Composition containing orotic acid as well as preparation method and application thereof

By synergistically combining orotic acid with additives, the problems of thermal stability, compatibility, and storage of orotic acid in polymer materials have been solved, enabling the application of highly efficient and environmentally friendly biodegradable materials. This significantly improves the processing adaptability and storage stability of orotic acid, achieving the application of high-performance biodegradable materials.

CN121160102APending Publication Date: 2025-12-19CHENGDU BAISHIXING SCI & TECH IND
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Patent Information

Application Number
CN202511714907.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-11-21
Publication Date
2025-12-19

AI Technical Summary

Technical Problem

The application of orotic acid in the field of polymer materials has problems such as low thermal decomposition temperature, poor compatibility with resins such as polylactic acid, easy electrostatic aggregation, and lack of UV resistance and antioxidant properties, which limit its application in high-value-added environmentally friendly materials such as biodegradable films and biodegradable containers.

Method used

By adding additives such as microcrystalline cellulose, zinc oxide, epoxidized soybean oil, and tributyl acetylacetate to synergistically compound with orotic acid, a dynamic stable-plasticized system is formed, which improves thermal stability and flowability, antistatic and UV resistance, and enhances storage stability.

Benefits of technology

It significantly improves the processing adaptability and stability of whey acid-based materials, realizing high-performance biodegradable materials that meet the requirements of injection molding and casting processes, and possesses antistatic, anti-UV and antioxidant properties. It also meets food contact safety standards and is biodegradable.

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Abstract

The invention relates to the technical field of bio-based materials, and particularly discloses a composition containing orotic acid and a preparation method and application thereof, and the composition comprises the following components in parts by weight: 85.0-95.0 parts of orotic acid; 0.3 to 1.2 parts of microcrystalline cellulose; 0.05 to 1.5 parts of zinc oxide; 1.5 to 6.0 parts of epoxidized soybean oil; 0.05 to 0.8 part of vitamin E; and 2.0 to 7.0 parts of acetyl tributyl citrate. According to the invention, the auxiliary agent is added to be synergistically compounded with the orotic acid, so that the processing adaptability is successfully improved, and the melt flow rate is increased to meet the technological requirements of injection molding, tape casting and the like; the stability of the material is fundamentally improved, and the problem of caking during storage is solved; the material is endowed with composite functional characteristics, and the synergistic effect of static electricity resistance, ultraviolet resistance and oxidation resistance is achieved. Finally, a high-performance orotic acid-based material formula which is environment-friendly, biodegradable and suitable for high-added-value environment-friendly products is formed.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of bio-based materials, and relates to a composition containing orotic acid as well as a preparation method and application thereof. BACKGROUND

[0002] Orotic acid, with a chemical name of 1,2,3,6-tetrahydro-2,6-dioxo-4-pyrimidinecarboxylic acid, has a molecular weight of 156.1 and is a naturally occurring pyrimidine compound. It is known as “vitamin B13” in the medical and nutritional fields, and its derivatives (such as potassium orotate and magnesium orotate) are widely used in the auxiliary treatment of liver diseases and the nutrition fortification of infants (see: Grand View Research market report, 2024).

[0003] However, with the increasing demand for bio-based and degradable materials, it has become a promising research direction to expand the application of orotic acid, which is a widely available and degradable molecule of biological origin, from high-value small molecule applications to the field of bulk high polymer materials, such as degradable biofilms, degradable bio-based food packaging materials, and degradable bio-based adsorption materials.

[0004] At present, this research direction is still in its early stages and there are significant technical bottlenecks. In the prior art, the application of orotic acid in the field of high polymer materials is mainly focused on its chelated form. For example, patent CN102863580A discloses a orotic acid chelated resin for heavy metal ion adsorption. However, in terms of directly using orotic acid as a main raw material or a key component to construct bio-based materials, the prior art exposes the following defects that need to be solved urgently: (1) The thermal decomposition initiation temperature of orotic acid is relatively low, and it will decompose when the temperature exceeds 250°C. However, the conventional high polymer processing temperature range is 150-300°C, which makes orotic acid have a risk of thermal degradation during processing, affecting the material performance and appearance.

