A kind of amaryllis bulb sealing wax material and preparation method thereof

Abstract

The present invention belongs to the field of chemical synthesis, and specifically relates to a wax sealing material for Amaryllis bulbs and a preparation method thereof. The method comprises: (1) preparing raw materials according to the following weight percentages: 33-37 wt% hexafluoropropylene oligomer, 4-6 wt% beeswax, 0.5-1.0 wt% tackifier, and the balance being high-melting-point paraffin wax; (2) mixing and stirring the hexafluoropropylene oligomer and beeswax to prepare a first-stage mixture; (3) mixing and stirring the first-stage mixture with high-melting-point paraffin wax to prepare a second-stage mixture; (4) uniformly mixing the second-stage mixture and the tackifier, and naturally cooling to obtain the wax sealing material for Amaryllis bulbs. The wax sealing material of the present invention can not only play a good waterproof and antibacterial role as well as a mechanical protective role, but also further optimize the respiratory environment of Amaryllis bulbs, thereby improving their respiration and increasing the flowering rate and flowering period of the wax-sealed Amaryllis.

Description

Technical Field

[0001] The invention belongs to the field of chemical synthesis, and particularly relates to a wax sealing material for amaryllis bulbs and a preparation method thereof. Background Art

[0002] Amaryllis is a perennial herbaceous plant in the Amaryllidaceae family, native to Peru and Brazil. Its upright, beautifully shaped flowers, large, elegantly arranged, and vibrantly colored, make it a highly ornamental plant. In southern China, it blooms from April to May, typically with four flowers per stem, each blooming for about seven days, or 14 days per plant. It is often used for cut flowers, potted plants, and garden beautification. Amaryllis prefers warm, humid, and sunny environments. Its bulbs contain a rich reservoir of nutrients and water, which supports growth and flowering after its dormant period. Furthermore, under adverse conditions, the bulbs help the plant survive drought and other stressful periods. Under favorable growing conditions, the bulbs serve as the source of new leaves and flower stalks, further promoting the growth of new plant tissue. Mature Amaryllis bulbs produce daughter bulbs, which can be divided and propagated. Once separated, the daughter bulbs can be cultivated into independent plants.

[0003] The wax-sealed amaryllis technique is a unique treatment method that allows amaryllis to grow and bloom normally in a soilless environment. This technique involves encasing the base of the bulb in a waxy substance, leaving only the flower buds at the top exposed. By sealing the base of the bulb with wax, the wax-sealed amaryllis technique effectively reduces water loss, ensuring a continuous supply of moisture and nutrients within the bulb to the developing flower buds. The wax-sealed design allows amaryllis to grow in a soilless environment, requiring no watering or fertilizer. This makes them ideal low-maintenance interior decorations. Since they don't require traditional planting, wax-sealed amaryllis can be easily placed anywhere in the home, such as on tabletops and windowsills, increasing their placement flexibility. Furthermore, wax-sealed amaryllis boasts an exceptionally high flowering rate, typically exceeding 90%. Simply place them in suitable temperature and light conditions, and they will bloom within approximately 30 days.

[0004] However, with the recent increase in sales of wax-sealed amaryllis, the original flowering rate has gradually fallen short of expectations, resulting in numerous customer complaints about insufficient flowering rates. Our R&D staff identified a key issue: While wax sealing effectively locks in and preserves the bulb's nutrients, protecting it from common diseases like insects and root rot, thereby maintaining a healthy, long-lasting flowering period and vibrant color, it also effectively protects the flower. However, the wax seal also affects the plant's respiration. This is primarily due to the characteristics of the wax used in wax-sealed amaryllis. During the wax sealing process, a blank area is created 1.5 to 2.5 cm below the top of the bulb's bud, eliminating the need for protective wax. This protects the bud and ensures proper budding and flowering. This is because the bulb undergoes normal respiration and evaporation processes. Excessive blanking can prematurely deplete the bulb's moisture and nutrients. The main purpose is to limit evaporation from wax-sealed amaryllis bulbs, as they typically have an excess of nutrients. However, due to the nature of wax-sealed bulbs, water loss cannot be replenished, which can lead to a decrease in flowering rate. Therefore, our company has focused on researching how to inhibit evaporation from amaryllis bulbs while improving their respiratory environment. Summary of the Invention

[0005] In order to solve the problems that the existing wax-sealed amaryllis has a limited flowering rate and the existing wax-sealing technology reduces the evaporation water loss of the bulb while excessively suppressing its respiration, the present invention provides an amaryllis bulb sealing wax material and a preparation method of the sealing wax material.

[0006] The main objectives of the present invention are:

[0007] 1. It can further improve the water and air permeability of wax seal materials;

[0008] 2. Ensure that the wax sealing material can more effectively maintain the effective respiration of Amaryllis after wax sealing;

[0009] 3. It has good protective effect.

