Preparation process and device of environment-friendly color fixing agent

Abstract

The invention discloses a preparation process and device of an environment-friendly color fixing agent, and belongs to the field of preparation of environment-friendly color fixing agents. The device comprises a reaction kettle, a stirrer, a heating device, a dropwise adding device, a cooling device and a filtering device; the reaction kettle serves as a core reaction container and is used for bearing raw materials and carrying out various chemical reactions. A feeding hole is formed in the top of the reaction kettle and is connected with a raw material storage tank through a pipeline, and raw materials such as triethylenetriamine and acrylics can be conveyed into the reaction kettle; a discharge hole is formed in the bottom, is connected with a cooling device through a pipeline, and can convey reacted materials to the cooling device for cooling treatment; on the basis of the traditional raw materials, the monomer containing the ultraviolet absorbing group and the monomer containing the chlorine stabilizing group are introduced, so that the color fastness to sunlight and the color fastness to chlorine of the color fixing agent can be effectively improved, the performance of the color fixing agent is expanded, the color fixing agent is suitable for more types of dyes and dyeing scenes, and the applicability and the competitiveness of the product are improved.

Description

Technical Field

[0001] This invention relates to the field of environmentally friendly color-fixing agent preparation technology, and in particular to a preparation process and apparatus for an environmentally friendly color-fixing agent. Background Technology

[0002] With increasing awareness of environmental protection and health, many existing dyes and chemicals have been banned internationally, posing challenges to the requirements of color-fixing agents. Currently, most color-fixing agents on the market contain formaldehyde, failing to meet environmental demands, especially for infant and toddler clothing, which requires vibrant colors, good color-fixing effects, and no pollution to ensure infants' health. Existing methods for preparing color-fixing agents primarily employ simple polymerization methods, with modifications to the reaction conditions. This results in color-fixing agents requiring higher dosages, higher fixing temperatures, and longer fixing times, leading to higher production costs and room for improvement in wet rubbing fastness.

[0003] Publication (Announcement) No.: CN103422370A discloses a preparation process for an environmentally friendly color-fixing agent. Step 1: Heat one-third of the formulated amount of triethylenetriamine to 70-80℃, add the formulated amount of acrylate dropwise, react for 2-3 hours, then add the formulated amounts of initiator and acrylic acid comonomer, controlling the temperature at 50-60℃ to complete the polymerization reaction, obtaining product A; Step 2: Heat two-thirds of the formulated amount of triethylenetriamine to 90-100℃, add the formulated amount of propylene oxide dropwise, after the dropwise addition is complete, quickly lower the temperature to below 40℃, maintain the low temperature, and react for another 4-6 hours to obtain product B; Step 3: Mix product A and product B, adjust the pH value to 2-3, add water to the solid mass fraction to 60%-65%, and the product is ready. The preparation process yields a better color-fixing effect than existing direct polymerization reaction processes, especially in terms of wet rubbing fastness, which can be improved by 1 grade. This effectively solves the weakness of poor wet rubbing fastness of reactive dyes. The washing fastness and perspiration fastness are also better than existing color-fixing agents.

[0004] However, this patent only uses a few raw materials such as triethylenetriamine, acrylates, and propylene oxide. The limited variety of raw materials makes it difficult to meet the needs for further improvement and diversification of the performance of color-fixing agents, and it has shortcomings in terms of color fastness to sunlight and chlorine.

[0005] Furthermore, its preparation process suffers from harsh reaction conditions and complex process steps, requiring high standards for production equipment and operating techniques, which is not conducive to large-scale production and stable quality control.

[0006] Therefore, there is a need for an environmentally friendly process and apparatus for preparing color-fixing agents to improve the performance of color-fixing agents, simplify the preparation process, reduce production costs, and improve production efficiency and product quality stability. Summary of the Invention

[0007] To address the shortcomings of existing technologies, this invention provides a process and apparatus for preparing an environmentally friendly color-fixing agent. By introducing novel raw materials and improving the preparation process, the performance of the color-fixing agent is enhanced, the preparation process is simplified, production costs are reduced, and production efficiency and product quality stability are improved.