[0005] (2) The compatibility of orotic acid with mainstream degradable resins such as polylactic acid (PLA) and polybutylene adipate terephthalate (PBAT) is extremely poor. The interfacial tension between unmodified orotic acid and PLA is as high as 35 mN / m, resulting in a very low melt flow rate (190°C / 2.16kg) of the blend, only 1.2-2.5 g / 10 min. This flowability is far from meeting the basic requirements of conventional high polymer processing techniques such as injection molding and casting, making processing difficult and product formability poor. The published literature also confirms that the impact strength of orotic acid / PLA blend is reduced by 30%-50% compared with pure PLA, which severely limits its application.

[0006] (3) The orotic acid powder is easy to produce static electricity in normal state, resulting in serious agglomeration between particles (scanning electron microscope observation shows that the original particles are obviously adhered). Especially after being stored in an environment with humidity > 60% for 15 days, serious caking phenomenon occurs, affecting the uniformity and fluidity of subsequent processing.

[0007] (4) The material prepared from pure orotic acid and its simple blend lacks the properties of anti-ultraviolet and anti-oxidation. Experiments show that after being irradiated in an ultraviolet aging test box for 72 hours, the tensile strength retention rate of the material is significantly reduced, which cannot meet the requirements of durability of the material for outdoor packaging or long-term use scenarios.

[0008] In summary, the prior art fails to provide a special formula that can simultaneously solve the defects of orotic acid in processability, stability and functionality, which greatly limits the application of orotic acid in the field of high-value-added environmentally friendly materials such as biodegradable films and degradable containers. Therefore, there is an urgent need in the art to develop a new orotic acid-containing composition to overcome the above technical obstacles. SUMMARY

[0009] To solve the above problems, the present application provides an orotic acid-containing composition, its preparation method and application. By adding additives and synergistically compounding with orotic acid, the technical bottleneck of orotic acid as a material raw material is successfully overcome, the processing adaptability is significantly improved, the melt flow rate is improved, and the process requirements such as injection molding and flow casting are met; the stability of the material is fundamentally improved, not only the thermal decomposition temperature is improved, but also the storage caking problem is solved through antistatic and hygroscopic effect; the material is also given composite functional characteristics, realizing the synergistic effect of antistatic, anti-ultraviolet and anti-oxidation. Finally, an environmentally friendly, biodegradable and high-performance orotic acid-based material formula suitable for high-value-added environmentally friendly products is formed.

[0010] To achieve the above purpose, the technical scheme of the present application is as follows: An orotic acid-containing composition, including the following components by weight: Orotic acid 85.0-95.0 parts; microcrystalline cellulose 0.3-1.2 parts; zinc oxide 0.05-1.5 parts; epoxy soybean oil 1.5-6.0 parts; vitamin E 0.05-0.8 parts; acetyl tri-butyl citrate 2.0-7.0 parts.

[0011] The synergistic mechanism of each component of the above-mentioned orotic acid-containing composition of the present application is as follows: (1) Epoxy soybean oil (ESO) and acetyl tributyl citrate (ATBC) are compounded: the compounding of ESO and ATBC is the core of realizing high performance of the composition, and the two complement each other in function at the molecular level to build a dynamic stabilizing-plasticizing system. The high-activity epoxy groups in the ESO molecule can act as efficient "acid traps" to actively capture the H + , which may be generated by orotic acid due to heat during thermal processing, thereby significantly improving thermal stability; ATBC, as a high-efficiency plasticizer, can form a wide dynamic hydrogen bond network with the polar groups (such as carboxyl and amide groups) of orotic acid molecules. On the one hand, this network effectively weakens the intermolecular forces of orotic acid, plays an internal lubricating role, greatly reduces the melt viscosity, and improves the processing fluidity; on the other hand, this hydrogen bond network acts as a "molecular scaffold" to stabilize the molecular conformation of orotic acid, reduce the exposure of its degradation sites under thermal shear, and provide additional thermal protection from a physical perspective. (2) Microcrystalline cellulose (MCC) reduces the surface resistance of the powder through the fiber network structure, and its porous structure can adsorb free water, so that the rest angle change rate of the powder is reduced when stored for 30 days under RH 85%; (3) Nano zinc oxide improves the weather resistance of the material by reflecting and scattering ultraviolet light (200-400 nm), and when the addition amount is 0.5%, the ultraviolet transmittance (UV-Vis spectrum) of the material decreases, and the Zn 2+ O can form a coordination bond with the carboxyl group of orotic acid, further improving the thermal stability; the above-mentioned components form a multi-level synergistic effect with the orotic acid matrix, systematically solving the inherent defects of orotic acid as a material raw material from the physical, chemical and functional levels. (4) Vitamin E inhibits the oxidation chain reaction by capturing free radicals, so that the tensile strength retention rate of the material is improved in the 120℃ aging test (GB / T 7141-2021).

