Irreversible thermochromic pigment capable of memorizing temperature and preparation method thereof

By preparing a mixed solution of rare earth elements, transition metals and active metals, adding an alkaline mineralizing agent and treating it, an irreversible thermochromic pigment with temperature memory was prepared, which solved the shortcomings of temperature memory in the existing technology and realized the color change memory function within the range of room temperature to 400 degrees Celsius.

CN121591253APending Publication Date: 2026-03-03JILIN INST OF CHEM TECH
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Patent Information

Application Number
CN202511714068.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-15
Publication Date
2026-03-03

AI Technical Summary

Technical Problem

In existing technologies, it is difficult to achieve irreversible color changes in pigments to memorize temperature ranges and fault locations, especially in temperature ranges from room temperature to 400 degrees Celsius.

Method used

By preparing solutions of rare earth element nitrates, transition metal chlorides, and active metal chlorides, and adding alkaline inorganic compounds as mineralizing agents, followed by stirring, cooling, and drying, an irreversible thermochromic pigment with temperature memory can be prepared, achieving irreversible color changes of the pigment at different temperatures.

Benefits of technology

This pigment can achieve irreversible color changes within a range of room temperature to 400 degrees Celsius. It uses color changes to remember the location of the fault point and the highest heating temperature, providing intelligent temperature memory characteristics.

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Abstract

The invention belongs to the technical field of pigments, and particularly relates to an irreversible thermochromic pigment capable of memorizing temperature and a preparation method thereof.The irreversible thermochromic pigment capable of memorizing temperature can serve as a pigment to be coated on the surface of a normally-working machine or part, and once an instrument breaks down and is heated, the irreversible thermochromic pigment can memorize temperature. The position of a fault point and the comprehensive effect of the highest heating temperature can be memorized according to the color change of the surface material; the preparation method of the irreversible thermochromic pigment capable of memorizing the temperature comprises the following steps: step 1, preparing and storing a solution; step 2, stirring; step 3, adding a mineralizing agent; 4, cooling and transferring: after stirring for a certain time, spontaneously cooling the small beaker at room temperature, and transferring the reactant into a reaction kettle after the reactant is uniformly stirred; and 5, carrying out a drying reaction.
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Description

Technical Field

[0001] This invention relates to the field of pigment technology, specifically to an irreversible thermochromic pigment with temperature memory and its preparation method. Background Technology

[0002] Chromium oxides exhibit different strongest absorption peaks in the visible spectrum due to their different valence states, and the material can produce different concentrations of high-valence chromium when heated. By controlling the irreversible chemical reaction pathway through which the material can be transformed into high-valence chromium to varying degrees at different temperatures and heating times, it is possible to achieve the phenomenon that the material's color varies at different heating temperatures.

[0003] Therefore, the material claimed in this invention can be used as a temperature memory material in the range of room temperature to 400 degrees Celsius. This material can be used as a pigment to coat the surface of a normally functioning machine or part. Once the instrument malfunctions and is heated, it can remember the location of the malfunction point and the highest heating temperature based on the color change of its surface material. Summary of the Invention

[0004] The purpose of this section is to outline some aspects of the embodiments of the present invention and to briefly describe some preferred embodiments. Simplifications or omissions may be made in this section, as well as in the abstract and title of this application, to avoid obscuring the purpose of these documents; however, such simplifications or omissions should not be construed as limiting the scope of the invention.

[0005] In view of the problems existing in the above and / or existing irreversible thermochromic pigments with memorizable temperature and their preparation methods, the present invention is proposed.

[0006] Therefore, the object of this invention is to provide an irreversible thermochromic pigment capable of remembering temperature and its preparation method, which can remember the location and maximum heating temperature of the coated pigment and / or the fault point of the component based on the color change of its surface material. This irreversible thermochromic pigment can provide irreversible color changes within the range of room temperature to 400°C, thereby achieving intelligent temperature memory characteristics. According to one aspect of the invention, the invention provides the following technical solution:

[0007] An irreversible thermochromic pigment capable of remembering its temperature and its preparation method thereof, the formulation of the irreversible thermochromic pigment capable of remembering its temperature and its preparation method include the following steps:

[0008] Step 1: Solution preparation and storage: First, prepare reaction solutions of certain concentrations for rare earth element nitrates, transition metal chlorides, and active metal chlorides, and store them in a wide-mouth bottle with a seal.

[0009] Step 2: Stirring: According to the stoichiometric ratio, transfer a certain proportion of rare earth element nitrate, transition metal chloride, active metal chloride, etc. solution into a 50 ml beaker and stir evenly at room temperature using a magnetic stirrer.