[0008] Technical solution: To solve the above-mentioned technical problems, according to one aspect of the present invention, more specifically, an apparatus for preparing an environmentally friendly color-fixing agent, comprising a reaction vessel, a stirrer, a heating device, a dripping device, a cooling device, and a filtration device;

[0009] Reactor: As the core reaction vessel, it is used to hold raw materials and carry out various chemical reactions. It has a feed inlet at the top, which is connected to the raw material storage tank through a pipeline, allowing raw materials such as triethylenetriamine and acrylates to be transported into the reactor; and a discharge outlet at the bottom, which is connected to the cooling device through a pipeline, enabling the reaction materials to be transported to the cooling device for cooling treatment.

[0010] Agitator: Installed inside the reactor and driven by a motor, it stirs the materials within the reactor. During the reaction, continuous stirring ensures thorough mixing and uniform contact of the raw materials, accelerating the reaction rate, ensuring complete reaction, and improving the quality and consistency of the reaction products.

[0011] Heating device: Surrounding the outside of the reactor and closely fitted to it, it provides heat to the reactor through electric heating or heat transfer oil circulation. A temperature sensor monitors the internal temperature of the reactor in real time and is connected to the control system, allowing for precise adjustment of the reaction temperature according to process requirements, ensuring the reaction proceeds within a set temperature range.

[0012] Dropping device: Connected to the raw material storage tank, it controls the dropping rate and amount of raw materials through a metering pump and pipeline. During the reaction, raw materials such as acrylates and propylene oxide can be slowly and precisely dripped into the reaction vessel according to process requirements, ensuring the orderly progress and effectiveness of the reaction.

[0013] Cooling device: Utilizing either air or water cooling, this device receives the high-temperature material from the reactor and cools it down to room temperature. The outlet of the cooling device is connected to the filtration device via a pipeline, transporting the cooled material there.

[0014] Filtration device: It adopts precision filtration equipment, which can effectively filter the cooled mixture, remove unreacted impurities and insoluble substances, and finally obtain a pure and environmentally friendly color fixing agent product.

[0015] According to one aspect of the present invention, and more specifically, a process for preparing an environmentally friendly color-fixing agent, using an apparatus for preparing an environmentally friendly color-fixing agent as described, comprising the following steps:

[0016] S1. Raw material preparation: Prepare triethylenetriamine, acrylates, propylene oxide, monomers containing ultraviolet absorbing groups, monomers containing chlorine stabilizing groups, and dispersants.

[0017] S2, First stage reaction: Triethylenetriamine is added to the reactor through the connecting pipe between the feed inlet at the top of the reactor and the raw material storage tank. The heating device is started and heated to 50°C by its contact heating with the reactor. The stirrer is turned on and, under stirring conditions, acrylates are slowly added dropwise through the pipe connected to the raw material storage tank by the dropping device. The dropping time is controlled within 1 hour. After the dropping is completed, the temperature is raised to 70°C by the heating device and the reaction is carried out for 2 hours to obtain the first reaction product.

[0018] S3. Second stage reaction: Add monomers containing ultraviolet absorbing groups and monomers containing chlorine stabilizing groups to the product of the first reaction above, heat the mixture to 80°C using a heating device, and slowly add propylene oxide again using a dropping device under stirring conditions. The dropping time is controlled at 1.5 hours. After the dropping is completed, keep the mixture at the temperature for 3 hours using a heating device to obtain the second reaction product.

[0019] S4. Dispersion treatment: Add a dispersant to the second reaction product, adjust the temperature to 40°C using a heating device, and stir and mix for 1 hour at this temperature to ensure that the dispersant is fully dispersed in the reaction product, thus obtaining a mixture.

[0020] S5. Post-processing: The mixture is transported to the cooling device through the pipe connected to the discharge port at the bottom of the reactor. After cooling to room temperature, it is sent to the filtration device through the pipe connected to the filtration device to remove unreacted impurities and insoluble substances, thus obtaining the environmentally friendly color-fixing agent product.