[0012] Preferably, the particle size of the microcrystalline cellulose is 40-120 μm, the bulk density is 0.20-0.40 g / cm³, and the pH value is 5.0-7.0.

[0013] Selecting this particle size range can achieve full stretching of the microcrystalline cellulose in the orotic acid matrix to form a uniform and dense three-dimensional network structure. This structure is the physical basis for achieving efficient and stable antistatic and anti-caking functions. Limiting the pH value (10% aqueous solution) of the microcrystalline cellulose to the near-neutral range of 5.0-7.0 is a key success factor, which effectively avoids catalyzing the hydrolysis or degradation reaction of orotic acid molecules due to local over-acidification or over-alkalization during processing or storage, thereby ensuring the long-term chemical stability of the material system.

[0014] Preferably, the zinc oxide is nanoscale, with an average particle size of 15-60 nm and a specific surface area of ≥25 m² / g.

[0015] Zinc oxide is nanoscale (average particle size 15-60 nm) and has a high specific surface area (≥25 m² / g), which is the core of maximizing its light stabilization function. Nanoscale gives the particle stronger scattering and reflection ability when it interacts with ultraviolet light, thereby achieving efficient ultraviolet shielding with lower addition amount. At the same time, the huge specific surface area increases the contact probability of zinc ions and carboxyl groups of orotic acid, making the coordination bond formed more sufficient, thereby more significantly improving the thermal stability of the composite material.

[0016] Preferably, the purity of the acetyl tri-butyl citrate is ≥98.5%, and the moisture content is ≤0.2%.

[0017] The acetyl tri-butyl citrate is set to have a high purity (≥98.5%) and a low moisture content (≤0.2%), which directly serves the processing stability and the quality of the final product. The low impurity content ensures the specificity of its function in the system, avoiding side reactions; the extremely low moisture completely eliminates the risk of foaming, defects or orotic acid hydrolysis caused by water vaporization during thermal processing.

[0018] Preferably, the epoxy value of the epoxy soybean oil is ≥5.8%.

[0019] The epoxy value of the epoxy soybean oil is limited to be ≥5.8%, which essentially ensures that it contains a high enough concentration of active epoxy groups in its molecules. A high epoxy value means that the additive per unit mass has stronger thermal stabilization ability and can more effectively inhibit the thermal degradation chain reaction during processing.

[0020] Preferably, the above orotic acid raw material formula consists of the following components by weight: Orotic acid 88.0-92.0 parts; microcrystalline cellulose 0.5-0.8 parts; zinc oxide 0.3-0.7 parts; epoxy soybean oil 3.0-4.5 parts; vitamin E 0.1-0.3 parts; acetyl tri-butyl citrate 4.0-5.5 parts.

[0021] Preferably, the above orotic acid raw material formula consists of the following components by weight: Orotic acid 90.0 parts; microcrystalline cellulose 0.6 parts; zinc oxide 0.5 parts; epoxy soybean oil 3.5 parts; vitamin E 0.2 parts; acetyl tri-butyl citrate 5.2 parts.