[0010] Step 3: Add mineralizing agent: Add a certain amount of alkaline inorganic compound as a mineralizing agent to the small beaker of mixed liquid while stirring. At this time, a large amount of gray-green flocculent matter will appear in the beaker.

[0011] Step 4: Cooling and Transfer: After stirring for a certain period of time, allow the small beaker to cool spontaneously at room temperature. Once the reactants are stirred evenly, transfer them to the reaction vessel.

[0012] Step 5: Drying reaction: Rinse the reactant raw materials with deionized water, seal the reaction vessel, and transfer it to a forced-air drying oven. React at 240-300 degrees Celsius for a certain period of time to prepare the target material.

[0013] In a preferred embodiment of the preparation method of the irreversible thermochromic pigment with memory temperature described in this invention, the rare earth element nitrate is one of lanthanum nitrate, praseodymium nitrate, neodymium nitrate, samarium nitrate, dysprosium nitrate, holmium nitrate, lutetium nitrate, thulium nitrate, erbium nitrate, and ytterbium nitrate; the transition metal chloride is one of titanium chloride, chromium chloride, manganese chloride, ferric chloride, cobalt chloride, nickel chloride, and copper chloride; the active metal chloride is one of potassium chloride, sodium chloride, calcium chloride, magnesium chloride, and aluminum chloride; and the inorganic alkaline solid is one of sodium bicarbonate, potassium bicarbonate, sodium carbonate, potassium carbonate, sodium hydroxide, and potassium hydroxide. The rare earth element nitrate, transition metal chloride, and active metal chloride are mixed in a ratio of 25-50 parts by weight.

[0014] In a preferred embodiment of the method for preparing the irreversible thermochromic pigment with memory temperature as described in this invention, the room temperature condition is 18-35℃.

[0015] As a preferred embodiment of the irreversible thermochromic pigment with memorizable temperature and its preparation method described in this invention, the reaction time in step five is 2-4 hours.

[0016] As a preferred embodiment of the irreversible thermochromic pigment with memorizable temperature and its preparation method described in this invention, wherein the reaction vessel in step five is an electrically heated reaction vessel.

[0017] As a preferred embodiment of the irreversible thermochromic pigment with memory temperature and its preparation method described in this invention, the magnetic stirrer operates at a medium speed and the stirring time is 25-60 minutes.

[0018] As a preferred embodiment of the irreversible thermochromic pigment with memorizable temperature and its preparation method described in this invention, wherein: the stoichiometric ratio is defined as follows:

[0019] Suppose that titrant T reacts with substance B as follows:

[0020] tT+bB=cC+dD

[0021] When the reaction reaches the stoichiometric point, the amount of substance n of the substance being dropped can be determined from the reaction equation. B The amount of titrant n T The following relationship exists between them:

[0022]

[0023] but or This is called the stoichiometric ratio. It can be easily obtained from the stoichiometric coefficients t, b, c, and d in the reaction equation. or Further obtain n B With n T The measurement relationship.

[0024] Compared with existing technologies: When pigments are applied to the surface of normally functioning machines or parts, once the instrument malfunctions and is heated, the location of the malfunction and the highest heating temperature can be remembered based on the color change of the surface material. Attached Figure Description

[0025] To more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. Wherein:

[0026] Figures 1-5 Structural data and temperature-dependent color change data for materials with different proportions;

[0027] Figure 6 This invention provides a schematic diagram illustrating the color change of an irreversible thermochromic pigment, LaCr1-xAlxO3, which can remember temperatures, obtained by using lanthanum nitrate as a rare earth nitrate, chromium chloride as a transition metal chloride, and aluminum chloride as an active metal chloride.

[0028] Figure 7This invention provides a schematic diagram illustrating the temperature-dependent changes in the color coordinates of an irreversible thermochromic pigment, LaCr1-xAlxO3, which uses lanthanum nitrate as a rare-earth nitrate, chromium chloride as a transition metal chloride, and aluminum chloride as an active metal chloride. Detailed Implementation

[0029] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

[0030] Many specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of the invention. Therefore, the invention is not limited to the specific embodiments disclosed below.

[0031] Secondly, the present invention is described in detail with reference to the schematic diagrams. When detailing the embodiments of the present invention, for ease of explanation, the cross-sectional views illustrating the device structure may be partially enlarged, not according to the usual scale. Furthermore, the schematic diagrams are merely examples and should not limit the scope of protection of the present invention. In addition, actual fabrication should include three-dimensional spatial dimensions of length, width, and depth.

