阅读说明：本技术 畜禽用水溶型纳米单质硒的制备方法 (Preparation method of water-soluble nano elemental selenium for livestock and poultry ) 是由 杨彩梅 邵彦婕 李慧 刘金松 曾新福 孔随飞 于 2019-09-09 设计创作，主要内容包括：本发明公开了一种畜禽用水溶型纳米单质硒的制备方法,包括以下步骤：1)按质量分数分别称取亚硒酸盐、分散剂、还原剂及载体备用；2)将亚硒酸盐加入至水中溶解,搅拌均匀后备用；3)向步骤2)中加入分散剂,并持续搅拌至无色透明溶液变成红色溶液且颜色不再加深,然后停止搅拌；4)持续搅拌,加入还原剂溶液颜色逐渐变成红色,持续25min,搅拌至还原剂全部溶解后反应基本完成；5)向步骤4)的溶液中加入载体搅拌均匀,然后剪切均质。本发明制备的纳米单质硒,通过还原剂对亚硒酸钠进行还原,将剧毒物质转变为动物可利用的单质硒,丰富了单质硒的生产途径。并使用分散剂和载体,结合固体分散技术,制得稳定的纳米单质硒微囊。(The invention discloses a preparation method of water-soluble nano elemental selenium for livestock and poultry, which comprises the following steps: 1) respectively weighing selenite, a dispersant, a reducing agent and a carrier according to mass fractions for later use; 2) adding selenite into water to dissolve, and stirring uniformly for later use; 3) adding a dispersing agent into the step 2), continuously stirring until the colorless transparent solution becomes a red solution and the color is not deepened, and then stopping stirring; 4) continuously stirring, adding a reducing agent solution, gradually changing the color into red, continuously stirring for 25min until the reducing agent is completely dissolved, and basically completing the reaction; 5) adding the carrier into the solution obtained in the step 4), uniformly stirring, and then shearing and homogenizing. The nano elemental selenium prepared by the invention reduces sodium selenite by a reducing agent, so that highly toxic substances are converted into elemental selenium which can be utilized by animals, and the production way of the elemental selenium is enriched. And a dispersing agent and a carrier are used, and a solid dispersion technology is combined to prepare the stable nano elemental selenium microcapsule.)

1. A preparation method of water-soluble nano elemental selenium for livestock and poultry is characterized by comprising the following steps:

1) respectively weighing selenite, a dispersant, a reducing agent and a carrier according to mass fractions for later use;

2) adding selenite into water to dissolve, and stirring uniformly for later use;

3) adding a dispersing agent into the step 2), continuously stirring until the colorless transparent solution becomes a red solution and the color is not deepened, and then stopping stirring;

4) continuously stirring, adding a reducing agent solution, gradually changing the color into red, continuously stirring for 25min until the reducing agent is completely dissolved, and basically completing the reaction;

5) adding the carrier into the solution obtained in the step 4), uniformly stirring, and then shearing and homogenizing;

6) and (3) passing the homogenized mixture obtained in the step 5) through a centrifugal spraying system, adjusting spraying parameters, and drying to obtain nano selenium particles.

2. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 1, which is characterized in that: 1.0-2.0 parts of selenite, 0.2-0.8 part of dispersant, 2-3 parts of reducing agent and 40-70 parts of carrier which are weighed according to mass fraction in the step 1).

3. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 1, which is characterized in that: the pressure during stirring in the step 4) is 40-60MPa, the stirring time is 20-40min, and the stirring temperature is normal temperature.

4. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 1, which is characterized in that: the color of the wear-resistant selenium particles prepared in the step 5) is orange red to red, the moisture content is less than or equal to 8.0%, and the particle size of the nano selenium particles is 60-100 nm.

5. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 1, which is characterized in that: the selenite is one or more of sodium selenite, potassium selenite, and zinc selenite.

6. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 4, which is characterized in that: the dispersant is one or more of polyvinylpyrrolidone K30, sodium carboxymethylcellulose, sodium carboxymethyl starch, sucrose fatty acid ester, polysorbate, polyethylene glycol, sodium dodecyl benzene sulfonate, etc.

7. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 5, which is characterized in that: the reducing agent is one or more of tea polyphenol and L-ascorbic acid; the carrier is a water-soluble inert carrier.

8. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 1, which is characterized in that: the parameters of the spray drying system are that the air inlet temperature is 180-185 ℃, the air outlet temperature is 88-96 ℃, and the spray frequency is 420-450 HZ.

9. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 7, which is characterized in that: the selenite is sodium selenite, the dispersing agent is sodium carboxymethyl starch, the reducing agent is L-ascorbic acid, and the carrier is dextrin.

10. The method for preparing water-soluble nano elemental selenium for livestock and poultry according to claim 9, which is characterized in that: weighing 1.5 parts of sodium selenite, 2 parts of L-ascorbic acid, 0.5 part of sodium carboxymethyl starch and 40 parts of dextrin according to mass fraction.

Technical Field

The invention belongs to the technical field of feed additives, and particularly relates to a preparation method of water-soluble nano elemental selenium for livestock and poultry.

Background

The two forms of inorganic selenium and organic selenium are the main forms of selenium in nature, seleno-amino acid, seleno-nucleotide and selenium-enriched yeast are represented by organic selenium, and selenite and selenate are represented by inorganic selenium. Inorganic selenium sources are abundant, but because of strong toxicity and low absorption and utilization rate of animals and plants, organic selenium sources such as selenoprotein and other forms of selenium such as nano selenium are gradually abandoned in recent years.

Selenium is a necessary trace element for animal body, and the biggest limitation of its application is its toxicity. It is well recognized that selenium is more toxic than calcium and potassium. Moreover, the safety range between the effective amount and the toxic amount is narrower than that of calcium and potassium, so that the excessive amount is easy to cause, and compared with other selenium compounds, the elemental selenium (nano selenium) has the greatest advantage of low toxicity, namely, higher safety.

The electron spin resonance experiment proves that: the hydroxyl radical scavenging efficiency of the elemental selenium (nano selenium) is 5 times of that of sodium selenite. The comparative experiment proves that: under the condition of lower selenium dosage supplement, sodium selenite does not show the effects of inhibiting tumor and regulating immunity, but elemental selenium (nano selenium) can effectively inhibit tumor and can improve cellular immunity, humoral immunity and nonspecific phagocytosis.

The selenium content in animal body is generally 0.02-0.5mg/kg, wherein the total selenium content in muscle is the most, the selenium concentration in kidney is the highest, and the selenium deficiency of body can cause diseases such as myocardial necrosis and skeletal muscle pathological changes. Selenium is also a prosthetic group of glutathione peroxidase, and has irreplaceable effect on maintaining the antioxidant function of the body. Researches in recent years show that selenium has the effects of promoting growth, improving immunity and improving the quality of livestock and poultry products.

Disclosure of Invention

The invention provides a preparation method of water-soluble nano elemental selenium for livestock and poultry, which is non-toxic and has a good absorption effect, and aims to overcome the defects of the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of water-soluble nano elemental selenium for livestock and poultry comprises the following steps:

a preparation method of water-soluble nano elemental selenium for livestock and poultry comprises the following steps:

1) respectively weighing selenite, a dispersant, a reducing agent and a carrier according to mass fractions for later use;

2) adding selenite into water to dissolve, and stirring uniformly for later use;

3) adding a dispersing agent into the step 2), continuously stirring until the colorless transparent solution becomes a red solution and the color is not deepened, and then stopping stirring;

4) continuously stirring, adding a reducing agent solution, gradually changing the color into red, continuously stirring for 25min until the reducing agent is completely dissolved, and basically completing the reaction;

5) adding the carrier into the solution obtained in the step 4), uniformly stirring, and then shearing and homogenizing;

6) and (3) passing the homogenized mixture obtained in the step 5) through a centrifugal spraying system, adjusting spraying parameters, and drying to obtain nano selenium particles.

Preferably, 1.0-2.0 parts of selenite, 0.2-0.8 part of dispersant, 2-3 parts of reducing agent and 40-70 parts of carrier are weighed according to mass fraction in the step 1).

Preferably, the pressure during stirring in the step 4) is 40-60MPa, the stirring time is 20-40min, and the stirring temperature is normal temperature.