[0022] Preferably, the above orotic acid raw material formula consists of the following components by weight: Oxalic acid 89.0 parts; microcrystalline cellulose 0.7 parts; zinc oxide 0.4 parts; epoxy soybean oil 4.0 parts; vitamin E 0.2 parts; acetyl tri-butyl citrate 5.7 parts.

[0023] The present application also provides a preparation method of the above-mentioned oxalic acid-containing composition, comprising the following steps: (1) Liquid gradient addition: first uniformly mix the epoxy soybean oil and acetyl tri-butyl citrate to obtain an epoxy soybean oil-acetyl tri-butyl citrate composite liquid, then add the epoxy soybean oil-acetyl tri-butyl citrate composite liquid to the oxalic acid raw material in three times according to the proportion, to obtain a first mixture, and each time interval is 5-8 minutes, and at the same time, vacuum degassing is started, and the vacuum degree is-0.08 MPa, to avoid the entry of air bubbles; (2) Solid premixing: put the first mixture obtained in step (1), microcrystalline cellulose and nano-zinc oxide into a mixer, and alternately perform low-speed stirring and high-speed shearing to obtain a second mixture, the low-speed stirring is 300 rpm-400 rpm, and the high-speed shearing is 2000 rpm-2100 rpm, and the initial agglomeration is broken by shearing force; (3) Secondary dispersion: transfer the second mixture into a horizontal screw ribbon mixer, and maintain at a low speed of 150 rpm-180 rpm for 15-20 minutes, so that the liquid additives are uniformly penetrated into the solid network pores, to obtain the oxalic acid-containing composition.

[0024] The liquid gradient addition and synchronous vacuum degassing can make the composite liquid formed by ESO and ATBC preliminarily penetrate into the surface layer of the oxalic acid powder under a low disturbance environment, effectively remove air bubbles, and lay a foundation for subsequent homogenization, to avoid air bubbles inducing degradation in thermal processing.

[0025] The subsequent solid premixing can break the initial agglomeration of nano-ZnO and MCC under the action of high-speed shearing force (2000 rpm), to ensure that all solid components are preliminarily homogenized in the oxalic acid matrix, and to provide a physical platform for the uniform action of functional additives.

[0026] The final secondary dispersion step utilizes the extrusion and overturning flexible shearing force of the horizontal screw ribbon mixer to stereoscopically comb the material for a long time (15 min) at a low speed (150 rpm). This process can promote the ESO-ATBC composite liquid which has been preliminarily infiltrated to further penetrate and diffuse into the micro-pores of the solid particles, and finally realize the molecular-level uniform distribution of the liquid additives in the entire solid network, so as to maximize the degradation inhibition-flow enhancement synergistic effect of ESO and ATBC, and ensure the uniformity of the MCC antistatic network and the nano-ZnO ultraviolet shielding function.

[0027] Use of a composition containing orotic acid for preparing a biodegradable film material by melt blending, extrusion casting, or for preparing a degradable container by mixing, injection molding.

[0028] Advantages of the present application: (1) The orotic acid-containing composition of the present application fundamentally improves the practical performance of orotic acid as a material raw material. Its most significant effect is to greatly improve the processing adaptability of the material, increase the melt flow rate of the composite system, and enable it to be successfully applied to conventional polymer processing processes such as injection molding and casting, thereby solving the technical bottleneck of orotic acid which is difficult to form due to poor compatibility and high melt viscosity.

[0029] (2) The orotic acid-containing composition of the present application has achieved a double breakthrough in stability. First, the thermal stability is significantly enhanced, the thermal decomposition temperature of the material is increased, and the thermal degradation phenomenon during processing is effectively inhibited. Second, the storage stability is completely improved, the problem of easy agglomeration and caking of orotic acid powder is solved through antistatic and hygroscopic effects, and the material maintains good flow characteristics during storage.

[0030] (3) The orotic acid-containing composition of the present application successfully endows the material with the functional properties of composite. The material exhibits excellent antistatic properties, with surface resistance stable in a strong antistatic range; it also has reliable weather resistance, maintaining good tensile strength after UVB ultraviolet aging for 72 hours, and the yellowing index is controlled at a low level; the antioxidant performance is also outstanding, with an increase in the retention rate of mechanical properties after thermal oxidation.