[0010] To achieve the above objectives, the present invention adopts the following technical solutions.

[0011] A preparation method for amaryllis bulb sealing wax material,

[0012] The method comprises:

[0013] (1) The raw materials are prepared according to the following weight percentages: hexafluoropropylene oligomer 33-37 wt%, beeswax 4-6 wt%, tackifier 0.5-1.0 wt%, and the balance is high melting point paraffin wax;

[0014] The high melting point paraffin wax is C28-C30 paraffin wax, which generally has a melting point of 61-65.5°C. The melting point of standard C28 paraffin wax is 61.1°C, and the melting point of standard C30 paraffin wax is 65.5°C. Unless otherwise specified, the standard C28 paraffin wax with a melting point of 61.1°C is used in the present invention.

[0015] (2) mixing hexafluoropropylene oligomer and beeswax and stirring them to react to prepare a first-stage mixture;

[0016] (3) Mixing the first stage mixture with high melting point paraffin wax and stirring to react to prepare the second stage mixture;

[0017] (4) The second-stage mixture and the viscosity enhancer are mixed evenly, and the mixture is cooled naturally to obtain the wax sealing material for the amaryllis bulbs.

[0018] As a preference,

[0019] The hexafluoropropylene oligomer in step (1) is prepared by the following method:

[0020] The perfluorinated compound, nitrile compound, polymer and metal fluoride salt are uniformly mixed in proportion, and stirred and thermally reacted under high pressure conditions to obtain the directionally prepared hexafluoropropylene oligomer.

[0021] As a preference,

[0022] The perfluorinated compound is liquid hexafluoropropylene that has been subjected to a pressure treatment;

[0023] The nitrile compound is acetonitrile;

[0024] The polymer is polyethylene glycol;

[0025] The metal fluoride salt is potassium fluoride;

[0026] The perfluorinated compound, nitrile compound, polymer and metal fluoride salt are uniformly mixed in a mass ratio of 1.5: (4-6): (0.04-0.06): 0.02.

[0027] As a preference,

[0028] The high pressure condition is an ambient pressure of 1.0 to 1.2 MPa;

[0029] The stirring thermal reaction is carried out at 75-85° C. and 80-120 rpm for 40-45 min.

[0030] As a preference,

[0031] The mixing and stirring reaction in step (2) is carried out at 0.3-0.4 MPa, 95-105°C, and at a stirring speed of 40-60 rpm for 45-75 min.

[0032] As a preference,

[0033] The mixing and stirring reaction in step (3) is carried out at 0.3-0.4 MPa, 120-140°C, and at a stirring speed of 70-90 rpm for 60-90 min.

[0034] As a preference,

[0035] The uniform mixing in step (4) is carried out by stirring and mixing at a speed of 30 to 50 rpm for 60 to 90 minutes under the conditions of 0.3 to 0.4 MPa and 100 to 120°C.

[0036] A wax sealing material for amaryllis bulbs.

[0037] For technical solution of the present invention, actual research and development thinking is to derive from the PTFE preservative film used for part plant transplanting. PTFE preservative film has a large amount of use in protecting root and branch during plant transplanting, and it has the effect of good hydrophobic water-proof and waterproof, but has certain air permeability, allows gas to pass through. But when it is used for amaryllis wax seal, but there are many problems again, such as how it is mixed into wax seal material, and its air permeability is too strong and may also cause the respiration of amaryllis bulb to be too vigorous, causing its nutrients to be lost too fast, causing the situations such as shortening of flowering period, decline in flowering rate to occur, and PTFE is usually difficult to build a stable supporting structure to form mechanical protection, and for example the most critical PTFE has the possibility of fluorine diffusion, fluorine has cytotoxicity, and all has influence on the metabolic process of plant and the processes such as cell division, and although PTFE is very stable, has outstanding chemical resistance, but in the case of direct contact and in the wax seal process of melt-plated aluminum, fluorine diffusion is still likely to occur. For example, in early experiments, the standard DGT (dynamic adsorption gel technology) was used to characterize the diffusion of fluorine in Amaryllis bulbs when PTFE was added or directly encapsulated with PTFE, confirming the existence of this process.

[0038] After experimenting with different materials, technicians discovered the unique properties of hexafluoropropylene oligomers. Because they have low melting and boiling points, the wax sealing process can be performed at lower temperatures to minimize damage to the Amaryllis bulbs. Furthermore, after mixing and solidifying, the materials synergistically create a dual-layer structure of separation and support layers, effectively enhancing gas exchange while ensuring excellent mechanical support and waterproofing.

