Production process of feed-grade high-protein calcium d-pantothenate granules

Abstract

The application discloses a production process of a feed-grade high-protein D-calcium pantothenate particle, and the process comprises the following steps: (1) after inactivation of D-calcium pantothenate mash, ceramic filtrate and ceramic membrane residue liquid are obtained through membrane filtration; (2) after heating of the ceramic filtrate, wood active carbon is added for decolorization; decolorized liquid is obtained through suction filtration; (3) the decolorized liquid is mixed with part of the ceramic membrane residue liquid to prepare a mixed liquid with a dry basis purity of 52-58%; (4) after concentration of the mixed liquid to a dry solid content of 52-58%, auxiliary materials are added to prepare a dry basis purity of 42-48%, and a 42-48% D-calcium pantothenate particle product is obtained through granulation bed drying. The production process effectively reduces the production cost and environmental protection pressure, and meanwhile, the bacterial protein and auxiliary materials are used to prepare an animal-friendly feed D-calcium pantothenate product which is better in flowability and richer in nutrition.

Description

Technical Field

[0001] This invention belongs to the field of vitamin production, specifically relating to a production process for feed-grade high-protein D-calcium pantothenate granules. Background Technology

[0002] Vitamin B5, also known as D-calcium pantothenate, is the calcium salt of water-soluble vitamin D-pantothenic acid. It is a component of coenzyme A and acyl carrier proteins. Industrial production of VB5 is primarily achieved through chemical synthesis. Enterprises typically use the isobutyraldehyde-formaldehyde-hydrocyanic acid method to synthesize DL-pantolactone. DL-pantolactone is further resolved chemically or enzymatically to obtain L-pantolactone. Finally, L-pantolactone is combined with β-alanine, produced from acrylonitrile, to synthesize VB5. The main raw materials for chemical synthesis of VB5 are flammable, explosive, and highly toxic. The production process generates cyanide-containing wastewater, which is difficult to treat, making VB5 a heavily polluting industry.

[0003] Another method is fermentation, which directly obtains D-calcium pantothenate through microbial fermentation, and then purifies it to obtain D-calcium pantothenate with a purity of 70% or 98%. For example, CN 115745827 A discloses an extraction process for producing calcium pantothenate by fermentation. This extraction process includes: acidification of fermentation broth, filtration, primary nanofiltration concentration, ion exchange, secondary nanofiltration concentration, decolorization, neutralization, evaporation concentration, crystallization, and centrifugal drying; or acidification of fermentation broth, filtration, primary nanofiltration concentration, decolorization, ion exchange, secondary nanofiltration concentration, neutralization, evaporation concentration, crystallization, and centrifugal drying to obtain calcium pantothenate crystals with a purity >98.5%. This type of method is costly, uses strong acids and alkalis in the fermentation extraction process, and generates a large amount of acidic and alkaline wastewater, resulting in high wastewater treatment pressure.

[0004] One major use of D-calcium pantothenate is in the processing of premixed feeds. In this case, D-calcium pantothenate is added to other nutrients to formulate premixed feeds. The inventors have found that these nutrients overlap to some extent with D-calcium pantothenate mash (which contains proteins, amino acids, and vitamins). Therefore, extracting high-purity D-calcium pantothenate from the D-calcium pantothenate mash is not a necessary operation. At the same time, pure D-calcium pantothenate may clump due to water absorption, and its powder form can make processing more difficult when premixing feed. Summary of the Invention

[0005] This invention provides a production process for feed-grade high-protein D-calcium pantothenate granules. This process solves the problems of high cost and environmental pressure associated with existing fermentation methods for producing D-calcium pantothenate. Furthermore, it enriches the product's nutrition by retaining the protein, amino acids, and vitamins produced during fermentation. Finally, it optimizes feed reprocessing by adding excipients to provide structural support for the production of granule formulations.

[0006] The technical solution of the present invention is as follows:

[0007] A production process for feed-grade high-protein D-calcium pantothenate granules includes the following steps:

[0008] (1) After inactivating and breaking the cell wall of D-calcium pantothenate mash, ceramic filtrate and ceramic membrane residue were obtained by membrane filtration;

[0009] (2) After heating the filtrate, wood-based activated carbon was added for decolorization, and the decolorized solution was obtained by suction filtration;

[0010] (3) The decolorizing solution and part of the ceramic membrane slag solution are remixed to prepare a mixed solution;

[0011] (4) After concentrating the mixture, add the auxiliary materials, and then granulate and dry it in a fluidized bed to obtain D-calcium pantothenate granules.

[0012] The inventors have discovered that, due to the presence of a certain amount of protein in D-calcium pantothenate products and the use of a coating granulation process to prepare granules, the product's flowability and anti-caking properties can be effectively improved, dust reduction facilitates automated processing in the feed industry. Simultaneously, the fermentation and metabolic process involves the trace generation of B vitamins or amino acids; retaining these components can enhance feed nutritional balance, improve animal growth performance, and the cell wall components (such as nucleotides and small peptides) can regulate intestinal flora, improve feed conversion rate, enhance palatability, and provide better nutritional value.

