阅读说明：本技术 饲料级谷氨酸锌的生产工艺 (Production process of feed-grade zinc glutamate ) 是由 邵勇杰 吴兵 李达昌 吕宗良 于 2021-08-03 设计创作，主要内容包括：本发明涉及谷氨酸锌生产技术领域,具体公开了饲料级谷氨酸锌的生产工艺,采用湿法合成工艺,采用锌与谷氨酸在溶液中进行反应,通过控制反应温度、反应时间,得到谷氨酸锌的溶液,通过冷却结晶得到谷氨酸锌产物,经过干燥,除去表面水分,再经过筛分,除去大颗粒产物,得到饲料级谷氨酸锌。工艺能耗低,绿色环保,不产生对环境污染物质,且产品含量、重金属等各项指标均能达到饲料级谷氨酸锌质量要求；由于生产过程只需要升温及搅拌,不需要超声等复杂操作,设备成本小；合成过程在水中进行,无有害副产物产生,母液可循环使用,不需要采用有机溶剂萃取,工艺绿色环保,后处理简单,无三废产生；本合成工艺环保、经济、高效。(The invention relates to the technical field of zinc glutamate production, and particularly discloses a production process of feed-grade zinc glutamate. The process has low energy consumption, is green and environment-friendly, does not generate substances polluting the environment, and can meet the quality requirements of feed-grade zinc glutamate on the product content, heavy metals and other indexes; the production process only needs heating and stirring, and complex operations such as ultrasound and the like are not needed, so that the equipment cost is low; the synthesis process is carried out in water, no harmful by-product is generated, the mother solution can be recycled, organic solvent extraction is not needed, the process is green and environment-friendly, the post-treatment is simple, and no three wastes are generated; the synthesis process is environment-friendly, economical and efficient.)

1. The production process of feed-grade zinc glutamate is characterized by comprising the following steps of: the production process comprises the following steps:

(1) adding deionized water or mother liquor into the reaction kettle;

(2) adding feed-grade glutamic acid, stirring, heating to 55-65 ℃, slowly adding zinc, and controlling the molar ratio of the total zinc content to the glutamic acid to be 1: 1;

(3) after the feeding is finished, continuously heating, controlling the reaction temperature to be 75-85 ℃, and preserving the temperature for 30min to ensure that the raw materials are fully reacted to generate a target product;

(4) stopping heating, transferring the materials in the reaction kettle into a crystallizing tank, reducing the temperature of the materials to 25-30 ℃, and obtaining a zinc glutamate product in a cooling crystallization mode;

(5) obtaining solid-phase zinc glutamate through a centrifugal or filter pressing separation mode, and recycling the separated liquid phase as mother liquor;

(6) removing the surface moisture of the solid-phase zinc glutamate through drying, controlling the surface moisture to be 0-1%, and screening to remove large-particle products to obtain qualified products.

2. The production process of feed-grade zinc glutamate according to claim 1, characterized in that: in the step (2), the zinc can be one or more of zinc oxide, zinc hydroxide, zinc carbonate or zinc derivative.

3. Production facility of feed grade zinc glutamate which characterized in that: including reation kettle (1), the upper end of reation kettle (1) sets up the opening, and its opening part sets up first closing cap (2), the opening side of reation kettle (1) still is provided with slowly annotates ware (3), slowly annotate ware (3) and be used for slowly adding reation kettle (1) with zinc in, the lower extreme delivery outlet of reation kettle (1) is connected with the inlet port of crystallizer (4), the delivery outlet of crystallizer (4) is connected with the inlet port of drying cabinet (9), and the material gets into after accomplishing the reaction in reation kettle (1) crystallizer (4) crystallization, the crystallization part gets into through the drying obtain feed level zinc glutamate in drying cabinet (9).

4. The production facility of feed-grade zinc glutamate according to claim 3, characterized in that: slowly annotate ware (3) including slowly annotating pipe (301), slowly annotate pipe (301) run through in the upper wall of reation kettle (1), just the output of slowly annotating pipe (301) is the throat, under no exogenic action, the material is the state of stewing in slowly annotating pipe (301), the inside sliding connection of slowly annotating pipe (301) has pressure plug (302), the upper end opening part of slowly annotating pipe (301) can be dismantled and be connected with second closing cap (303), second closing cap (303) run through there is first connecting pipe (304), through to input malleation messenger in first connecting pipe (304) pressure plug (302) move down the extrusion zinc extremely in reation kettle (1).

