Preparation method and application of anti-caking agent for amylase

Abstract

The invention provides a preparation method and application of an anti-caking agent for amylase, and the preparation method comprises the following steps: step 1, uniformly mixing metered calcium silicate, calcium stearate 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. Hydrophobic long chains of calcium stearate are adsorbed on the surface of calcium silicate to form a hydrophobic coating layer, and are uniformly dispersed on the surfaces of amylase particles, so that water contact is blocked, and moisture absorption and caking are reduced; on the other hand, the hydrophilic end of calcium stearate and ions on the surface of calcium silicate are subjected to weak ion exchange or coordination, the microenvironment around amylase is changed, the hydrophilicity of the amylase is reduced, meanwhile, the surface activity of the anti-caking agent is enhanced through structural change generated by ball milling, and the anti-caking agent can be used for improving the anti-caking effect through hydrogen bonds formed with amylase molecules, Van der Waals force and other interactions. The starch is tightly attached to the surfaces of amylase particles to prevent moisture absorption and caking, so that the performance of the amylase is ensured.

Description

Technical Field

[0001] The present invention relates to the field of chemical engineering technology, and more particularly, to a method for preparing an anti-caking agent for amylase and its application. Background Art

[0002] As a powdery enzyme preparation, amylase is prone to absorb moisture and caking in a humid environment, resulting in a decrease in dispersibility. After caking, it is difficult to dissolve evenly, affecting the catalytic efficiency. For example, in the food industry, caked amylase may cause uneven fermentation of bread, affecting the taste. In addition, after caking, the interaction between enzyme molecules is enhanced, which may damage the spatial structure, reduce the ability to catalyze starch hydrolysis, and cause its activity to decay. Research experiments have shown that the activity of caked amylase may decrease by more than 30%.

[0003] Therefore, there is an urgent need for a method for preparing an anti-caking agent for amylase to solve the above problems. Summary of the Invention

[0004] The main object of the present invention is to provide an anti-caking agent for amylase and a method for preparing the same, so as to at least solve the problem that amylase is prone to absorb moisture and caking in a humid environment in the prior art.

[0005] To achieve the above object, the present invention provides a method for preparing an anti-caking agent for amylase, including:

[0006] Step 1: Mix the measured calcium silicate, calcium stearate and water evenly to obtain a first treated product; wherein, the mass ratio of calcium silicate, calcium stearate and water is 10-20:1-5:100-200;

[0007] Step 2: Ball-mill the first treated product in a ball mill to obtain a second treated product;

[0008] Step 3: Filter the second treated product by suction and then dry it to obtain the target anti-caking agent.

[0009] Optionally, in Step 1, the mass ratio of calcium silicate, calcium stearate and water is 20:2:150.

[0010] Optionally, in Step 2, the ball-milling time is 20-40 min.

[0011] Optionally, in Step 2, the ball-milling time is 30 min.

[0012] Optionally, qualitative filter paper is used in the suction filtration process in Step 3.

[0013] Optionally, the drying temperature in Step 3 is 60-70 °C, and the drying time is 2.5-3.5 h.

[0014] Optionally, the drying temperature in step 3 is 70 °C and the drying time is 3 h.

[0015] The present application also provides an application of an anti-caking agent prepared by the preparation method of the present application in amylase.

[0016] A preparation method and application of an anti-caking agent for amylase according to the technical solution of the present invention include: Step 1, mixing metered calcium silicate, calcium stearate and water evenly to obtain a first treated product; wherein, the mass ratio of calcium silicate, calcium stearate and water is 10-20:1-5:100-200; 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 then drying it to obtain the target anti-caking agent. Thus, the hydrophobic long chain of calcium stearate adsorbs on the surface of calcium silicate to form a hydrophobic coating layer, which is evenly dispersed on the surface of amylase particles, blocking the contact with moisture and reducing moisture absorption and caking; on the other hand, the hydrophilic end of calcium stearate undergoes weak ion exchange or coordination with the surface ions of calcium silicate, changing the microenvironment around amylase to reduce its hydrophilicity. At the same time, the structural changes generated by ball milling enhance the surface activity of the anti-caking agent. Through interactions such as hydrogen bonding and van der Waals forces with amylase molecules, it adheres tightly to the surface of amylase particles, preventing them from absorbing moisture and caking, thereby ensuring the performance of amylase. Description of the Drawings

[0017] 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:

[0018] Figure 1 is a flowchart of the preparation method of the anti-caking agent provided by the embodiment of the present application. Detailed Embodiments

[0019] 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.

