Monensin sodium premix and preparation method thereof

Abstract

The invention mainly relates to a monensin sodium premix and a preparation method thereof, and belongs to the technical field of veterinary drugs. The preparation method comprises the following steps: carrying out enzyme wall breaking inactivation, ionic solution system pore forming and sodium loading on a monensin fermentation solution to obtain a monensin sodium treatment solution, and carrying out auxiliary material dispersion, solid-liquid separation and preparation on the treatment solution to obtain the monensin sodium premixing agent. According to the preparation method disclosed by the invention, Na < + > loading of monensin can be promoted by adopting enzyme wall breaking and ionic solution system pore forming, formation of monensin sodium is facilitated, loss of Na < + > in a solid-liquid separation process is avoided, the sodium loading amount is remarkably increased, and improvement of the pesticide effect is facilitated; meanwhile, the process preparation is simple, the heating and organic solvent extraction processes are avoided, the filtrate can form recyclable reclaimed water after purification treatment, and the method is more energy-saving, environment-friendly and safe.

Description

Technical Field

[0001] The invention belongs to the technical field of veterinary drugs, and in particular relates to a monensin sodium premix and a preparation method thereof. Background Art

[0002] Monensin is a fermentation product of Streptomyces cinnamomi (an acidic antibiotic with a pentacyclic polyether structure) and is one of the most widely used drugs among polyether ion carrier antibiotics. The preparation is its sodium salt, which has a broad spectrum of anticoccidial activity. The insecticidal mechanism of monensin sodium is to interfere with the Na + Normal osmotic pressure, a certain amount of Na + In order to balance the osmotic pressure, a large number of water molecules enter the cells, causing swelling. + , coccidia cells need to consume a certain amount of metabolic energy, Na + Too much sodium will cause the coccidia to die due to energy exhaustion and excessive swelling. Therefore, increasing the sodium loading of monensin plays an important role in improving the efficacy of monensin sodium.

[0003] Monensin is synthesized by the secondary metabolism of producing bacteria through biological fermentation, using soybean oil, glucose, soybean cake powder, ammonium sulfate, potassium dihydrogen phosphate and other food chemical raw materials. After the metabolism is completed, since monensin is insoluble in water and exists in the mycelium of the producing bacteria, it is impossible to directly obtain the sodium monensin product. The commonly used processes for converting monensin to sodium monensin are the solvent method and the pH adjustment method. The solvent method requires the use of organic solvents, and the process is relatively complicated. There are also environmental pollution and safety risks. In the pH adjustment method, since the fermentation level of monensin has been greatly improved, the mass proportion of monensin in the dry bacteria is about 30% to 35%, but the monensin fermentation broth cannot fully load Na by adjusting the pH to 8 to 9 with alkali. + , resulting in Na + Therefore, a method for increasing the Na content of monensin is provided. + A method for preparing monensin sodium that is high in quantity, simple in process, energy-saving, environmentally friendly and safe is very necessary. Summary of the invention

[0004] In view of this, the object of the present invention is to provide a monensin sodium premix and a preparation method thereof, to simplify the preparation process, to increase the sodium loading of monensin, to avoid the use of a large amount of organic solvents and heating processes in the preparation process of monensin sodium, and to achieve the effect of improving drug efficacy and energy saving and environmental protection.

[0005] The present invention provides a method for preparing a monensin sodium premix, comprising the following steps:

[0006] After the monensin fermentation broth was mixed with cellulase and inactivated, NaOH was added to adjust the pH to 8-11, and the ion solution system Na + -EDTANa2-BF4, forming a mixed solution, stirring to obtain a monensin sodium treatment solution;

[0007] The monensin sodium treatment liquid is mixed with auxiliary materials, and the solid-liquid separation is performed to obtain a solid part, and the solid part is prepared to obtain a monensin sodium premix.

[0008] Preferably, the content of monensin in the monensin fermentation broth is 4 to 4.8 g / 100 mL.

