Slow-release composite acetate low-freezing-point filler and preparation method thereof
By preparing a slow-release composite acetate low-freezing-point filler, and utilizing the composite technology of acetate and porous carrier and phenolic resin coating technology, the problems of excessively rapid acetate release and corrosiveness were solved, achieving a highly efficient and environmentally friendly snow melting and de-icing effect.
Patent Information
- Application Number
- CN202510902247.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-01
- Publication Date
- 2025-10-31
AI Technical Summary
Existing acetate-based de-icing agents are highly water-soluble during use, resulting in an excessively rapid release of active ingredients, which reduces their service life and economic efficiency. Furthermore, traditional chloride-based de-icing agents are corrosive to facilities and the environment.
By combining acetate with porous carriers such as lignin fiber and diatomaceous earth, and using phenolic resin coating technology, a slow-release composite acetate low-freezing-point filler was prepared to control the uniform adsorption and slow release of acetate in the pores of the carrier.
It achieves slow release of acetate, extends service life, reduces environmental pollution, reduces corrosiveness to facilities, and improves snow melting and de-icing efficiency and environmental friendliness.
Smart Images
Figure CN120865843A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of composite acetate, specifically to a slow-release composite acetate low-freezing-point filler and its preparation method. Background Technology
[0002] In cold regions, roads, bridges, and airport runways often become slippery due to snowfall or ice, severely impacting traffic safety. Traditionally, chloride-based de-icing agents, such as sodium chloride and calcium chloride, are widely used to lower the freezing point and accelerate snow and ice melting. However, chloride-based de-icing agents are highly corrosive, causing varying degrees of damage to road infrastructure, vehicle chassis, and the surrounding environment, particularly affecting metal components and concrete structures. Long-term use can also lead to soil salinization. Therefore, developing environmentally friendly, efficient, and low-corrosion novel low-freezing-point fillers has become a research hotspot. Acetate-based de-icing agents, due to their excellent low-temperature performance and low corrosivity, have been widely used in airports and other locations with high corrosion control requirements. Common organic salts such as sodium acetate, calcium acetate, and magnesium acetate exhibit good environmental adaptability and low toxicity during snow and ice removal. However, their high water solubility allows them to be quickly washed away by rainwater or snowmelt, resulting in an excessively rapid release of active ingredients, reducing their service life and economic efficiency. Therefore, it is essential to design a slow-release composite acetate low-freezing-point filler with excellent slow-release performance and its preparation method. Summary of the Invention
[0003] (a) Technical problems to be solved
[0004] To address the shortcomings of existing technologies, this invention provides a slow-release composite acetate low-freezing-point filler and its preparation method, which has advantages such as PPP and solves the problems mentioned in the background technology.
[0005] (II) Technical Solution
[0006] To achieve the aforementioned PPP objective, this invention provides the following technical solution: a method for preparing a sustained-release composite acetate, comprising the following steps: Select any two or more acetates from sodium acetate, calcium acetate, potassium acetate or magnesium acetate according to a preset ratio, and mix them evenly to obtain an acetate mixture. According to the target sustained-release performance requirements, any two or more carriers from lignin fiber, diatomaceous earth, bentonite, zeolite, and attapulgite are selected and uniformly mixed to obtain a composite carrier. Place deionized water in an oil bath stirring pot, control the heating temperature to 60℃, add the acetate mixture, maintain a constant stirring speed of 500r / min, and continue stirring until all acetate is dissolved to form a homogeneous solution. The composite carrier was slowly added within 10 minutes after the acetate was completely dissolved, and stirring was maintained for 2 hours to ensure that the acetate was uniformly adsorbed into the pores and surface structure of the carrier. The adsorbed slurry was transferred to a constant temperature drying oven and dried at 120°C for 68 hours to ensure that the moisture content was below 2%. The dried solid material is mechanically crushed to control the particle size at 0.06 mm, and then an intermediate product with uniform particle size is obtained by ultrasonic sieving. The intermediate product is coated with phenolic resin through an atomizing nozzle. The phenolic resin used for coating is pre-diluted to 30% solid content, and uniform coating is achieved by spray coating. The coated material is then dried, pulverized, and sieved again to obtain a slow-release composite acetate product.
[0007] Preferably, the acetate is a mixture of two or more of sodium acetate, calcium acetate, potassium acetate and magnesium acetate, the carrier is a mixture of two or more of lignin fiber, diatomaceous earth, zeolite, bentonite and attapulgite, and the coating material is phenolic resin.
