阅读说明：本技术 含水量检测试剂及检测液体中含水量的方法 (Water content detection reagent and method for detecting water content in liquid ) 是由 王允军 翟伟 于 2020-04-24 设计创作，主要内容包括：本申请公开了一种含水量检测试剂及检测液体中含水量的方法。含水量检测试剂,包括：有机溶剂；A<Sub>4</Sub>BX<Sub>6</Sub>型钙钛矿量子点,分散于所述有机溶剂中,其中,A为一价阳离子,B为二价阳离子,X为一价阴离子；该含水量检测试剂用于检测液体中的含水量。该含水量检测试剂与荧光检测技术相结合,检测灵敏度高,使用寿命长,可有效检测液体中低至0.03wt％的含水量。(The application discloses a water content detection reagent and a method for detecting water content in liquid. A water content detecting reagent comprising: an organic solvent; a. the 4 BX 6 The perovskite-type quantum dots are dispersed in the organic solvent, wherein A is monovalent cation, B is divalent cation, and X is monovalent anion; the water content detection reagent is used for detecting the water content in liquid. The water content detection reagent is combined with a fluorescence detection technology, has high detection sensitivity and long service life, and can effectively detect the water content of as low as 0.03 wt% in liquid.)

1. A water content detecting reagent, comprising:

an organic solvent;

A₄BX₆the perovskite-type quantum dots are dispersed in the organic solvent, wherein A is monovalent cation, B is divalent cation, and X is monovalent anion;

the water content detection reagent is used for detecting the water content in liquid.

2. The reagent for detecting water content according to claim 1, wherein the polarity parameter of the organic solvent is less than 3.

3. The reagent for detecting water content according to claim 1, wherein the organic solvent comprises at least one of n-pentane, toluene, n-hexane, cyclohexane, n-heptane, and cyclooctane.

4. The reagent for detecting water content according to claim 1, wherein A is contained in the organic solvent₄BX₆The concentration of the perovskite quantum dots is less than 3 wt%.

5. The reagent for detecting water content according to claim 4, wherein A is contained in the organic solvent₄BX₆The concentration of the perovskite quantum dots is 0.1 wt% to 2 wt%.

6. The moisture content test of claim 1The test agent is characterized in that A is Cs⁺Or Rb⁺B is Pb²⁺、Ge²⁺Or Sn²⁺Wherein X is Cl^-、Br^-Or I^-At least one of (1).

7. The reagent for detecting water content according to claim 6, wherein A is a₄BX₆The perovskite quantum dot comprises Cs₄PbCl₆、Rb₄PbCl₆、Cs₄GeCl₆、Rb₄GeCl₆、Cs₄SnCl₆、Rb₄SnCl₆、Cs₄PbBr₆、Rb₄PbBr₆、Cs₄GeBr₆、Rb₄GeBr₆、Cs₄SnBr₆、Rb₄SnBr₆、Cs₄PbI₆、Rb₄PbI₆、Cs₄GeI₆、Rb₄GeI₆、Cs₄SnI₆、Rb₄SnI₆、Cs₄PbBr₃I₃、Rb₄PbBr₃I₃、Cs₄PbCl₃Br₃、Rb₄PbCl₃Br₃、Cs₄SnBr₃I₃、Rb₄SnBr₃I₃、Cs₄SnCl₃Br₃、Rb₄SnCl₃Br₃、Cs₄GeBr₃I₃、Rb₄GeBr₃I₃、Cs₄GeCl₃Br₃Or Rb₄GeCl₃Br₃At least one of (1).

8. A method of detecting the water content of a liquid, comprising the steps of:

mixing the water amount detecting reagent according to any one of claims 1 to 7 with a liquid to be detected, and detecting the fluorescence intensity thereof;

and comparing the fluorescence intensity with a water content-fluorescence intensity standard curve of the water amount detection reagent to determine the water content in the liquid to be detected.

9. The method of claim 8, wherein the mixing is performed for a period of 1 to 10 minutes.

10. The method for detecting the water content in liquid according to claim 8, wherein the main component of the liquid to be detected is a nonpolar organic solvent.

Technical Field

The application relates to the field of detection, in particular to a water content detection reagent and a method for detecting water content in liquid.