[0031] (4) The orotic acid-containing composition of the present application has high environmental friendliness, all components meet the food contact material standards and are biodegradable, with a degradation rate of more than 90% within 180 days, and completely free of restricted phthalate substances. The final orotic acid-based material has improved mechanical properties such as impact strength compared to the unmodified system, and truly realizes the upgrading and conversion from biomass raw materials to high-performance environmentally friendly materials.

[0032] (5) The preparation method of the present application effectively protects the activity of each functional component through temperature control, humidity adjustment and other detailed designs, avoiding component failure during processing. At the same time, the entire process does not have additional harmful additives, and each step is focused on improving the degradability of the material and the safety of food contact, so that the final product meets the environmental friendliness and safety standards, and meets the preparation needs of high-value-added environmentally friendly products such as biodegradable films and degradable containers. BRIEF DESCRIPTION OF DRAWINGS

[0033] Figure 1 The molecular structure of orotic acid in the present application.

[0034] Figure 2SEM cross-section of the orotic acid composition prepared from the orotic acid raw material formulation in Example 1 of the present application.

[0035] Figure 3 Thermogravimetric analysis curve of the orotic acid-containing composition in Example 2 of the present application. DETAILED DESCRIPTION

[0036] Example 1 This example provides an orotic acid-containing composition comprising the following components in parts by weight: orotic acid 90.0 parts (structural formula as shown Figure 1 microcrystalline cellulose 0.8 parts; nano-zinc oxide (average particle size 30 nm) 0.5 parts; epoxy soybean oil (epoxy value 6.3%) 3.0 parts; vitamin E 0.2 parts; acetyl tri-butyl citrate 5.5 parts.

[0037] The preparation method of the orotic acid-containing composition of this example comprises the following steps: (1) Liquid addition: first uniformly mix the epoxy soybean oil and acetyl tri-butyl citrate to obtain an epoxy soybean oil-acetyl tri-butyl citrate complex liquid, add the epoxy soybean oil-acetyl tri-butyl citrate complex liquid to the orotic acid raw material in three times according to the proportion, obtain a first mixture, and interval 5 minutes between each time of adding, and at the same time, start vacuum degassing with a vacuum degree of -0.08 MPa to avoid the entry of air bubbles; (2) Solid premixing: put the first mixture obtained in step (1), microcrystalline cellulose and nano-zinc oxide into a mixer, and alternately perform low-speed stirring and high-speed shearing to obtain a second mixture, the low-speed stirring is 300 rpm, and the high-speed shearing is 2100 rpm, and the initial agglomeration is broken by using the shearing force; (3) Secondary dispersion: transfer the second mixture into a horizontal screw ribbon mixer, maintain at a low speed of 150 rpm for 20 minutes to make the liquid additives uniformly penetrate into the solid network pores, and obtain the orotic acid-containing composition of this example.

[0038] Example 2 This example provides an orotic acid-containing composition comprising the following components in parts by weight: orotic acid 88.0 parts; microcrystalline cellulose 1.0 parts; nano-zinc oxide (average particle size 30 nm) 0.8 parts; epoxy soybean oil (epoxy value 6.3%) 4.0 parts; vitamin E 0.3 parts; acetyl tri-butyl citrate 5.9 parts.

[0039] The preparation method of the orotic acid-containing composition of this example is as in Example 1.

[0040] Comparative Example 1 The comparative example 1 provides a composition containing orotic acid, which includes the following components by weight parts: orotic acid 90.0 parts; microcrystalline cellulose 0.8 parts; nano zinc oxide (average particle size 30 nm) 0.5 parts; epoxy soybean oil (epoxy value 6.3%) 3 parts; vitamin E 0.2 parts; acetyl tri-butyl citrate 7 parts.

[0041] The preparation method of the composition containing orotic acid of the present example is as described in the example 1.

