditional chemical analysis methods
[0004] "GBT 14849.4-2014 Industrial Silicon Chemical Analysis Methods Part 4 Determination of Impurity Element Content Inductively Coupled Plasma Atomic Emission Spectrometry" only stipulates the determination method of element copper in industrial silicon, but the domestic research literature has not been found. Study on the Method of Elemental Copper in Organosilicon Slurry

Method used

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  • Method for analyzing elemental copper in organosilicone slag slurry

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Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 20g of the slurry from the washing tower reboiler or the slurry distillation device of the organosilicon monomer synthesis device and place it in a 200ml beaker, add 100ml of ethanol to completely soak the slurry, stir and let it stand for 2 hours before removing the slurry The solution was filtered with suction, and then the filter cake was dried in an oven at 60°C for 2 hours.

[0023] After cooling, weigh 0.25g into the crucible, add 10ml of hydrofluoric acid, and after the violent reaction stops, add nitric acid dropwise until the sample is completely dissolved, then add 1ml of perchloric acid, continue heating to dissolve the sample completely, until no more sparks Take off the white smoke of perchloric acid, take it out and cool it, add 5ml of hydrochloric acid, wash the wall of the dish with a little water, heat until the residue is completely dissolved, cool to room temperature, transfer it into a 100ml volumetric flask, dilute with water to the mark and sh...

Embodiment 2

[0028] Weigh 40g of the slurry from the washing tower reboiler or the slurry distillation device of the organosilicon monomer synthesis unit and place it in a 500ml beaker, add 200ml of ethanol to completely soak the slurry, stir and let it stand for 2 hours before the slurry The solution was filtered with suction, and then the filter cake was dried in an oven at 60°C for 2 hours.

[0029] After cooling, weigh 0.4g into the crucible, add 10ml of hydrofluoric acid, and after the violent reaction stops, add nitric acid dropwise until the sample is completely dissolved, then add 1ml of perchloric acid, continue heating to dissolve the sample completely, until no more sparks Take off the white smoke of perchloric acid, take it out and cool it, add 5ml of hydrochloric acid, wash the wall of the dish with a little water, heat until the residue is completely dissolved, cool to room temperature, transfer it into a 100ml volumetric flask, dilute with water to the mark and shake well, us...

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Abstract

The invention discloses an analysis method for detecting the elemental copper in organosilicone slag slurry. The method is mainly characterized in that when an organosilicone monomer is produced, slaggenerated by an organosilicone monomer synthesizer is subjected to chemical reagent treatment so as to enable the slag to lose the activity, then the slag slurry is subjected to high-temperature digestion by using hydrofluoric acid and nitric acid, the elements such as silicon and fluorine are removed by using perchloric acid, finally, the slag is prepared into a sample solution by using hydrochloric acid, and the content of the copper element in the sample solution is measured under the selected optimal measurement condition by utilizing an inductively coupled plasma spectrometer. Practice proves that the chemical activity of the slag slurry treated through the method is reduced, the safety is enhanced, the experimental operation steps are simple, the detection result of the element of the copper is accurate, and guidance data are provided for guiding the monomer synthesis production process adjustment and recycling the metal copper in the slag slurry in the subsequent process.

Description

technical field [0001] The invention belongs to the field of chemical organosilicon production and provides an analysis method for detecting elemental copper in organosilicon slurry. Background technique [0002] With the improvement of our people's living standards and comprehensive national strength, the demand for organosilicon monomers and organosilicon materials is increasing rapidly. According to statistics, in 2016, the global organosilicon monomer production capacity was 5.53 million tons, and the domestic production capacity accounted for 50%. In the process of synthesizing organosilicon monomer, a certain amount of copper powder is needed as a catalyst, and the usage ratio is about 2.5- 3.5kg / t, the copper powder catalyst is taken out of the fluidized bed through the cyclone separator and exists in the by-product slurry. For the organosilicon monomer unit with an annual production capacity of 400,000 tons / year, it is conservatively estimated that about 500 tons of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 颜昌锐周魁周治国温丽崔宜
Owner 湖北环宇化工有限公司
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