Preparation method and application of anti-caking agent for betaine

Abstract

The invention provides a preparation method and application of an anti-caking agent for betaine, and the preparation method comprises the following steps: step 1, uniformly mixing metered calcium silicate, stearic acid and water to obtain a first treated substance; step 2, performing ball milling on the first treated object in a ball mill to obtain a second treated object; and 3, carrying out suction filtration on the second treated substance, and drying to obtain the target anti-caking agent. The calcium silicate and the stearic acid are compounded, so that the porous structure of the calcium silicate preferentially adsorbs environmental moisture and reduces water films on the surfaces of betaine particles, the hydrophobicity of the stearic acid forms a hydrophobic layer through coating and chemical reaction, the moisture is further isolated, adhesion among the particles is reduced, and the caking rate of the betaine is reduced. Low-cost raw materials such as calcium silicate and stearic acid are used, and simple process steps such as mixing, ball milling, suction filtration and drying are adopted in the preparation process, so that the preparation cost of the anti-caking agent is reduced while the preparation process is simplified. In addition, the whole preparation process is environment-friendly, less in wastewater discharge and free of waste residue discharge.

Description

Technical Field

[0001] The present invention relates to the field of chemical engineering technology, and in particular, to a preparation method and application of an anti-caking agent for betaine. Background Art

[0002] Betaine (chemical name: N,N,N-trimethylglycine) is a natural quaternary ammonium base substance widely present in animals and plants. Its chemical structure contains polar groups (carboxyl and quaternary ammonium groups), with strong hygroscopicity and high solubility in water. Its multiple application scenarios as a feed additive (improving lean meat rate, regulating osmotic pressure), pharmaceutical intermediate (anti-tumor, liver protection), food nutritional fortifier, and daily chemical raw material require it to have good flowability and stability. However, its strong hygroscopicity leads to easy caking during storage and transportation, directly affecting the convenience of use and the mixing uniformity. Therefore, the research on anti-caking agents has become a key direction for improving the application performance of betaine.

[0003] To solve this problem, the application of anti-caking agents becomes the key. Anti-caking agents change the surface properties of betaine particles through physical or chemical actions, forming a hydrophobic barrier or steric hindrance, thereby inhibiting the adhesion and caking between particles. Its principles mainly include surface modification (such as coating with hydrophobic materials), eutectic technology (forming stable eutectic crystals with excipients), and microstructural regulation (such as porous materials adsorbing moisture), etc. Currently, the research and development of betaine anti-caking agents mainly focus on the following directions:

[0004] 1) Nano-scale anti-caking agents: Utilize the high specific surface area and surface effect of nano-materials to develop anti-caking agents such as nano-silica and nano-calcium carbonate. These materials can adsorb on the surface of betaine particles through van der Waals forces or hydrogen bonding to form a hydrophobic layer, effectively inhibiting moisture absorption and caking.

[0005] 2) Eutectic crystallization technology: Form composite crystals of betaine and excipients (such as sodium chloride, potassium chloride) through eutectic crystallization technology. The eutectic crystals not only have anti-caking properties but also can maintain the functional activity of betaine. However, the eutectic crystallization technology has high requirements for process control, and precise control of crystallization conditions is required to ensure the stability and uniformity of the crystals.

[0006] 3) Bio-based anti-caking agents: Develop bio-based materials such as modified starch and cellulose as anti-caking agents, which have the advantages of wide sources and biodegradability. However, the anti-caking performance of bio-based materials needs to be further optimized to meet the stability requirements of betaine in high-humidity environments.

[0007] Despite the diverse R & D directions, the industrial application of betaine anti-caking agents still faces many challenges: Technical bottlenecks: Difficulty in screening anti-caking agents: It is necessary to balance hydrophobicity and functional activity to avoid chemical reactions with betaine; Complex co-crystallization process: During the industrial scale-up process, it is difficult to control the crystallization conditions, which easily leads to crystal defects or poor uniformity. Cost issues: High cost of nanomaterials: For example, nano-silica is expensive, increasing the overall cost of anti-caking agents; Insufficient performance of bio-based materials: Their performance needs to be improved through modification, but the modification process may increase process complexity and cost. Environmental impact: Difficulty in wastewater treatment: Traditional anti-caking agent production may generate high-salt wastewater, with high treatment costs; Degradability of bio-based materials: Although they are biodegradable, their long-term impact on the ecological environment needs to be evaluated for large-scale applications.

