Preparation method and application of polymer hydrogel for detecting volatile phenolic compounds

By preparing a polymer hydrogel containing a phenolic compound sensitive indicator, the problem of complex detection of volatile phenolic compounds in the prior art has been solved, and a rapid, simple and sensitive detection effect has been achieved.

CN121495053APending Publication Date: 2026-02-10DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202411089318.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-08-08
Publication Date
2026-02-10

AI Technical Summary

Technical Problem

Existing technologies are not suitable for the rapid, convenient, and sensitive detection of volatile phenolic compounds. Gas chromatography requires complex instrument operation, and spectrophotometry cannot directly respond to volatile phenolic gases.

Method used

A polymer hydrogel containing a phenolic compound sensitive indicator was prepared by reacting polyethylene glycol, polyvinylpyrrolidone, acrylamide and other materials to form a hydrogel, adding 4-aminoantipyrine and potassium ferricyanide indicators, reacting under ultraviolet light, and drying for the detection of volatile phenolic compounds.

Benefits of technology

It achieves highly sensitive and stable detection of volatile phenolic compounds, requiring only 10 minutes of contact reaction for color development, and is easy to operate.

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Abstract

The invention discloses a preparation method of polymer hydrogel for detecting volatile phenolic compounds, and the method at least comprises the following steps: 1, dispersing polyethylene glycol, polyvinylpyrrolidone and acrylamide in water, adding an indicator solution and an initiator, reacting, and adding an alkaline reagent to obtain transparent hydrogel; 2, the transparent hydrogel obtained in the step 1 is soaked in water and dried, the polymer hydrogel for detecting the volatile phenolic compounds is obtained, and indicators in the indicator solution are 4-aminoantipyrine and potassium ferricyanide. The hydrogel can react with volatile gas of phenolic compounds at room temperature, is high in sensitivity, good in stability and visible in result, and is suitable for application scenes such as timely and effective monitoring of the volatile phenolic compound emission process in related factories.
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Description

Technical Field

[0001] This application relates to a method for preparing a polymer hydrogel for detecting volatile phenolic compounds and its application, belonging to the field of rapid detection of volatile gases. Background Technology

[0002] Volatile phenolic compounds generally refer to phenolic compounds with boiling points below 230°C, which can evaporate with water vapor. Volatile phenolic compounds are toxic to humans; acute poisoning symptoms include vomiting, diarrhea, and dizziness, while long-term exposure may lead to headaches, rashes, itching, anemia, and neurological symptoms. Due to their wide range of industrial applications and potential environmental risks, volatile phenolic compounds require strict management and control during production, use, and emission; therefore, monitoring of these compounds is necessary.

[0003] Existing methods for detecting volatile phenolic compounds mainly include gas chromatography and spectrophotometry. Gas chromatography offers high sensitivity and accuracy, but requires specialized instruments and is relatively cumbersome to operate. Spectrophotometry uses chemical colorimetric reagents to react with phenols under specific conditions to generate color products, primarily targeting volatile phenolic compounds in aqueous media, but it cannot directly and effectively respond to volatile phenolic gaseous compounds. Both of these methods have limitations in practical applications; therefore, there is a need to develop a simple, sensitive, and visual colorimetric detection method for the rapid detection of volatile phenolic gaseous compounds in the environment.

[0004] Polymer hydrogels are composed of functional polymers and have a three-dimensional network structure. They contain hydrophilic groups and have a strong adsorption effect on water, which can provide an aqueous environment for chemical reactions and is beneficial for the preservation of chemical reagents. Therefore, they have broad application prospects in the field of analytical chemistry. Summary of the Invention

[0005] The purpose of this invention is to provide a polymer hydrogel containing a phenolic compound sensitive indicator. This hydrogel can directly react with phenolic compound gas, exhibiting high sensitivity, good stability, and wide applicability.

[0006] According to one aspect of this application, a method for preparing a polymer hydrogel for detecting volatile phenolic compounds is provided, the method comprising at least the following steps:

[0007] Step 1: Disperse polyethylene glycol, polyvinylpyrrolidone, and acrylamide in water to form a mixture, add indicator solution and initiator, react, add alkaline reagent, and obtain transparent hydrogel;

[0008] Step 2: Immerse the transparent hydrogel obtained in Step 1 in deionized water, dry it, and obtain a polymer hydrogel for detecting volatile phenolic compounds;

[0009] The indicator in the indicator solution is 4-aminoantipyrine and potassium ferricyanide.

[0010] Optionally, the mass ratio of polyethylene glycol, polyvinylpyrrolidone, and acrylamide is 1:(1.2-1.8):(3-8).

[0011] Optionally, the mass of the polyethylene glycol is 100 mg.

[0012] The volume of the deionized water is 20 mL.