[0009] Preferably, the ratio of the cellulase to the monensin fermentation broth is 0.1-1.0 g:100 mL, and the cell wall breaking and inactivation time is 60 min to 180 min.

[0010] Preferably, the Na + -EDTANa2-BF4 is composed of BF4, EDTANa2, NaOH solution and purified water; the weight volume ratio of BF4, EDTANa2, NaOH solution and purified water is 10-15g: 10-15g: 40-50mL: 100mL; the concentration of the NaOH solution is 30-40g / 100mL.

[0011] Preferably, the volume ratio of the ionic solution system to the monensin fermentation broth is 1.0-3.0:100.

[0012] Preferably, the stirring time is 60 min to 180 min, and the stirring speed is 30 to 45 rpm.

[0013] Preferably, the auxiliary materials include light calcium carbonate, attapulgite, diatomaceous earth and talc.

[0014] Preferably, the ratio of the light calcium carbonate to the sodium monensin treatment solution is 5-8 g:100 mL, the ratio of the attapulgite to the sodium monensin treatment solution is 0.5-2.0 g:100 mL; the ratio of the diatomaceous earth to the sodium monensin treatment solution is 0.5-2.0 g:100 mL; the ratio of the talc to the sodium monensin treatment solution is 0.25-0.5 g:100 mL.

[0015] Preferably, the solid-liquid separation is filtration, and the filtration is plate and frame filtration.

[0016] The invention also provides a monensin sodium premix prepared by the preparation method.

[0017] Beneficial effects of the present invention:

[0018] The present invention provides a method for preparing sodium monensin. By breaking the cell wall and inactivating the cell wall, not only the cumbersome process of high-temperature heating is avoided, but also the energy-saving effect is achieved. At the same time, the pore-forming of the cell by the ionic solution system can jointly promote the sodium loading of monensin, avoid the loss of sodium ions during the solid-liquid separation process, and be beneficial to the formation of sodium monensin. In addition, the extraction of organic solvents is avoided during the preparation process, and the filtrate obtained by solid-liquid separation after the sodium monensin treatment liquid is added with auxiliary materials is purified by an environmental protection system to form recyclable reclaimed water, and the auxiliary materials are light calcium carbonate, attapulgite, diatomaceous earth, talcum powder and other animal auxiliary materials, which are more environmentally friendly and safe. Therefore, the preparation method of the sodium monensin premix of the present invention achieves the effect of improving drug efficacy and energy saving and environmental protection. DETAILED DESCRIPTION

[0019] The present invention provides a method for preparing a monensin sodium premix, comprising the following steps:

[0020] After the monensin fermentation broth was mixed with cellulase and inactivated, NaOH was added to adjust the pH to 8-11, and the ion solution system Na + -EDTANa2-BF4, forming a mixed solution, stirring to obtain a monensin sodium treatment solution;

[0021] The monensin sodium treatment liquid is mixed with auxiliary materials, and the solid-liquid separation is performed to obtain a solid part, and the solid part is prepared to obtain a monensin sodium premix.

[0022] In the present invention, the monensin fermentation broth is preferably a fermentation broth produced by fermentation of Streptomyces cinnamomi, and the content of monensin in the monensin fermentation broth is 4-4.8 g / 100 mL. In one embodiment, 4 g / 100 mL, 4.5 g / 100 mL or 4.8 g / 100 mL can be selected; the solid content of the monensin fermentation broth is preferably 10% to 12% by mass, more preferably 10.5-11.5%, and further preferably 11%.

[0023] In the present invention, the monensin fermentation broth is mixed with cellulase, and the cellulase is used to enzymolyze the cellulase to achieve cell wall breaking and inactivation, and the cell wall breaking and inactivation is carried out at room temperature (20°C to 30°C). The enzymatic activity of the cellulase is preferably >5500U / g, and in one embodiment, 5637U / g, 5775U / g or 5912U / g can be selected; the ratio of the cellulase to the monensin fermentation broth is preferably 0.1 to 1.0g:100mL, and in one embodiment, 0.1g:100mL, 0.25g:100mL, 0.5g:100mL, 0.75g:100mL or 1g:100mL can be selected. The cell wall breaking and inactivation time is preferably 60min to 180min, and in one embodiment, 60min, 80min, 100min, 120min, 140min, 160min or 180min can be selected.