[0008] Therefore, there is an urgent need for a preparation method of an anti-caking agent for betaine to solve the above problems. Summary of the Invention

[0009] The main purpose of the present invention is to provide an anti-caking agent for betaine and its preparation method to at least solve the problem of high process control requirements in the prior art.

[0010] To achieve the above purpose, the present invention provides a preparation method of an anti-caking agent for betaine, including:

[0011] Step 1: Mix the metered calcium silicate, stearic acid and water evenly to obtain a first treatment product; wherein, the mass ratio of calcium silicate, stearic acid and water is 10 - 30:1 - 10:200 - 300;

[0012] Step 2: Ball-mill the first treatment product in a ball mill to obtain a second treatment product;

[0013] Step 3: Filter the second treatment product by suction and then dry it to obtain the target anti-caking agent.

[0014] Optionally, in Step 1, the mass ratio of calcium silicate, stearic acid and water is 20:5:250.

[0015] Optionally, in Step 2, the ball-milling time is 20 - 40 min.

[0016] Optionally, the ball-milling time is 30 min.

[0017] Optionally, qualitative filter paper is used in the suction filtration process in Step 3.

[0018] Optionally, the drying temperature in Step 3 is 60 - 70 °C, and the drying time is 2.5 - 3.5 h.

[0019] Optionally, the drying temperature in Step 3 is 70 °C, and the drying time is 3 h.

[0020] The present application also provides an application of an anti-caking agent prepared according to the method of the present application in betaine.

[0021] A method for preparing an anti-caking agent for betaine and its application according to the technical solution of the present invention includes: Step 1, mixing the metered calcium silicate, stearic acid and water evenly to obtain a first treated product; wherein, the mass ratio of calcium silicate, stearic acid and water is 10-30:1-10:200-300; Step 2, ball-milling the first treated product in a ball mill to obtain a second treated product; Step 3, filtering the second treated product by suction and drying to obtain the target anti-caking agent. Thus, the anti-caking agent prepared in the present application effectively prevents the caking of betaine through the synergistic effect of calcium silicate and stearic acid. Among them, the porous structure of calcium silicate preferentially adsorbs environmental moisture, reducing the water film on the surface of betaine particles, while the hydrophobicity of stearic acid forms a hydrophobic layer through coating and chemical reactions, further isolating moisture and reducing the adhesion between particles, reducing the caking rate of betaine and effectively preventing it from caking during storage. Moreover, the present application uses low-cost raw materials such as calcium silicate and stearic acid, and adopts simple process steps such as mixing, ball-milling, suction filtration and drying during the preparation process, which simplifies the preparation process and reduces the preparation cost of the anti-caking agent at the same time. In addition, calcium silicate is derived from natural minerals, is low-toxic and can be slowly degraded in the natural environment; stearic acid has biodegradability and can be decomposed into water and carbon dioxide under specific conditions, and has little direct impact on the human body and the environment. The whole preparation process is environmentally friendly, with less wastewater discharge and no waste residue discharge. Description of the Drawings

[0022] The specification drawings forming a part of the present application are used to provide a further understanding of the present invention. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation to the present invention. In the drawings:

[0023] Figure 1 is a flowchart of the method for preparing an anti-caking agent provided by an embodiment of the present application. Detailed Embodiments

[0024] It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The present invention will be described in detail below with reference to the drawings and in combination with the embodiments.

[0025] The present application provides a method for preparing an anti-caking agent for betaine, including:

[0026] Step 1, mixing the metered calcium silicate, stearic acid and water evenly to obtain a first treated product; wherein, the mass ratio of calcium silicate, stearic acid and water is 10-30:1-10:200-300;

[0027] Step 2: Ball-mill the first treated material in a ball mill to obtain a second treated material;

[0028] Step 3: Filter the second treated material by suction and then dry it to obtain the target anti-caking agent.

[0029] Specifically, in Step 1, weigh calcium silicate, stearic acid, and water in proportion and stir and mix them evenly to ensure that all components are fully dispersed, avoiding the formation of particle agglomerates, so that the materials can be uniformly processed during the subsequent ball-milling process to obtain the first treated material.

[0030] In Step 2, put the obtained first treated material into a ball mill for ball-milling. Through the action of mechanical force, physical and chemical changes occur on the surfaces of calcium silicate and stearic acid, forming a uniform dispersion system, and increasing the specific surface area and surface activity of the materials.