[0008] Preferably, the mass ratio of sodium acetate to calcium acetate is 6:4, and the mass ratio of diatomaceous earth to lignin fiber is 6:4.
[0009] Preferably, the mass percentage of acetate mixture to composite carrier is 74.975%, and the mass percentage of acetate mixture to phenolic resin is 95.238%.
[0010] Preferably, the heating temperature is 60°C.
[0011] Preferably, the mixing speed of the mixer is 500 r / min and the mixing time is 2 h.
[0012] Preferably, the temperature of the constant temperature drying oven is set to 120℃.
[0013] Preferably, the particle size of the material after crushing is 0~0.06mm.
[0014] (III) Beneficial Effects
[0015] Compared with the prior art, the present invention provides a slow-release composite acetate low-freezing-point filler and its preparation method, which has the following beneficial effects: This invention utilizes a compound of two or more acetates to effectively synergize the low freezing point characteristics and slow-release behavior of each component, thereby improving overall snow melting and de-icing efficiency. Secondly, the use of porous and highly absorbent composite carriers such as lignin fiber, diatomaceous earth, and bentonite not only enhances the loading capacity of acetates but also significantly improves the slow-release performance of the finished product, enabling long-term release in low-temperature environments and effectively extending its service life. Furthermore, by controlling process parameters such as heating, stirring, and drying, the full adsorption and uniform distribution of acetates within the carrier pores are ensured, improving the product's structural stability and performance consistency. Subsequent phenolic resin spray coating technology further enhances the acetates' resistance to runoff in high-humidity or rainy / snowy environments, reducing environmental pollution and material waste. The resulting product exhibits uniform particle size and good flowability, facilitating on-site application and construction, demonstrating good feasibility for industrial production and promotional value. It is a green, environmentally friendly, highly efficient, and durable low-freezing-point functional filler. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the method of the present invention; Figure 2 This is an image showing the effect of corrosion on a Q235 steel sheet. Detailed Implementation
[0017] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0018] Example 1: Please refer to Figure 1 As shown in the embodiment of the present invention, a method for preparing a sustained-release composite acetate is characterized by comprising the following steps: Select any two or more acetates from sodium acetate, calcium acetate, potassium acetate or magnesium acetate according to a preset ratio, and mix them evenly to obtain an acetate mixture. According to the target sustained-release performance requirements, any two or more carriers from lignin fiber, diatomaceous earth, bentonite, zeolite, and attapulgite are selected and uniformly mixed to obtain a composite carrier. Place deionized water in an oil bath stirring pot, control the heating temperature to 60℃, add the acetate mixture, maintain a constant stirring speed of 500r / min, and continue stirring until all acetate is dissolved to form a homogeneous solution. The composite carrier was slowly added within 10 minutes after the acetate was completely dissolved, and stirring was maintained for 2 hours to ensure that the acetate was uniformly adsorbed into the pores and surface structure of the carrier. The adsorbed slurry was transferred to a constant temperature drying oven and dried at 120°C for 68 hours to ensure that the moisture content was below 2%. The dried solid material is mechanically crushed to control the particle size at 0.06 mm, and then an intermediate product with uniform particle size is obtained by ultrasonic sieving. The intermediate product is coated with phenolic resin through an atomizing nozzle. The phenolic resin used for coating is pre-diluted to 30% solid content, and uniform coating is achieved by spray coating. The coated material is then dried, pulverized, and sieved again to obtain a slow-release composite acetate product.
[0019] The acetate is a mixture of two or more of sodium acetate, calcium acetate, potassium acetate and magnesium acetate, the carrier is a mixture of two or more of lignin fiber, diatomaceous earth, zeolite, bentonite and attapulgite, and the coating material is phenolic resin.
[0020] The mass ratio of sodium acetate to calcium acetate is 6:4, and the mass ratio of diatomaceous earth to lignin fiber is 6:4.
[0021] The mass percentage of the acetate mixture to the composite carrier is 74.975%, and the mass percentage of the acetate mixture to the phenolic resin is 95.238%.
[0022] The heating temperature is 60°C.
[0023] The mixer has a mixing speed of 500 r / min and a mixing time of 2 h.
[0024] The temperature of the constant temperature drying oven is set to 120℃.
[0025] The particle size of the material after pulverization is 0~0.06mm.