[0039] To this end, the present invention stirs a hexafluoropropylene oligomer under a specific temperature and pressure to form a stable oligomer solution. This solution is then mixed with additives in a specific ratio to produce a first-stage mixed material. The first-stage mixed material is then further mixed with other ingredients to produce a second-stage mixed material. Finally, the second-stage mixed material is stirred and mixed under suitable conditions to produce a wax sealing material for Amaryllis bulbs. This preparation method yields a wax sealing material with excellent physical and chemical properties, effectively protecting Amaryllis bulbs and extending their shelf life.

[0040] The key point lies in the nucleophilic addition reaction of hexafluoropropylene. Due to the significant electron-withdrawing properties of the fluorine atoms attached to its double bond, hexafluoropropylene is more susceptible to nucleophilic addition reactions than common alkenes. Liquid-phase oligomerization is a common method for preparing hexafluoropropylene oligomers. This process is typically carried out in a dry, aprotic, polar solvent containing a catalyst under specific temperature and pressure conditions. The products are primarily composed of hexafluoropropylene dimers and trimers. By selecting different reaction conditions, such as solvents and catalysts, oligomers with specific structures can be prepared. Hexafluoropropylene oligomers, including dimers and trimers, exhibit excellent chemical and thermodynamic stability, making them useful as solvents and media in specialized environments and as raw materials for the synthesis of polymers, intermediates, and surfactants. The different solubility of different isomers in solvents and their varying reactivity with nucleophiles also contribute to their diverse applications. Due to the high reactivity of the carbon-carbon double bond, hexafluoropropylene dimers react with a variety of nucleophiles, enabling the synthesis of a variety of fluorinated heterocyclic organic compounds through a series of chemical reactions. Surfactants are substances that can reduce surface tension and are usually composed of two groups, hydrophilic and hydrophobic. Fluorosurfactants are hydrocarbon surfactants in which hydrogen is replaced by fluorine, and their fluorinated carbon chains have hydrophobic and oleophobic properties. Compared with ordinary hydrocarbon surfactants, fluorinated surfactants have higher efficiency and stronger stability, so they can be used as high-efficiency fine chemicals in complex environments. The carbon atoms of hexafluoropropylene oligomers are connected to fluorine atoms. Due to the strong electronegativity of fluorine, unlike ordinary hydrocarbon alkenes, they are not easy to react with electrophilic reagents. The carbon-carbon double bond of hexafluoropropylene oligomers and the fluorine atoms connected to them have good activity. Through a series of reactions with nucleophilic reagents, fluorinated surfactants derived from hexafluoropropylene oligomers can be prepared.

[0041] Experiments have shown that under controlled, low room temperature conditions, the oligomerization of hexafluoropropylene in acetonitrile exhibits high selectivity for dimers. The addition of polyethylene glycol further directs the selective conversion of hexafluoropropylene to trimers. In the system of the present invention, polyethylene glycol acts as both a solvent and a catalyst. Unlike acetonitrile, its addition exhibits unique selectivity in the experiments, promoting the formation of highly polymerized (trimeric) hexafluoropropylene and improving its conversion rate to a certain extent. Combined with the relatively higher reaction temperature of the present invention, trimer selectivity in the oligomers of the present invention is significantly improved. While hexafluoropropylene oligomers, as fluorinated polymers, are inherently susceptible to fluorine diffusion, trimers are more effective at suppressing this diffusion than dimers. Furthermore, research indicates that when acetonitrile combines with halides to form complex salts, these complex salts can complex with cations in alkali metal fluorides, accelerating the dissociation of fluoride anions and thus increasing the reaction rate. The choice of acetonitrile as a solvent is primarily influenced by the radius of the alkali metal fluoride cation. This invention achieves the goal of enhancing material strength, improving wear resistance, and enhancing chemical corrosion resistance by blending different hexafluoropropylene oligomers with paraffin wax. Considering both performance enhancement and cost-effectiveness, blending modification has proven to be the most promising method for modifying sealing wax materials.

[0042] The unique structure of the resulting hexafluoropropylene oligomers imparts exceptional performance. Incorporating hexafluoropropylene oligomers into wax sealing materials significantly improves their thermal stability. Due to their unique chemical structure, hexafluoropropylene oligomers maintain excellent physical and chemical properties even at high temperatures, a crucial requirement for wax sealing materials. In practical applications, this material can withstand higher operating temperatures, extending the service life of the wax sealing material and maintaining excellent sealing performance even in high-temperature environments. Furthermore, the addition of hexafluoropropylene oligomers imparts excellent water and chemical resistance to the wax sealing material, ensuring its stability in harsh industrial environments and effectively protecting sealed items from damage.

