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A method for measuring acetic acid content in biomass pretreatment liquid

A technology for the content of pretreatment liquid and acetic acid, which is used in measuring devices, instruments, scientific instruments, etc., can solve the problems of gas chromatography column and chromatography separation hazards, reduce detection speed, block liquid chromatography column and other problems, and achieve the elimination of matrix effect, simple sample preparation, high detection precision and accuracy

Inactive Publication Date: 2016-08-31
FUJIAN AGRI & FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The complexity of the components of the biomass pretreatment solution (interferences such as formic acid, levulinic acid, polybasic weak acids, etc.) makes the acid-base titration and potentiometric titration methods usually greatly overestimate the acetic acid content in the biomass pretreatment solution, while the ultraviolet-visible Pretreatment solutions with high color values ​​are usually not able to be measured
Although high-performance liquid chromatography and gas chromatography can separate acetic acid from other interfering substances through chromatography; however, the biomass pretreatment liquid contains a large amount of solid particles and non-acetic acid soluble substances (high boiling point substances and inorganic salts, etc.), These will cause great harm to the inlet, column and chromatographic separation of gas chromatography
Of course, larger solid particles can be removed by centrifugation and filtration, but small solid particles that are difficult to remove often block the liquid chromatography column; or affect the chromatographic separation effect of acetic acid, and also generate coke at the inlet of the gas chromatograph or the front end of the chromatographic column; greatly reducing the speed of detection and increasing the cost of determination

Method used

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  • A method for measuring acetic acid content in biomass pretreatment liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1) Accurately measure 1mL of bamboo ethanol pretreatment solution with a pipette gun and place it in a dry headspace bottle, add 50mL sulfuric acid solution (0.2mol / L), shake vigorously until mixed evenly to obtain the test solution, the test solution The concentration of hydrogen ions is 10 -2 mol / L, and placed in an ultrasonic oscillator for 5 minutes to remove air bubbles in the solution to be tested.

[0054] (2) Filter the solution to be tested in (1) with a 0.45mm water filter head, use a micro syringe to accurately measure 5mL of the filtered solution to be tested and add it to a dry headspace bottle (20mL), and use a The aluminum cap of the tetrafluoroethylene / butyl rubber gasket sealed the headspace bottle to obtain the headspace bottle to be tested.

[0055] (3) Place the headspace vial to be tested in (2) in an automatic headspace sampler for equilibration. Measure and record the acetic acid gas chromatography signal value A 0 =151.7. The conditions of t...

Embodiment 2

[0060] (1) Accurately measure 1 mL of eucalyptus dilute acid pretreatment solution with a pipette gun, place it in a dry headspace bottle, add 100 mL of oxalic acid solution (0.1 mol / L), shake vigorously until mixed uniformly to obtain the solution to be tested, and wait for The concentration of hydrogen ions in the solution is 10 -3 mol / L, and placed in an ultrasonic oscillator for 1 minute to remove air bubbles in the solution to be tested.

[0061] (2) Filter the solution to be tested in (1) with a 0.45mm water filter head, use a microsyringe to accurately measure 11mL of the filtered solution to be tested and add it to a dry headspace bottle (20mL), and use a The aluminum cap of the tetrafluoroethylene / butyl rubber gasket sealed the headspace bottle to obtain the headspace bottle to be tested.

[0062] (3) Place the headspace vial to be tested in (2) in an automatic headspace sampler for equilibration. Measure and record the acetic acid gas chromatography signal value A ...

Embodiment 3

[0067] (1) Use a pipette gun to accurately measure 1mL of the southern pine green liquid pretreatment solution and place it in a dry headspace bottle, add 300mL of phosphoric acid solution (2mol / L), shake vigorously until it is evenly mixed to obtain the solution to be tested. The hydrogen ion concentration of the solution was 0.1 mol / L, and placed in an ultrasonic oscillator for 3 minutes to remove air bubbles in the solution to be tested.

[0068] (2) Filter the solution to be tested in (1) with a 0.45mm water phase filter head, use a micro syringe to accurately measure 8mL of the filtered solution to be tested and add it to a dry headspace bottle (20mL), and use a poly The aluminum cap of the tetrafluoroethylene / butyl rubber gasket sealed the headspace bottle to obtain the headspace bottle to be tested.

[0069] (3) Place the headspace vial to be tested in (2) in an automatic headspace sampler for equilibration. Measure and record the acetic acid gas chromatography signal ...

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Abstract

The invention discloses a method for determining acetic acid content in a biomass preprocessing fluid, and relates to the detection of acetic acid content. The method comprises the following steps: adding a non-volatile acid solution to a biomass preprocessing fluid so as to obtain a to-be-detected solution, wherein hydrogen ion concentration of the to-be-detected solution is 10-4mol / L-5.0mol / L; respectively adding the to-be-detected solution and multiple acetic acid standard solutions differing in concentration to different upper-space bottles and sealing to obtain to-be-detected upper-space bottles, wherein the volume of solutions in the to-be-detected upper-space bottles is no more than 0.55mL / mL of the capacity of each upper-space bottle; transferring the acetic acid to a gas chromatograph by virtue of an all-volatile upper-space gas chromatography technology so as to detect a gas chromatography signal value of the acetic acid; and finally, calculating the acetic acid content in the biomass preprocessing fluid. The method for determining the acetic acid content in the biomass preprocessing fluid, disclosed by the invention, has the advantages of being simple and rapid in sample making, high in determination accuracy, good in repeatability and the like, and is widely applied to the detection of the acetic acid content in the biomass preprocessing fluid.

Description

technical field [0001] The present invention relates to the detection of acetic acid content, more specifically, to a detection method of acetic acid content in pretreatment liquid in biomass refining and related fields. Background technique [0002] Acetic acid, a simple carboxylic acid consisting of a methyl group and a carboxyl group, is an important chemical reagent. In the chemical industry, it is used to make polyethylene terephthalate, which is the main part of beverage bottles. Acetic acid is also used to make cellulose acetate for motion picture film and polyvinyl acetate in wood adhesives, as well as many synthetic fibers and fabrics. In households, a dilute solution of acetic acid is often used as a descaling agent. In the food industry, acetic acid is a regulated acidity regulator in the food additive list E260. The annual worldwide demand for acetic acid is about 6.5 million tons. Among them, about 1.5 million tons are recycled, and the remaining 5 million t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 胡会超陈礼辉黄六莲何婷婷杨雪芳
Owner FUJIAN AGRI & FORESTRY UNIV
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