[0013] Optionally, the concentration of 4-aminoantipyrine in the indicator solution is 20–40 g / L.

[0014] Optionally, the concentration of 4-aminoantipyrine in the indicator solution can be independently selected from any value among 20 g / L, 25 g / L, 30 g / L, 35 g / L, and 40 g / L, or a range between any two of the above points.

[0015] Optionally, the concentration of potassium ferricyanide in the indicator solution is 40–80 g / L.

[0016] Optionally, the concentration of potassium ferricyanide in the indicator solution can be independently selected from any value among 40 g / L, 50 g / L, 60 g / L, 70 g / L, and 80 g / L, or a range between any two of the above points.

[0017] Optionally, the initiator is selected from at least one of hydrogen peroxide, potassium persulfate, and cerium ammonium nitrate.

[0018] Optionally, the initiator is hydrogen peroxide.

[0019] Optionally, the concentration of the initiator in the mixture is 0.02 to 0.10 mol / L.

[0020] Optionally, the reaction conditions in step one are as follows:

[0021] The reaction was carried out under ultraviolet light irradiation;

[0022] The reaction time is 5 to 10 hours;

[0023] The reaction temperature is 50–80°C.

[0024] Optionally, the alkaline reagent is selected from at least one of tetrabutylammonium hydroxide, sodium hydroxide, and potassium hydroxide.

[0025] Optionally, the alkaline reagent is tetrabutylammonium hydroxide.

[0026] Optionally, the concentration of the alkaline reagent in the mixture is 1 to 2 mol / L.

[0027] Optionally, the drying time in step two is 8 to 12 hours;

[0028] The drying temperature is 30-35℃.

[0029] According to another aspect of this application, an application of a polymer hydrogel for detecting volatile phenolic compounds is provided, wherein the volatile phenolic compounds react with the polymer hydrogel for detecting volatile phenolic compounds upon contact.

[0030] Optionally, the volatile phenolic compound is selected from at least one of phloroglucinol, hydroquinone, catechol, and resorcinol.

[0031] Optionally, the contact reaction time is 5 to 10 minutes.

[0032] The beneficial effects that this application can produce include:

[0033] 1) The polymer hydrogel constructed for the detection of volatile phenolic compounds has high stability and good repeatability because it is rich in water molecules and can provide an aqueous environment for the indicator used for the detection of volatile phenolic compounds.

[0034] 2) The polymer hydrogel constructed for the detection of volatile phenolic compounds can directly measure phenolic compound gases. It only requires 10 minutes of contact reaction to obtain obvious color change results. It has high detection sensitivity and is easy to operate. Attached Figure Description

[0035] Figure 1 This application describes the colorimetric effect of a polymer hydrogel containing a phenolic compound sensitive indicator on the detection of volatile phenolic compounds. Detailed Implementation

[0036] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments.

[0037] Unless otherwise specified, all raw materials used in the embodiments of this application were purchased through commercial channels.

[0038] Example 1.

[0039] Preparation of a polymeric hydrogel containing a phenolic compound sensitive indicator: Polyethylene glycol, polyvinylpyrrolidone, and acrylamide were dispersed in water at a mass ratio of 1:1.2:3, with 100 mg of polyethylene glycol and 20 mL of water. 2 mL of 40 g / L 4-aminoantipyrine and 80 g / L potassium ferricyanide were added to the solution, and after thorough mixing, hydrogen peroxide was added as an initiator to a concentration of 0.10 mol / L. The mixture was reacted under ultraviolet light for 8 hours, with 1 mL of 1 mol / L tetrabutylammonium hydroxide added dropwise during the reaction to obtain a transparent hydrogel. The transparent hydrogel was then immersed in deionized water to remove unreacted monomers and initiator, and dried in a 35°C oven for 8 hours to constant weight, yielding a polymeric hydrogel capable of testing volatile phenolic compound gases.

[0040] Example 2.

[0041] Preparation of a polymeric hydrogel containing a phenolic compound sensitive indicator: Polyethylene glycol, polyvinylpyrrolidone, and acrylamide were dispersed in water at a mass ratio of 1:1.8:8, with 100 mg of polyethylene glycol and 20 mL of water. 2 mL of 30 g / L 4-aminoantipyrine and 60 g / L potassium ferricyanide were added to the solution, and the mixture was thoroughly mixed. Hydrogen peroxide was added as an initiator to a concentration of 0.05 mol / L. The mixture was reacted under ultraviolet light for 10 hours, with 0.8 mL of 1.5 mol / L tetrabutylammonium hydroxide added dropwise during the reaction to obtain a transparent hydrogel. The transparent hydrogel was then immersed in deionized water to remove unreacted monomers and initiator, and dried in a 35°C oven for 12 hours to constant weight, yielding a polymeric hydrogel capable of testing volatile phenolic compound gases.

