A water-sensitive fluorescent capillary based on aminosilanized zinc oxide and its preparation method and application

An aminosilanization and capillary technology, which is applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the problems of high environmental requirements, insensitive end point, and long measurement time, and achieve a portable detection system and intuitive quantitative methods , the effect of short detection time

Active Publication Date: 2018-10-12
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The co-distillation method is to co-distill the oil sample with the same volume of solvent such as toluene, and the toluene will take out the water in the oil product. The volume ratio of the latter to the original sample is the water content of the sample. The measurement error of this method is large , only suitable for the determination of constant moisture; Karl Fischer method is a common method for the determination of moisture in oil, and its titration solution involves the use of iodine, sulfur dioxide, pyridine, methanol and other substances, which are prone to side reactions. Insensitive, poor reproducibility, this method is suitable for the determination of trace moisture, but there are troublesome operations, the use of Cal . Most of the Fischer reagents are toxic, poor in accuracy, and take a long time to measure. Although gas chromatography is easy to operate and is suitable for the determination of a large number of samples, the instrument is large, expensive, time-consuming, and requires high environmental requirements, which is not conducive to on-site detection and Product Process Control

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  • A water-sensitive fluorescent capillary based on aminosilanized zinc oxide and its preparation method and application
  • A water-sensitive fluorescent capillary based on aminosilanized zinc oxide and its preparation method and application
  • A water-sensitive fluorescent capillary based on aminosilanized zinc oxide and its preparation method and application

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Effect test

Embodiment 1

[0037] A water-sensitive fluorescent capillary based on aminosilanized nano-zinc oxide, which is composed of capillary and aminosilanized nano-zinc oxide (APS-ZnO) cured on the inner surface of the capillary, and the loading of APS-ZnO on the inner surface of the capillary is 0.03mg / mm 2 ; The APS-ZnO is a colorless transparent sol.

[0038] The capillary is a colorless and transparent glass capillary with openings at both ends, with an inner diameter of 1.0 mm, a thickness of 0.08 mm, and a length of 10.0 cm.

[0039] The water-sensitive fluorescent capillary based on aminosilanized nano zinc oxide has a colorless and transparent initial color and a size of about 3 nm.

[0040] The preparation method comprises the following steps:

[0041] 1) Preparation of fluorescent APS-ZnO water-sensitive nanosol: Zn(AC) 2 2H 2 O was dissolved in absolute ethanol at a concentration of 0.066 g / mL, sonicated at room temperature for 10 min, and then LiOH·H 2 O, Zn(AC) 2 2H 2 O and Li...

Embodiment 2

[0045] 1) Preparation of fluorescent APS-ZnO water-sensitive nanosol: Zn(AC) 2 2H 2 O was dissolved in absolute ethanol at a concentration of 0.033 g / mL, sonicated at room temperature for 10 min, and then LiOH·H 2 O, Zn(AC) 2 2H 2 O and LiOH·H 2 The ratio of the amount of O to the substance is 1.0, and continue to sonicate until it is completely dissolved to obtain a nano-zinc oxide material. Ethoxysilane, the ratio of 3-aminopropyltriethoxysilane to the amount of zinc oxide in the nano-zinc oxide material is 1: 40, sealed, protected from light, stirred at room temperature overnight, to obtain fluorescent APS-ZnO water sensitive nano sol;

[0046] 2) Hydrophobic treatment of the capillary: soak the capillary matrix material in a mixed solution of concentrated sulfuric acid and hydrogen peroxide with a volume ratio of 7:3 for 12 h, wash off the excess acid on the surface with water, and introduce hydroxyl groups on the surface, dry it and soak it in ten In the ethanol sol...

Embodiment 3

[0049] 1) Preparation of fluorescent APS-ZnO water-sensitive nanosol: Zn(AC) 2 2H 2 O was dissolved in absolute ethanol at a concentration of 0.011 g / mL, sonicated at room temperature for 10 min, and then LiOH·H 2 O, Zn(AC) 2 2H 2 O and LiOH·H 2 The ratio of the amount of O to the substance is 1.4, continue to sonicate until it is completely dissolved, and obtain a nano-zinc oxide material. The concentration of zinc oxide in the nano-zinc oxide material is 0.050mol / L, and then add 3-aminopropyl three Ethoxysilane, the ratio of 3-aminopropyltriethoxysilane to the amount of zinc oxide in the nano-zinc oxide material is 1: 60, sealed, protected from light, stirred at room temperature overnight, to obtain fluorescent APS-ZnO water-sensitive nano sol;

[0050] 2) Hydrophobic treatment of the capillary: soak the capillary matrix material in a mixed solution of concentrated sulfuric acid and hydrogen peroxide with a volume ratio of 7:3 for 12 h, wash off the excess acid on the s...

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Abstract

The invention discloses a water-sensitive fluorescent capillary tube based on amino silanization zinc oxide as well as a preparation method and application of the water-sensitive fluorescent capillary tube. The water-sensitive fluorescent capillary tube consists of a capillary tube and amino silanization zinc oxide (APS-ZnO) which is cured on the surface inside the capillary tube. As silanization nano zinc oxide sol with fluorescence characteristics and water sensitivity is prepared and cured on the surface of a capillary substrate material, the APS-ZnO water-sensitive capillary tube can be prepared, a sample solution can be automatically sucked due to the own capillary function of the capillary tube, and due to the ZnO fluorescence quenching property caused by hydrolysis of an APS-ZnO material, the moisture content of an organic sample can be judged according to fluorescent intensity. Reagents used in the water-sensitive fluorescent capillary tube are safe and non-toxic and simple to operate, and both quantitative analysis and qualitative testing can be achieved; no complex instrument operation is involved, and the water-sensitive fluorescent capillary tube has the characteristics of being low in cost, convenient to carry and integral in design, the quantitative mode is visible, rapid and high in sensitivity, and the water-sensitive fluorescent capillary tube has the advantages of being rapid in detection, sensitive, automatic, micro-scale, convenient in on-site rapid test application, and the like.

Description

technical field [0001] The invention belongs to the field of energy and chemical detection, and relates to a water-sensitive fluorescent capillary based on aminosilanized nano-zinc oxide and a preparation method thereof, which can be applied to rapid detection of moisture in oil plants. Background technique [0002] Petroleum and its products are often mixed with some water, which may be introduced during the storage and transportation process, and the oil itself has a certain degree of water absorption, and can absorb and dissolve part of the water from the atmosphere or contact with water. There are roughly three forms of water in petroleum, including: suspended water, which is more common in crude oil and residual fuel oil; emulsified water, which is evenly dispersed in oil with very fine microbeads, and is difficult to separate; dissolved water, which generally exists in aviation fuel. In particular, the moisture in these oils is likely to cause varying degrees of damag...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64C09K11/06C09K11/54
CPCC09K11/06C09K11/54C09K2211/10G01N21/64
Inventor 王桦李淑英郑滢亭鲁叶白玉龙张营窦晓萌
Owner QUFU NORMAL UNIV
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