[0020] The present application provides a preparation method of an anti-caking agent for amylase, including:

[0021] Step 1, mixing metered calcium silicate, calcium stearate and water evenly to obtain a first treated product; wherein, the mass ratio of calcium silicate, calcium stearate and water is 10-20:1-5:100-200;

[0022] Step 2, ball-milling the first treated product in a ball mill to obtain a second treated product;

[0023] Step 3, filtering the second treated product by suction and then drying it to obtain the target anti-caking agent.

[0024] Specifically, the development of the amylase anti-caking agent aims to solve the problem of performance attenuation caused by moisture absorption and caking of amylase, while meeting the application requirements in multiple fields and improving industrial efficiency. The anti-caking agent forms a barrier by adsorbing moisture, maintaining the loose state and activity of amylase, significantly improving its processing fluidity and extending the storage period.

[0025] In step 1, calcium silicate, calcium stearate and water are weighed in proportion and then stirred and mixed 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 product.

[0026] In step 2, the obtained first treated product is put 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 calcium stearate, forming a uniform dispersion system, and improving the specific surface area and surface activity of the materials.

[0027] In step 3, the ball-milled material is filtered by suction to remove the excess liquid, and then put into an oven to be dried to a constant weight to ensure that the product is dry and avoid moisture residue affecting the anti-caking effect, and finally the target anti-caking agent applicable to amylase is obtained.

[0028] Among them, during the ball milling process, the impact and shear forces generated by the grinding balls will damage the crystal structure of calcium silicate, and then generate a variety of active sites. On the one hand, broken Si-O and Ca-O bonds will be formed, increasing the surface energy; on the other hand, newly exposed Ca 2+ and SiO3 2- ions will appear, thus enhancing the reaction activity. In addition, amorphous calcium silicate will also be formed during this process. The hydrophobic long chain (C 17 H 35 -) of calcium stearate is adsorbed on the surface of calcium silicate by van der Waals force, and then a hydrophobic coating layer is formed, while its hydrophilic calcium ion end (-COO-Ca 2+ ) undergoes weak ion exchange or coordination with Ca 2+ or SiO3 2- on the surface of calcium silicate.

[0029] In this application, water molecules cause partial hydrolysis reaction on the surface of calcium silicate, thus generating Si-OH and Ca-OH groups. The generation of these groups can enhance the interaction between calcium silicate and calcium stearate; and water, as a carrier, evenly disperses calcium stearate, so that it can fully contact the surface of calcium silicate particles.

[0030] Generally speaking, for the anti-caking agent prepared in this application, the hydrophobic long chains of calcium stearate adsorb on the surface of calcium silicate to form a hydrophobic coating layer, which is evenly dispersed on the surface of amylase particles, blocking the contact with moisture and reducing moisture absorption and caking. On the other hand, the hydrophilic end of calcium stearate undergoes weak ion exchange or coordination with the surface ions of calcium silicate, changing the microenvironment around amylase to reduce its hydrophilicity. At the same time, the structural changes caused by ball milling enhance the surface activity of the anti-caking agent. Through interactions such as hydrogen bonding and van der Waals forces with amylase molecules, it tightly adheres to the surface of amylase particles, preventing them from absorbing moisture and caking, thus ensuring the performance of amylase, ensuring the uniform distribution and activity of amylase during application, and thereby improving the catalytic efficiency; reducing problems such as production interruption and equipment blockage caused by amylase caking, and reducing maintenance costs and downtime. Moreover, the anti-caking agent helps to maintain the stability of amylase, extend its storage period, and reduce inventory losses.

[0031] In a possible implementation manner, in step 1, the mass ratio of calcium silicate, calcium stearate, and water is 20:2:150.

[0032] Specifically, if there is too much calcium silicate, on the one hand, during the ball milling process, there is a relative shortage of calcium stearate, making it difficult to fully adsorb on the surface of calcium silicate to form a complete and uniform hydrophobic coating layer, resulting in some calcium silicate particles being exposed, being easily hygroscopic and reducing the anti-caking effect; on the other hand, it may lead to uneven distribution of active sites, weakening the surface activity and reaction activity of the material, affecting the interaction with amylase molecules, and weakening the protective effect on amylase. If there is too little calcium silicate, it may not provide enough attachment basis for calcium stearate, resulting in an unstable structure of the formed anti-caking agent, also affecting its anti-caking performance on amylase. Too much calcium stearate will increase the cost, and the excessive hydrophobic long chains may affect the dispersibility of the material to a certain extent; too little will make it difficult to form an effective hydrophobic coating layer and ionic interaction, reducing the anti-caking ability. If the proportion of water is too much, the material will be too soft and mushy during the ball milling process, affecting the grinding effect and the formation of active sites. Too little water is not enough to fully initiate the hydrolysis reaction of calcium silicate, and is also not conducive to the uniform mixing and dispersion of each component, thereby affecting the overall performance of the anti-caking agent.