[0021] Furthermore, in the S1 raw material preparation step, the monomer containing the ultraviolet absorbing group is 2-hydroxy-4-acrylate benzophenone; the monomer containing the chlorine stabilizing group is 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester; and the dispersant is sodium lignosulfonate.

[0022] Furthermore, in the S1 raw material preparation step, the amounts of monomer (A) containing ultraviolet absorbing groups, monomer (B) containing chlorine stabilizing groups, and dispersant (C) added satisfy the color fastness synergistic enhancement index formula:

[0023]

[0024] In the formula: A is the mass (kg) of the monomer containing the ultraviolet absorbing group, and the monomer is 2-hydroxy-4-acrylate benzophenone;

[0025] B represents the mass (kg) of the monomer containing the chlorine-containing stabilizing group, wherein the monomer is 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester;

[0026] C represents the mass (kg) of the dispersant, which is sodium lignosulfonate.

[0027] A0=0 and B0=0 represent the equivalent addition amounts of UV-absorbing monomers and chlorine-stabilizing monomers that are not introduced into traditional color-fixing agents, respectively.

[0028] C0 represents the conventional dosage (kg) of traditional dispersants, ranging from 8 to 12 kg.

[0029] The SCI value is ≥1.5 to achieve synergistic enhancement of lightfastness and chlorinefastness.

[0030] The beneficial effects of the preparation process and apparatus for the environmentally friendly color-fixing agent of the present invention are as follows:

[0031] (1) Based on traditional raw materials, this invention introduces monomers containing ultraviolet absorbing groups and monomers containing chlorine stabilizing groups, which can effectively improve the light fastness and chlorine fastness of the fixing agent, expand the performance of the fixing agent, make it suitable for more types of dyes and dyeing scenarios, and improve the applicability and competitiveness of the product.

[0032] (2) This invention rationally adjusts the reaction steps and conditions, reduces unnecessary operational steps, lowers the stringent requirements for reaction conditions, and makes the process simpler and easier to control, which is conducive to large-scale production. At the same time, precise dropwise control and stirring ensure the sufficiency and uniformity of the reaction, and improves the stability of product quality.

[0033] (3) The preparation device of the present invention has a reasonable structure and the components work together to meet the requirements of the preparation process, realize the precise addition of raw materials, effective control of reaction temperature, and rapid cooling and filtration of materials, thereby improving production efficiency and reducing the intensity of manual operation and production costs. Attached Figure Description

[0034] The present invention will now be described in further detail with reference to the accompanying drawings and specific implementation methods.

[0035] Figure 1 This is a schematic diagram of the preparation apparatus in this invention;

[0036] Figure 2 This is a schematic diagram of the preparation process in this invention. Detailed Implementation

[0037] The present invention will be described in detail below with reference to the accompanying drawings and embodiments. It should be noted that, unless otherwise specified, the embodiments and features described in the present application can be combined with each other.

[0038] To make the technical solution of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0039] Reference Figure 1 An apparatus for preparing an environmentally friendly color-fixing agent includes a reaction vessel, a stirrer, a heating device, a dripping device, a cooling device, and a filtration device.

[0040] Reactor: As the core reaction vessel, it is used to hold raw materials and carry out various chemical reactions. It has a feed inlet at the top, which is connected to the raw material storage tank through a pipeline, allowing raw materials such as triethylenetriamine and acrylates to be transported into the reactor; and a discharge outlet at the bottom, which is connected to the cooling device through a pipeline, enabling the reaction materials to be transported to the cooling device for cooling treatment.

[0041] Agitator: Installed inside the reactor and driven by a motor, it stirs the materials within the reactor. During the reaction, continuous stirring ensures thorough mixing and uniform contact of the raw materials, accelerating the reaction rate, ensuring complete reaction, and improving the quality and consistency of the reaction products.

