Composite acidifier as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of feed additives, and discloses a compound acidifier as well as a preparation method and application thereof. The preparation method of the composite acidifying agent comprises the following steps: evaporating and concentrating filtered yellow water, adding auxiliary materials into the concentrated yellow water, uniformly stirring, and carrying out spray drying; the air inlet temperature of the spray drying is 120-190 DEG C, the air outlet temperature of the spray drying is 80-110 DEG C, and the flow velocity of feed liquid is 80-100 mL / min. The composite acidifying agent for feed is prepared by taking the wine-brewing yellow water as a raw material through evaporation concentration, auxiliary material addition and spray drying, the development cost is low, the preparation process is simple and convenient, no complex reaction is needed, a large amount of yellow water can be consumed, reducing sugar and amino acid in the yellow water can serve as nutrient substances of feed, and alcohol and ester can improve the palatability of animals, so that the feed can be used as a feed additive. The prepared compound acidifier is higher in nutrient content and better in palatability.

Description

Technical Field

[0001] The invention relates to the technical field of feed additives, and in particular to a composite acidulant and a preparation method and application thereof. Background Art

[0002] Yellow water, also known as yellow pulp water, is a by-product of the liquor brewing process. In essence, after sorghum and other raw and auxiliary materials are added to the koji and undergo solid-state fermentation in the mud cellar, the fermented grains produce a large amount of free water after the microbial decomposition and metabolism. Some of the free water dissolves the acid, soluble starch, yeast extract, reducing sugar, tannin, alcohol and aroma precursors in the fermented grains, and settles together with the water in the fermented grains that is not used by microorganisms, and finally precipitates into a brown-yellow, slightly viscous turbid liquid. Yellow water is mainly composed of acids, aldehydes, alcohols, esters, sugars, nitrogen-containing compounds and a small amount of pigments and tannins and other organic substances, and its content varies slightly depending on the raw and auxiliary materials. At present, the most important and bulk use of yellow water is in the production of Luzhou-flavor liquor. This includes esterifying yellow water for serial distillation and aroma enhancement and filling the cellar, directly using yellow water to cultivate artificial cellar mud and maintain the cellar, blending liquor, and producing discarded yellow water liquor. The main problem with using yellow water directly in the production of Luzhou-flavor liquor is that it can only produce medium- and low-end liquors. In addition, the accumulation of excessive acid and tannin during repeated use of yellow water may cause the reconstruction of the brewing microbial flora, resulting in the deterioration of the quality of the entire liquor. Other applications are mostly at the experimental research stage due to small scale and high cost. Therefore, new technologies for the resource utilization of yellow water with low cost, good benefits and large-scale consumption should be developed based on the composition characteristics of yellow water. Summary of the invention

[0003] In order to solve the problems in the background technology, the present invention provides a composite acidifier and a preparation method and application thereof. Yellow water is prepared as a feed acidifier, which can realize the resource utilization of yellow water. At the same time, the beneficial microorganisms in the yellow water are added to the feed to improve the palatability.

[0004] To achieve the above object, the first technical solution adopted by the present invention is: The preparation method of the composite acidifier comprises: evaporating and concentrating the filtered yellow water, adding auxiliary materials to the concentrated yellow water, stirring evenly and then spray drying; the inlet air temperature of the spray drying is 120°C to 190°C, the outlet air temperature is 80°C to 110°C, and the feed liquid flow rate is 80 to 100 mL / min.

[0005] Preferably, the evaporation concentration temperature is 50-100° C., and the solid content of the yellow water after evaporation concentration is 15%-30%.

[0006] Preferably, the auxiliary material comprises any one or more of soluble starch, β-cyclodextrin, chitosan, and sodium carboxymethyl cellulose, and the amount of the auxiliary material added is 5% to 25% of the mass of the yellow water after filtration. After the auxiliary material is added, the solid content of the yellow water is 15% to 50%.

[0007] The auxiliary material of the present invention is used as an excipient and is added before spray drying. In order to overcome the defects of yellow water that has high viscosity and is difficult to form due to high sugar content, an appropriate amount of auxiliary material needs to be added. The amount of auxiliary material added is 5% to 25% of the mass of the yellow water after filtration. If the amount of auxiliary material added is less than 5%, the yellow water cannot be effectively spray dried to form a dry powder. If the amount of auxiliary material added is greater than 25%, the effective ingredient content of the composite acidifier obtained by spray drying is reduced, and the effect is reduced. Secondly, the addition of the auxiliary material can effectively increase the stability of the composite acidifier, prevent its oxidative decomposition, and improve the bioavailability.

[0008] The second technical solution adopted by the present invention is: The composite acidulant is obtained by any preparation method in the first technical solution.

[0009] The third technical solution adopted by the present invention is: The second technical solution is the use of the composite acidifier in animal feed.

[0010] Preferably, the animal comprises any one or more of poultry, piglets, beef cattle, dairy cows, and sheep.

[0011] Preferably, the added amount of the composite additive is 0.1% to 3% of the mass of the animal feed.

[0012] Compared with the prior art, the present invention has the following beneficial effects: The invention uses brewing yellow water as a raw material, and prepares a composite acidulant for feed by evaporation concentration, auxiliary material addition and spray drying. The invention has low development cost and simple preparation process, does not require complex reactions, and can consume yellow water in large quantities. Meanwhile, reducing sugars and amino acids in the yellow water can be used as nutrients for feed, and alcohols and esters can improve the palatability of animals. The prepared composite acidulant has higher nutrients and better palatability. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 The following are the actual product pictures of the experimental group and the control group in Experimental Example 2. DETAILED DESCRIPTION

[0014] The technical scheme in the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Although the representative embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that various modifications and changes can be made to the present invention without departing from the scope of the present invention. Therefore, the scope of the present invention should not be limited to the embodiments, but should be limited by the attached claims and their equivalents.

[0015] Example 1 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 50° C. to increase the solid content of the yellow water to 15%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 15 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the slurry treated in step (3) is spray dried, the inlet air temperature is set to 120°C, the outlet air temperature is set to 80°C, the slurry flow rate is set to 80 mL / min, and after cyclone separation, the sample is collected.

[0016] Example 2 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 70° C. to increase the solid content of the yellow water to 25%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 10 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 130° C., the outlet air temperature is set to 90° C., the liquid flow rate is set to 90 mL / min, and after cyclone separation, the sample is collected.

[0017] Example 3 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 80° C. to increase the solid content of the yellow water to 30%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 5 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the slurry treated in step (3) is spray dried, the inlet air temperature is set to 140° C., the outlet air temperature is set to 100° C., the slurry flow rate is set to 100 mL / min, and after cyclone separation, the sample is collected.

[0018] Example 4 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 90° C. to increase the solid content of the yellow water to 35%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 5 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 160° C., the outlet air temperature is set to 110° C., the liquid flow rate is set to 90 mL / min, and after cyclone separation, the sample is collected.

[0019] Example 5 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 80° C. to increase the solid content of the yellow water to 25%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 15 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 180°C, the outlet air temperature is set to 100°C, the liquid flow rate is set to 80 mL / min, and after cyclone separation, the sample is collected.

[0020] Example 6 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 90° C. to increase the solid content of the yellow water to 30%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 15 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 190°C~, the outlet air temperature is set to 110°C, the liquid flow rate is set to 90mL / min, and after cyclone separation, the sample is collected.

[0021] Example 7 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 60° C. to increase the solid content of the yellow water to 15%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 25 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 110°C~, the outlet air temperature is set to 85°C, the liquid flow rate is set to 80mL / min, and after cyclone separation, the sample is collected.

[0022] Example 8 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 70° C. to increase the solid content of the yellow water to 20%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 20 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 150°C, the outlet air temperature is set to 90°C, the liquid flow rate is set to 90 mL / min, and after cyclone separation, the sample is collected.

[0023] Example 9 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 80° C. to increase the solid content of the yellow water to 25%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 25 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 180°C, the outlet air temperature is set to 95°C, the liquid flow rate is set to 90 mL / min, and after cyclone separation, the sample is collected.