[0032] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0033] This invention provides an irreversible thermochromic pigment with memorizable temperature and its preparation method:

[0034] Implementation Method 1

[0035] The irreversible thermochromic pigment capable of remembering temperature and its preparation method include the following steps:

[0036] Step 1: Solution preparation and storage: Prepare reaction solutions of certain concentrations for rare earth nitrates, transition metal chlorides, and active metal chlorides respectively, and store them in wide-mouth bottles in a sealed container.

[0037] Step 2: Stirring: First, by weight: according to the stoichiometric ratio, transfer a certain proportion of the solution of the rare earth nitrate (25 parts), the transition metal chloride (65 parts), and the active metal chloride (20 parts) into a 50 ml beaker, and stir evenly with a magnetic stirrer at room temperature (35°C) for 25 minutes.

[0038] Step 3: Add mineralizing agent: Add a certain amount of alkaline inorganic compound as a mineralizing agent to the small beaker of mixed liquid while stirring. At this time, a large amount of gray-green flocculent matter will appear in the beaker.

[0039] Step 4: Cooling and Transfer: After stirring for a certain period of time, allow the small beaker to cool spontaneously at room temperature (35°C). Once the reactants are stirred evenly, transfer them to the reaction vessel.

[0040] Step 5: Drying reaction: Rinse the reactant raw materials with deionized water, seal the reaction vessel, and transfer it to a forced-air drying oven. The reaction vessel is an electrically heated reaction vessel. Under the condition of 240 degrees Celsius, the reaction time is 4 hours, and the target material can be prepared.

[0041] The stoichiometric ratio is defined as follows:

[0042] Suppose that titrant T reacts with substance B as follows:

[0043] tT+bB=cC+dD

[0044] When the reaction reaches the stoichiometric point, the amount of substance n of the substance being dropped can be determined from the reaction equation. B The amount of titrant n T The following relationship exists between them:

[0045]

[0046] but or This is called the stoichiometric ratio. It can be easily obtained from the stoichiometric coefficients t, b, c, and d in the reaction equation. or Further obtain n B With n T The measurement relationship.

[0047] Implementation Method 2

[0048] The irreversible thermochromic pigment capable of remembering temperature and its preparation method include the following steps:

[0049] Step 1: Solution preparation and storage: Prepare reaction solutions of certain concentrations for rare earth nitrates, transition metal chlorides, and active metal chlorides respectively, and store them in wide-mouth bottles in a sealed container.

[0050] Step 2: Stirring: First, by weight: according to the stoichiometric ratio, transfer a certain proportion of the solution of rare earth nitrate (50 parts), transition metal chloride (36 parts), and active metal chloride (38 parts) into a 50 ml beaker, and stir evenly with a magnetic stirrer at room temperature (18°C) for 60 minutes.

[0051] Step 3: Add mineralizing agent: Add a certain amount of alkaline inorganic compound as a mineralizing agent to the small beaker of mixed liquid while stirring. At this time, a large amount of gray-green flocculent matter will appear in the beaker.

[0052] Step 4: Cooling and Transfer: After stirring for a certain period of time, allow the small beaker to cool spontaneously at room temperature of 18°C. After the reactants are stirred evenly, transfer them to the reaction vessel.

[0053] Step 5: Drying reaction: Rinse the reactant raw materials with deionized water, seal the reaction vessel, and transfer it to a forced-air drying oven. The reaction vessel is an electrically heated reaction vessel. Under the condition of 300 degrees Celsius, the reaction time is 2 hours, and the target material can be prepared.

[0054] The stoichiometric ratio is defined as follows:

[0055] Suppose that titrant T reacts with substance B as follows:

[0056] tT+bB=cC+dD

[0057] When the reaction reaches the stoichiometric point, the amount of substance n of the substance being dropped can be determined from the reaction equation. B The amount of titrant n T The following relationship exists between them:

[0058]

[0059] but or This is called the stoichiometric ratio. It can be easily obtained from the stoichiometric coefficients t, b, c, and d in the reaction equation. or Further obtain n B With n T The measurement relationship.

[0060] Implementation Method 3

[0061] The irreversible thermochromic pigment capable of remembering temperature and its preparation method include the following steps:

[0062] Step 1: Solution preparation and storage: Prepare reaction solutions of certain concentrations for rare earth nitrates, transition metal chlorides, and active metal chlorides respectively, and store them in wide-mouth bottles in a sealed container.

[0063] Step 2: Stirring: First, by weight, transfer a certain proportion of the rare earth nitrate solution (37.5 parts), the transition metal chloride solution (55 parts), and the active metal chloride solution (26 parts) into a 50 ml beaker using a pipette according to the stoichiometric ratio. Stir the mixture evenly at room temperature (27°C) using a magnetic stirrer at medium speed for 42.5 minutes.