[0042] Heating device: Surrounding the outside of the reactor and closely fitted to it, it provides heat to the reactor through electric heating or heat transfer oil circulation. A temperature sensor monitors the internal temperature of the reactor in real time and is connected to the control system, allowing for precise adjustment of the reaction temperature according to process requirements, ensuring the reaction proceeds within a set temperature range.

[0043] Dropping device: Connected to the raw material storage tank, the dropping rate and amount of raw materials are controlled by a metering pump and pipeline. During the reaction, acrylate and propylene oxide raw materials can be slowly and precisely dripped into the reactor according to process requirements, ensuring the orderly progress and effectiveness of the reaction.

[0044] Cooling device: Utilizing either air or water cooling, this device receives the high-temperature material from the reactor and cools it down to room temperature. The outlet of the cooling device is connected to the filtration device via a pipeline, transporting the cooled material there.

[0045] Filtration device: It adopts precision filtration equipment, which can effectively filter the cooled mixture, remove unreacted impurities and insoluble substances, and finally obtain a pure and environmentally friendly color fixing agent product.

[0046] Preferably, in the S1 raw material preparation step, the amounts of monomer (A) containing ultraviolet absorbing groups, monomer (B) containing chlorine stabilizing groups, and dispersant (C) added satisfy the color fastness synergistic enhancement index formula:

[0047]

[0048] In the formula: A is the mass (kg) of the monomer containing the ultraviolet absorbing group, and the monomer is 2-hydroxy-4-acrylate benzophenone;

[0049] B represents the mass (kg) of the monomer containing the chlorine-containing stabilizing group, wherein the monomer is 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester;

[0050] C represents the mass (kg) of the dispersant, which is sodium lignosulfonate.

[0051] A0=0 and B0=0 represent the equivalent addition amounts of UV-absorbing monomers and chlorine-stabilizing monomers that are not introduced into traditional color-fixing agents, respectively.

[0052] C0 represents the conventional dosage (kg) of traditional dispersants, ranging from 8 to 12 kg.

[0053] The SCI value is ≥1.5 to achieve synergistic enhancement of lightfastness and chlorinefastness.

[0054] Example 1

[0055] Raw material preparation: Accurately weigh 100 kg of triethylenetriamine, 150 kg of acrylates, 80 kg of propylene oxide, 20 kg of 2-hydroxy-4-acrylate benzophenone, 15 kg of 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester, and 10 kg of sodium lignosulfonate.

[0056] First stage reaction: Triethylenetriamine was added to the reactor through the feed inlet at the top of the reactor. The heating device was started and the temperature was raised to 50°C. The stirrer was turned on and stirred at a speed of 100 r / min. Acrylic esters were slowly added dropwise using a dropping device. The addition was completed in 1 hour. Then the temperature was raised to 70°C and the reaction was carried out for 2 hours to obtain the first reaction product.

[0057] Second stage reaction: Add 2-hydroxy-4-acrylate benzophenone and 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester to the product of the first reaction, heat to 80°C, and slowly add propylene oxide dropwise under stirring. The addition is completed in 1.5 hours. Keep the reaction at this temperature for 3 hours to obtain the product of the second reaction.

[0058] Dispersion treatment: Sodium lignosulfonate was added to the second reaction product, the temperature was adjusted to 40℃, and the mixture was stirred at 80r / min for 1 hour to obtain the mixture.

[0059] Post-processing: The mixture is transported through the bottom outlet of the reactor to a cooling device to cool to room temperature, and then sent to a filtration device for filtration to obtain the environmentally friendly color-fixing agent product.

[0060] This embodiment achieves effective improvement in the color fastness to sunlight and chlorine by precisely controlling the raw material ratio and reaction conditions, while ensuring the stability and feasibility of the preparation process.

[0061] Example 2

[0062] Raw material preparation: Weigh 120 kg of triethylenetriamine, 180 kg of acrylates, 90 kg of propylene oxide, 25 kg of 2-hydroxy-4-acrylate benzophenone, 20 kg of 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester, and 12 kg of sodium lignosulfonate.