[0042] Example 3.

[0043] Preparation of a polymeric hydrogel containing a phenolic compound sensitive indicator: Polyethylene glycol, polyvinylpyrrolidone, and acrylamide were dispersed in water at a mass ratio of 1:1.5:5, with 100 mg of polyethylene glycol and 20 mL of water. 2 mL of 20 g / L 4-aminoantipyrine and 40 g / L potassium ferricyanide were added to the solution, and the mixture was thoroughly mixed. Hydrogen peroxide was added as an initiator to a concentration of 0.02 mol / L. The mixture was reacted under ultraviolet light for 5 hours, with 0.5 mL of 1.8 mol / L tetrabutylammonium hydroxide added dropwise during the reaction to obtain a transparent hydrogel. The transparent hydrogel was then immersed in deionized water to remove unreacted monomers and initiator, and dried in a 35°C oven for 10 hours to constant weight to obtain a polymeric hydrogel capable of testing volatile phenolic compound gases.

[0044] Example 4.

[0045] The polymeric hydrogel prepared in Example 1 was reacted with volatile phenolic compounds, including phloroglucinol (10 ppm), hydroquinone (10 ppm), catechol (10 ppm), and resorcinol (10 ppm), at room temperature for 10 minutes. Visible results were observed. Figure 1 The hydrogels containing phloroglucinol, hydroquinone, catechol, and resorcinol exhibit significant color changes; see [link to details]. Figure 1 .

[0046] Comparative Example 1

[0047] The polymer-type hydrogel prepared using Example 1 does not come into contact with volatile phenolic compounds, and the hydrogel's color is visible. Figure 1 The control group.

[0048] Comparative Example 2

[0049] A mixed indicator solution of 2 mL of 4-aminoantipyrine (concentration 40 g / L) and potassium ferricyanide (concentration 80 g / L) was spotted onto porous filter paper. After drying, the sample was exposed to volatile phenolic compounds for 10 minutes. The color of the spotted indicator did not change.

[0050] The above description is merely a few embodiments of this application and is not intended to limit this application in any way. Although this application discloses preferred embodiments as described above, it is not intended to limit this application. Any changes or modifications made by those skilled in the art without departing from the scope of the technical solution of this application using the disclosed technical content are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. A method for preparing a polymer hydrogel for detecting volatile phenolic compounds, characterized in that, The method includes at least the following steps: Step 1: Disperse polyethylene glycol, polyvinylpyrrolidone, and acrylamide in water to form a mixture, add indicator solution and initiator, react, add alkaline reagent, and obtain transparent hydrogel; Step 2: Immerse the transparent hydrogel obtained in Step 1 in [the solution], dry it, and obtain a polymer hydrogel by detecting volatile phenolic compounds; The indicator in the indicator solution is 4-aminoantipyrine and potassium ferricyanide.

2. The preparation method according to claim 1, characterized in that, The mass ratio of polyethylene glycol, polyvinylpyrrolidone, and acrylamide is 1:(1.2-1.8):(3-8).

3. The preparation method according to claim 1, characterized in that, The concentration of 4-aminoantipyrine in the indicator solution is 20–40 g / L; Preferably, the concentration of potassium ferricyanide in the indicator solution is 40–80 g / L.

4. The preparation method according to claim 1, characterized in that, The initiator is selected from at least one of hydrogen peroxide, potassium persulfate, and cerium ammonium nitrate. Preferably, the concentration of the initiator in the mixture is 0.02 to 0.10 mol / L.

5. The preparation method according to claim 1, characterized in that, The reaction conditions in step one are as follows: The reaction was carried out under ultraviolet light irradiation; The reaction time is 5 to 10 hours; The reaction temperature is 50–80°C.

6. The preparation method according to claim 1, characterized in that, The alkaline reagent is selected from at least one of tetrabutylammonium hydroxide, sodium hydroxide, and potassium hydroxide; Preferably, the concentration of the alkaline reagent in the mixture is 1 to 2 mol / L.

7. The preparation method according to claim 1, characterized in that, In step two The drying time is 8 to 12 hours; The drying temperature is 30-35℃.

8. An application of a polymer hydrogel for detecting volatile phenolic compounds, characterized in that, The volatile phenolic compounds react with the polymer hydrogel used to detect the volatile phenolic compounds; The polymer hydrogel for detecting volatile phenolic compounds is prepared by the preparation method according to any one of claims 1 to 7.

9. The application according to claim 8, characterized in that, The volatile phenolic compound is selected from at least one of phloroglucinol, hydroquinone, catechol, and resorcinol.

10. The application according to claim 8, characterized in that, The contact reaction time is 5 to 10 minutes.