阅读说明：本技术 一种控缓释型mof骨架补钒剂的制备方法 (Preparation method of controlled-release MOF framework vanadium supplement ) 是由 姚志通 夏枚生 孙清平 于 2020-05-09 设计创作，主要内容包括：一种控缓释型MOF骨架补钒剂的制备方法,属于饲料添加剂领域,通过配置质量浓度3-5%的2-甲基咪唑溶液和3-10%的偏钒酸钠溶液,用蠕动泵缓慢将偏钒酸钠溶液滴入超声分散的2-甲基咪唑溶液中；静置老化0.5-3小时后转入具有内衬的高压反应釜,在100-140℃反应3-5小时后过滤干燥得到MOF骨架补钒剂前驱体；将前驱体以2-5℃/min的升温速率缓慢升温至200-400℃,自然冷却后得到含锡量5-10%的控缓释型MOF骨架补钒剂。本发明制备方法原理清晰,具有高孔隙率、低密度、大比表面积、孔道规则、孔径可调以及拓扑结构多样性和可裁剪性等优点,较好地解决了纳米粒子团聚和稳定性问题,适宜工业化生产,可为MOF材料在高新技术领域的应用提供新的途径和生长点。(A method for preparing a controlled slow release type MOF framework vanadium supplement agent belongs to the field of feed additives, and comprises the steps of preparing a 2-methylimidazole solution with the mass concentration of 3-5% and a sodium metavanadate solution with the mass concentration of 3-10%, and slowly dripping the sodium metavanadate solution into the ultrasonically dispersed 2-methylimidazole solution by using a peristaltic pump; standing and aging for 0.5-3 hours, transferring the mixture into a high-pressure reaction kettle with a lining, reacting for 3-5 hours at the temperature of 100 ℃ and 140 ℃, and filtering and drying to obtain an MOF framework vanadium supplement agent precursor; slowly heating the precursor to 200 ℃ and 400 ℃ at the heating rate of 2-5 ℃/min, and naturally cooling to obtain the controlled slow release MOF framework vanadium supplement agent with the tin content of 5-10%. The preparation method disclosed by the invention is clear in principle, has the advantages of high porosity, low density, large specific surface area, regular pore channels, adjustable pore diameter, diversity and tailorability of topological structures and the like, well solves the problems of nanoparticle aggregation and stability, is suitable for industrial production, and can provide a new path and a new growth point for the application of MOF materials in the high and new technical field.)

1. A preparation method of a controlled-release MOF framework vanadium supplement agent is characterized by comprising the following steps:

(1) preparing a 2-methylimidazole solution with the mass concentration of 3-5% and a sodium metavanadate solution with the mass concentration of 3-10%;

(2) slowly dripping the sodium metavanadate solution into the ultrasonically dispersed 2-methylimidazole solution by using a peristaltic pump;

(3) standing and aging for 0.5-3 hours, transferring the mixture into a high-pressure reaction kettle with a lining, reacting for 3-5 hours at the temperature of 100 ℃ and 140 ℃, and filtering and drying to obtain an MOF framework vanadium supplement agent precursor;

(4) slowly heating the precursor to 200 ℃ and 400 ℃ at the heating rate of 2-5 ℃/min, and naturally cooling to obtain the controlled slow release MOF framework vanadium supplement agent with the tin content of 5-10%.

Technical Field

The invention belongs to the field of feed additives, and particularly relates to a preparation method of a controlled slow-release MOF framework vanadium supplement.

Background

Vanadium was formally identified as one of the essential trace elements for humans and animals in the 70's of the 20 th century. Although the content of vanadium in animals is not very high, vanadium plays important and complex physiological roles in animal life activities, such as the stimulation of hematopoiesis, the inhibition of cholesterol synthesis, insulin-like action and the like. Vanadium is an essential trace element for the growth and development of the chickens, and the mass concentration of vanadium in each tissue of the chickens is relatively higher than that of vanadium in other animals. Pig, rabbit and mouse vanadium are mainly present in bones, liver and kidney, and the vanadium content in bones is highest. The commonly used feed additives are ammonium vanadate and the like, but have the defects of low absorptivity, large addition amount or high absorptivity but relatively high price and the like, so that the development of the novel high-efficiency vanadium additive has important significance for feed and animal husbandry in China.

The slow-release control system has selectivity and controllability on release positions, speed and modes of medicines, pesticides, fertilizers and spices, can realize targeted transmission and controlled slow release of target objects, improves the utilization rate and action effect of the target objects, and brings a new technical revolution to related industries through research and application of the slow-release control system. The controlled-release technology also shows huge application prospect and theoretical significance in the research and development aspect of feed additives, can promote the high performance and environmental friendliness of products, and can provide material and technical guarantee for the sustainable development of animal husbandry at a new level. The key of the controlled-release technology is the selection of a controlled-release carrier. The mineral material can be used as a miniature nano reactor and a carrier and a medium for manufacturing a nano structure assembly material because the pore diameter is small enough and the pore volume is large, so that the size effect and the surface effect of pores can be shown, but most of the mineral materials have small specific surface area and limited metal loading capacity, so that the addition amount is large.

Disclosure of Invention

The invention aims to provide a preparation method of a controlled-release type MOF framework vanadium supplement, aiming at the problems of complex production process, large particle size of products, difficult absorption by animal bodies, low bioavailability and the like of the traditional tin supplement.

The technical scheme of the invention is as follows: a preparation method of a controlled-release MOF framework vanadium supplement agent is characterized by comprising the following steps:

(1) preparing a 2-methylimidazole solution with the mass concentration of 3-5% and a sodium metavanadate solution with the mass concentration of 3-10%;

(2) slowly dripping the sodium metavanadate solution into the ultrasonically dispersed 2-methylimidazole solution by using a peristaltic pump;

(3) standing and aging for 0.5-3 hours, transferring the mixture into a high-pressure reaction kettle with a lining, reacting for 3-5 hours at the temperature of 100 ℃ and 140 ℃, and filtering and drying to obtain an MOF framework vanadium supplement agent precursor;

(4) slowly heating the precursor to 200 ℃ and 400 ℃ at the heating rate of 2-5 ℃/min, and naturally cooling to obtain the controlled slow release MOF framework vanadium supplement agent with the tin content of 5-10%.

The invention has the beneficial effects that: the preparation method of the controlled slow release type MOF framework vanadium supplement agent provided by the invention has clear principle of the preparation method, the MOF framework vanadium supplement agent has the advantages of high porosity, low density, large specific surface area, regular pore channels, adjustable pore diameter, diversity and tailorability of topological structure and the like, and is widely applied to the fields of catalysis, energy storage, separation and the like.

Detailed Description

The invention is further illustrated by the following examples: