Precise electronic moisture-proof storage humidity color-developing indicator card composition

Abstract

The invention discloses a moisture-proof storage humidity color-developing indicator card composition for precision electronics. The moisture-proof storage humidity color-developing indicator card composition comprises the following raw materials in parts by weight: 10-15 parts of ferric sulfate, 3-8 parts of a sulfonic compound and 20 parts of a buffer solution, the sulfonyl compound is prepared by the following steps: S1, adding 1, 3-propane sultone and 2, 2 '-dipyridyl into toluene to prepare an intermediate 1; s2, 4-phenylazo phenol and 1, 6-dibromohexane are added into absolute ethyl alcohol, and an intermediate 2 is prepared; s3, adding the intermediate 2 and the intermediate 1 into N, N-dimethylformamide, and carrying out heat preservation reaction for 24 hours to prepare a sulfonic compound; the sulfonyl compound structurally comprises sulfonate ions, quaternary ammonium salt ions and an azophenol structure, and the quaternary ammonium salt ions have good hygroscopicity and can absorb water vapor in air in time when being used for a color developing agent, so that color change is caused.

Description

Technical Field

[0001] The invention relates to the technical field of color developers, in particular to a precision electronic moisture-proof storage humidity color indicator card composition. Background Art

[0002] When shipping or storing many types of materials, especially electronic and semiconductor components, it is desirable to know whether these components have been exposed to a particular level of humidity in the surrounding atmosphere that could cause damage to these components. For example, electronic components can be damaged by exposure to an atmosphere having humidity exceeding a certain threshold level, even when the threshold level is low and the exposure is only for a short time.

[0003] To meet the needs of detection, humidity indicators have been developed. Most humidity indicator cards manufactured today use cobalt chloride as an indicator, which changes color based on the different degrees of hydration of the cobalt chloride under different humidity environments. Cobalt chloride can change from blue (when it has a hydration of monohydrate) to pink (when it has a hydration of hexahydrate). As the degree of hydration increases, the blue gradually changes to red. Therefore, based on the different colors presented on the card to determine its approximate humidity, an array including different humidity indication areas can be provided on the card, where increasing humidity levels are required to change different indication areas on the card from blue to pink.

[0004] The problem with humidity sensitive coatings for humidity indicator cards using cobalt chloride is that cobalt chloride is a known heavy metal irritant and toxin and cannot be used as a dry humidity indicator card when used in food and pharmaceutical products. Therefore, the application of cobalt chloride humidity indicator cards is not available in the food and pharmaceutical industries.

[0005] At the same time, the 2004 EU environmental regulations (2004 / 73 / EC) listed cobalt chloride as a Class II carcinogen, requiring the prohibition of using humidity indicator cards containing this component in electronic products. Therefore, companies are in urgent need of providing a dry humidity indicator composition that does not contain heavy metal elements such as cobalt as a humidity sensitive coating for dry humidity indicator cards. Summary of the invention

[0006] In order to solve the above technical problems, the present invention provides a precision electronic moisture-proof storage humidity color indicator card composition.

[0007] The purpose of the present invention can be achieved through the following technical solutions: A precision electronic moisture-proof storage humidity color indicator card composition comprises the following raw materials in parts by weight: 10-15 parts of ferric sulfate, 3-8 parts of sulfonic acid compounds, and 20 parts of buffer solution; The sulfonic acid compound is prepared by the following steps: Step S1, adding 1,3-propane sultone and 2,2'-bipyridine to toluene, heating to 35-40°C, stirring at a constant speed for 4 hours, filtering to obtain intermediate 1, wherein the dosage ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene is controlled to be 0.02-0.05mmol:0.02-0.05mmol:10mL; In step S1, 1,3-propane sultone and 2,2'-bipyridine react to prepare intermediate 1, and the structure of intermediate 1 contains sulfonate ions and quaternary ammonium salt ions.

[0008] Step S2, adding 4-phenylazophenol and 1,6-dibromohexane to anhydrous ethanol, heating to 75-80°C, stirring at a uniform speed and sequentially adding potassium carbonate and potassium iodide, continuing stirring and reacting for 24 hours to obtain intermediate 2, wherein the amount ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and anhydrous ethanol is controlled to be 0.01-0.02mmol: 0.05-0.08mmol: 0.22-0.25mmol: 0.01-0.02mmol: 10mL; In step S2, the phenolic hydroxyl group on 4-phenylazophenol reacts with the bromine element on 1,6-dibromohexane to prepare intermediate 2; Step S3, adding intermediate 2 and intermediate 1 to N,N-dimethylformamide, introducing nitrogen to expel air, raising the temperature to 70-80°C, and keeping the temperature for reaction for 24 hours to obtain a sulfonic acid compound, wherein the amount ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide is controlled to be 0.03-0.05mmol:0.08-0.1mmol:10mL.