5. The production facility of feed-grade zinc glutamate according to claim 4, characterized in that: install positive press (5) on the lateral wall of crystallizer (4), crystallizer (4) with be connected with second connecting pipe (6) between drying cabinet (9), be provided with filter screen (7) in second connecting pipe (6).

6. The production facility of feed-grade zinc glutamate according to claim 4, characterized in that: reation kettle (1) with be connected with third connecting pipe (8) between crystallizer (4), install the pump body on third connecting pipe (8), will through pump body work mother liquor follows in crystallizer (4) third connecting pipe (8) are taken back extremely in reation kettle (1).

7. The production facility of feed-grade zinc glutamate according to claim 4, characterized in that: the outside of slowly annotating pipe (301) is provided with the reinforcement subassembly, the reinforcement subassembly includes go-between (12), go-between (12) fixed connection in slowly annotate on the lateral wall of pipe (301), go-between (12) with be connected with bracing piece (10) between the upper wall of reation kettle (1).

8. The production facility of feed-grade zinc glutamate according to claim 4, characterized in that: a cooling jacket (11) is arranged outside the crystallization tank (4), and cold fluid is introduced into the cooling jacket (11) to reduce the temperature in the crystallization tank (4).

Technical Field

The invention relates to the technical field of zinc glutamate production, in particular to a production process of feed-grade zinc glutamate.

Background

The use of zinc glutamate to replace other zinc sources has been proven to have higher safety and antibacterial activity, reduce the toxic and side effects of high zinc on animals, and the Chinese patent, the granted publication number is: CN101785534B discloses application of zinc glutamate or derivatives thereof as animal growth promoting feed additives, wherein the technical scheme refers to the application effect of the zinc glutamate or derivatives thereof as the animal growth promoting feed additives, the zinc glutamate has low water solubility, strong acid resistance and high bioavailability, the zinc glutamate is used as the growth promoting feed additives, and has higher safety and antibacterial activity compared with other zinc sources (including zinc oxide, basic zinc chloride, zinc glycinate and the like), the addition amount of zinc ions can be reduced by 80-90%, the production cost can be reduced, the environmental pollution can be reduced, and the toxic and side effects of high zinc on animals can be reduced.

However, the existing production process for synthesizing zinc glutamate is only limited to laboratory synthesis, the synthesis mode adopts a microwave synthesis method or organic solvent extraction, the energy consumption is high, the pollution is large, and the process is difficult to be applied to actual production, so that the production process of feed-grade zinc glutamate is provided.

Disclosure of Invention

The invention aims to provide a production process of feed-grade zinc glutamate and a manufacturing process and equipment thereof, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: the production process of feed-grade zinc glutamate comprises the following steps:

(1) adding deionized water or mother liquor into the reaction kettle;

(2) adding feed-grade glutamic acid, stirring, heating to 55-65 ℃, slowly adding zinc, and controlling the molar ratio of the total zinc content to the glutamic acid to be 1: 1;

(3) after the feeding is finished, continuously heating, controlling the reaction temperature to be 75-85 ℃, and preserving the temperature for 30min to ensure that the raw materials are fully reacted to generate a target product;

(4) stopping heating, transferring the materials in the reaction kettle into a crystallizing tank, reducing the temperature of the materials to 25-30 ℃, and obtaining a zinc glutamate product in a cooling crystallization mode;

(5) obtaining solid-phase zinc glutamate through a centrifugal or filter pressing separation mode, and recycling the separated liquid phase as mother liquor;

(6) removing the surface moisture of the solid-phase zinc glutamate through drying, controlling the surface moisture to be 0-1%, and screening to remove large-particle products to obtain qualified products.

Preferably, the zinc in step (2) may be one or more of an oxide, a hydroxide, a carbonate or a derivative thereof.

Feed-grade zinc glutamate production equipment comprises a reaction kettle, wherein the reaction kettle provides a reaction space for glutamic acid and zinc, the upper end of the reaction kettle is provided with an opening, the opening part of the reaction kettle is provided with a first sealing cover, the opening is an addition port of glutamic acid, a buffer injector is arranged beside the opening of the reaction kettle and used for slowly adding zinc into the reaction kettle, a lower end output port of the reaction kettle is connected with an inlet port of a crystallization tank, a material can automatically enter the crystallization tank under the action of gravity by opening a lower end output port valve of the reaction kettle, an output port of the crystallization tank is connected with an inlet port of a drying box, the material enters the crystallization tank for crystallization after reaction in the reaction kettle, a crystallized part enters the drying box and is dried to obtain feed-grade zinc glutamate, and the feed-grade zinc glutamate preparation is completed by matching with a zinc glutamate wet synthesis process, the method has the advantages of replacing complex operations such as ultrasound and the like, along with low equipment cost, and no harmful by-products generated during the synthesis process in water, so that the preparation of the zinc glutamate is environment-friendly, economical and efficient, and is suitable for industrial production.