[0063] First stage reaction: Triethylenetriamine was added to the reactor and heated to 55°C. The stirring speed was set to 120 r / min. Acrylic esters were slowly added dropwise using a dropping device. The addition was completed within 2 hours. Then the temperature was raised to 75°C and the reaction was carried out for 2.5 hours to obtain the first reaction product.

[0064] Second stage reaction: Add monomers containing ultraviolet absorbing groups and monomers containing chlorine stabilizing groups to the product of the first reaction, heat to 85°C, add propylene oxide dropwise over 2 hours, and then keep the reaction at the temperature for 3.5 hours to obtain the product of the second reaction.

[0065] Dispersion treatment: Add sodium lignosulfonate and stir at 45°C for 1.2 hours to obtain a mixture.

[0066] Post-processing: Cool the mixture to room temperature and filter to obtain the environmentally friendly color-fixing agent product.

[0067] This embodiment further optimizes the performance of the environmentally friendly color-fixing agent by adjusting the amount of raw materials and reaction parameters. The prepared color-fixing agent not only performs well in terms of resistance to sunlight and chlorine, but also shows a significant improvement in overall color fastness.

[0068] Example 3

[0069] Raw material preparation: Take 150 kg of triethylenetriamine, 200 kg of acrylates, 100 kg of propylene oxide, 30 kg of 2-hydroxy-4-acrylate benzophenone, 25 kg of 2-methyl-2-acrylate-2-[bis(2-chloroethyl)amino]ethyl ester, and 15 kg of sodium lignosulfonate.

[0070] First stage reaction: Triethylenetriamine was placed in a reaction vessel, heated to 60°C, and stirred at 150 r / min. Acrylic esters were added dropwise over 1.5 hours. After the addition was completed, the temperature was raised to 80°C and the reaction was carried out for 3 hours to obtain the first reaction product.

[0071] Second stage reaction: Add a monomer containing a special group, heat to 90°C, add propylene oxide dropwise, take 2.5 hours, keep the temperature for 4 hours, and obtain the second reaction product.

[0072] Dispersion treatment: Add dispersant and stir at 50°C for 1.5 hours to obtain a mixture.

[0073] Post-processing: Cooling and filtration yield the environmentally friendly color-fixing agent product.

[0074] This embodiment, by increasing the input of raw materials and extending the reaction time, fully stimulates the chemical reaction between the raw materials. The prepared environmentally friendly color-fixing agent achieves a high level in all performance indicators, especially in terms of resistance to harsh environments. The process and apparatus of this invention have great potential to improve product performance.