[0033] In a possible implementation manner, in step 2, the ball milling time is 20 - 40 min.

[0034] In a possible implementation manner, in step 2, the ball milling time is 30 min.

[0035] Specifically, in step 2, the ball milling time is preferably 30 min. The impact and shear forces of the grinding balls can act on the material more fully, so that the crystal structure of calcium silicate is more thoroughly destroyed, generating more highly active fracture surfaces and newly exposed ions, greatly increasing the specific surface area and surface activity of the material. The formed hydrophobic coating layer will be more uniform and dense, effectively isolating the contact between moisture and amylase. Moreover, the interaction between calcium stearate and calcium silicate will be further enhanced, and the ion exchange and coordination effects will be more sufficient. The increase in multiple active sites also makes the binding between the anti-caking agent and amylase molecules more stable. If the ball milling time is short, the degree of destruction of the calcium silicate crystal structure is limited, the number of active sites is insufficient, the surface energy is limitedly increased, the surface activity and reaction activity of the anti-caking agent are not ideal, calcium stearate is difficult to adsorb and act sufficiently, the hydrophobic coating layer and ion interaction are imperfect, and it cannot prevent amylase from absorbing moisture and caking well, ultimately affecting the anti-caking effect.

[0036] In a possible implementation manner, in step 3, qualitative filter paper is used in the suction filtration process.

[0037] 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 simple operation, ensuring the purity of the anti-caking agent particles and avoiding the influence of impurities and residual liquid.

[0038] In a possible implementation manner, in step 3, the drying temperature is 60 - 70 °C, and the drying time is 2.5 - 3.5 h.

[0039] In a possible implementation manner, in step 3, the drying temperature is 70 °C, and the drying time is 3 h.

[0040] Specifically, in step 3, the drying temperature is preferably 70 °C, and the drying time is preferably 3 h. Appropriate drying temperature and drying time can not only effectively remove the moisture in the anti-caking agent and ensure that the particles are dry, but also will not damage its chemical structure and hydrophobic properties. Excessive temperature may damage the stability of the anti-caking agent, while too low temperature may lead to 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. It can balance the drying efficiency and product quality and ensure the stability and performance of the anti-caking agent.

[0041] The anti-caking agent prepared in this application is applied to amylase.

[0042] Implementation Case 1

[0043] Mix 20 g of calcium silicate, 2 g of calcium stearate, and 150 g of water evenly, ball mill for 30 min, then perform suction filtration and drying, denote it as A1, and add it to the amylase.

[0044] Example 2

[0045] Mix 20 g of calcium silicate, 2 g of sodium lignosulfonate, and 150 g of water evenly, ball mill for 30 min, then perform suction filtration and drying, denote it as A2, and add it to the amylase.

[0046] Example 3

[0047] Mix 20 g of silicon dioxide, 2 g of sodium lignosulfonate, and 150 g of water, ball mill for 30 min, then perform suction filtration and drying, denote it as A3, and add it to the amylase.

[0048] Anti-caking agent performance test method: Mix 10 kg of amylase and 3.5% 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 and packed under a uniform force of 1 ton for 31 days.

[0049] 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:

[0050] Caking rate (%) = (m / 10 kg) * 100%

[0051] Table 1 Anti-caking agent test data

[0052]

[0053] It can be seen from Table 1 that the anti-caking agent with the A1 formulation has the best effect in this pilot experiment, the lowest average caking rate, and the optimal caking rate reaches 2.63%.

[0054] 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, various changes and modifications can be made to the present invention. 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 amylase, characterized in that, Including: Step 1: Mix the measured calcium silicate, calcium stearate and water evenly to obtain a first treatment product; wherein, the mass ratio of calcium silicate, calcium stearate and water is 10-20:1-5:100-200; 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 preparation method of the anti-caking agent for amylase according to claim 1, characterized in that, In the step 1, the mass ratio of calcium silicate, calcium stearate and water is 20:2:

150.

3. The preparation method of the anti-caking agent for amylase according to claim 1, characterized in that, In the step 2, the ball-milling time is 20-40 min.

4. The preparation method of the anti-caking agent for amylase according to claim 3, characterized in that, In the step 2, the ball-milling time is 30 min.

5. The preparation method of the anti-caking agent for amylase according to claim 1, wherein In the step 3, qualitative filter paper is used in the suction filtration process.

6. The preparation method of the anti-caking agent for amylase according to claim 1, wherein In the step 3, the drying temperature is 60-70 °C and the drying time is 2.5-3.5 h.

7. The method for preparing an anti-caking agent for amylase according to claim 6, wherein In the 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 amylase.

Images