[0024] In the present invention, after cell wall inactivation, NaOH is added to adjust the pH to 8-11. In one embodiment, the pH can be adjusted to 8, 8.5, 9, 9.5, 10, 10.5 or 11. The present invention has no particular limitation on the concentration of NaOH. In one embodiment, a NaOH solution with a mass volume concentration of 30 g / 100 mL can be selected. + -EDTANa2-BF4 forms a mixed solution, the ion solution system Na +-EDTANa2-BF4 is preferably composed of BF4, EDTANa2, NaOH solution and purified water, and the ratio of BF4 to purified water is preferably 10-15g:100mL, more preferably 10g:100mL, 13g:100mL or 15g:100mL; the ratio of EDTANa2 to purified water is preferably 10-15g:100mL, more preferably 10g:100mL, 13g:100mL or 15g:100mL; the volume ratio of NaOH solution to purified water is preferably 40-50:100, more preferably 40:100, 45:100 or 50:100, and the concentration of NaOH solution is preferably 30-40g / 100mL, more preferably 30g / 100mL, 35g / 100mL or 40g / 100mL. The ionic solution system is preferably prepared by the following method: BF4 is dispersed in purified water, the ratio of BF4 to purified water is 10-15 g: 100 mL (such as 10 g: 100 mL, 13 g: 100 mL or 15 g: 100 mL), heated to 60-65°C (for example 60°C, 63°C or 65°C), EDTANa2 is added, the ratio of EDTANa2 to purified water is 10-15 g: 100 mL (such as 10 g: 100 mL, 13 g: 100 mL or 15 g: 100 mL), and the temperature is kept for 60-90 min (such as 60 min, 70 min, 80 min or 90 min). 90min), 30-45rpm (such as 30rpm, 35rpm, 40rpm or 45rpm) stirring for 30-60min (such as 30min, 40min, 50min or 60min), adding a sodium hydroxide solution with a mass volume concentration of 30-40g / 100mL (such as 30g / 100mL, 35g / 100mL, 40g / 100mL), the volume ratio of sodium hydroxide solution to purified water is 40-50:100 (such as 40:100, 45:100 or 50:100), stirring and cooling to 25-30°C (such as 25°C, 28°C or 30°C). Preferably, the volume ratio of the ionic solution system to the monensin fermentation broth is 1.0-3.0:100. In one embodiment, 1.0:100, 1.8:100, 2.0:100 or 3.0:100 can be selected. The molar ratio of sodium ions to monensin molecules in the mixed solution after the ionic solution system is added is 0.8-1.2. In one embodiment, it can be 0.8, 0.9, 1.0, 1.1 or 1.2.Stirring promotes the ion solution system to form pores on the bacteria, promotes sodium loading, and then forms a sodium monensin treatment solution. The stirring time is preferably 60 minutes to 180 minutes. In one embodiment, 60 minutes, 80 minutes, 90 minutes, 120 minutes or 180 minutes can be selected. The stirring speed is preferably 30 to 45 rpm. In one embodiment, 30 rpm, 35 rpm, 40 rpm or 45 rpm can be selected.

