A composition for a precision electronic moisture-proof storage humidity color display indicator card

Abstract

The present invention discloses a humidity color - showing indicating card composition for precision electronic moisture - proof storage, comprising the following raw materials in parts by weight: 10 - 15 parts of ferric sulfate, 3 - 8 parts of sulfonic acid - based compound, and 20 parts of buffer solution; the sulfonic acid - based compound is prepared through the following steps: Step S1: Add 1,3 - propane sultone and 2,2'-bipyridine into toluene to obtain intermediate 1; Step S2: Add 4 - phenylazo phenol and 1,6 - dibromohexane into absolute ethanol to obtain intermediate 2; Step S3: Add intermediate 2 and intermediate 1 into N,N - dimethylformamide, keep the temperature for reaction for 24 h to obtain the sulfonic acid - based compound; the structure of the sulfonic acid - based compound has sulfonate ions, quaternary ammonium salt ions and azophenol structure, and the quaternary ammonium salt ions have good hygroscopicity. When used as a color - showing agent, it can absorb water vapor in the air in time, thus causing a color change.

Description

Technical Field

[0001] The present invention relates to the technical field of color developers, and particularly relates to a humidity color - showing indicator card composition for precision electronic moisture - proof storage. 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 an ambient atmosphere at a particular level of humidity that can damage these components. For example, electronic components can be damaged by exposure to an atmosphere having a humidity above a specific threshold level, even when the threshold level is low and the exposure is only for a short time.

[0003] To meet the need for detection, humidity indicators have been developed. Most humidity indicator cards currently manufactured use cobalt chloride as the indicator, which changes color based on the degree of hydration of cobalt chloride in different humidity environments. Cobalt chloride can change from blue (when it has a hydration of one water) to pink (when it has a hydration of six waters). As the degree of hydration increases, the blue gradually changes to red. Therefore, to determine the approximate humidity based on the different colors presented on the card, an array including different humidity - indicating regions can be set on the card, where increasing humidity levels change different indicating regions on the card from blue to pink.

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

[0005] At the same time, the EU environmental protection regulation (2004 / 73 / EC) in 2004 listed cobalt chloride as a class - II carcinogenic substance, and required the prohibition of using humidity indicator cards containing this component in electronic products. Therefore, enterprises are in urgent need of providing a humidity - indicating composition without heavy - metal elements such as cobalt as the humidity - sensitive coating of humidity indicator cards. Summary of the Invention

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

[0007] The object of the present invention can be achieved by the following technical solutions:

[0008] A humidity color - showing indicator card composition for precision electronic moisture - proof storage, comprising the following raw materials in parts by weight: 10 - 15 parts of ferric sulfate, 3 - 8 parts of sulfonic - group compound, and 20 parts of buffer solution;

[0009] The sulfonic - group compound is prepared by the following steps:

[0010] Step S1: Add 1,3 - propanesultone and 2,2'-bipyridine into toluene, heat up to 35 - 40 °C, stir evenly for 4 h, then filter to obtain Intermediate 1. Control the dosage ratio of 1,3 - propanesultone, 2,2'-bipyridine and toluene as 0.02 - 0.05 mmol : 0.02 - 0.05 mmol : 10 mL;

[0011] In Step S1, 1,3 - propanesultone and 2,2'-bipyridine react to prepare Intermediate 1, and the structure of Intermediate 1 contains sulfonate ions and quaternary ammonium ions.