Background

With the development of scientific research and the progress of production technology, the quantitative analysis of water in liquid is listed as one of the basic items of physical and chemical analysis of various substances, and is used as an important quality index of liquid. The determination of the water content in the liquid has important significance in the chemical field, the detection field and the like.

The conventional method for detecting moisture in a substance includes: karl fischer moisture determination, coulomb moisture determination, dew point moisture determination, microwave moisture meter determination, infrared moisture determination, and the like. These methods are not suitable for, or cannot be applied at all for, detecting the water content in a liquid;

the development of a detection reagent or a detection method for the water content in a liquid is of great significance.

Disclosure of Invention

In view of the above technical problems, an object of the present application is to provide a detection reagent that can effectively detect the water content in a liquid.

One aspect of the present application provides a water content detection reagent, comprising:

an organic solvent;

A₄BX₆the perovskite-type quantum dots are dispersed in the organic solvent, wherein A is monovalent cation, B is divalent cation, and X is monovalent anion;

the water content detection reagent is used for detecting the water content in liquid.

In one embodiment, the organic solvent has a polarity parameter of less than 3.

In one embodiment, the organic solvent comprises at least one of n-pentane, toluene, n-hexane, cyclohexane, n-heptane, cyclooctane.

In one embodiment, a is in the organic solvent₄BX₆The concentration of the perovskite quantum dots is less than 3 wt%.

In one embodiment, a is in the organic solvent₄BX₆The concentration of the perovskite quantum dots is 0.1 wt% to 2 wt%.

In one embodiment, a is Cs⁺Or Rb⁺B is Pb²⁺、Ge²⁺Or Sn²⁺Wherein X is Cl^-、Br^-Or I^-At least one of (1).

In one embodiment, said a₄BX₆The perovskite quantum dot comprises Cs₄PbCl₆、Rb₄PbCl₆、Cs₄GeCl₆、Rb₄GeCl₆、Cs₄SnCl₆、Rb₄SnCl₆、Cs₄PbBr₆、Rb₄PbBr₆、Cs₄GeBr₆、Rb₄GeBr₆、Cs₄SnBr₆、Rb₄SnBr₆、Cs₄PbI₆、Rb₄PbI₆、Cs₄GeI₆、Rb₄GeI₆、Cs₄SnI₆、Rb₄SnI₆、Cs₄PbBr₃I₃、Rb₄PbBr₃I₃、Cs₄PbCl₃Br₃、Rb₄PbCl₃Br₃、Cs₄SnBr₃I₃、Rb₄SnBr₃I₃、Cs₄SnCl₃Br₃、Rb₄SnCl₃Br₃、Cs₄GeBr₃I₃、Rb₄GeBr₃I₃、Cs₄GeCl₃Br₃Or Rb₄GeCl₃Br₃At least one of (1).

Another aspect of the present application provides a method for detecting water content in a liquid, comprising the steps of:

mixing the water quantity detection reagent with the liquid to be detected, and detecting the fluorescence intensity of the liquid to be detected;

and comparing the fluorescence intensity with a water content-fluorescence intensity standard curve of the water amount detection reagent to determine the water content in the liquid to be detected.

In one embodiment, the mixing process is for a time period of 1 to 10 minutes.

In one embodiment, the main component of the liquid to be detected is a non-polar organic solvent.

Has the advantages that:

1. the present application makes use of A without fluorescence effect₄BX₆ABX with high fluorescence efficiency generated by perovskite quantum dots after meeting water₃The principle of perovskite quantum dots, thereby realizing a detection reagent which is easy to detect the water content in liquid.

2、A₄BX₆The perovskite quantum dots are dispersed in an organic solvent with small polarity parameters, so that external water vapor can be effectively inhibited from acting on A₄BX₆The effect of perovskite quantum dots.

3. The water content detection reagent is combined with a fluorescence detection technology, has high detection sensitivity, and can effectively detect the water content of as low as 0.03 wt% in liquid.

Drawings

FIG. 1 is a graph showing a standard curve of water content versus fluorescence intensity of a water content detecting reagent according to an embodiment of the present application.

Detailed Description

The technical solutions in the examples will be described in detail below with reference to the embodiments of the present application. It should be noted that this embodiment is only a partial way, not a complete one.