[0026] Example 2: Preparation of acetate low freezing point filler (1) Weigh a certain amount of sodium acetate and calcium acetate and put them into a constant temperature drying oven at 60℃ for 2 hours; weigh 30g of sodium acetate and 20g of sodium acetate according to the mass ratio of sodium acetate to calcium acetate of 6:4.
[0027] (2) Weigh 100g of deionized water and add it to the acetate in step 1. Stir in an oil bath at 60°C for 0.5h to obtain a saturated acetate solution.
[0028] (3) Weigh a certain amount of diatomaceous earth and lignin fiber and put them into a constant temperature drying oven at 100℃ for 2 hours; and weigh 40g of diatomaceous earth and 24g of lignin fiber in a ratio of 5:3.
[0029] (4) The diatomaceous earth and lignin weighed in step 3 are slowly added to the acetate solution prepared in step 2, and stirred in an oil bath at 60°C for 1 hour at a speed of 500 r / min to obtain a low freezing point acetate solution.
[0030] (5) Place the mixed solution prepared in step 4 into a constant temperature drying oven at 120°C and dry it. After drying, grind it into powder and sieve it through a 0.06mm sieve to obtain acetate low freezing point filler.
[0031] Example 3: Preparation of sustained-release composite acetate low-freezing-point filler (1) Weigh 52g of water-soluble phenolic resin and 100g of ethanol. Slowly add the ethanol to the phenolic resin and stir with a mixer at a speed of 500 r / min to obtain a diluted phenolic resin solution.
[0032] (2) The acetate low freezing point filler prepared in Example 1 was slowly added to the phenolic resin dilution solution, and the stirring speed was kept constant for 1 hour to obtain a mixture.
[0033] (3) The mixture prepared in step 2 is placed in a constant temperature drying oven at 80°C and dried. After drying, it is ground into powder and sieved through a 0.06mm sieve to obtain a slow-release acetate low freezing point filler.
[0034] Example 4:
[0035] I. Ice-melting test Take 2g of the slow-release composite acetate low-freezing-point filler prepared in Example 2 and the control samples sodium chloride and MF, respectively. Set up two parallel experimental groups for each salt material, and set up two blank control groups. Place all the above samples in a low-temperature constant temperature chamber at 5℃ for 1 hour to complete the pretreatment. Prepare 8 beakers of the same size, add 100g of deionized water to each, and place them in a constant temperature environment at -10℃ for 4 hours to make ice blocks. Then, evenly sprinkle the pretreated salt materials of each experimental group and control group on the surface of the ice blocks in the corresponding beakers, and then place all beakers together in a constant temperature environment chamber at 5℃ for melting test. During the test, accurately weigh the melting mass of each ice block every 20 minutes and record the data in detail. The test results are shown in Table 2 below.
[0036] Table 1. Cumulative ice melt volume (g) As shown in Table 1, the ice melting amount of the blank control group under natural conditions was significantly lower than that of the experimental groups with added sodium chloride (NaCl), MF, and slow-release composite acetate low-freezing-point filler. This fully demonstrates that the slow-release composite acetate low-freezing-point filler has excellent ice melting performance. Specifically, although the ice melting amount of the experimental group with added slow-release composite acetate low-freezing-point filler was less than that of the experimental group with added NaCl, it was close to that of the experimental group with added MF. Behind this seemingly similar ice melting effect, the two have fundamentally different mechanisms of action. MF mainly relies on its own chemical structure to form a eutectic with ice to achieve ice melting, while the slow-release composite acetate low-freezing-point filler, through the coating effect of the gel membrane, precisely controls the release rate of inorganic salts, allowing the salt to continuously and slowly contact the ice and snow, effectively avoiding the problem of ice melting efficiency decay due to excessively high local concentrations. It is worth noting that, based on careful observation during the experiment, the experimental group with the addition of slow-release composite acetate low-freezing-point filler formed a more uniform meltwater film on the ice and snow surface, which was completely different from the water puddles formed by the NaCl experimental group due to localized excessive melting.
[0037] II. Environmental Protection Test To evaluate the environmental performance of the slow-release composite acetate low-freezing-point filler, the following experiment was conducted: First, the surface of Q235 steel sheets was wiped with anhydrous alcohol to remove grease and impurities, followed by cleaning and drying with deionized water. Next, solutions of 3% slow-release composite acetate low-freezing-point filler, 3% sodium chloride solution, and 3% MF solution were prepared, with deionized water used as a control group. Finally, a wet-dry cycle was performed. The pre-treated steel sheets were marked and immersed in the corresponding solutions, maintaining the liquid level at 3 / 4 of the steel sheet. A 30-day wet-dry cycle test was conducted, with the steel sheets removed every 24 hours, allowed to air dry in a dry environment, and then returned to the original solution for further immersion, thus simulating the corrosion process in a real environment. The cycle was repeated for 30 days.