[0012] Step S2: Add 4 - phenylazophenol and 1,6 - dibromohexane into absolute ethanol, heat up to 75 - 80 °C, stir evenly and successively add potassium carbonate and potassium iodide, continue to stir and react for 24 h to obtain Intermediate 2. Control the dosage ratio of 4 - phenylazophenol, 1,6 - dibromohexane, potassium carbonate, potassium iodide and absolute ethanol as 0.01 - 0.02 mmol : 0.05 - 0.08 mmol : 0.22 - 0.25 mmol : 0.01 - 0.02 mmol : 10 mL;

[0013] In Step S2, the phenolic hydroxyl group on 4 - phenylazophenol reacts with the bromine element on 1,6 - dibromohexane to further prepare Intermediate 2;

[0014] Step S3: Add Intermediate 2 and Intermediate 1 into N,N - dimethylformamide, introduce nitrogen to expel air, heat up to 70 - 80 °C, keep the temperature for reaction for 24 h to obtain the sulfonic acid group compound. Control the dosage ratio of Intermediate 2, Intermediate 1 and N,N - dimethylformamide as 0.03 - 0.05 mmol : 0.08 - 0.1 mmol : 10 mL.

[0015] In Step S3, the bromine element on Intermediate 2 reacts with the pyridine on Intermediate 1 to prepare the sulfonic acid group compound; the structure of this sulfonic acid group compound has sulfonate ions, quaternary ammonium ions and azophenol structure. The quaternary ammonium ions have good hygroscopicity. When used as a color developer, they can absorb water vapor in the air in time, resulting in a change in the pH value of the system's acidity and alkalinity, thus affecting the combination of Fe ions and sulfonate ions, causing a color change. Moreover, the azophenol structure can form hydrogen bonds with water molecules, further causing a color change and further improving the color development performance.

[0016] Further, the buffer solution is 15% dilute hydrochloric acid by mass fraction.

[0017] Advantages of the present invention:

[0018] The present invention prepares a humidity color - indicating card composition for precision electronic moisture - proof storage. First, a sulfonic acid - based compound is synthesized. During the preparation process, intermediate 1 is prepared by reacting 1,3 - propane sultone with 2,2'-bipyridine. The structure of intermediate 1 contains sulfonate ions and quaternary ammonium ions. Then, the phenolic hydroxyl group on 4 - phenylazophenol reacts with the bromine element on 1,6 - dibromohexane to prepare intermediate 2. Finally, the bromine element on intermediate 2 reacts with the pyridine on intermediate 1 to prepare the sulfonic acid - based compound. The structure of the sulfonic acid - based compound has sulfonate ions, quaternary ammonium ions, and an azophenol structure. The quaternary ammonium ions have good hygroscopicity. When used as a color - developing agent, it can absorb water vapor in the air in a timely manner, causing a change in the pH value of the system, thereby affecting the combination of iron ions and sulfonate ions, resulting in a color change. Moreover, the azophenol structure can form hydrogen bonds with water molecules, further causing a color change and improving the color - developing performance. Detailed implementation mode

[0019] Next, the technical solutions in the embodiments of the present invention will be described clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention. Embodiment 1

[0020] A humidity color - indicating card composition for precision electronic moisture - proof storage, comprising the following raw materials in parts by weight: 10 parts of ferric sulfate, 3 parts of sulfonic acid - based compound, and 20 parts of buffer solution;

[0021] The sulfonic acid - based compound is prepared through the following steps:

[0022] Step S1: Add 1,3 - propane sultone and 2,2'-bipyridine to toluene, heat up to 35°C, stir evenly for 4 h, and then filter to obtain intermediate 1. Control the dosage ratio of 1,3 - propane sultone, 2,2'-bipyridine, and toluene as 0.02 mmol:0.02 mmol:10 mL;

[0023] Step S2: Add 4 - phenylazophenol and 1,6 - dibromohexane to absolute ethanol, heat up to 75 - 80°C, stir evenly and sequentially add potassium carbonate and potassium iodide, continue to stir and react for 24 h to obtain intermediate 2. Control the dosage ratio of 4 - phenylazophenol, 1,6 - dibromohexane, potassium carbonate, potassium iodide, and absolute ethanol as 0.01 mmol:0.05 mmol:0.22 mmol:0.01 mmol:10 mL;

[0024] Step S3: Add intermediate 2 and intermediate 1 into N,N-dimethylformamide, introduce nitrogen to expel air, heat up to 70 - 80 °C, keep the temperature for reaction for 24 h to obtain the sulfonic acid group compound, and control the dosage ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide to be 0.03 mmol:0.08 mmol:10 mL.