[0042] Comparative example 2 The comparative example 2 provides a composition containing orotic acid, which includes the following components by weight parts: orotic acid 90.0 parts; microcrystalline cellulose 0.8 parts; nano zinc oxide (average particle size 30 nm) 0.5 parts; epoxy soybean oil (epoxy value 6.3%) 4.5 parts; vitamin E 0.2 parts; acetyl tri-butyl citrate 5.4 parts.

[0043] The preparation method of the composition containing orotic acid of the present example is as described in the example 1.

[0044] Comparative example 3 The comparative example 3 provides a composition containing orotic acid, which includes the following components by weight parts: orotic acid 90.0 parts; microcrystalline cellulose 0.8 parts; nano zinc oxide (average particle size 30 nm) 0.5 parts; epoxy soybean oil (epoxy value 6.3%) 6 parts; vitamin E 0.2 parts.

[0045] The preparation method of the composition containing orotic acid of the present example is as described in the example 1.

[0046] Comparative example 4 The comparative example 4 provides a composition containing orotic acid, which includes the following components by weight parts: orotic acid 90.0 parts; microcrystalline cellulose 0.8 parts; nano zinc oxide (average particle size 30 nm) 0.5 parts; vitamin E 0.2 parts; acetyl tri-butyl citrate 7 parts.

[0047] The preparation method of the composition containing orotic acid of the present example is as described in the example 1.

[0048] Comparative example 5 The comparative example 5 is designed according to the formulation ratio of the example 1, and the present example provides a preparation method of a composition containing orotic acid, which includes the following steps: (1) Composition mixing: the epoxy soybean oil, acetyl tri-butyl citrate, microcrystalline cellulose and nano-zinc oxide are added into the whey acid raw material in proportion, and the mixed material is put into a mixing machine, and the mixture is obtained by alternating low-speed stirring and high-speed shearing, the low-speed stirring is 400 rpm, and the high-speed shearing is 2000 rpm, and the shearing force is used to break the agglomeration; (2) Secondary dispersion: the mixture is transferred into a horizontal screw ribbon mixer, and the liquid additive is uniformly penetrated into the solid network pores under the low speed of 180 rpm for 15 minutes, and the whey acid-containing composition of the embodiment is obtained.

[0049] Experimental example 1 Thermal weight loss temperature and acid value change The whey acid-containing compositions of examples 1-2 and comparative examples 1-5 are subjected to 5% thermal weight loss temperature and acid value change determination, and the determination results are shown in table 1: Table 1. Physicochemical properties of the whey acid-containing compositions prepared in examples 1-2 and comparative examples 1-5

[0050] It can be seen from the above that: as shown in table 1, in the whey acid-containing composition, the compounding use of epoxy soybean oil (ESO) and acetyl tri-butyl citrate (ATBC) and the ratio of the two have a decisive influence on the thermal stability and degradation inhibition ability of the whey acid-containing composition, when there is no epoxy soybean oil (ESO=0 parts, ATBC=7 parts), the composition obviously lacks the acid capture effect of ESO, and the whey acid is prone to degradation reactions such as decarboxylation and molecular chain rupture during the heating process, and the thermal stability is very poor; when there is no acetyl tri-butyl citrate (ATBC=0 parts, ESO=6 parts), the composition is slightly improved compared with the system without ESO, but the thermal stability is still much lower than that of the compounding system, which shows that the role of ATBC in stabilizing the conformation of whey acid molecules by forming a dynamic hydrogen bond network is indispensable.

[0051] When ESO and ATBC coexist, the 5% weight loss temperature of the composition is greatly improved to above 180℃, and the acid value change is controlled below 0.67 mg KOH / g, which is significantly better than the single additive system. When ESO=4 parts and ATBC=4.7 parts, the 5% weight loss temperature of the composition reaches 239℃, which is significantly improved compared with pure whey acid and other compounding ratios, indicating that the acid capture ability of ESO and the hydrogen bond stabilization effect of ATBC are most sufficient at this ratio, and the thermal protection effect is the strongest.