[0031] In Step 3, the ball-milled material is filtered by suction to remove the excess liquid, and then put into an oven and dried to constant weight to ensure that the product is dry, avoiding the influence of residual moisture on the anti-caking effect, and finally obtaining the target anti-caking agent applicable to betaine.

[0032] Among them, stearic acid is a single-component stearic acid, which is weakly acidic and partially dissociates into stearate ions C 17 H 35 COO- and H + .

[0033] During the ball-milling process, the impact and shear force of the grinding balls in the ball mill will destroy the crystal structure of calcium silicate particles, generating a large number of fresh surfaces and active sites (such as broken Si-O and Ca-O bonds), significantly increasing the chemical activity of calcium silicate. The stearate ions combine with the Ca 2+ on the surface of calcium silicate to form calcium stearate (Ca(C 17 H 35 COO)2):

[0034] CaSiO3 + 2C 17 H 35 COOH → Ca(C 17 H 35 COO)2 + H2SiO3CaSiO3 + 2C 17 H 35 COOH → Ca(C 17 H 35 COO)2 + H2SiO3

[0035] The unreacted stearic acid molecules are coated on the surface of calcium silicate through physical adsorption or hydrogen bonding to form a hydrophobic layer.

[0036] In this application, water is used as a dispersant to help stearic acid disperse evenly and promote ionic dissociation.

[0037] Generally speaking, the anti-caking agent prepared in this application can effectively prevent the caking of betaine through the synergistic effect of calcium silicate and stearic acid. Among them, the porous structure of calcium silicate preferentially adsorbs environmental moisture, reducing the water film on the surface of betaine particles, while the hydrophobicity of stearic acid forms a hydrophobic layer through coating and chemical reactions, further isolating moisture and reducing the adhesion between particles, reducing the caking rate of betaine, and thus effectively preventing its caking during storage. This application uses low-cost raw materials such as calcium silicate and stearic acid, and adopts simple process steps such as mixing, ball milling, suction filtration and drying during the preparation process. While simplifying the preparation process, it also reduces the preparation cost of the anti-caking agent. Moreover, calcium silicate is derived from natural minerals, is low-toxic and can be slowly degraded in the natural environment; stearic acid has biodegradability and can be decomposed into water and carbon dioxide under specific conditions, and has low toxicity with little direct impact on the human body and the environment. The entire preparation process is environmentally friendly, with less wastewater discharge and no waste residue discharge.

[0038] In a possible implementation manner, in step 1, the mass ratio of calcium silicate, stearic acid and water is 20:5:250.

[0039] Specifically, the mass ratio of calcium silicate, stearic acid and water is preferably 20:5:250. A reasonable proportion of calcium silicate can not only effectively adsorb moisture in the environment, reduce the water film on the surface of betaine particles, but also avoid excessive cost increase. And the appropriate proportion of stearic acid ensures the formation of an appropriate hydrophobic layer on the surface of calcium silicate, preventing the adhesion between particles, so as not to excessively affect the mixing uniformity and the overall effect of the anti-caking agent. The appropriate amount of water can ensure the good dispersion and mixing of each component.

[0040] In a possible implementation manner, in step 2, the ball milling time is 20-40 min.

[0041] In a possible implementation manner, in step 2, the ball milling time is at least 30 min.

[0042] Specifically, during the ball milling process, the crystal structure of calcium silicate particles is destroyed by the action of mechanical force, increasing its specific surface area and active sites, thereby improving the moisture absorption and isolation effect. At the same time, ball milling ensures that stearic acid is evenly coated on the surface of calcium silicate, forming a stable hydrophobic layer. Sufficient ball milling time can make the impact and shear action of the grinding balls on the material more sufficient and thorough, the crystal structure of calcium silicate can be more deeply damaged, generating a large number of fresh surfaces and abundant active sites, greatly improving the specific surface area and surface activity of the material. Secondly, the reaction between stearic acid and calcium silicate will be more complete, and stearate ions and Ca on the surface of calcium silicate 2+It can more fully combine to form calcium stearate, and the unreacted stearic acid molecules can also be more evenly coated on the surface of calcium silicate through physical adsorption or hydrogen bonding to form a denser and more stable hydrophobic layer, which can further enhance the protective effect of the anti-caking agent on betaine and more effectively reduce the caking rate of betaine.

[0043] In a possible implementation, qualitative filter paper is used in the suction filtration process in step 3.