[0025] In the present invention, the sodium monensin treatment solution is mixed with auxiliary materials to disperse the sodium monensin, and the auxiliary materials preferably include light calcium carbonate, attapulgite, diatomaceous earth and talcum powder. The ratio of the light calcium carbonate to the sodium monensin treatment solution is preferably 5 to 8 g:100 mL. In one embodiment, 5 g:100 mL, 6 g:100 mL, 6.5 g:100 mL, 7 g:100 mL or 8 g:100 mL can be selected; the ratio of the attapulgite to the sodium monensin treatment solution is preferably 0.5 to 2 g:100 mL. In one embodiment, 0.5 g:100 mL, 1 g:100 mL, 1.5 g:100 mL or 2 g:100 mL can be selected; The ratio of diatomaceous earth to sodium monensin treatment liquid is preferably 0.5-2g:100mL, and in one embodiment, 0.5g:100mL, 1g:100mL, 1.5g:100mL or 2g:100mL can be selected; the ratio of talcum powder to sodium monensin treatment liquid is preferably 0.25-0.5g:100mL, and in one embodiment, 0.25g:100mL, 0.35g:100mL, 0.45g:100mL or 0.5g:100mL can be selected. After the sodium monensin treatment liquid is mixed with the auxiliary materials, it is preferred that stirring is also included, and the stirring speed is preferably 20-30rpm, and in one embodiment, 20rpm, 25rpm or 30rpm can be selected; the stirring time is preferably 60min-120min, and in one embodiment, 60min, 70min, 80min, 90min, 100min, 110min or 120min can be selected. After stirring, solid-liquid separation is performed, and the solid-liquid separation is preferably filtration, and the filtration is preferably plate-frame filter press, and the volume of the plate-frame filtration is preferably 5m 3 ~7m 3 / board frame, in one embodiment, 5m can be selected 3 / Plate frame, 6m 3 / Plate frame or 7m 3 / plate frame, the air pressure of the plate frame filtration is 0.4-0.5 MPa, in one embodiment, 0.4 MPa, 0.45 MPa or 0.5 MPa can be selected, and the moisture content of the monensin sodium filter cake obtained is controlled to be 30%-40%, in one embodiment, 30%, 35% or 40% can be selected. After filtration, a filtrate and the monensin sodium filter cake are obtained. The filtrate is tested to have a pH of 8.5 and a sodium ion content of 0.01%-0.015% (W / V). The filtrate can also be preferably purified by an environmental protection system to obtain recycled water with a COD of 20-50.

[0026] In the present invention, after obtaining the monensin sodium filter cake, it is preferred that a preparation process can also be performed. In one embodiment, a granule preparation can be selected. The present invention has no special limitation on the preparation process of the granule preparation, and it can be prepared by a conventional granule preparation method in the art. It is preferably prepared by crushing, screening, extrusion granulation, and drying.

[0027] The present invention also provides a monensin sodium premix prepared by the above preparation method, wherein the main components of the monensin sodium premix are monensin sodium, C 37 H 63 NaO 11 , molecular weight 706.89, structural formula as shown in formula I. The content of monensin sodium in the monensin sodium premix is ​​greater than 19% (W / W), such as 19.6%, 20% or 22%; the content of sodium ions in the monensin sodium premix is ​​greater than 0.7% (W / W), such as 0.779%, 0.736% or 0.816%.

[0028]

[0029] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0030] In the following embodiments, unless otherwise specified, all of them are conventional methods.

[0031] Unless otherwise specified, the materials and reagents used in the following examples can be obtained from commercial sources.

[0032] In the following examples and comparative examples, Na +-EDTANa2-BF4 was prepared by the following method: BF4 was dispersed in purified water, the ratio of BF4 to purified water was 13g:100mL, heated to 63°C, EDTANa2 was added, the ratio of EDTANa2 to purified water was 13g:100mL, kept warm for 70min, stirred at 35rpm for 40min, sodium hydroxide solution with a mass volume concentration of 35g / 100mL was added, the volume ratio of sodium hydroxide solution to purified water was 45:100, stirred and cooled to 28°C to obtain Na + -EDTANa2-BF4 ion solution system.