[0043] The present invention also utilizes conventional paraffin wax components in its wax sealing material. By introducing hexafluoropropylene oligomers into the paraffin wax molecules, some C-H bonds are converted into C-F bonds. Given that fluorine atoms have significantly higher electronegativity than hydrogen atoms, C-F bonds exhibit stronger polarity and shorter bond lengths, which enhances intermolecular interactions. Furthermore, the larger van der Waals volume of fluorine atoms results in greater steric hindrance, leading to a tighter molecular arrangement. These enhanced forces increase intermolecular attraction, requiring more energy to overcome these forces, resulting in a more stable structure and support. Due to the steric hindrance effect of fluorine atoms, the fluorinated paraffin wax molecules are more tightly packed in the solid state. However, due to the support provided by the dimer, micropores for breathing air are formed, which increases the stability of the crystal structure and addresses the problem of paraffin wax's poor air permeability. A more stable crystal structure requires higher temperatures to disrupt this orderly arrangement, leading to increased thermal stability. To precisely control the temperature at which the wax melts, the present invention proposes a novel wax sealing material for Amaryllis bulbs and its preparation method. The method includes the following steps: first, paraffin wax and hexafluoropropylene oligomer are selected in a specific proportion for mixing. Then, by precisely controlling the heating temperature and time, it is ensured that the hexafluoropropylene oligomer can be evenly dispersed in the paraffin wax to form a stable mixture. During the mixing process, a specific stirring device is required to ensure mixing uniformity to avoid local overheating or insufficient mixing. Then, the mixture is cooled to room temperature to form a solid sealing wax material. Finally, the sealing wax material is evenly coated on the amaryllis bulb through a specific packaging device to form a protective film. The melting point of the sealing wax material prepared by this method is precisely controlled, and it can adapt to the storage and transportation requirements under different ambient temperatures while keeping the amaryllis bulb in good condition.

[0044] Another key element of the present invention's technical solution lies in the use of co-polymerization to create a membrane structure that can be modified by relative humidity. In this invention, the wax layer treated with wax can be divided into two components based on their structural functions: a support layer and a separation layer. The support layer, primarily composed of trimers, forms an effective support structure with its excellent anti-swelling properties, while the separation layer, primarily composed of hexafluoropropylene dimers, exhibits weak inter-chain interactions. In high-humidity environments, the separation layer experiences slippage, creating a creep effect that shrinks the molecular pores within the wax material, effectively blocking water penetration and achieving the dual effects of water retention and breathability. Hexafluoropropylene oligomers can be used both as a matrix material and as a filler to enhance the properties of other polymers. To address the brittleness of blends caused by uneven phase distribution and a tendency toward densification, a multi-component blend was successfully prepared by introducing hexafluoropropylene oligomers as modifiers into the blend system. This blend combines high tensile modulus with excellent ductility, significantly improving impact resistance. The wax sealing material of the present invention also has good biocompatibility and does not adversely affect the growth of Hippeastrum bulbs, i.e., it reduces the occurrence of fluorine diffusion. This is because during the preparation of the oligomer, the present invention directs the preparation and construction of oligomers with a higher trimer content, which can reach more than 72%. The remaining dimer will form fluorine exchange during the mixing process with paraffin wax. The stability of fluorine in the incompletely fluorinated paraffin wax after fluorine exchange and the dimer after the molecular structure slip is further enhanced, thereby ensuring the stability of fluorine and the controllability of fluorine diffusion.

[0045] In practical applications, the fluorine-containing wax layer can effectively resist the penetration and invasion of pathogens during the storage and transportation of the bulbs after wax sealing, reducing the risk of bulb rot, thereby improving the survival rate and planting efficiency of Amaryllis. At the same time, the wax sealing material is simple to use, easy to operate, and suitable for large-scale production applications. Experimental verification shows that the wax sealing material of the present invention can maintain good stability and protective effects under different temperature and humidity conditions, providing reliable technical support for the long-term storage and long-distance transportation of Amaryllis bulbs.

[0046] The beneficial effects of the present invention are:

[0047] The present invention constructs a wax sealing material for amaryllis bulbs with good biocompatibility by directionally constructing oligomers and mixing the oligomers. The wax sealing material can not only play a good waterproof and antibacterial role as well as a mechanical protective role, but also further optimize the respiratory environment of the amaryllis bulbs, thereby improving their respiration and increasing the flowering rate and flowering period of the wax-sealed amaryllis. DETAILED DESCRIPTION

[0048] The present invention is further described in detail below with reference to specific embodiments. Those skilled in the art will be able to implement the present invention based on these descriptions. Furthermore, the embodiments of the present invention described below are generally only a portion of the embodiments of the present invention, rather than all of the embodiments. Therefore, all other embodiments derived by those skilled in the art based on the embodiments of the present invention without inventive effort should fall within the scope of protection of the present invention.

[0049] Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all methods known to those skilled in the art.