As used herein, a statement such as "at least one (one)" modifies an entire list of elements as it precedes or succeeds the list of elements without modifying individual elements of the list. Unless otherwise defined, all terms (including technical and scientific terms) in the specification may be defined as commonly understood by one of ordinary skill in the art. Terms defined in commonly used dictionaries should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present disclosure, and may not be interpreted in an idealized or overly formal sense unless expressly so defined. Furthermore, unless expressly stated to the contrary, the terms "comprises" and "comprising," when used in this specification, specify the presence of stated features, regions, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, regions, integers, steps, operations, elements, components, and/or groups thereof. Thus, the above wording will be understood to mean that the stated elements are included, but not to exclude any other elements.

As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The term "or" means "and/or".

It will be understood that, although the terms first, second, third, etc. may be used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms.

As used herein, "about" or "approximately" includes the stated value and is meant to be within an acceptable range of deviation for the particular value as determined by one of ordinary skill in the art in view of the measurement in question and the error associated with measurement of the particular quantity (i.e., limitations of the measurement system). For example, "about" may mean a deviation from the stated value within one or more standard deviation ranges, or within ± 10%, ± 5%.

In one embodiment of the present application, there is provided a water content detecting reagent including an organic solvent; a dispersed in an organic solvent₄BX₆The perovskite quantum dot comprises a perovskite quantum dot; the water content detection reagent is used for detecting the water content in the liquid.

In the present application, by using A₄BX₆The perovskite quantum dot can generate ABX when meeting water₃The water content detection reagent is prepared by the perovskite quantum dots and the fluorescence enhancement principle. Due to synthetically obtained A₄BX₆The perovskite quantum dot has no fluorescence characteristic (or is very weak and can be basically ignored), and the dispersion liquid under a certain concentration presents milk white color under the room temperature condition, but can be converted into ABX with very high fluorescence efficiency in a short time after being in contact with water₃Perovskite quantum dots. Due to conversion to ABX₃The quantity of the perovskite quantum dots has a direct relation with the water content in the environment to be detected, so that the water content in the liquid to be detected can be determined through the change of the fluorescence intensity.

A₄BX₆The perovskite quantum dots are dispersed in an organic solvent, so that the water content detection reagent is very suitable for detecting the water content in liquid. The water content detection reagent can quantitatively detect the water content in liquid, and only needs to directly mix the water content detection reagent with the liquid to be detected and then measure the change of the fluorescence intensity of the liquid during detection.

In a preferred embodiment, the organic solvent has a polarity parameter of less than 3. That is, the polarity of the organic solvent is very small. The polarity parameters of organic solvents are referred to the solvent handbook. The inventor finds that A is₄BX₆The perovskite quantum dots are very sensitive to water, and A can be caused by a very small amount of water₄BX₆The perovskite quantum dots react to cause the crystal to be recombined. When the polarity parameter of the organic solvent is less than 3, the organic solvent is a solvent havingThe compatibility between the organic solvent and water is poor, and the organic solvent can not absorb the water vapor in the air basically, so that the A can be effectively inhibited₄BX₆The perovskite quantum dots are affected by water vapor in the air, so that the storage and the service life of the water content detection reagent are prolonged.

The organic solvent includes, but is not limited to, n-pentane (polarity parameter 0), toluene (polarity parameter 2.4), n-hexane (polarity parameter 0.06), cyclohexane (polarity parameter 0.1), n-heptane (polarity parameter 0.2), or cyclooctane (polarity parameter 0.1). In addition, other solvents having a polarity parameter of less than 3 can be used as the organic solvent of the water content detection reagent in the present application.

In an organic solvent A₄BX₆The concentration of perovskite quantum dots is less than 3 wt%, more preferably between 0.1 wt% and 2 wt%. Due to A₄BX₆The surface of the perovskite quantum dot generally contains hydrophobic ligands such as oleylamine, oleic acid and the like, A₄BX₆The dispersibility of the perovskite quantum dots in an organic solvent is very good, such as 10 wt% or even 20 wt%. But when A is₄BX₆When the concentration of perovskite-type quantum dots is too high, although these A' s₄BX₆The perovskite quantum dots can be dissolved in an organic solvent, but when the perovskite quantum dots are used for a water content detection reagent, the detection accuracy of the reagent is not high. And when A is an organic solvent₄BX₆When the concentration of the perovskite quantum dots is less than 3 wt%, A can be ensured₄BX₆The perovskite quantum dots are fully and well uniformly dispersed in an organic solvent, A₄BX₆The probability of forming agglomeration among the perovskite quantum dots is very small, so that the detection accuracy is effectively improved.