[0064] Step 3: Add mineralizing agent: Add a certain amount of alkaline inorganic compound as a mineralizing agent to the small beaker of mixed liquid while stirring. At this time, a large amount of gray-green flocculent matter will appear in the beaker.

[0065] Step 4: Cooling and Transfer: After stirring for a certain period of time, allow the small beaker to cool spontaneously at room temperature of 26°C. After the reactants are stirred evenly, transfer them to the reaction vessel.

[0066] Step 5: Drying reaction: Rinse the reactant raw materials with deionized water, seal the reaction vessel, and transfer it to a forced-air drying oven. The reaction vessel is an electrically heated reaction vessel. Under the condition of 270 degrees Celsius, the reaction time is 3 hours, and the target material can be prepared.

[0067] The stoichiometric ratio is defined as follows:

[0068] Suppose that titrant T reacts with substance B as follows:

[0069] tT+bB=cC+dD

[0070] When the reaction reaches the stoichiometric point, the amount of substance n of the substance being dropped can be determined from the reaction equation. B The amount of titrant n T The following relationship exists between them:

[0071]

[0072] but or This is called the stoichiometric ratio. It can be easily obtained from the stoichiometric coefficients t, b, c, and d in the reaction equation. or Further obtain n B With n T The measurement relationship.

[0073] Example 1: Using lanthanum nitrate as a rare earth nitrate, chromium chloride as a transition metal chloride, and aluminum chloride as an active metal chloride, an irreversible thermochromic pigment with temperature memory, LaCr1-xAlxO3, can be obtained through the above implementation method in a certain proportion. This pigment can achieve temperature memory function within the range of room temperature to 400 degrees Celsius. Its color and chromaticity coordinates change with temperature as follows: Figure 6 and Figure 7As shown.

[0074] In summary, the above embodiments demonstrate that the temperature-memory-memory irreversible thermochromic pigment and its preparation method can memorize the location of the fault point and the maximum heating temperature based on the color change of its surface material, thus offering significant economic benefits.

[0075] Although the present invention has been described above with reference to embodiments, various modifications can be made and components can be replaced with equivalents without departing from the scope of the invention. In particular, as long as there is no structural conflict, the features in the disclosed embodiments can be combined with each other in any manner. The lack of an exhaustive description of these combinations in this specification is merely for the sake of brevity and resource conservation. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. An irreversible thermochromic pigment with memoryable temperature and its preparation method, characterized in that: The formulation and preparation method of this temperature-memory-capable irreversible thermochromic pigment include the following steps: Step 1: Solution preparation and storage: First, prepare reaction solutions of certain concentrations for rare earth nitrates, transition metal chlorides, and active chlorine metal chlorides, and store them in a wide-mouth bottle with a seal. Step 2: Stirring: According to the stoichiometric ratio, transfer a certain proportion of rare earth nitrate, transition metal chloride, and chlorinated active metal chloride solution into a 50 ml beaker and stir evenly at room temperature using a magnetic stirrer. Step 3: Add mineralizing agent: Add a certain amount of alkaline inorganic compound as a mineralizing agent to the small beaker of mixed liquid while stirring. At this time, a large amount of gray-green flocculent matter will appear in the beaker. Step 4: Cooling and Transfer: After stirring for a certain period of time, allow the small beaker to cool spontaneously at room temperature. Once the reactants are stirred evenly, transfer them to the reaction vessel. Step 5: Drying reaction: Rinse the reactant raw materials with deionized water, seal the reaction vessel, and transfer it to a forced-air drying oven. React at 240-300 degrees Celsius for a certain period of time to prepare the target material.

2. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: This pigment can achieve irreversible thermochromic changes within a temperature range of room temperature to 400 degrees Celsius, enabling intelligent temperature memory functionality.

3. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: By weight: 25-50 parts of lanthanum nitrate, 36-65 parts of chromium chloride, and 20-38 parts of aluminum chloride are mixed together.

4. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: The room temperature conditions are 18-35℃.

5. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: The reaction time in step five is 2-4 hours.

6. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: The reactor in step five is an electrically heated reactor.

7. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: The magnetic stirrer operates at a medium speed, with a stirring time of 25-60 minutes.

8. The irreversible thermochromic pigment with memoryable temperature and its preparation method according to claim 1, characterized in that: The definition of stoichiometry is Suppose that titrant T reacts with substance B as follows: tT+bB=cC+dD When the reaction reaches the stoichiometric point, the amount of substance n of the substance being dropped can be determined from the reaction equation. B The amount of titrant n T The following relationship exists between them: but or This is called the stoichiometric ratio. It can be easily obtained from the stoichiometric coefficients t, b, c, and d in the reaction equation. or Further obtain n B With n T The measurement relationship.