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Method for chromatographic determination of crude furfuryl alcohol composition

A determination method and technology of alcohol content, applied in the field of chromatographic analysis, can solve the problems of little attention to the meaning of determination of crude furfuryl alcohol content, inability to effectively guide production, large errors, etc., achieve the best reaction effect, improve product yield and product quality , low cost effect

Active Publication Date: 2010-09-01
濮阳宏业高新科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in actual production, because the factors that affect the reaction, such as furfural raw material quality, catalyst quality, feed amount and reaction temperature, pressure, etc. change at any time, it will inevitably affect the content of the main product furfuryl alcohol in the result of the reaction. In order to understand the reaction Effect, control and adjustment of the reaction are carried out under optimal conditions, it is necessary to monitor the composition and content of furfuryl alcohol; but on the one hand, due to the less attention to the significance of the determination of the content of furfuryl alcohol in the industry, on the other hand, due to the There are too many mechanical and chemical impurities in the medium, and they cannot be directly put into the chromatographic column for chromatographic analysis. Therefore, although there are also chemical methods for determination, at present, only two components can be made and the time is long and the error is large, which cannot effectively guide production.

Method used

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  • Method for chromatographic determination of crude furfuryl alcohol composition
  • Method for chromatographic determination of crude furfuryl alcohol composition
  • Method for chromatographic determination of crude furfuryl alcohol composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The chromatographic determination method of crude furfuryl alcohol, the steps are as follows:

[0023] A, extract a part of crude furfuryl alcohol from the furfuryl alcohol reactor with a sealed container;

[0024] B, take out a part of crude furfuryl alcohol from the sealed container with a syringe, filter with an organic phase nylon needle filter, and the specification of the organic phase nylon needle filter is 13mm*0.22μm;

[0025] c. The relatively clear filtrate filtered out is quickly injected into a gas chromatographic sample injector for sample analysis, and the gas chromatographic conditions are as follows: the gas chromatograph adopts an FID detector, the chromatographic column specification is 30m*0.32mm*0.25 μm, and the carrier gas is nitrogen, The flow rate is 50ml / min; the hydrogen flow rate is 35ml / min, the air is 110ml / min, and the split ratio is 3:1; the makeup is nitrogen, and the flow rate is 25ml / min; 130°C, injection volume 0.1 μL.

[0026] The a...

Embodiment 2

[0031] In the gas chromatography conditions, the carrier gas is nitrogen, the flow rate is 50ml / min; the hydrogen flow rate is 50ml / min, the air is 120ml / min, and the split ratio is 4:1; the makeup is nitrogen, the flow rate is 30ml / min; the temperature of the injector is 190°C , the detector temperature was 190°C, the column temperature was 140°C, and the injection volume was 0.15 μL.

[0032] Others are the same as embodiment 1.

[0033] Its measurement result is:

[0034]

[0035] The chromatogram of sample 4 is shown in figure 2 .

Embodiment 3

[0037] In the gas chromatography conditions, the carrier gas is nitrogen, the flow rate is 50ml / min; the hydrogen flow rate is 40ml / min, the air is 90ml / min, and the split ratio is 5:1; the makeup is nitrogen, the flow rate is 20ml / min; the temperature of the injector is 200°C , the detector temperature was 200°C, the column temperature was 130°C, and the injection volume was 0.2 μL. Other is the same as embodiment 1 precision test

[0038] Get 5 parts of No. 1 sample, filter and measure under the condition of embodiment 1, RSD% is 2.1%. One part of No. 1 sample was weighed, filtered under the conditions of Example 1 and continuously sampled 5 times for measurement, and the RSD% was 0.2%.

[0039] Recovery experiment

[0040] Among the two 100 gram samples, one of them (sample 1) added 5 grams of furfuryl alcohol (alcohol content is 98.9%) and another part of (sample 2) did not handle the sample parallel analysis, did not add furfuryl alcohol sample 2 The content of measure...

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Abstract

The invention belongs to the technical field of chromatographic analysis and particularly relates to a method for the chromatographic determination of crude furfuryl alcohol composition. The method comprises: filtering a sample of crude furfuryl alcohol; and performing gas chromatography of sampled filtrate, wherein the gas chromatography is performed in an FID detector, nitrogen is used as a carrier gas, the hydrogen flow rate is 30 to 50ml / min, the air flow rate is 90 to 120ml / min, the split ratio is 2-5:1, nitrogen is used as a make-up gas, the flow rate of the make-up gas is 16 to 30ml / min, the temperature of a sampler is 190 to 220 DEG C, the temperature of a detector is 190 to 220 DEG C, and the column temperature is 120 to 150 DEG C. In the invention, a complete method for analyzing the crude furfuryl alcohol is established to determine the content of the components of the crude furfuryl alcohol quickly and accurately. The method is simple, quick in detection, low in cost and wide in application range and can create great economic benefits.

Description

(1) Technical field [0001] The invention belongs to the technical field of chromatographic analysis, in particular to a chromatographic determination method for the content of crude furfuryl alcohol. (2) Background technology [0002] Furfuryl alcohol is an important fine chemical raw material, which is mainly used to produce furfuryl alcohol resin, furan resin, etc. Furfuryl alcohol is mainly industrially produced by furfural and hydrogen in the presence of a catalyst. The production unit of this method is divided into four units: batching, reaction, rectification, and finished product storage. The classic process is: mix furfural with catalyst, preheat, mix with hydrogen after preheating, and enter the tubular reactor or reaction The reaction is carried out in the kettle to generate crude furfuryl alcohol, which is cooled by a cooler, and then filtered to separate the catalyst, and then the crude alcohol filtrate is subjected to a rectification process to produce finished ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
Inventor 陈志勇任万法贾贵芳
Owner 濮阳宏业高新科技发展有限公司