[0024] Example 10 This embodiment provides a method for preparing a composite acidulant, specifically: (1) Pre-treating yellow wine water with a coarse filter to remove coarse solid matter; (2) evaporating and concentrating the yellow water filtered in step (1) at a temperature of 70° C. to increase the solid content of the yellow water to 15%; (3) adding an auxiliary material to the solution of step (2), wherein the auxiliary material is soluble starch, and the amount added is 20 wt % based on the mass of the yellow water after filtration, and stirring evenly; (4) Before spray drying of yellow water, spray lubricant in the drying tower, the lubricant is Tween 80, and the concentration of Tween 80 is 0.5wt‰; (5) After spraying Tween, the liquid treated in step (3) is spray dried, the inlet air temperature is set to 170°C, the outlet air temperature is set to 95°C, the liquid flow rate is set to 90 mL / min, and after cyclone separation, the sample is collected.

[0025] Test Example 1 Composite Acidifier Performance Determination 1.1 Determination of moisture content The method for determining the moisture content of the acidifier shall refer to GB / T 606-2003 General method for determination of moisture in chemical reagents - Karl Fischer method.

[0026] Determination of water content in samples: Add a certain volume of methanol or solvent specified in the product standard to the reaction bottle (immerse the platinum electrode), and titrate to the endpoint with Karl Fischer reagent under stirring. Quickly add the amount of sample specified in the product standard, and titrate to the endpoint with Karl Fischer reagent.

[0027] The mass fraction of water in the sample, ω, is expressed in "%" and is calculated according to formula (1) or formula (2): ω=V1T / m×100…………………………(1) or ω=V1T / V2ρ×100……………………(2) Where: V1 is the volume of Karl Fischer reagent when titrating the sample, in milliliters (mL); T is the exact value of the titer of Karl Fischer reagent, in grams per milliliter (g / mL); m is the mass of the sample, in grams (g); V2 is the volume of the liquid sample, in milliliters (mL); ρ is the density of the liquid sample, in grams per milliliter (g / mL).

[0028] 1.2 Determination of the fineness of composite acidifier Weigh about 10 g of sample (accurate to 0.01 g), place it on a 1000 μm analytical sieve for sieving, and weigh the material under the sieve (accurate to 0.01 g). Calculate the percentage of the mass of the material under the sieve to the total mass of the sample. The difference between the results of two parallel sample measurements should not exceed 1%.

[0029] 1.3 Determination of pH value of 1% aqueous solution of composite acidifier After dissolving 1g of acidifier in 100g of water, the pH of the aqueous solution is measured, which corresponds to the H + concentration.

[0030] 1.4 Determination of total acid content of composite acidifier The method for determining the total acid content of the acidulant shall refer to the method for determining the total acid in food by the indicator method of acid-base titration in GB / T 12456-2008.

[0031] Preparation of sample: Take at least 200 g of representative sample, place it in a mortar or tissue pestle, add water equal to the sample, grind or mash it, mix well, and place it in a sealed glass container.

[0032] Analytical steps: (1) Take 25.00-50.00 mL of test solution to make it contain 0.035-0.070 g of acid and place it in a 250 mL conical flask. Add 40-60 mL of water and 0.2 mL of 1% phenolphthalein indicator, and titrate with 0.1 mol / L sodium hydroxide standard titration solution (if the sample acidity is low, 0.01 mol / L or 0.05 mol / L sodium hydroxide standard titration solution can be used) until it turns slightly red and does not fade for 30 seconds. Record the number of milliliters of 0.1 mol / L sodium hydroxide standard titration solution consumed (V1). The same sample to be tested must be measured twice. (2) For the blank test, replace the test solution with water. Follow the analytical step (1) below. Record the number of milliliters of 0.1 mol / L sodium hydroxide standard titration solution consumed (V2).

[0033] Analysis results: Total acid The total acid content is expressed as mass fraction X, and the value is expressed in grams per kilogram (g / kg).