[0052] The results of Comparative Example 1 and Comparative Example 5 can be known: under the premise that the compounding ratio of epoxy soybean oil (ESO) and acetyl tri-butyl citrate (ATBC) is fixed, the degree of refinement of the mixing process has a significant regulatory effect on the thermal stability (5% weight loss temperature) of the orotic acid-containing composition, and is a key link to ensure the full play of the synergistic effect of the additive.

[0053] Experimental Example 2: Preparation of a degradable biological film The orotic acid-containing composition prepared in Example 1 was prepared into a degradable biological film according to the following method: S1: melt extrusion granulation: the orotic acid-containing composition prepared in Example 1 was melt blended and granulated by using a twin-screw extruder (model TE-34, length-diameter ratio 40:1). The temperature of each section of the extruder was set to zone 1 140°C, zone 2 160°C, zone 3 180°C, and zone 4 170°C, the screw rotation speed was 300 rpm, and the length of the granulation was 3-5 mm.

[0054] S2: casting film formation: the obtained granules were put into a casting machine (model SJ-65), the die temperature was set to 170°C, the cooling roll temperature was set to 40°C, and the pulling speed was controlled to 2.5 m / min, and finally a film with a thickness of about 50 μm was prepared.

[0055] The film was tested for performance, and the results are shown in Table 2: Table 2. Film performance test results

[0056] From the above results, it can be known that the biological film prepared from the orotic acid composition prepared by the preparation method of the present application has stable mechanical strength, suitable flexibility, and good gas and water vapor barrier ability, and has potential application value in the field of degradable packaging materials, etc.

[0057] Experimental Example 3: injection molding of a degradable container The orotic acid-containing composition prepared in Example 2 was prepared into an injection molded degradable container according to the following method: S1: injection molding: the orotic acid-containing composition prepared in Example 2 was molded using an injection molding machine (model HTF86X1). The process parameters were: barrel temperature 180-200°C, mold temperature 40-50°C, injection pressure 80-100 bar, holding pressure 60-80 bar, and cooling time 25 seconds. A disposable lunch box with a capacity of 100 mL and a wall thickness of 1.5 mm was prepared in this way.

[0058] S2: post-treatment: the molded lunch box was placed in a 60°C air oven for annealing for 4 hours to eliminate internal stress.

[0059] The performance test was conducted on the above degradable container, and the results are shown in Table 3. Table 3. Performance test results of the degradable container

[0060] From the above results, it can be seen that the degradable container prepared from the whey acid composition prepared by the preparation method has good mechanical toughness, suitable heat resistance, high-efficiency composting degradation capacity and reliable food contact safety, and has significant application potential in the field of environmental protection such as disposable food packaging.

[0061] Experimental Example 4 SEM The SEM test was conducted on the whey acid-containing composition prepared in Example 1, and the results are shown in Figure 2 It can be seen from Figure 2 that the whey acid particles (white area) prepared by the preparation method of the application are uniformly dispersed without obvious agglomeration.

[0062] Experimental Example 5 Thermogravimetric analysis The thermogravimetric analysis experiment was conducted on the whey acid-containing composition of Example 2 and pure whey acid material, respectively, and the results are shown in the attached Figure 3 It can be seen from the thermogravimetric analysis curve in the attached Figure 3 that the maximum weight loss rate temperature of the whey acid-containing composition of Example 3 is 312℃, which is 58℃ higher than that of pure whey acid (254℃).

[0063] In summary, the whey acid-containing composition and its preparation method and application of the application successfully overcome the multiple technical bottlenecks of the application of whey acid in the field of high polymer materials, build a complete technical system of formula cooperation, process adaptation, performance upgrade and environmental protection adaptation, and through systematic technical innovation, not only improve the practical value of whey acid-based materials, but also promote the diversified development of biobased degradable materials, and provide a new technical path for solving the problem of traditional plastic pollution.