[0013] Preferably, in step (1), the D-calcium pantothenate mash contains 5-10 wt% D-calcium pantothenate and also contains other proteins, amino acids, and vitamins, which are derived from the fermentation broth formed by preparing D-pantothenic acid by fermentation.

[0014] Preferably, in step (1), the membrane filtration uses a ceramic membrane with a pore size of 30~70nm, and more preferably a ceramic membrane with a pore size of 50nm.

[0015] Preferably, in step (2), the heating temperature is 70~90℃ and the time is 1~5h.

[0016] Preferably, in step (2), the decolorizing activated carbon used includes, but is not limited to, one or more of 311, 301, 313, 303, 305, and 307. Furthermore, the decolorizing effect of activated carbon used for decolorization is best with 307.

[0017] As a preferred option, in step (2), the proportion of activated carbon added can be adjusted according to the actual material state and the type of activated carbon. It can be operated by adding 5 to 20g of activated carbon per liter of liquid, and more preferably by adding 10g of activated carbon per liter of liquid.

[0018] In this invention, in step (3), D-calcium pantothenate feed products with specifications ranging from 20% to 70% can be obtained by adjusting the mixing ratio of the decolorizing liquid and the residue liquid and the ratio of the auxiliary materials. Preferably, 45% D-calcium pantothenate can balance cost and product content, but other specifications of products prepared by the method of this patent are also within the scope of protection of this patent.

[0019] In this invention, in step (4), different excipients have different lower limits for granulation. If the amount added is too low, granular products cannot be obtained, but powdered formulations can still be obtained through drying equipment such as spray towers. Preferably, granular products are significantly better than powdered products in terms of hygroscopicity and flowability. The excipients include one or more of white dextrin, calcium carbonate, rice husk powder, maifanite, white corn cob, and zeolite powder, and the amount used is 17.5-37.5% of the dry weight of the solids in the mixed liquid. Preferably, when the excipient is corn cob, the amount added for granulation can be lower, which is more economical, and the minimum ratio is 17.5% of the dry weight of the solids in the mixed liquid.

[0020] Preferably, in step (4), the granulation fluidized bed is dried at 65~75℃ for 1~4h.

[0021] In this invention, step (4) involves granulation and drying using a pre-granulation and secondary spraying process. Utilizing the characteristics of the fluidized bed granulation system, a segmented spraying method is employed. In the fluidized bed feeding section, the mixture of auxiliary materials is pumped to a two-fluid spray gun, atomized into fine droplets by compressed air, and sprayed onto the seed crystals after large particles are crushed. Through agglomeration, the droplets gradually grow larger, completing the pre-granulation. In the discharge section, the auxiliary material slurry is sprayed separately through a two-fluid spray gun, coating the particles and completing the secondary spraying. The slurry is then discharged through a discharge valve. The particle size is controlled by the residence time; unqualified large particles are crushed by a crusher and used as seed crystals for re-granulation. The auxiliary materials used in the secondary spraying account for 0.02 to 2 wt% of the total auxiliary materials.

[0022] The feed-grade high-protein D-calcium pantothenate granules prepared by this invention have improved flowability and anti-caking properties. They contain D-calcium pantothenate and preferably include most of the other components in the fermentation broth, wherein the biomass content generated during fermentation is 0-82.5%. These D-calcium pantothenate granules have the following advantages:

[0023] 1.1 Contains D-calcium pantothenate at a concentration of 30 to 90 wt% of the total content.

[0024] 1.2 Bulk density is 0.7~0.9 g / mL.

[0025] 1.3 The pigment content in the fermentation broth was reduced by at least 70%.

[0026] Compared with the prior art, the beneficial effects of the present invention are reflected in:

[0027] (1) The process of the present invention does not require the use of acid and alkali, which solves the environmental protection problem. Moreover, the D-calcium pantothenate granules obtained retain the fermented microbial protein (the crude protein content in the product is >30%), which improves the product nutrition and can be better applied in the field of animal husbandry.

[0028] (2) The product obtained by the process of the present invention has a bulk density of 0.7~0.9 g / mL, which is close to the bulk density of premixed feed (the bulk density of mixed feed is generally around 0.7~0.8 g / mL), which is beneficial for feed companies to keep their products uniform during production, storage and transportation. Attached Figure Description

[0029] Figure 1 This is a flowchart of the entire production process of D-calcium pantothenate according to the present invention.

[0030] Figure 2 Images of the finished D-calcium pantothenate products prepared in Example 1 and Comparative Example 2. Detailed Implementation

[0031] The raw material D-calcium pantothenate mash applicable to this invention can be obtained by existing methods, and its source is not strictly limited. Any fermentation broth formed by the production of D-calcium pantothenate by fermentation method can be used as the raw material D-calcium pantothenate mash of this invention. For example, the fermentation broth containing D-calcium pantothenate can be obtained by referring to the method in the embodiment of CN 116024278 A.

[0032] Unless otherwise specified, all percentages mentioned in the following examples are weight percentages.