[0044] Specifically, in step 3, the ball-milled anti-caking agent mixture is poured into a suction filtration device, and the excess liquid is removed by vacuum suction filtration. The pore size of the qualitative filter paper is moderate, which can effectively intercept particles and ensure the integrity and purity of the filter cake. The qualitative filter paper has good filtration efficiency and operational simplicity, ensuring the purity of the anti-caking agent particles and avoiding the influence of impurities and residual liquid.

[0045] In a possible implementation, the drying temperature in step 3 is 60 - 70 °C, and the drying time is 2.5 - 3.5 h.

[0046] In a possible implementation, the drying temperature in step 3 is 70 °C, and the drying time is 3 h.

[0047] Specifically, appropriate drying temperature and drying time can not only effectively remove the moisture in the anti-caking agent to ensure that the particles are dry, but also will not damage its chemical structure and hydrophobic properties. Too high a temperature may damage the stability of the anti-caking agent, while too low a temperature may result in incomplete drying and affect the storage effect. The drying time is long enough to ensure that the moisture is fully evaporated, but not too long to cause energy waste or potential thermal damage. This setting takes into account both drying efficiency and product quality, ensuring the stability and performance of the anti-caking agent.

[0048] The anti-caking agent prepared in this application is applied to betaine.

[0049] Example 1

[0050] Mix 20 g of calcium silicate, 5 g of stearic acid, and 250 g of water, ball mill for 30 min, then suction filter, and dry at 70 °C for 3 h until constant weight, denoted as R1, and add it to 98% betaine.

[0051] Comparative Example 1

[0052] Mix 20 g of calcium silicate, 5 g of sodium glutamate, and 250 g of water, ball mill for 30 min, then suction filter, and dry until constant weight, denoted as R2, and add it to 98% betaine.

[0053] Comparative Example 2

[0054] Mix 20 g of calcium silicate, 5 g of polyvinylpyrrolidone, and 250 g of water, ball mill for 30 min, then filter by suction and dry to constant weight, denoted as R3, and add it to 98% betaine.

[0055] Anti-caking agent performance test method: Mix 10 kg of betaine and 2.5% of the anti-caking agent evenly using a high-speed mixer, pack it in a bag and seal it, and conduct 4 parallel experiments; all samples are pressed into bales under an equal force of 1 ton for 31 days.

[0056] After 31 days, open the packaging bag, sieve the sample through a 40-mesh sieve, weigh and record the sample that has not passed through the sieve on the sieve, and record the mass as m. Among them:

[0057] Caking rate (%) = (m / 10 kg) * 100%

[0058] Table 1 Anti-caking agent test data

[0059]

[0060] It can be seen from Table 1 that the anti-caking agent with the R1 formula has the best effect in this pilot experiment, the lowest average caking rate, and the optimal caking rate reaches 1.27%.

[0061] The above are only the preferred embodiments of the present invention and are not used to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A preparation method of an anti-caking agent for betaine, characterized in that, Comprising: Step 1: Mix the measured calcium silicate, stearic acid and water evenly to obtain a first treatment product; wherein, the mass ratio of calcium silicate, stearic acid and water is 10 - 30:1 - 10:200 - 300; Step 2: Ball-mill the first treatment product in a ball mill to obtain a second treatment product; Step 3: Filter the second treatment product by suction and then dry it to obtain the target anti-caking agent.

2. The method for preparing an anti-caking agent for betaine according to claim 1, characterized in that, In the said Step 1, the mass ratio of calcium silicate, stearic acid and water is 20:5:

250.

3. The method for preparing an anti-caking agent for betaine according to claim 1, characterized in that, In the said Step 2, the ball-milling time is 20 - 40 min.

4. The method for preparing an anti-caking agent for betaine according to claim 3, characterized in that, The ball-milling time is 30 min.

5. The preparation method of the anti-caking agent for betaine according to claim 1, characterized in that, In the suction filtration process of the said Step 3, qualitative filter paper is used.

6. The preparation method of the anti-caking agent for betaine according to claim 1, characterized in that, In the said Step 3, the drying temperature is 60 - 70 °C and the drying time is 2.5 - 3.5 h.

7. The preparation method of the anti-caking agent for betaine according to claim 6, characterized in that, In the said Step 3, the drying temperature is 70 °C and the drying time is 3 h.

8. Application of an anti-caking agent prepared as claimed in claim 1 in betaine.

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