[0050] Example 1: A method for preparing a wax sealing material for Amaryllis bulbs,

[0051] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0052]

[0053] The method comprises:

[0054] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and potassium fluoride were mixed uniformly in a mass ratio of 1.5:4:0.04:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 75 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0055] The oligomer products were characterized and the conversion of hexafluoropropylene and the selectivity of dimers and trimers were calculated. The characterization and calculation results showed that the conversion of hexafluoropropylene was 87.32% (the conversion rate of the target products dimers and trimers), the dimer selectivity was 26.31%, and the trimer selectivity was 73.70% (the selectivity was calculated only based on the total amount of dimers and trimers).

[0056] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0057] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0058] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0059] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0060] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0061] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0062] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0063] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0064] The experimental and test results are shown in the following table.

[0065]

[0066] The above characterization results show that the wax sealant of the present invention can significantly improve the respiratory environment of Amaryllis, thereby significantly increasing its flowering rate and average flowering period. Because more efficient respiration can promote the transformation of substances, the plant growth condition is better and the flowering period is significantly longer. The DGT characterization results show that although the wax sealant of the present invention uses fluorine-containing raw materials, except for the presence of contact residues on the epidermis, there is almost no diffusion. The fluorine diffusion phenomenon cannot be detected at 0.5mm below the skin, indicating that the wax sealant of the present invention also shows very excellent biocompatibility.

[0067] On the other hand, the wax-sealed amaryllis of the experimental group and the wax-sealed amaryllis of the blank control group were immersed in clean water, with the water immersion height reaching about two-thirds of the height of the wax sealing layer. After immersion for 6 hours, the samples were taken out and the mass change rate was characterized. The results showed that the change rate was ≤1%, indicating that the wax sealing material of the present invention has a waterproof property that is basically equivalent to that of the traditional wax sealing material.

[0068] Example 2: A method for preparing a wax sealing material for Amaryllis bulbs,

[0069] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0070]

[0071] The method comprises:

[0072] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and potassium fluoride were mixed uniformly in a mass ratio of 1.5:5:0.05:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 75 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0073] The oligomer product was characterized and the hexafluoropropylene conversion rate and dimer and trimer selectivity of this process were calculated. The characterization and calculation results showed that the hexafluoropropylene conversion rate was 86.83%, the dimer selectivity was 26.89%, and the trimer selectivity was 73.11%.

[0074] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0075] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0076] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0077] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0078] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0079] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0080] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0081] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0082] The experimental and test results are shown in the following table.

[0083]

[0084] Compared to Example 1, this example used a relatively higher amount of oligomer, and the amounts of polyethylene glycol and acetonitrile in the oligomer were also relatively increased. During the preparation process, the selectivity of the trimer decreased slightly. However, in terms of overall product performance, the flowering rate and average flowering period were almost identical, and the air permeability and DGT characterization results were also essentially the same. This indicates that the wax sealing material product of the present invention has good performance stability.

[0085] Example 3: A method for preparing a wax sealing material for Amaryllis bulbs,

[0086] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0087]

[0088] The method comprises:

[0089] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and potassium fluoride were mixed uniformly in a mass ratio of 1.5:6:0.06:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 75 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0090] The oligomer product was characterized and the hexafluoropropylene conversion rate and dimer and trimer selectivity of this process were calculated. The characterization and calculation results showed that the hexafluoropropylene conversion rate was 86.02%, the dimer selectivity was 27.71%, and the trimer selectivity was 72.29%.

[0091] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0092] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0093] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0094] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0095] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0096] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0097] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0098] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0099] The experimental and test results are shown in the following table.

[0100]

[0101] Compared to Examples 1 and 2, this example further increased the amount of oligomer used, and also relatively increased the amount of polyethylene glycol and acetonitrile in the oligomer. This resulted in a further decrease in trimer content during the preparation process. In terms of overall product performance, the flowering rate and average flowering period decreased slightly, while the air permeability and DGT characterization results remained essentially the same. This indicates that the wax sealing material product of the present invention has good performance stability, but the amount of oligomer used should not be too large, and the amounts of acetonitrile and polyethylene glycol should also be controlled accordingly.

[0102] Comparative Example 1: A method for preparing a wax sealing material for Amaryllis bulbs. The specific preparation method is the same as that in Example 2. In the comparative example, only the catalyst for preparing the hexafluoropropylene oligomer in the present invention is changed. Specifically, an equal amount of lithium fluoride is used instead to prepare the hexafluoropropylene oligomer, and the performance is tested by referring to the wax sealing experiment in Example 2. The specific characterization results and operation process are as follows.