[0025] The buffer solution is 15% dilute hydrochloric acid by mass fraction.

[0026] Apply the prepared color display indicator card composition evenly on the humidity indicator card substrate, air dry naturally, and the card will change color at a relative humidity of 10 - 20%. Example 2

[0027] A precision electronic moisture-proof storage humidity color display indicator card composition, comprising the following raw materials in parts by weight: 12 parts of ferric sulfate, 5 parts of sulfonic acid group compound, 20 parts of buffer solution;

[0028] The sulfonic acid group compound is prepared through the following steps:

[0029] Step S1: Add 1,3-propane sultone and 2,2'-bipyridine into toluene, heat up to 35 °C, stir evenly for 4 h, then filter to obtain intermediate 1, and control the dosage ratio of 1,3-propane sultone, 2,2'-bipyridine and toluene to be 0.03 mmol:0.03 mmol:10 mL;

[0030] Step S2: Add 4-phenylazophenol and 1,6-dibromohexane into absolute ethanol, heat up to 75 °C, stir evenly and add potassium carbonate and potassium iodide in sequence, continue to stir and react for 24 h to obtain intermediate 2, and control the dosage ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and absolute ethanol to be 0.01 mmol:0.06 mmol:0.23 mmol:0.01 mmol:10 mL;

[0031] Step S3: Add intermediate 2 and intermediate 1 into N,N-dimethylformamide, introduce nitrogen to expel air, heat up to 70 - 80 °C, keep the temperature for reaction for 24 h to obtain the sulfonic acid group compound, and control the dosage ratio of intermediate 2, intermediate 1 and N,N-dimethylformamide to be 0.04 mmol:0.08 mmol:10 mL.

[0032] The buffer solution is 15% dilute hydrochloric acid by mass fraction.

[0033] Apply the prepared color display indicator card composition evenly on the humidity indicator card substrate, air dry naturally, and the card will change color at a relative humidity of 10 - 20%. Example 3

[0034] A humidity color - indicating card composition for precision electronic moisture - proof storage, comprising the following raw materials in parts by weight: 14 parts of ferric sulfate, 5 parts of sulfonic acid - group compound, and 20 parts of buffer solution;

[0035] The sulfonic acid - group compound is prepared through the following steps:

[0036] Step S1: Add 1,3 - propane sultone and 2,2'-bipyridine into toluene, heat up to 40°C, stir evenly for 4 h, then filter to obtain Intermediate 1, and control the dosage ratio of 1,3 - propane sultone, 2,2'-bipyridine and toluene as 0.04 mmol:0.04 mmol:10 mL;

[0037] Step S2: Add 4 - phenylazophenol and 1,6 - dibromohexane into absolute ethanol, heat up to 75 - 80°C, stir evenly and successively add potassium carbonate and potassium iodide, continue stirring and reacting for 24 h to obtain Intermediate 2, and control the dosage ratio of 4 - phenylazophenol, 1,6 - dibromohexane, potassium carbonate, potassium iodide and absolute ethanol as 0.02 mmol:0.08 mmol:0.24 mmol:0.01 mmol:10 mL;

[0038] Step S3: Add Intermediate 2 and Intermediate 1 into N,N - dimethylformamide, introduce nitrogen to expel air, heat up to 70 - 80°C, keep warm and react for 24 h to obtain the sulfonic acid - group compound, and control the dosage ratio of Intermediate 2, Intermediate 1 and N,N - dimethylformamide as 0.04 mmol:0.09 mmol:10 mL.

[0039] The buffer solution is 15% dilute hydrochloric acid by mass fraction.