Preferably, the wear-resistant selenium particles prepared in the step 5) are orange red to red, the moisture content is less than or equal to 8.0%, and the particle size of the nano selenium particles is 60-100 nm.

Preferably, the selenite is one or more of sodium selenite, potassium selenite and zinc selenite.

Preferably, the dispersant is one or more of polyvinylpyrrolidone K30, sodium carboxymethylcellulose, sodium carboxymethyl starch, sucrose fatty acid ester, polysorbate, polyethylene glycol, sodium dodecyl benzene sulfonate, etc.

Preferably, the carrier is a water-soluble inert carrier.

Preferably, the parameters of the spray drying system are that the air inlet temperature is 180-185 ℃, the air outlet temperature is 88-96 ℃, and the spray frequency is 420-450 HZ.

Preferably, the selenite is sodium selenite, the dispersant is sodium carboxymethyl starch, the reducing agent is L-ascorbic acid, and the carrier is dextrin.

Preferably, 1.5 parts of sodium selenite, 2 parts of L-ascorbic acid, 0.5 part of sodium carboxymethyl starch and 40 parts of dextrin are weighed according to mass fraction.

In summary, the present invention has the following effects:

(1) the nano elemental selenium prepared by the invention reduces sodium selenite by a reducing agent, so that highly toxic substances are converted into elemental selenium which can be utilized by animals, and the production way of the elemental selenium is enriched. And a dispersing agent and a carrier are used, and a solid dispersion technology is combined to prepare the stable nano elemental selenium microcapsule; solves the defects of poor stability and easy ash generation of red elemental selenium. The reducing agent, the dispersing agent and the carrier are commonly used in food and medicine, cannot cause pollution, meets the industrial production condition, and has great technical advantages.

(2) The nano elemental selenium prepared by the invention has good water solubility at 25-37 ℃, can be dispersed in water automatically, and the solution is clear and transparent, and is still stable after being placed for 3-5 days according to concentration difference. The 5% water solution can be kept in water for 24h without precipitation, is stable and is suitable for drinking water of livestock and poultry. The nano-selenium particles are uniform and fine, and have large surface area. Has many surface atoms and unsaturated bonds, high surface activity, improved adhesion to gastrointestinal mucosa, easy absorption by animal intestinal tract, and high bioavailability.

(3) The nano elemental selenium prepared by the invention has good fluidity after being adsorbed by a carrier and spray-dried by microencapsulation treatment, good stability and no discoloration or agglomeration after being hermetically placed at 40 ℃ and normal temperature. Convenient to use, the fodder misce bene of being convenient for.

(4) The preparation process provided by the invention has the advantages of simple flow, easiness in reproduction, shorter production process time, low energy consumption and high efficiency. Compared with the traditional process for producing nano-selenium by culturing microorganisms or fungi, the process only needs 1/10 time for producing equivalent products, greatly improves the efficiency, can meet the modern large-scale culture requirement, and greatly reduces the energy consumption. In addition, the process adopts excessive reducing agent for production, can convert 100 percent of inorganic selenium into nano selenium, and the obtained final product has low toxicity and high safety; the used raw and auxiliary materials are common raw and auxiliary materials, so that the production and popularization are facilitated, and the cost is low.

Drawings

FIG. 1 is a schematic diagram of the construction of a centrifugal spray system of the present invention;

FIG. 2 is a schematic view of the structure of a drying tower according to the present invention;

FIG. 3 is a cross-sectional view of a drying tower of the present invention;

FIG. 4 is an exploded view of a drying tower of the present invention;

FIG. 5 is a schematic structural view of a heating element according to the present invention;

FIG. 6 is a first cross-sectional view of a heating element of the present invention;

FIG. 7 is a second cross-sectional view of the heating element of the present invention;

FIG. 8 is a schematic structural view of the cartridge of the present invention;

FIG. 9 is a partial schematic view of a spray assembly according to the present invention;

fig. 10 is a partial structural schematic view of a spray member of the present invention.

Detailed Description

In order to make the technical solutions of the present invention better understood, technical solutions in the embodiments of the present invention are clearly and completely described.