[0103] A preparation method for amaryllis bulb sealing wax material,

[0104] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0105]

[0106] The method comprises:

[0107] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and lithium fluoride were mixed uniformly in a mass ratio of 1.5:5:0.05:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 75 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0108] The oligomer product was characterized and the hexafluoropropylene conversion rate and dimer and trimer selectivity of this process were calculated. The characterization and calculation results showed that the hexafluoropropylene conversion rate was 71.37%, the dimer selectivity was 37.62%, and the trimer selectivity was 62.38%.

[0109] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0110] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0111] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0112] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0113] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0114] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0115] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0116] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0117] The experimental and test results are shown in the following table.

[0118]

[0119] Analysis of the above characterization data shows that the flowering rate in this example remains relatively good, while the oxygen permeability in the air permeability increases and the carbon dioxide permeability decreases, while the average flowering period decreases significantly compared with Examples 1 to 3. Observation of the DGT characterization results shows that fluorine diffusion occurs. Combined with the analysis of the composition of the hexafluoropropylene oligomer in this example, it is found that the dimer component accounts for a large proportion in the hexafluoropropylene oligomer. The dimer may have a positive effect on expanding respiratory stomata, but when the dimer content accounts for too high a proportion, slippage will occur prematurely and first inhibit the passage of larger carbon dioxide molecules, resulting in a polarized trend in the permeability change, and residual free fluorine atoms enter the plant, causing fluorine diffusion, and thus the metabolism and other processes of the experimental group plants may be relatively affected. Although the flowering rate remains basically the same, this is mainly because the plant metabolic rate is higher after flowering, and the fluorine diffusion may be more intense or the impact is more significant.

[0120] Comparative Example 2: A method for preparing a wax sealing material for Amaryllis bulbs. The specific preparation method is the same as that in Example 2. In the comparative example, only the amount of polyethylene glycol used in the preparation process of the hexafluoropropylene oligomer in the present invention is adjusted to prepare the hexafluoropropylene oligomer. The specific characterization results and operation process are as follows.

[0121] A preparation method for amaryllis bulb sealing wax material,

[0122] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0123]

[0124] The method comprises:

[0125] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and potassium fluoride were mixed uniformly in a mass ratio of 1.5:5:0.02:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 75 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0126] The oligomer product was characterized and the hexafluoropropylene conversion rate and dimer and trimer selectivity of this process were calculated. The characterization and calculation results showed that the hexafluoropropylene conversion rate was 69.87%, the dimer selectivity was 69.72%, and the trimer selectivity was 30.28%.

[0127] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0128] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0129] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0130] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0131] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0132] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0133] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0134] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0135] The experimental and test results are shown in the following table.

[0136]

[0137] Analysis of the above characterization data reveals that, with the use of less polyethylene glycol, both the product conversion rate and selectivity of the oligomers undergo significant changes. Particularly noticeable is the dramatic increase in dimer selectivity and the sharp decrease in trimer selectivity. The final product exhibits very poor results, with both the flowering rate and average flowering period far below those reported in Examples 1-3. Air permeability also decreases significantly, due to slippage and accumulation caused by the excess dimer. In earlier experiments, a high dimer content in thin films did not actually result in a sharp drop in air permeability. However, due to the layered slippage, this leads to a different air permeability trend in thicker wax layers than in thin films. Furthermore, the increase in dimer content also significantly reflects the initial fluorine diffusion. Based on the DGT characterization results, a significant increase in fluorine diffusion is evident. This is similar to the results of earlier PTFE experiments. In these experiments, a 0.5 mm thick PTFE film was applied to the surface of the treated Amaryllis bulbs before wax coating. Subsequently, wax sealing was performed using the same well-established beeswax + paraffin wax process. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm. The results showed a significant decrease in flowering rate and flowering period. Similarly, DGT characterization results detected fluorine diffusion in Ep0 to Ep0.15. This suggests that fluorine diffusion can significantly affect the growth and development of wax-sealed Amaryllis.

[0138] Comparative Example 3: A method for preparing a wax sealing material for Amaryllis bulbs. The specific preparation method is the same as that in Example 2. In the comparative example, only the preparation environment of the hexafluoropropylene oligomer in the present invention is changed, specifically, the reaction temperature of the hexafluoropropylene trimer is changed. The specific characterization results and operation process are as follows.

[0139] A preparation method for amaryllis bulb sealing wax material,

[0140] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0141]

[0142] The method comprises:

[0143] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and potassium fluoride were mixed uniformly in a mass ratio of 1.5:5:0.05:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 30 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0144] The oligomer product was characterized and the conversion rate of hexafluoropropylene and the selectivity of dimer and trimer in this process were calculated. The characterization and calculation results showed that the conversion rate of hexafluoropropylene was 71.20%, the dimer selectivity was 68.71%, and the trimer selectivity was 31.29%.

[0145] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0146] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0147] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0148] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0149] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0150] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0151] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0152] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0153] The experimental and test results are shown in the following table.