Preferably, the slow filling device comprises a slow filling pipe, the slow filling pipe penetrates through the upper wall of the reaction kettle, the output end of the slow filling pipe is a necking, the material in the slow filling pipe is in a standing state under the action of no external force, a press plug is connected inside the slow filling pipe in a sliding mode, the press plug can be used in a sliding mode through cooperation of a sliding block and a sliding way, a strip-shaped sliding way is formed in the inner side wall of the slow filling pipe, the sliding block is connected to the outer side wall of the press plug, therefore, the press plug can stably move in the slow filling pipe, a second sealing cover is detachably connected to an opening at the upper end of the slow filling pipe, a first connecting pipe penetrates through the second sealing cover, the press plug can move downwards to the inside of the reaction kettle through inputting positive pressure into the first connecting pipe, the second sealing cover is opened, and liquid zinc oxide is added into the slow filling pipe, and closing the second closing cover, starting an external press, wherein proper pressure input can be selected according to the requirement of injection speed, the press plug slowly moves downwards under the action of air pressure, and the liquid zinc oxide in the slow injection pipe is slowly added into the reaction kettle, so that glutamic acid and zinc react more fully.

Preferably, install positive press on the lateral wall of crystallizer, the crystallizer with be connected with the second connecting pipe between the drying cabinet, be provided with the filter screen in the second connecting pipe, through positive press work, can with crystal in the crystallizer blows in the drying cabinet, the crystal is at the entering in-process, the process the second connecting pipe reaches the filter screen, through filter screen filter-pressing, the bold crystal becomes the fritter crystal and gets into in the drying cabinet, promote the finished product qualification rate.

Preferably, reation kettle with be connected with the third connecting pipe between the crystallizer, install the pump body on the third connecting pipe, will through pump body work mother liquor follows in the crystallizer the third connecting pipe is taken back to in the reation kettle, mother liquor recycles, saves the raw materials and does benefit to the environmental protection simultaneously.

Preferably, the outside of slowly annotating the pipe is provided with the reinforcement subassembly, the reinforcement subassembly includes the go-between, the go-between fixed connection in slowly annotate on the lateral wall of pipe, the go-between with be connected with the bracing piece between reation kettle's the upper wall, the bracing piece is right the go-between plays supporting role, makes slowly annotate the stable connection of pipe in reation kettle's upper wall.

Preferably, a cooling jacket is arranged outside the crystallization tank, and cold fluid is introduced into the cooling jacket to reduce the temperature in the crystallization tank, so that crystallization is facilitated.

The invention has the beneficial effects that: the preparation method comprises the steps of adopting a wet synthesis process, adopting zinc oxide, hydroxide, carbonate or derivative to react with glutamic acid in a solution, controlling reaction temperature and reaction time to obtain a zinc glutamate solution, cooling and crystallizing to obtain a zinc glutamate product, drying, removing surface moisture, screening, and removing large-particle products to obtain feed-grade zinc glutamate. The process has low energy consumption, is green and environment-friendly, does not generate substances polluting the environment, and can meet the quality requirements of feed-grade zinc glutamate on the product content, heavy metals and other indexes; the production process only needs heating and stirring, and complex operations such as ultrasound and the like are not needed, so that the equipment cost is low; the synthesis process is carried out in water, no harmful by-product is generated, the mother solution can be recycled, organic solvent extraction is not needed, the process is green and environment-friendly, the post-treatment is simple, and no three wastes are generated; the synthesis process is environment-friendly, economical and efficient.

Drawings

FIG. 1 is a sectional view of the main structure of the present invention;

FIG. 2 is a front view of the main structure of the present invention;

FIG. 3 is an enlarged view taken at A in FIG. 1 according to the present invention;

FIG. 4 is a schematic view of a structure of a buffer according to the present invention;

fig. 5 is a schematic structural view of the drying box of the present invention.