[0034] ; Where: c: concentration of sodium hydroxide standard titration solution (moL / L); V1: Volume of sodium hydroxide standard titration solution consumed when titrating the test solution (mL); V2: Volume of sodium hydroxide standard titration solution consumed during blank test (mL); F: dilution factor of the test solution; m: sampling volume of the test sample (g or mL); K: Acid conversion coefficient: malic acid, 0.067; acetic acid, 0.060; tartaric acid, 0.075; citric acid, 0.064; citric acid, 0.070 (containing one molecule of crystal water); lactic acid, 0.090; hydrochloric acid, 0.036; phosphoric acid, 0.049.

[0035] The calculation result shall be accurate to the second decimal place. If the difference between the two measurement results is within the allowable range, the arithmetic mean of the two measurement results shall be taken and reported.

[0036] The above measurement results are shown in Table 1-2.

[0037] Table 1 Moisture content and fineness of composite acidulant in Example .

[0038] Table 2 pH value and total acid content of 1% aqueous solution of composite acidifier in Example .

[0039] 1.5 Acidifier composition test The main components of the acidulant are organic acids, alcohols, esters, aldehydes, sugars, microorganisms and other aromatic and flavoring substances. The organic acid content of yellow water is 3.5-5.5%, alcohols are 5.5-10.0%, esters are 1.5-3.6%, aldehydes are 0.15-1.5%, and amino acids are 0.15-0.18%. The specific content of the components contained in the acidulant prepared in Example 1 was further determined by high performance liquid chromatography. The test conditions of high performance liquid chromatography (HPLC) are as follows: the mobile phase is 5 mM H2SO4, the detector is an ultraviolet detector, the detection wavelength is 210 nm, the flow rate is 0.6 mL / min, the injection volume is 20 μL, and the column temperature is 50 °C. The standard substance retention time, linear equation and correlation coefficient of each organic acid are shown in Table 3, the standard substance retention time, linear equation and correlation coefficient of each alcohol and ester are shown in Table 4, and the main substance content of the detected acidulant is shown in Table 5.

[0040] Table 3 Retention time, linear equation and correlation coefficient of standard substances of organic acids (HPLC) .

[0041] Table 4 Retention time, linear equation and correlation coefficient of standard substances of alcohols and esters (GC) .

[0042] Table 5 Content of main substances in acidifier .

[0043] The reducing sugars and amino acids in the acidifier can be used as nutrients in feed, and the alcohols and esters can improve the palatability of animals.

[0044] Test Example 2 The composite acidifier prepared in Example 1 was used as the experimental group, and the following control groups were set up at the same time. The control groups had the following differences compared with the experimental groups: control group 1, no auxiliary materials were added; control group 2, 3% auxiliary materials were added; control group 3, 30% auxiliary materials were added.

[0045] The actual pictures of the products in the experimental group and control group 1-3 are as follows Figure 1 shown. Figure 1 In the figure, a is control group 1, b is control group 2, c is experimental group, and d is control group 3.

[0046] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that the technical solutions described in the above embodiments may still be modified, or some or all of the technical features thereof may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. Preparation method of composite acidifier, It is characterized in that The method comprises: evaporating and concentrating the filtered yellow water, adding auxiliary materials to the concentrated yellow water, stirring evenly and then spray drying; the inlet air temperature of the spray drying is 120°C to 190°C, the outlet air temperature is 80°C to 110°C, and the feed liquid flow rate is 80 to 100 mL / min.

2. The preparation method according to claim 1, It is characterized in that The evaporation concentration temperature is 50-100° C., and the solid content of the yellow water after evaporation concentration is 15%-30%.

3. The preparation method according to claim 1, It is characterized in that The auxiliary material comprises any one or more of soluble starch, beta-cyclodextrin, chitosan, and sodium carboxymethyl cellulose. The amount of auxiliary material added is 5% to 25% of the mass of the yellow water after filtration. After the auxiliary material is added, the solid content of the yellow water is 15% to 50%.

4. A composite acidulant obtained by the preparation method according to any one of claims 1 to 3.

5. Use of the composite acidulant as claimed in claim 4 in animal feed.

6. The use according to claim 5, It is characterized in that The animals include any one or more of poultry, piglets, beef cattle, dairy cows, and sheep.

7. The use according to claim 6, It is characterized in that The added amount of the composite additive is 0.1% to 3% of the mass of the animal feed.

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