[0033] Example 1

[0034] 1. Treatment of Monensin Fermentation Broth

[0035] 1.1 Cellulase inactivation, the conditions are as follows: 0.1% (W / V) cellulase is added to a monensin fermentation broth having a solid content of 11% (W / W) and a monensin content of 4.5 g / 100 mL, and the cellulase activity is 5637 U / g, and the cellulase is inactivated by cell wall breaking for 120 min;

[0036] 1.2 Breaking the wall and forming pores: Use 30g / 100mL NaOH solution to adjust the pH to 11, add 2% (V / V) ion solution system Na + -EDTANa2-BF4, to form a mixed solution, in which the molar ratio of sodium ions to monensin molecules was 1.0, and stirred at 30 rpm for 120 min to promote sodium loading.

[0037] 2. Dispersion of monensin sodium treatment solution: add 8% (W / V) light calcium carbonate, 0.5% (W / V) attapulgite, 0.5% (W / V) diatomaceous earth, and 0.25% (W / V) talc, and stir at 30 rpm for 120 min.

[0038] 3. Solid-liquid separation: put the dispersed monensin sodium treated liquid into the plate frame, adjust the air pressure to 0.5mpa, and 3 / plate and frame filtration volume was subjected to high pressure closed plate and frame filtration (the moisture content of the monensin sodium filter cake was controlled at 30%) to obtain a filtrate and a monensin sodium filter cake. The pH of the filtrate was tested to be 8.5, and the sodium ion content was 0.0113% (W / V).

[0039] 4. Filtrate purification: The filtrate is purified by the environmental protection system to form recyclable grey water with a COD of 30.

[0040] 5. Granulation: The filter cake of monensin sodium was crushed by a pulverizer, and 100% passed through a 24-mesh sieve; it was conveyed to a rotary extrusion granulator by a screw conveyor, with a feeding speed of 30 Hz, a rotary extrusion speed of 90 rpm, and a spheronization speed of 90 rpm to form spherical wet granules.

[0041] 6. Drying: The wet granules were vacuum-sucked into a fluidized bed dryer and dried for 60 min at an inlet air temperature of 160° C., an outlet air temperature of 60° C., and a wind speed of 160 Hz to obtain a monensin sodium premix with a moisture content of 4% (W / W), a monensin sodium content of 22% (W / W), and a sodium ion content of 0.816% (W / W), thereby achieving sodium loading.

[0042] Example 2

[0043] 1. Treatment of Monensin Fermentation Broth

[0044] 1.1 Cellulase inactivation, the conditions are as follows: 0.1% (W / V) cellulase is added to a monensin fermentation broth with a solid content of 10% (W / W) and a monensin content of 4.5 g / 100 mL, and the cellulase activity is 5637 U / g, and the cellulase is inactivated by cell wall breaking for 120 min;

[0045] 1.2 Breaking the wall and forming pores: Use 30g / 100mL NaOH solution to adjust the pH to 11, add 1.8% (V / V) ion solution system Na + -EDTANa2-BF4, to form a mixed solution, in which the molar ratio of sodium ions to monensin molecules was 0.9, and stirred at 30 rpm for 90 min to promote sodium loading.

[0046] 2. Dispersion of monensin sodium treatment solution: add 6.5% (W / V) light calcium carbonate, 1.0% (W / V) attapulgite, 1.0% (W / V) diatomaceous earth, and 0.5% (W / V) talc, and stir at 30 rpm for 90 min.

[0047] 3. Solid-liquid separation: put the dispersed monensin sodium treated liquid into the plate frame, adjust the air pressure to 0.4mpa, and 3 / plate and frame filtration volume was subjected to high pressure closed plate and frame filtration (the moisture content of the monensin sodium filter cake was controlled at 35%) to obtain a filtrate and a monensin sodium filter cake. The pH of the filtrate was tested to be 8.5, and the sodium ion content was 0.0146% (W / V).

[0048] 4. Filtrate purification: The filtrate is purified by the environmental protection system to form recyclable grey water with a COD of 40.

[0049] 5. Granulation: The filter cake of monensin sodium was crushed by a pulverizer, and 100% passed through a 24-mesh sieve; it was conveyed to a rotary extrusion granulator by a screw conveyor, with a feeding speed of 20 Hz, a rotary extrusion speed of 45 rpm, and a spheronization speed of 60 rpm to form spherical wet granules.