[0154]

[0155] Analysis of the above characterization data shows that the experimental group showed no improvement in air permeability and other properties, and was accompanied by severe fluorine diffusion, resulting in results similar to those in Comparative Example 3. This, in turn, inhibited the growth and metabolism of the experimental plants, severely affecting their photosynthesis and respiration, and interfering with the activity of various enzymes in the plants, resulting in slow growth, leaf yellowing, and even necrosis in the experimental plants. This indicates that temperature and polyethylene glycol have a significant impact on the directed construction of the specific oligomers of the present invention, and together have a significant impact on the performance of the wax sealant.

[0156] Comparative Example 4: A method for preparing a wax sealing material for Amaryllis bulbs. The specific preparation method is the same as that of Example 2. In the comparative example, only the preparation environment of the hexafluoropropylene oligomer in the present invention is changed, specifically, the reaction temperature of the hexafluoropropylene trimer is changed. The specific characterization results and operation process are as follows.

[0157] A preparation method for amaryllis bulb sealing wax material,

[0158] The described amaryllis bulb wax sealing material comprises the following raw materials in percentage by weight:

[0159]

[0160] The method comprises:

[0161] (1) Liquid hexafluoropropylene, acetonitrile, polyethylene glycol, and potassium fluoride were mixed uniformly in a mass ratio of 1.5:5:0.05:0.02, and stirred at a speed of 100 r / min for 45 min under nitrogen atmosphere, temperature of 90 °C, and pressure of 1.1 MPa to prepare hexafluoropropylene oligomers;

[0162] The oligomer product was characterized and the hexafluoropropylene conversion rate and dimer and trimer selectivity of this process were calculated. The characterization and calculation results showed that the hexafluoropropylene conversion rate was 79.33%, the dimer selectivity was 46.72%, and the trimer selectivity was 53.28%.

[0163] (2) Hexafluoropropylene oligomer and beeswax were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.25 h under the environmental conditions of temperature of 95 °C, pressure of 0.3 MPa, and stirring rate of 50 r / min to prepare the first stage mixture;

[0164] (3) The first stage mixture and high melting point paraffin were mixed and stirred according to the above raw material ratio, and stirred and mixed for 1.5 h under the environmental conditions of temperature 120 °C, pressure 0.3 MPa, and stirring rate 80 r / min to prepare the second stage mixture;

[0165] (4) The second stage mixture and the viscosity enhancer were mixed and stirred according to the above raw material ratio. The mixture was stirred for 0.6 h at a temperature of 100 °C, a pressure of 0.3 MPa, and a stirring rate of 40 r / min. The mixture was then cooled naturally to obtain the wax sealing material for Amaryllis bulbs.

[0166] A wax sealing experiment was carried out on the wax sealing material prepared in this example.

[0167] Take mature Amaryllis bulbs, remove the leaves and roots, and retain the bulbs. Wash and disinfect the bulbs to obtain seed bulbs. During the disinfection process, boiled, cooled water is diluted with 75% alcohol to create a 25% disinfectant. Soak the bulbs in this disinfectant. Disinfect the bulbs twice, soaking them for 25 minutes each time. Refresh the disinfectant before each soaking.

[0168] Coat the surface of the seed bulbs with protective wax. Leave a blank area 1.5 to 2.5 cm below the top of the bulb's bud. This blank area does not need to be coated with protective wax (i.e., sealing wax). Immerse the sterilized bulbs in 70°C molten wax and then remove them. Repeat this process several times until the bulbs are evenly coated with protective wax. Each immersion lasts approximately 1 second. Repeat this process until a uniform protective wax layer forms on the bulb surface, with a total thickness of approximately 10 mm. This serves as the experimental group.

[0169] After 105 days of simulated storage (including normal storage) at 8°C, the samples were removed and placed in an environment receiving normal sunlight (at least 7 hours of sunshine on sunny days) at a temperature of 20-22°C. The total number of flowers and flowering rate were calculated from the first blooming sample until the flower withered, as well as the average peak flowering period after the flowers of all blooming samples. All samples were displayed and counted in the laboratory or in a garden exhibition area within the same factory under essentially identical conditions. Conventionally wax-sealed Hippeastrum paniculatum was used as a blank control for comparison, following the same storage and flowering conditions. Conventionally wax-sealed Hippeastrum paniculatum was wax-sealed using the established beeswax + paraffin wax process, with all other treatments remaining the same. The beeswax layer thickness was 2.7 ± 0.1 cm, and the paraffin layer thickness was 7.3 ± 0.1 cm.