[0009] In step S3, the bromine element on the intermediate 2 reacts with the pyridine on the intermediate 1 to prepare a sulfonic acid compound; the sulfonic acid compound has a sulfonate ion, a quaternary ammonium salt ion and an azophenol structure in its structure; the quaternary ammonium salt ion has good hygroscopicity and can absorb water vapor in the air in time when used as a developer, causing the pH value of the system to change, thereby affecting the combination of Cu ions and sulfonate ions, thereby causing a color change; and the azophenol structure can form hydrogen bonds with water molecules, thereby causing a color change, further improving the color development performance.

[0010] Furthermore, the buffer solution is 15% by mass of dilute hydrochloric acid.

[0011] Beneficial effects of the present invention: The invention prepares a precision electronic moisture-proof storage humidity color indicator card composition. A sulfonic acid compound is firstly synthesized. In the preparation process, an intermediate 1 is firstly prepared by reacting 1,3-propane sultone and 2,2'-bipyridine. The intermediate 1 contains sulfonate ions and quaternary ammonium salt ions. Then, the phenolic hydroxyl group on 4-phenylazophenol reacts with the bromine element on 1,6-dibromohexane to prepare an intermediate 2. Finally, the bromine element on the intermediate 2 reacts with the pyridine on the intermediate 1 to prepare the sulfonic acid compound. The sulfonic acid compound has a sulfonate ion, a quaternary ammonium salt ion and an azophenol structure. The quaternary ammonium salt ion has good hygroscopicity and can absorb water vapor in the air in time when used as a color developer, resulting in a change in the pH value of the system, thereby affecting the combination of iron ions and sulfonate ions, thereby causing a color change. In addition, the azophenol structure can form a hydrogen bond with a water molecule, thereby causing a color change, and further improving the color development performance. DETAILED DESCRIPTION

[0012] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Example

[0013] A precision electronic moisture-proof storage humidity color indicator card composition comprises the following raw materials in parts by weight: 10 parts of ferric sulfate, 3 parts of sulfonic acid compounds, and 20 parts of buffer solution; The sulfonic acid compound is prepared by the following steps: Step S1, adding 1,3-propane sultone and 2,2'-bipyridine to toluene, heating to 35°C, stirring at a constant speed for 4 hours, filtering to obtain intermediate 1, wherein the amount ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene is controlled to be 0.02 mmol: 0.02 mmol: 10 mL; Step S2, adding 4-phenylazophenol and 1,6-dibromohexane to anhydrous ethanol, heating to 75-80°C, stirring at a uniform speed and sequentially adding potassium carbonate and potassium iodide, continuing stirring and reacting for 24 hours to obtain intermediate 2, wherein the amount ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and anhydrous ethanol is controlled to be 0.01mmol:0.05mmol:0.22mmol:0.01mmol:10mL; Step S3, adding intermediate 2 and intermediate 1 to N,N-dimethylformamide, introducing nitrogen to expel air, raising the temperature to 70-80°C, and keeping the temperature for reaction for 24 hours to obtain a sulfonic acid compound, wherein the amount ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide is controlled to be 0.03mmol:0.08mmol:10mL.

[0014] The buffer solution is 15% by mass dilute hydrochloric acid.

[0015] The prepared color indicator card composition is evenly applied on a humidity indicator card substrate and dried naturally. When the relative humidity is 10-20%, the card changes color. Example

[0016] A precision electronic moisture-proof storage humidity color indicator card composition comprises the following raw materials in parts by weight: 12 parts of ferric sulfate, 5 parts of sulfonic acid compound, and 20 parts of buffer solution; The sulfonic acid compound is prepared by the following steps: Step S1, adding 1,3-propane sultone and 2,2'-bipyridine to toluene, heating to 35°C, stirring at a constant speed for 4 hours, filtering to obtain intermediate 1, wherein the amount ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene is controlled to be 0.03 mmol: 0.03 mmol: 10 mL; Step S2, adding 4-phenylazophenol and 1,6-dibromohexane to anhydrous ethanol, heating to 75°C, stirring at a uniform speed and sequentially adding potassium carbonate and potassium iodide, continuing stirring and reacting for 24 hours to obtain intermediate 2, wherein the amount ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and anhydrous ethanol is controlled to be 0.01mmol:0.06mmol:0.23mmol:0.01mmol:10mL; Step S3, adding intermediate 2 and intermediate 1 to N,N-dimethylformamide, introducing nitrogen to expel air, raising the temperature to 70-80°C, and keeping the temperature for reaction for 24 hours to obtain a sulfonic acid compound, wherein the amount ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide is controlled to be 0.04mmol:0.08mmol:10mL.

[0017] The buffer solution is 15% by mass dilute hydrochloric acid.