[0050] 6. Drying: The wet granules were vacuum-sucked into a fluidized bed dryer and dried for 40 min at an inlet air temperature of 130° C., an outlet air temperature of 40° C., and a wind speed of 120 Hz to obtain a monensin sodium premix with a moisture content of 6% (W / W), a monensin sodium content of 19.6% (W / W), and a sodium ion content of 0.736% (W / W).

[0051] Example 3

[0052] 1. Treatment of Monensin Fermentation Broth

[0053] 1.1 Cellulase inactivation, the conditions are as follows: 0.5% (W / V) cellulase, the cellulase activity is 5637U / g, and cellulase inactivation is carried out by cell wall breaking for 180min to monensin fermentation broth with a solid content of 12% (W / W) and a monensin content of 4.5g / 100mL;

[0054] 1.2 Breaking the wall and forming pores: Use 30g / 100mL NaOH solution to adjust the pH to 11, add 1.8% (V / V) ion solution system Na + -EDTANa2-BF4, to form a mixed solution, in which the molar ratio of sodium ions to monensin molecules was 0.9, and stirred at 45 rpm for 60 min to promote sodium loading.

[0055] 2. Dispersion of monensin sodium treatment solution: add 5% (W / V) light calcium carbonate, 2.0% (W / V) attapulgite, 2.0% (W / V) diatomaceous earth, and 0.25% (W / V) talc, and stir at 20 rpm for 60 min.

[0056] 3. Solid-liquid separation: put the dispersed monensin sodium treated liquid into the plate frame, adjust the air pressure to 0.4mpa, and 3 / plate and frame filtration volume was subjected to high pressure closed plate and frame filtration (the moisture content of the monensin sodium filter cake was controlled at 40%) to obtain a filtrate and a monensin sodium filter cake. After testing, the pH of the filtrate was 8.5 and the sodium ion content was 0.0101% (W / V).

[0057] 4. Filtrate purification: The filtrate is purified by the environmental protection system to form recyclable grey water with a COD of 35.

[0058] 5. Granulation: The filter cake of monensin sodium was crushed by a pulverizer, and 100% passed through a 24-mesh sieve; it was conveyed to a rotary extrusion granulator by a screw conveyor, with a feeding speed of 25 Hz, a rotary extrusion speed of 75 rpm, and a spheronization speed of 80 rpm to form spherical wet granules.

[0059] 6. Drying: The wet granules were vacuum-sucked into a fluidized bed dryer and dried for 50 min at an inlet air temperature of 150° C., an outlet air temperature of 50° C., and a wind speed of 140 Hz to obtain a monensin sodium premix with a moisture content of 5.2% (W / W), a monensin sodium content of 20% (W / W), and a sodium ion content of 0.779% (W / W).

[0060] Comparative Example 1

[0061] 1. Treatment of Monensin Fermentation Broth

[0062] 1.1 Heating inactivation, the conditions are as follows: a monensin fermentation broth with a solid content of 11% (W / W) and a monensin content of 4.5 g / 100 mL, without adding cellulase, is heated to 60°C for inactivation for 120 min;

[0063] 1.2 Sodium loading: Use 30 g / 100 mL NaOH solution to adjust the pH of the solution to 11, the molar ratio of sodium ions to monensin molecules in the solution is 0.14, and stir at 30 rpm for 120 min.

[0064] 2. Dispersion of monensin sodium treatment solution: add 8% (W / V) light calcium carbonate, 0.5% (W / V) attapulgite, 0.5% (W / V) diatomaceous earth, and 0.25% (W / V) talc, and stir at 30 rpm for 120 min.

[0065] 3. Solid-liquid separation: put the dispersed monensin sodium treated liquid into the plate frame, adjust the air pressure to 0.5mpa, and 3 / plate and frame filtration volume was subjected to high pressure closed plate and frame filtration (the moisture content of the monensin sodium filter cake was controlled at 30%) to obtain a filtrate and a monensin sodium filter cake. After testing, the pH of the filtrate was 8.5 and the sodium ion content was 0.01692% (W / V).