[0033] Example 1

[0034] 25 L of inactivated and cell-wall-broken D-calcium pantothenate mash (7% concentration) was filtered through a ceramic membrane with a pore size of 50 nm to obtain 19.2 L of D-calcium pantothenate filtrate (density 1.02 g / ml) and 5.8 L of residue. 10 L of the filtrate was heated to 80 °C and held at that temperature for 2 hours. 50 g of 303 activated carbon was added, and the mixture was stirred for 30 minutes before plate and frame filtration. The filtrate was mixed with 1.93 L of ceramic membrane residue (approximately 30% solids) and concentrated to a solids content of 55%. Add 256g of white dextrin (20% of the dry weight of the mixture), granulate and dry in a fluidized bed at 70℃ for 2 hours. During drying, a segmented spraying method is used. In the feeding section of the fluidized bed, the mixture with added auxiliary materials is pumped to a two-fluid spray gun by a feed pump. It is atomized into fine droplets by compressed air and sprayed onto the seed crystals after the large particles are crushed. Through agglomeration, the crystals gradually grow and complete the pre-granulation. In the discharge section, the auxiliary material slurry (containing 6.4g of white dextrin) is sprayed separately through a two-fluid spray gun. Under the action of the coating, the particles are coated, completing the secondary spraying. The particles are discharged through the discharge valve to obtain off-white D-calcium pantothenate granules.

[0035] Tests showed that the product has a direct content of 45.18%, a moisture content of 3.15%, a protein content of 34.79%, is rich in nutrients, has a bulk density of 0.75 g / mL, a moisture absorption rate of 5.15%, and good flowability, meeting the mixing requirements of premixed feed.

[0036] Figure 2 The D-calcium pantothenate sample prepared in this embodiment has good particle size and light color.

[0037] Examples 2-6

[0038] The preparation process is basically the same as in Example 1, except that the mixing ratio of residue and liquid and the types and proportions of additives are different. The specific conditions for the changes are listed in Table 1 below.

[0039] Comparative Example 1

[0040] The preparation process is basically the same as in Example 1, except for the different proportions of excipients added. The specific conditions for the changes are listed in Table 1 below.

[0041] Comparative Example 2

[0042] The preparation process is basically the same as in Example 1, except that the D-calcium pantothenate mash is concentrated and then the excipient (white dextrin) is added for preparation, granulation and drying to obtain the product.

[0043] Figure 2 Images of the finished product samples prepared for this comparative example are provided by [author's name]. Figure 2 It can be seen that the product obtained by this comparative ratio has a darker color.

[0044] Comparative Example 3

[0045] The preparation process is basically the same as in Example 1, except that segmented spraying is not used during drying, and the product is obtained by one-time spray granulation.

[0046] Table 1

[0047]

[0048] Note 1: Hygroscopicity data testing conditions: constant temperature and humidity chamber, 25℃, 80% relative humidity, stored for 24 hours;

[0049] Note 2: The moisture absorption rate of 98% D-calcium pantothenate is 10-11% under the conditions described in Note 1.

Claims

1. A production process for feed-grade high-protein D-calcium pantothenate granules, characterized in that, Includes the following steps: (1) After inactivating and breaking the cell wall of D-calcium pantothenate mash, ceramic filtrate and ceramic membrane residue were obtained by membrane filtration; (2) After heating the filtrate, wood-based activated carbon was added for decolorization, and the decolorized solution was obtained by suction filtration; (3) The decolorizing solution and part of the ceramic membrane slag solution are remixed to prepare a mixed solution; (4) After concentrating the mixture, add the auxiliary materials, and then granulate and dry it in a fluidized bed to obtain D-calcium pantothenate granules.

2. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (1), the membrane filtration uses a ceramic membrane with a pore size of 30~70nm.

3. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (2), the heating temperature is 70~90℃ and the time is 1~5h.

4. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (2), the wood-based activated carbon used includes one or more of the following types: 311, 301, 313, 303, 305, and 307.

5. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (2), the amount of decolorizing activated carbon used is 0.5 to 2% of the liquid volume.

6. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (3), the volume ratio of the decolorizing solution to the ceramic membrane slag solution is 10:0.3~2.

7. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (4), the excipients include one or more of the following: white dextrin, calcium carbonate, rice husk powder, maifanite, white corn cob, and zeolite powder, and the amount used is 17.5 to 37.5% of the dry weight of the solids in the mixture.

8. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (4), the granulation fluidized bed granulation drying adopts a segmented spraying process: in the fluidized bed feeding section, the mixture containing auxiliary materials is atomized by a two-fluid spray gun and sprayed onto the seed crystals, and the particles grow through agglomeration to complete the pre-granulation; in the fluidized bed discharging section, the auxiliary material slurry prepared by the auxiliary materials and water is sprayed separately by a two-fluid spray gun to coat the surface of the particles to form a coating, thus completing the secondary spraying.

9. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (4), the granulation fluidized bed is dried at 65~75℃ for 1~4h.

10. The production process of feed-grade high-protein D-calcium pantothenate granules according to claim 1, characterized in that, In step (4), the bulk density of the product particles obtained is 0.7~0.9 g / mL.

Images