[0075] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A preparation device of an environmentally friendly color fixing agent, comprising a reaction kettle, a stirrer, a heating device, a dropping device, a cooling device and a filtering device, characterized in that: the top of the reaction kettle is provided with a feeding port connected with a raw material storage tank through a pipeline, so that triethylenetriamine and acrylate raw materials can be transported into the reaction kettle; the bottom is provided with a discharging port connected with the cooling device through a pipeline, so that the reacted materials can be transported to the cooling device for cooling treatment; the stirrer is installed in the reaction kettle and driven by a motor, so that the materials in the reaction kettle can be stirred; the heating device is wrapped around the outside of the reaction kettle and closely adheres to the reaction kettle, so that the reaction kettle is provided with heat by electric heating or heat conduction oil circulation; the dropping device is connected with the raw material storage tank, so that the dropping speed and dropping amount of the raw materials are controlled through a metering pump and a pipeline; the discharging end of the cooling device is connected with the filtering device through a pipeline, so that the cooled materials are transported to the filtering device; the filtering device can effectively filter the cooled mixed materials, remove the unreacted impurities and insoluble substances, and finally obtain pure environmentally friendly color fixing agent products. The reaction kettle is a core reaction container for carrying raw materials and performing various chemical reactions; the stirrer continuously stirs the raw materials during the reaction to make them fully mixed and uniformly contacted, accelerates the reaction rate, ensures the full reaction, and improves the quality and consistency of the reaction products; the heating device monitors the temperature in the reaction kettle in real time through a temperature sensor and is connected with a control system, so that the reaction temperature can be accurately adjusted according to the process requirements, so that the reaction is carried out in the set temperature range; the dropping device can slowly and accurately drop acrylate and propylene oxide raw materials into the reaction kettle according to the process requirements during the reaction, so as to ensure the orderly progress and reaction effect of the reaction; the cooling device adopts air cooling or water cooling to receive high-temperature materials from the reaction kettle, cool and cool them, and reduce the temperature of the materials to room temperature. The preparation device comprises the following steps: S1, raw material preparation: prepare triethylenetriamine, acrylate, propylene oxide, monomer containing ultraviolet absorbing group, monomer containing chlorine stabilizing group and dispersing agent; S2, first stage reaction: triethylenetriamine is added into the reaction kettle through the connecting pipeline of the feeding port at the top of the reaction kettle and the raw material storage tank, the heating device is started, the temperature is heated to 50℃ by the close heating mode of the heating device and the reaction kettle, the stirrer is started, acrylate is slowly dropped through the pipeline connected with the raw material storage tank by the dropping device under stirring condition, the dropping time is controlled within 1 hour, after the dropping is completed, the temperature is raised to 70℃ by the heating device, and the reaction is carried out for 2 hours to obtain the first reaction product; S3, second stage reaction: the monomer containing ultraviolet absorbing group and the monomer containing chlorine stabilizing group are added into the first reaction product, the temperature is raised to 80℃ by the heating device, propylene oxide is slowly added again by the dropping device under stirring condition, the dropping time is controlled within 1.5 hours, after the dropping is completed, the temperature is kept by the heating device for 3 hours to obtain the second reaction product. ​ 2. The preparation device of an environmentally friendly color fixing agent according to claim 1, characterized in that: ​ ​ ​ ​ ​ 3. A process for preparing an environmentally friendly fixing agent, using the apparatus for preparing an environmentally friendly fixing agent according to claim 2, characterized in that, ​ ​ ​ ​ S4, dispersion treatment: adding a dispersant into the second reaction product, adjusting the temperature to 40 DEG C by using a heating device, stirring the mixture by a stirrer at the temperature for 1 hour to make the dispersant fully dispersed in the reaction product, obtaining a mixture; S5, post-treatment: conveying the mixture through a pipeline connected between a bottom outlet of a reaction kettle and a cooling device to the cooling device, cooling to room temperature, then conveying the mixture through a pipeline connected between the cooling device and a filtering device to the filtering device to remove unreacted impurities and insoluble substances, obtaining an environment-friendly color fixing agent product.

4. The preparation process of the environment-friendly color fixing agent according to claim 3, characterized in that: In the S1 raw material preparation step, the monomer containing an ultraviolet absorption group is 2-hydroxy-4-acrylate benzophenone; the monomer containing a chlorine stabilizing group is 2-methyl-2-acrylic acid-2-[bis(2-chloroethyl) amino] ethyl ester; and the dispersant is sodium lignosulfonate.

5. The preparation process of the environment-friendly color fixing agent according to claim 3, characterized in that: In the S1 raw material preparation step, the adding amount of the monomer (A) containing an ultraviolet absorption group, the monomer (B) containing a chlorine stabilizing group and the dispersant (C) satisfies a color fastness synergistic enhancement index formula: In the formula: A is the mass of the monomer containing an ultraviolet absorption group, which is 2-hydroxy-4-acrylate benzophenone; B is the mass of the monomer containing a chlorine stabilizing group, which is 2-methyl-2-acrylic acid-2-[bis(2-chloroethyl) amino] ethyl ester; C is the mass of the dispersant, which is sodium lignosulfonate; A0 and B0 are respectively the equivalent adding amount of the monomer containing an ultraviolet absorption group and the monomer containing a chlorine stabilizing group which are not introduced in a traditional color fixing agent; C0 is the conventional amount of a traditional dispersant, and the value range is 8-12 kg; The SCI value is greater than or equal to 1.5 to realize the synergistic enhancement of the fastness to sunlight and the fastness to chlorine.

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