[0066] 4. Filtrate purification: The filtrate is purified by the environmental protection system to form recyclable grey water with a COD of 30.

[0067] 5. Granulation: The filter cake of monensin sodium was crushed by a pulverizer, and 100% passed through a 24-mesh sieve; it was conveyed to a rotary extrusion granulator by a screw conveyor, with a feeding speed of 30 Hz, a rotary extrusion speed of 90 rpm, and a spheronization speed of 90 rpm to form spherical wet granules.

[0068] 6. Drying: The wet granules were vacuum-sucked into a fluidized bed dryer and dried for 60 min at an inlet air temperature of 160° C., an outlet air temperature of 60° C., and a wind speed of 160 Hz to obtain a monensin sodium premix with a moisture content of 3.8% (W / W), a monensin sodium content of 20% (W / W), and a sodium ion content of 0.11% (W / W).

[0069] Comparative Example 2

[0070] 1. Treatment of Monensin Fermentation Broth

[0071] 1.1 Heating inactivation, the conditions are as follows: 0.5% (W / V) cellulase with an enzyme activity of 5637 U / g was added to a monensin fermentation broth with a solid content of 10% (W / W) and a monensin content of 4.5 g / 100 mL, and heated to 60°C for inactivation for 120 min;

[0072] 1.2 Sodium loading: Use 30 g / 100 mL NaOH solution to adjust the pH to 11, the molar ratio of sodium ions to monensin molecules is 0.14, and stir at 45 rpm for 60 min.

[0073] 2. Dispersion of monensin sodium treatment solution: add 5% (W / V) light calcium carbonate, 2.0% (W / V) attapulgite, 2.0% (W / V) diatomaceous earth, and 0.25% (W / V) talc, and stir at 20 rpm for 60 min.

[0074] 3. Solid-liquid separation: put the dispersed monensin sodium treated liquid into the plate frame, adjust the air pressure to 0.4mpa, and 3 / plate and frame filtration volume was subjected to high pressure closed plate and frame filtration (the moisture content of the monensin sodium filter cake was controlled at 40%) to obtain a filtrate and a monensin sodium filter cake. After testing, the pH of the filtrate was 8 and the sodium ion content was 0.00682% (W / V).

[0075] 4. Filtrate purification: The filtrate is purified by the environmental protection system to form recyclable grey water with a COD of 35.

[0076] 5. Granulation: The filter cake of monensin sodium was crushed by a pulverizer, and 100% passed through a 5-mesh sieve; it was conveyed to a rotary extrusion granulator by a screw conveyor, with a feeding speed of 20 Hz, a rotary extrusion speed of 45 rpm, and a spheronization speed of 60 rpm to form spherical wet granules.

[0077] 6. Drying: The wet granules were vacuum-sucked into a fluidized bed dryer and dried for 40 min at an inlet air temperature of 130° C., an outlet air temperature of 40° C., and a wind speed of 120 Hz to obtain a monensin sodium premix with a moisture content of 6% (W / W), a monensin sodium content of 20% (W / W), and a sodium ion content of 0.43% (W / W).

[0078] Comparative Example 3

[0079] 1. Treatment of Monensin Fermentation Broth

[0080] 1.1 Heating inactivation, the conditions are as follows: 0.5% (W / V) cellulase with an enzyme activity of 5637 U / g was added to a monensin fermentation broth with a solid content of 10% (W / W) and a monensin content of 4.5 g / 100 mL, and heated to 60°C for inactivation for 120 min;

[0081] 1.2 Sodium loading: Use 30 g / 100 mL NaOH solution to adjust the pH to 11, and use sodium chloride solution to supplement sodium ions to obtain a mixed solution, so that the molar ratio of sodium ions to monensin molecules in the mixed solution is 0.9, and stir at 45 rpm for 60 min.

