Nanogold enrichment tube and preparation method thereof, and device and method for sampling mercury in flue gas

A sampling device and nano-gold technology, applied in sampling devices, chemical instruments and methods, separation methods, etc., can solve problems such as inapplicability to mercury, penetration, poor repeatability, and inability to collect particulate mercury.

Pending Publication Date: 2021-08-31
福建省锅炉压力容器检验研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

①Since mercury exists in three forms in flue gas, namely elemental mercury Hg 0 , mercury oxide Hg 2+ and particulate mercury Hg p , this method cannot collect particulate mercury Hg in flue gas p
②SO in flue gas 2 , NO x It will inhibit the capture of mercury by activated carbon, mainly because the moisture content of flue gas is extremely high after desulfurization, SO 2 , NO x Acid mist is formed, and SO 2 , NO x The molecular polarity itself is strong, and the binding ability of the activated carbon exceeds that of the halogen and the activated carbon, so that the halogen with a strong binding ability to mercury is pushed away from the activated carbon, resulting in the ability of the adsorption tube to capture mercury in the flue gas and the stability of the complex. Significantly decreased, resulting in various results such as penetration, poor repeatability, etc.
Therefore, activated carbon is not suitable for sampling mercury in flue gas from solid waste incineration.
③ Only the flue position with low concentration of particulate matter can be collected (after dust removal), because high dust will block the fine-grained activated carbon, resulting in failure to sample normally
④ Activated carbon sampling and adsorption tubes are expensive and cannot be reused. On-site pre-test is required, and the test cost is high
⑤ Mercury captured by activated carbon is easy to re-release into the environment because its volatile properties have not changed, resulting in low test results

Method used

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  • Nanogold enrichment tube and preparation method thereof, and device and method for sampling mercury in flue gas
  • Nanogold enrichment tube and preparation method thereof, and device and method for sampling mercury in flue gas

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preparation example Construction

[0024] The present invention provides a kind of preparation method of nano-gold enrichment tube, comprising the following steps:

[0025] Step 1: put the carrier into 10% dilute nitric acid solution, heat and boil for 1 hour, wash it with distilled water several times, dry it at a constant temperature of 110°C for 1 hour, and cool it for later use;

[0026] Step 2: Add 0.1-0.2M sodium borohydride solution 3-5mL and 0.9-1.0wt% tetrakis hydroxymethyl phosphorus chloride solution 1-2mL in 100mL of 0.01-0.03% tetrachloroauric acid solution, at 1000r / min heated and stirred at a temperature of 70° C. to obtain a brown gold sol;

[0027] Step 3: Continue heating and stirring the gold sol, and at the same time add 1.0-4.0 mL of a 1% trisodium citrate solution to prepare gold nanoparticles with a particle size of 10-30 nm;

[0028] Step 4: Immerse the carrier obtained in step 1 in the mixed solution obtained in step 3 with uniform stirring, and then put it into a microwave oven to hea...

Embodiment 1

[0057] A preparation method of nano-gold enrichment tube, comprising the following steps:

[0058] Step 1: put the carrier into 10% dilute nitric acid solution, heat and boil for 1 hour, wash it with distilled water several times, dry it at a constant temperature of 110°C for 1 hour, and cool it for later use;

[0059] Step 2: Add 0.15M sodium borohydride solution 4mL and 0.95wt% tetrakishydroxymethyl phosphorus chloride solution 1.5mL in the 0.02% tetrachloroauric acid solution of 100mL, with the rotating speed of 1000r / min, the temperature condition of 70 ℃ Heat and stir to obtain brown gold sol;

[0060] Step 3: continuously heating and stirring the gold sol, and adding 2.5 mL of a 1% trisodium citrate solution at the same time to obtain gold nanoparticles with a particle size of 20 nm;

[0061] Step 4: Immerse the carrier obtained in step 1 in the mixed solution obtained in step 3 with uniform stirring, and then put it into a microwave oven for heating and drying with a m...

Embodiment 2

[0065] A preparation method of nano-gold enrichment tube, comprising the following steps:

[0066] Step 1: put the carrier into 10% dilute nitric acid solution, heat and boil for 1 hour, wash it with distilled water several times, dry it at a constant temperature of 110°C for 1 hour, and cool it for later use;

[0067] Step 2: Add 0.1M sodium borohydride solution 3mL and 0.9wt% tetrakishydroxymethyl phosphorus chloride solution 1mL in 100mL of 0.01% tetrachloroauric acid solution, carry out with the rotating speed of 1000r / min, the temperature condition of 70 ℃ Heat and stir to obtain brown gold sol;

[0068] Step 3: continuously heating and stirring the gold sol, and adding 1 mL of a 1% trisodium citrate solution at the same time to obtain gold nanoparticles with a particle size of 10 nm;

[0069] Step 4: Immerse the carrier obtained in step 1 in the mixed solution obtained in step 3 with uniform stirring, and then put it into a microwave oven for heating and drying with a m...

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Abstract

The invention relates to the technical field of environmental monitoring, in particular to a nanogold enrichment tube and a preparation method thereof, and a device and a method for sampling mercury in flue gas. The nanogold enrichment tube prepared by the preparation method has the advantages of large specific surface area, strong adsorption activity, high repeated utilization rate and the like, and can complete efficient enrichment of mercury in a short time. According to the sampling device adopting the nanogold enrichment tube and the corresponding sampling method, the content of the particulate mercury is measured by separating and capturing the particulate mercury and the gaseous mercury in the flue gas; and by utilizing the trapping capability of the nanogold on the gaseous mercury, the content of the gaseous mercury in the flue gas is accurately sampled and measured.

Description

technical field [0001] The invention relates to the technical field of environmental monitoring, in particular to a nano-gold enrichment tube and a preparation method thereof, and a sampling device and method for mercury in flue gas. Background technique [0002] At present, 1,900 to 2,200 tons of mercury are emitted into the atmosphere by man-made pollution sources around the world every year, of which 70% are emitted from coal combustion and solid waste incineration. . With the official signing of the international "Minamata Convention on Mercury" in 2013, the problem of mercury pollution has gradually been paid attention to by various countries. The UNEP research report shows that my country has become the hardest hit area of ​​mercury pollution, and the problem of controlling mercury pollution is imminent. At present, with the rapid development of the domestic solid waste incineration industry, the atmospheric mercury emissions caused by solid waste incineration are on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/24G01N1/22G01N1/34B01J20/02B01D15/10B01J20/28B01J20/30
CPCG01N1/24G01N1/2258G01N1/34B01J20/0233B01D15/10B01J20/28007G01N2001/227
Inventor 陈晖晖陈小韩李恭彦
Owner 福建省锅炉压力容器检验研究院
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