[0040] Apply the prepared color - indicating card composition evenly on the humidity - indicating card substrate, dry it naturally, and the card will change color at a relative humidity of 10 - 20%. Example 4

[0041] A humidity color - indicating card composition for precision electronic moisture - proof storage, comprising the following raw materials in parts by weight: 15 parts of ferric sulfate, 8 parts of sulfonic acid - group compound, and 20 parts of buffer solution;

[0042] The sulfonic acid - group compound is prepared through the following steps:

[0043] Step S1: Add 1,3 - propane sultone and 2,2'-bipyridine into toluene, heat up to 35 - 40°C, stir evenly for 4 h, then filter to obtain Intermediate 1, and control the dosage ratio of 1,3 - propane sultone, 2,2'-bipyridine and toluene as 0.05 mmol:0.05 mmol:10 mL;

[0044] Step S2: Add 4-phenylazophenol and 1,6-dibromohexane into absolute ethanol, heat up to 80 °C, stir evenly and sequentially add potassium carbonate and potassium iodide, continue stirring and reacting for 24 h to obtain Intermediate 2, and control the dosage ratio of 4-phenylazophenol, 1,6-dibromohexane, potassium carbonate, potassium iodide and absolute ethanol to be 0.02 mmol: 0.08 mmol: 0.25 mmol: 0.02 mmol: 10 mL;

[0045] Step S3: Add Intermediate 2 and Intermediate 1 into N,N-dimethylformamide, introduce nitrogen to expel air, heat up to 80 °C, keep the temperature and react for 24 h to obtain a sulfonic acid group compound, and control the dosage ratio of Intermediate 2, Intermediate 1 and N,N-dimethylformamide to be 0.05 mmol: 0.1 mmol: 10 mL.

[0046] The buffer solution is 15% by mass dilute hydrochloric acid.

[0047] Apply the prepared colorimetric indicator card composition evenly on the humidity indicator card substrate, air dry naturally, and the card will change color at a relative humidity of 10 - 20%.

[0048] The above content is only an example and illustration of the concept of the present invention. Those skilled in the art of this technology can make various modifications or supplements to the described specific embodiments or use similar methods to replace them. As long as they do not deviate from the concept of the invention or exceed the scope defined by this claim book, they should fall within the protection scope of the present invention.

Claims

1. A precision electronic moisture-proof storage humidity color-changing indicating card composition, characterized in that It includes the following raw materials in parts by weight: 10 - 15 parts of ferric sulfate, 3 - 8 parts of sulfonic acid group compound, and 20 parts of buffer solution; The sulfonic acid group compound is prepared through the following steps: Step S1: Add 1,3 - propanesultone and 2,2'-bipyridine into toluene, heat up to 35 - 40 °C, stir evenly for 4 h, then filter to obtain Intermediate 1; Step S2: Add 4 - phenylazophenol and 1,6 - dibromohexane into absolute ethanol, heat up to 75 - 80 °C, stir evenly and add potassium carbonate and potassium iodide in sequence, continue stirring and reacting for 24 h to obtain Intermediate 2; Step S3: Add Intermediate 2 and Intermediate 1 into N,N - dimethylformamide, introduce nitrogen to expel air, heat up to 70 - 80 °C, keep the temperature for reaction for 24 h to obtain the sulfonic acid group compound.

2. A precision electronic moisture-proof storage humidity color display indicating card composition according to claim 1, wherein The buffer solution is 15% dilute hydrochloric acid by mass fraction.

3. The composition of a precision electronic moisture-proof storage humidity color display indicator card according to claim 1, characterized in that, In Step S1, control the dosage ratio of 1,3 - propanesultone, 2,2'-bipyridine and toluene to be 0.02 - 0.05 mmol: 0.02 - 0.05 mmol: 10 mL.

4. The composition of a precision electronic moisture-proof storage humidity color display indicator card according to claim 1, characterized in that, In Step S2, control the dosage ratio of 4 - phenylazophenol, 1,6 - dibromohexane, potassium carbonate, potassium iodide and absolute ethanol 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 display indicating card composition according to claim 1, wherein, In Step S3, control the dosage ratio of Intermediate 2, Intermediate 1 and N,N - dimethylformamide to be 0.03 - 0.05 mmol: 0.08 - 0.1 mmol: 10 mL.