Analysis method for determining furfural content in extract oil and raffinate oil extracted by aromatic hydrocarbons

A technology for extracting aromatics and extracting oil, which is applied in the direction of analyzing materials, measuring devices, material separation, etc., to achieve the effect of simple operation, high precision and good accuracy

Active Publication Date: 2015-05-06
CHINA PETROLEUM & CHEM CORP
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Problems solved by technology

There is no report on the determination method of furfural content in the aromatics extraction oil and raffinate of catalytic oil slurry or back refining oil at present. Establish an accurate, sensitive, fast and simple analysis method for the determination of furfural content in medium, and provide strong technical support for guiding the extraction and production of heavy aromatics in catalytic oil slurry or refined oil

Method used

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  • Analysis method for determining furfural content in extract oil and raffinate oil extracted by aromatic hydrocarbons
  • Analysis method for determining furfural content in extract oil and raffinate oil extracted by aromatic hydrocarbons
  • Analysis method for determining furfural content in extract oil and raffinate oil extracted by aromatic hydrocarbons

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] The establishment of embodiment 1 standard curve

[0069] The analysis conditions are as follows:

[0070] Chromatographic column: stainless steel packed column, 2.4m×3.2mm, fixed solution is 1% SP-1000 (TPA modified polyethylene glycol), and support is 60 / 80 mesh Carbopack B.

[0071] Carrier gas: high-purity nitrogen N 2 , 40mL / min;

[0072] Combustion gas: high-purity hydrogen H 2 , 40mL / min;

[0073] Supporting gas: purified compressed air Air, 400mL / min;

[0074] Injection port temperature: 200°C;

[0075] Column temperature: Initial temperature is 180°C, raised to 200°C at 5°C / min, kept for 3 minutes, then raised to 240°C at 40°C / min;

[0076] Detector temperature: 300°C;

[0077] Balance: Sensitivity is 0.0001g;

[0078] Sample: 4g;

[0079] Formaldehyde: 4mL;

[0080] Constant temperature water bath: 60°C

[0081] Injection volume: 1uL.

[0082] Considering that in the production of heavy aromatics extraction, the content of furfural in catalytic oil...

Embodiment 2

[0086] The investigation of embodiment 2 precision

[0087] Under the analysis condition identical with embodiment 1, with the standard solution that furfural mass concentration is 3.00g / L, measure 6 times, the standard deviation that measures is 0.15g / L, and relative standard deviation is 5.0%; The mg / L standard solution was measured 6 times, the standard deviation was 1.77 mg / L, and the relative standard deviation was 4.4%.

Embodiment 3

[0088] Embodiment 3 standard addition recovery test

[0089] Add 0.050 g of furfural standard substance into 3.950 g of oil slurry to prepare sample A, and its furfural concentration is 1.25% (% (m / m)). Add 0.150g standard substance to 3.850g of extracted oil with a furfural concentration of 0.50% (% (m / m)), prepare sample B, and its furfural concentration is 4.23% (% (m / m)).

[0090] Under the same analytical conditions as in Example 1, sample A and sample B were pretreated, and the two preparations were measured 6 times respectively, and the furfural contained in the two samples was subjected to a standard addition recovery experiment, and the results are shown in the table 2. Table 3, the relative standard deviation of the determination is Figure 4 It is the analysis chromatogram of the methanol extraction sample of sample B. The retention time of the furfural chromatographic peak is 3.831min. It can be seen that the furfural analysis of the oil sample has no interference....

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Abstract

The invention relates to an analysis method for determining furfural content in extract oil and raffinate oil extracted by aromatic hydrocarbons, which employs steps of employing a polarity packed column and optimizing chromatographic analysis condition for completely separate a furfural component. Preferably, a methanol solvent and rotation separating are employed for extracting furfural in extract oil and raffinate oil extracted by aromatic hydrocarbons. A furfural standard sample is used, a furfural quantitative work curve is drafted by linear regression based on least square method, furfural content of the sample in the methanol extract can be obtained by using an external standard method, and then the furfural content of the sample can be calculated. The analysis method has the characteristics of high accuracy, low detection limit, fast analysis speed and simple operation, application prospect is wide, and the analysis method provides powerful technical support for guiding extracting production and scientific research of heavyweight aromatic hydrocarbon in catalyzed oil slurry or recycle oil.

Description

technical field [0001] The present invention relates to an analysis method for the determination of furfural content in aromatic hydrocarbon extraction oil and raffinate oil, in particular to a method for quantitative analysis of furfural content in catalytic oil slurry or re-refined aromatics extraction oil and raffinate oil by gas chromatography Methods. Background technique [0002] In oil refining production, furfural is used as a solvent to extract heavy aromatics from catalytic oil slurry or refined oil to obtain high-purity heavy aromatics and high-quality wax oil. This is an advanced production process, from the bottom of the extraction tower Both the extracted aromatics and the raffinate from the top of the extraction tower contain a large amount of furfural solvent, which needs to be recovered for recycling. At the same time, qualified extracted oil heavy aromatics and raffinate wax oil are obtained, which are required to be extracted during production. The furfur...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 赵惠菊王忠罗光刘明清万义芳贾咏梅蔡伟
Owner CHINA PETROLEUM & CHEM CORP
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