A₄BX₆The average size of the perovskite quantum dots is preferably between 1 and 20 nanometers. Chemical formula A₄BX₆In which A is Cs⁺Or Rb⁺B is Pb²⁺、Ge²⁺Or Sn²⁺At least one of (1), X is Cl^-、Br^-Or I^-At least one of (1). A. the₄BX₆Perovskite quantumPoints include, but are not limited to, Cs₄PbCl₆、Rb₄PbCl₆、Cs₄GeCl₆、Rb₄GeCl₆、Cs₄SnCl₆、Rb₄SnCl₆、Cs₄PbBr₆、Rb₄PbBr₆、Cs₄GeBr₆、Rb₄GeBr₆、Cs₄SnBr₆、Rb₄SnBr₆、Cs₄PbI₆、Rb₄PbI₆、Cs₄GeI₆、Rb₄GeI₆、Cs₄SnI₆、Rb₄SnI₆、Cs₄PbBr₃I₃、Rb₄PbBr₃I₃、Cs₄PbCl₃Br₃、Rb₄PbCl₃Br₃、Cs₄SnBr₃I₃、Rb₄SnBr₃I₃、Cs₄SnCl₃Br₃、Rb₄SnCl₃Br₃、Cs₄GeBr₃I₃、Rb₄GeBr₃I₃、Cs₄GeCl₃Br₃Or Rb₄GeCl₃Br₃。

A for use in this application₄BX₆The perovskite quantum dots can be prepared by a conventional method. For example, A₄BX₆The perovskite quantum dot is obtained by mixing a first precursor and a second precursor and then heating.

The first precursor is made of Cs⁺Or Rb⁺With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion; the second precursor is made of Pb²⁺、Ge²⁺Or Sn²⁺With at least one of a carboxylic acid anion or a halide anion; at least one of the first precursor and the second precursor comprises a halide anion.

In a specific embodiment of the present application, the first precursor comprises cesium oleate, rubidium oleate, cesium acetate, rubidium acetate, CsCl, CsBr, CsI, Cs₂CO₃、Rb₂CO₃At least one of RbCl or RbBr, the second precursor comprising PbCl₂、PbI₂、PbBr₂、GeCl₂、GeI₂、GeBr₂、SnCl₂、SnI₂Or SnBr₂At least one of (1). However, the exemplary embodiments of the present application are not limited thereto.

In another specific embodiment of the present application, A₄BX₆The preparation step of the perovskite quantum dot also comprises the step of preparing the obtained A₄BX₆And (3) carrying out purification treatment on the perovskite quantum dots to obtain the perovskite quantum dots with high purity. These purification treatment steps are well known in the art and will not be described in detail here.

The preparation of the reagent for measuring water content is very simple, and for example, A can be directly used₄BX₆The perovskite quantum dots can be uniformly dispersed in an organic solvent, and it is noted that the organic solvent used is anhydrous or has a very low water content, such as less than 0.001 wt%.

In one embodiment of the present application, a method of detecting water content in a liquid is disclosed, comprising the steps of: mixing a water quantity detection reagent with liquid to be detected, and detecting the fluorescence intensity of the liquid to be detected; and then, comparing the fluorescence intensity with a standard curve of water content-fluorescence intensity of the water quantity detection reagent so as to determine the water content in the liquid to be detected.

In the application, the obvious fluorescence enhancement phenomenon is detected 1 to 10 minutes after the water quantity detection reagent is mixed with the liquid to be detected, and the fluorescence intensity can be basically maintained unchanged for a long time. The main component of the liquid to be detected is preferably a non-polar organic solvent, such as alkane, alkene, ester, etc., so that the liquid to be detected and the water amount detection reagent can be uniformly mixed in a short time, and the detection accuracy is increased, wherein the main component refers to that the content of the component in the liquid to be detected is more than 95 wt%. In a preferred embodiment, the nonpolar organic solvent in the liquid to be detected and the organic solvent in the water content detection reagent are the same substance, such as n-heptane.

The detection method using the water amount detection reagent according to some exemplary embodiments of the present application will be described in more detail below with reference to examples; however, the exemplary embodiments of the present application are not limited thereto.