[0064] The technical solutions described in the above examples are only part of the embodiments of the application, not all embodiments. Based on the embodiments in the application, all other embodiments obtained by those of ordinary skill in the art without creative labor belong to the protection scope of the application. In addition, the technical solutions of each embodiment can be combined with each other, but it must be based on the realization of those of ordinary skill in the art, when the combination of technical solutions appears contradictory or unachievable, it should be considered that the combination of technical solutions does not exist, nor within the protection scope required by the application.

Claims

1. A composition containing orotic acid, characterized in that, The following components are included in parts by weight: 85.0-95.0 parts of whey acid; 0.3-1.2 parts of microcrystalline cellulose; 0.05-1.5 parts of zinc oxide; 1.5-6.0 parts of epoxidized soybean oil; 0.05-0.8 parts of vitamin E; 2.0-7.0 parts of acetylacetic acid tributyl ester.

2. The composition containing orotic acid according to claim 1, characterized in that, The microcrystalline cellulose has a particle size of 40-120 μm, a bulk density of 0.20-0.40 g / cm³, and a pH value of 5.0-7.

0.

3. The composition containing orotic acid according to claim 1, characterized in that, The zinc oxide is nanoscale, with an average particle size of 15-60 nm and a specific surface area ≥25 m² / g.

4. The composition containing orotic acid according to claim 1, characterized in that, The purity of the acetylglucosyl tributyl citrate is ≥98.5%, and the moisture content is ≤0.2%.

5. The composition containing orotic acid according to claim 1, characterized in that, The epoxy value of the epoxidized soybean oil is ≥5.8%.

6. The composition containing orotic acid according to claim 1, characterized in that, It consists of the following components in parts by weight: 88.0-92.0 parts of whey acid; 0.5-0.8 parts of microcrystalline cellulose; 0.3-0.7 parts of zinc oxide; 3.0-4.5 parts of epoxidized soybean oil; 0.1-0.3 parts of vitamin E; 4.0-5.5 parts of acetylated tributyl citrate.

7. The composition containing orotic acid according to claim 1, characterized in that, It consists of the following components in parts by weight: 90.0 parts of whey acid; 0.6 parts of microcrystalline cellulose; 0.5 parts of zinc oxide; 3.5 parts of epoxidized soybean oil; 0.2 parts of vitamin E; 5.2 parts of acetylated tributyl citrate.

8. The composition containing orotic acid according to claim 1, characterized in that, It consists of the following components in parts by weight: Orytic acid 89.0 parts; microcrystalline cellulose 0.7 parts; zinc oxide 0.4 parts; epoxidized soybean oil 4.0 parts; Vitamin E 0.2 parts; acetylsalicylate tributyl ester 5.7 parts.

9. A method for preparing the orotic acid-containing composition according to any one of claims 1-8, characterized in that, Includes the following steps: (1) Liquid addition: First, epoxidized soybean oil and acetylated tributyl citrate are mixed evenly to obtain epoxidized soybean oil-acetylated tributyl citrate composite liquid. The epoxidized soybean oil-acetylated tributyl citrate composite liquid is added to the orotic acid raw material in three batches according to the proportion to obtain the first mixture. The interval between each addition is 5-8 minutes. At the same time, vacuum degassing is turned on with a vacuum degree of -0.08 MPa to avoid air bubbles being entrained. (2) Solid premixing: The first mixture obtained in step (1), microcrystalline cellulose and nano zinc oxide are put into a mixer and the mixture is subjected to alternating low-speed stirring and high-speed shearing to obtain the second mixture. The low-speed stirring is 300 rpm-400 rpm and the high-speed shearing is 2000 rpm-2100 rpm. The initial agglomeration is broken by shearing force. (3) Secondary dispersion: The second mixture is transferred into a horizontal ribbon mixer and maintained at a low speed of 150 rpm-180 rpm for 15-20 minutes to allow the liquid additive to penetrate evenly into the pores of the solid network, thereby obtaining a composition containing orotic acid.

10. The use of the orotic acid-containing composition according to any one of claims 1-8, characterized in that, The whey acid-containing composition is used to prepare biodegradable membrane materials by melt blending and extrusion casting, or to prepare biodegradable containers by mixing and injection molding.

Citation Information

Patent Citations

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