[0018] The prepared color indicator card composition is evenly applied on a humidity indicator card substrate and dried naturally. When the relative humidity is 10-20%, the card changes color. Example

[0019] A precision electronic moisture-proof storage humidity color indicator card composition comprises the following raw materials in parts by weight: 14 parts of ferric sulfate, 5 parts of sulfonic acid compound, and 20 parts of buffer solution; The sulfonic acid compound is prepared by the following steps: Step S1, adding 1,3-propane sultone and 2,2'-bipyridine to toluene, heating to 40°C, stirring at a constant speed for 4 hours, filtering to obtain intermediate 1, wherein the amount ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene is controlled to be 0.04 mmol: 0.04 mmol: 10 mL; Step S2, adding 4-phenylazophenol and 1,6-dibromohexane to anhydrous ethanol, heating to 75-80°C, stirring at a uniform speed and sequentially adding potassium carbonate and potassium iodide, continuing stirring and reacting for 24 hours to obtain intermediate 2, wherein the amount ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and anhydrous ethanol is controlled to be 0.02mmol:0.08mmol:0.24mmol:0.01mmol:10mL; Step S3, adding intermediate 2 and intermediate 1 to N,N-dimethylformamide, introducing nitrogen to expel air, raising the temperature to 70-80°C, and keeping the temperature for reaction for 24 hours to obtain a sulfonic acid compound, wherein the amount ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide is controlled to be 0.04mmol:0.09mmol:10mL.

[0020] The buffer solution is 15% by mass dilute hydrochloric acid.

[0021] The prepared color indicator card composition is evenly applied on a humidity indicator card substrate and dried naturally. When the relative humidity is 10-20%, the card changes color. Example

[0022] A precision electronic moisture-proof storage humidity color indicator card composition comprises the following raw materials in parts by weight: 15 parts of ferric sulfate, 8 parts of sulfonic acid compound, and 20 parts of buffer solution; The sulfonic acid compound is prepared by the following steps: Step S1, adding 1,3-propane sultone and 2,2'-bipyridine to toluene, heating to 35-40°C, stirring at a constant speed for 4 hours, filtering to obtain intermediate 1, wherein the amount ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene is controlled to be 0.05mmol:0.05mmol:10mL; Step S2, adding 4-phenylazophenol and 1,6-dibromohexane to anhydrous ethanol, heating to 80°C, stirring at a uniform speed and sequentially adding potassium carbonate and potassium iodide, continuing stirring and reacting for 24 hours to obtain intermediate 2, wherein the amount ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and anhydrous ethanol is controlled to be 0.02mmol:0.08mmol:0.25mmol:0.02mmol:10mL; Step S3, adding intermediate 2 and intermediate 1 to N,N-dimethylformamide, introducing nitrogen to expel air, heating to 80°C, and keeping the temperature for reaction for 24 hours to obtain a sulfonic acid compound, wherein the amount ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide is controlled to be 0.05mmol:0.1mmol:10mL.

[0023] The buffer solution is 15% by mass dilute hydrochloric acid.

[0024] The prepared color indicator card composition is evenly applied on a humidity indicator card substrate and dried naturally. When the relative humidity is 10-20%, the card changes color.

[0025] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A precision electronic moisture-proof storage humidity color indicator card composition, It is characterized in that The method comprises the following raw materials in parts by weight: 10-15 parts of ferric sulfate, 3-8 parts of sulfonic acid compound, and 20 parts of buffer solution; The sulfonic acid compound is prepared by the following steps: Step S1, adding 1,3-propane sultone and 2,2'-bipyridine to toluene, heating to 35-40°C, stirring at a constant speed for 4 hours, and filtering to obtain intermediate 1; Step S2, adding 4-phenylazophenol and 1,6-dibromohexane to anhydrous ethanol, heating to 75-80° C., stirring at a uniform speed and sequentially adding potassium carbonate and potassium iodide, continuing stirring and reacting for 24 hours to obtain intermediate 2; Step S3, adding intermediate 2 and intermediate 1 into N,N-dimethylformamide, introducing nitrogen to expel air, raising the temperature to 70-80° C., and keeping the temperature for reaction for 24 hours to obtain a sulfonic acid compound.

2. A precision electronic moisture-proof storage humidity color indicator card composition according to claim 1, It is characterized in that The buffer solution is 15% by mass of dilute hydrochloric acid.

3. A precision electronic moisture-proof storage humidity color indicator card composition according to claim 1, It is characterized in that In step S1, the dosage ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene is controlled to be 0.02-0.05 mmol: 0.02-0.05 mmol: 10 mL.

4. A precision electronic moisture-proof storage humidity color indicator card composition according to claim 1, It is characterized in that In step S2, the dosage ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and anhydrous ethanol is controlled to be 0.01-0.02 mmol: 0.05-0.08 mmol: 0.22-0.25 mmol: 0.01-0.02 mmol: 10 mL.

5. A precision electronic moisture-proof storage humidity color indicator card composition according to claim 1, It is characterized in that In step S3, the usage ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide is controlled to be 0.03-0.05 mmol: 0.08-0.1 mmol: 10 mL.