[0038] according to Figure 2The experimental results show that each solution produced varying degrees of corrosion on pure Q235 steel sheets. Macroscopic morphological observation and analysis of the corroded steel sheets revealed the following order of corrosion severity from highest to lowest: sodium chloride solution > MF solution > slow-release composite acetate low-freezing-point filler > deionized water. The steel sheets immersed in sodium chloride solution exhibited the most significant corrosion, with a large, dense layer of reddish-brown rust forming on their surface, and localized rust accumulation and blocky peeling. The steel sheets in MF solution also showed a large amount of rust on their surface, exhibiting relatively obvious rust marks, indicating that MF solution has strong metallic corrosiveness. In contrast, deionized water and slow-release composite acetate low-freezing-point filler had significantly weaker corrosive effects on the steel sheets, with only a few scattered reddish-brown rust spots on the surface, and the corrosion product layer was thin, loose, and poorly adhered. The above test results fully demonstrate that, compared with sodium chloride solution and MF solution, the slow-release composite acetate low-freezing-point filler has significantly reduced corrosivity to metal materials and has excellent corrosion inhibition performance. In practical applications, it can effectively reduce corrosion damage to metal parts of roads, bridges and vehicles.
[0039] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.
[0040] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a sustained-release composite acetate, characterized in that, Includes the following steps: Select any two or more acetates from sodium acetate, calcium acetate, potassium acetate or magnesium acetate according to a preset ratio, and mix them evenly to obtain an acetate mixture. According to the target sustained-release performance requirements, any two or more carriers from lignin fiber, diatomaceous earth, bentonite, zeolite, and attapulgite are selected and uniformly mixed to obtain a composite carrier. Place deionized water in an oil bath stirring pot, control the heating temperature to 60℃, add the acetate mixture, maintain a constant stirring speed of 500r / min, and continue stirring until all acetate is dissolved to form a homogeneous solution. The composite carrier was slowly added within 10 minutes after the acetate was completely dissolved, and stirring was maintained for 2 hours to ensure that the acetate was uniformly adsorbed into the pores and surface structure of the carrier. The adsorbed slurry was transferred to a constant temperature drying oven and dried at 120°C for 68 hours to ensure that the moisture content was below 2%. The dried solid material is mechanically crushed to control the particle size at 0.06 mm, and then an intermediate product with uniform particle size is obtained by ultrasonic sieving. The intermediate product is coated with phenolic resin through an atomizing nozzle. The phenolic resin used for coating is pre-diluted to 30% solid content, and uniform coating is achieved by spray coating. The coated material is then dried, pulverized, and sieved again to obtain a slow-release composite acetate product.
2. The method for preparing a sustained-release composite acetate according to claim 1, characterized in that, Acetate is a mixture of two or more of sodium acetate, calcium acetate, potassium acetate and magnesium acetate, the carrier is a mixture of two or more of lignin fiber, diatomaceous earth, zeolite, bentonite and attapulgite, and the coating material is phenolic resin.
3. The method for preparing a sustained-release composite acetate according to claim 2, characterized in that, The mass ratio of sodium acetate to calcium acetate is 6:4, and the mass ratio of diatomaceous earth to lignin fiber is 6:
4.
4. The method for preparing a sustained-release composite acetate according to claim 1, characterized in that, The mass percentage of acetate mixture to composite carrier is 74.975%, and the mass percentage of acetate mixture to phenolic resin is 95.238%.
5. The method for preparing a sustained-release composite acetate according to claim 1, characterized in that, The heating temperature is 60℃.
6. The method for preparing a sustained-release composite acetate according to claim 1, characterized in that, The mixer's mixing speed is 500 r / min, and the mixing time is 2 hours.
7. The method for preparing a sustained-release composite acetate according to claim 1, characterized in that, The temperature of the constant temperature drying oven is set to 120℃.
8. The method for preparing a sustained-release composite acetate according to claim 1, characterized in that, The particle size of the material after crushing is 0~0.06mm.
9. A slow-release composite acetate low-freezing-point filler, characterized in that, It is prepared by the method described in any one of claims 1-8.