[0082] 2. Dispersion of monensin sodium treatment solution: add 5% (W / V) light calcium carbonate, 2.0% (W / V) attapulgite, 2.0% (W / V) diatomaceous earth, and 0.25% (W / V) talc, and stir at 20 rpm for 60 min.

[0083] 3. Solid-liquid separation: put the dispersed monensin sodium treated liquid into the plate frame, adjust the air pressure to 0.4mpa, and 3 / plate and frame filtration volume was subjected to high pressure closed plate and frame filtration (the moisture content of the monensin sodium filter cake was controlled at 40%) to obtain a filtrate and a monensin sodium filter cake. After testing, the pH of the filtrate was 8 and the sodium ion content was 0.1012% (W / V).

[0084] 4. Filtrate purification: The filtrate is purified by the environmental protection system to form recyclable grey water with a COD of 35.

[0085] 5. Granulation: The filter cake of monensin sodium was crushed by a pulverizer, and 100% passed through a 5-mesh sieve; it was conveyed to a rotary extrusion granulator by a screw conveyor, with a feeding speed of 20 Hz, a rotary extrusion speed of 45 rpm, and a spheronization speed of 60 rpm to form spherical wet granules.

[0086] 6. Drying: The wet granules were vacuum-sucked into a fluidized bed dryer and dried for 40 min at an inlet air temperature of 130° C., an outlet air temperature of 40° C., and a wind speed of 120 Hz to obtain a monensin sodium premix with a moisture content of 6% (W / W), a monensin sodium content of 20% (W / W), and a sodium ion content of 0.501% (W / W).

[0087] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a monensin sodium premix, characterized in that: The following steps are involved: After the monensin fermentation broth was mixed with cellulase and inactivated, NaOH was added to adjust the pH to 8-11, and the ion solution system Na + -EDTANa2-BF4, forming a mixed solution, stirring to obtain a monensin sodium treatment solution; The monensin sodium treatment liquid is mixed with auxiliary materials, and the solid-liquid separation is performed to obtain a solid part, and the solid part is prepared to obtain a monensin sodium premix.

2. The preparation method according to claim 1, characterized in that: The content of monensin in the monensin fermentation liquid is 4-4.8 g / 100 mL.

3. The preparation method according to claim 1, characterized in that: The ratio of the cellulase to the monensin fermentation liquid is 0.1-1.0 g:100 mL, and the cell wall breaking and inactivation time is 60 min-180 min.

4. The preparation method according to claim 1, characterized in that: The Na + -EDTANa2-BF4 is composed of BF4, EDTANa2, NaOH solution and purified water; the weight volume ratio of BF4, EDTANa2, NaOH solution and purified water is 10-15g: 10-15g: 40-50mL: 100mL; the concentration of the NaOH solution is 30-40g / 100mL.

5. The preparation method according to claim 1, characterized in that: The volume ratio of the ionic solution system to the monensin fermentation liquid is 1.0-3.0:

100.

6. The preparation method according to claim 1, characterized in that: The stirring time is 60 min to 180 min, and the stirring speed is 30 to 45 rpm.

7. The preparation method according to claim 1, characterized in that: The auxiliary materials include light calcium carbonate, attapulgite, diatomaceous earth and talc.

8. The preparation method according to claim 7, characterized in that: The ratio of the light calcium carbonate to the sodium monensin treatment solution is 5-8 g:100 mL, the ratio of the attapulgite to the sodium monensin treatment solution is 0.5-2.0 g:100 mL; the ratio of the diatomaceous earth to the sodium monensin treatment solution is 0.5-2.0 g:100 mL; the ratio of the talc to the sodium monensin treatment solution is 0.25-0.5 g:100 mL.

9. The preparation method according to claim 1, characterized in that: The solid-liquid separation is filtration, and the filtration is plate and frame filter pressing.

10. The monensin sodium premix prepared by the preparation method according to any one of claims 1 to 9.

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