[0170] During the above wax sealing experiment, the wax sealing material was sent to a third-party university to test its oxygen and carbon dioxide permeability (the thickness and layer distribution were the same as those of the experimental group and the blank control group). After the wax sealing experiment, two flowering samples and two non-flowering samples were taken (the sampling sites were the epidermis Ep0 after peeling off the wax layer, Ep0.05 0.5 mm below the epidermis, Ep0.1 1.0 mm below the epidermis, and Ep0.15 1.5 mm below the epidermis, and 10 samples were taken from each site). The samples were sent to a professional institution for DGT testing, and the fluorine detection limit was 0.02 μg / g.

[0171] The experimental and test results are shown in the following table.

[0172]

[0173] Analysis of the above characterization data shows that the air permeability of the experimental group in this example did not increase significantly, and there was no significant performance improvement in the growth and flowering period of Amaryllis. Combined with the analysis of the composition of the hexafluoropropylene oligomer in this example, due to the excessive proportion of hexafluoropropylene dimer, although more breathing micropores were formed by the cooperation and support of the fluorinated paraffin molecules and dimers, premature slippage occurred, resulting in poor optimization of the paraffin permeability and failure to achieve the expected optimization effect. Further comparative analysis of the data of the embodiment and comparative examples 3 and 4 clearly shows the effect of temperature on the synthesis reaction of hexafluoropropylene trimer. At lower reaction temperatures, the oligomer conversion rate is low. In the temperature range of 75-85 ° C, as the temperature increases, the polymerization reaction rate is effectively accelerated, thereby promoting the conversion rate of hexafluoropropylene and the increase in the yield of hexafluoropropylene trimer. Within a specific temperature range, an increase in temperature can significantly promote the increase in the polymerization reaction rate. However, when the temperature continues to rise above 85°C, the reaction rate and hexafluoropropylene conversion rate both decrease significantly, and the relative content of hexafluoropropylene trimers in the oligomerization product also decreases accordingly. This is because the hexafluoropropylene oligomerization process involves multiple chemical reactions, among which reactions with higher activation energy tend to proceed at higher temperatures. Because the degree of polymerization of hexafluoropropylene trimers is higher than that of dimers, increasing the temperature between 75°C and 85°C favors the formation of trimers. However, when the temperature exceeds 85°C, the content of byproducts in the oligomerization product increases significantly, the oligomer reactions and composition become more complex, and more impurities are generated, resulting in a decrease in the yield of hexafluoropropylene trimers.

Claims

1. A method for preparing a wax sealing material for Amaryllis bulbs, characterized in that: The method comprises: (1) The raw materials are prepared according to the following weight percentages: hexafluoropropylene oligomer 33-37 wt%, beeswax 4-6 wt%, tackifier 0.5-1.0 wt%, and the balance is high melting point paraffin wax; (2) mixing hexafluoropropylene oligomer and beeswax and stirring them to react to prepare a first-stage mixture; (3) Mixing the first stage mixture with high melting point paraffin wax and stirring to react to prepare the second stage mixture; (4) Evenly mixing the second-stage mixture and the viscosity enhancer, and naturally cooling the mixture to obtain the wax sealing material for the amaryllis bulb; The hexafluoropropylene oligomer in step (1) is prepared by the following method: The perfluorinated compound, nitrile compound, polymer and metal fluoride salt are mixed uniformly in proportion, and stirred and thermally reacted under high pressure to obtain a directionally prepared hexafluoropropylene oligomer. The perfluorinated compound is liquid hexafluoropropylene that has been subjected to a pressure treatment; The nitrile compound is acetonitrile; The polymer is polyethylene glycol; The metal fluoride salt is potassium fluoride; The perfluorinated compound, nitrile compound, polymer and metal fluoride salt are uniformly mixed in a mass ratio of 1.5: (4-6): (0.04-0.06): 0.02; The high pressure condition is an ambient pressure of 1.0 to 1.2 MPa; The stirring thermal reaction is carried out at 75-85° C. and 80-120 rpm for 40-45 min.

2. The method for preparing a wax sealing material for Amaryllis bulbs according to claim 1, wherein: The mixing and stirring reaction in step (2) is carried out at 0.3-0.4 MPa, 95-105°C, and at a stirring speed of 40-60 rpm for 45-75 min.

3. The method for preparing a wax sealing material for Hippeastrum bulbs according to claim 1, wherein: The mixing and stirring reaction in step (3) is carried out at 0.3-0.4 MPa, 120-140°C, and 70-90 rpm for 60-90 min.

4. The method for preparing a wax sealing material for Amaryllis bulbs according to claim 1, wherein: The uniform mixing in step (4) is carried out by stirring and mixing at a speed of 30 to 50 rpm for 60 to 90 minutes under the conditions of 0.3 to 0.4 MPa and 100 to 120°C.

5. A wax sealing material for Amaryllis bulbs prepared by the method according to any one of claims 1 to 4.

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