Wherein: 1-reaction kettle, 2-first closing cover, 3-slow injector, 301-slow injector, 302-press plug, 303-second closing cover, 304-first connecting pipe, 4-crystallizing tank, 5-positive press, 6-second connecting pipe, 7-filter screen, 8-third connecting pipe, 9-drying box, 10-support rod, 11-cooling jacket and 12-connecting ring.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1:

please refer to fig. 1-5:

(1) opening the first sealing cover 2, adding deionized water and feed-grade glutamic acid into the reaction kettle 1, and then closing the first sealing cover 2;

(2) opening the second closing cover 303, adding a zinc oxide solution into the slow filling pipe 301, closing the second closing cover 303, and inputting positive pressure into the first connecting pipe 304 to enable the press plug 302 to move downwards to press zinc oxide into the reaction kettle 1, wherein the molar ratio of the total zinc content to glutamic acid is 1: 1, stirring and heating to 55 ℃ in a reaction kettle 1;

(3) continuously heating, controlling the reaction temperature to be 75 ℃, and keeping the temperature for 30min to ensure that the raw materials are fully reacted to generate the zinc glutamate chelate;

(4) stopping heating, opening a valve at the output port of the reaction kettle 1, transferring the materials into the crystallization tank 4 under the action of gravity, and introducing cold fluid into the cooling jacket 11 to reduce the temperature in the crystallization tank 4 to 25 ℃ to obtain a zinc glutamate product;

(5) pumping the mother liquor in the crystallization tank 4 back into the reaction kettle 1 along a third connecting pipe 8 for recycling through the work of a pump body, blowing crystals in the crystallization tank 4 into a drying box 9 through a positive pressure machine 5, passing through a second connecting pipe 6, filtering through a filter screen 7, and then entering the drying box 9;

(6) drying the crystal through a drying box 9, removing the surface moisture of the solid-phase zinc glutamate to 0-1%, opening a door of the drying box 9, taking out the product, and screening to remove large-particle products to obtain qualified products.

Example 2:

please refer to fig. 1-5:

(1) opening the first sealing cover 2, adding deionized water and feed-grade glutamic acid into the reaction kettle 1, and then closing the first sealing cover 2;

(2) opening the second closing cover 303, adding a zinc oxide solution into the slow filling pipe 301, closing the second closing cover 303, and inputting positive pressure into the first connecting pipe 304 to enable the press plug 302 to move downwards to press zinc oxide into the reaction kettle 1, wherein the molar ratio of the total zinc content to glutamic acid is 1: 1, stirring and heating to 60 ℃ in a reaction kettle 1;

(3) continuously heating, controlling the reaction temperature to 80 ℃, and keeping the temperature for 30min to ensure that the raw materials are fully reacted to generate the zinc glutamate chelate;

(4) stopping heating, opening a valve at the output port of the reaction kettle 1, transferring the materials into the crystallization tank 4 under the action of gravity, and introducing cold fluid into the cooling jacket 11 to reduce the temperature in the crystallization tank 4 to 28 ℃ to obtain a zinc glutamate product;

(5) pumping the mother liquor in the crystallization tank 4 back into the reaction kettle 1 along a third connecting pipe 8 for recycling through the work of a pump body, blowing crystals in the crystallization tank 4 into a drying box 9 through a positive pressure machine 5, passing through a second connecting pipe 6, filtering through a filter screen 7, and then entering the drying box 9;

(6) drying the crystal through a drying box 9, removing the surface moisture of the solid-phase zinc glutamate to 0-1%, opening a door of the drying box 9, taking out the product, and screening to remove large-particle products to obtain qualified products.

Example 3:

please refer to fig. 1-5:

(1) opening the first sealing cover 2, adding deionized water and feed-grade glutamic acid into the reaction kettle 1, and then closing the first sealing cover 2;

(2) opening the second closing cover 303, adding a zinc oxide solution into the slow filling pipe 301, closing the second closing cover 303, and inputting positive pressure into the first connecting pipe 304 to enable the press plug 302 to move downwards to press zinc oxide into the reaction kettle 1, wherein the molar ratio of the total zinc content to glutamic acid is 1: 1, stirring and heating to 65 ℃ in a reaction kettle 1;

(3) continuously heating, controlling the reaction temperature to be 85 ℃, and keeping the temperature for 30min to ensure that the raw materials are fully reacted to generate the zinc glutamate chelate;

(4) stopping heating, opening a valve at the output port of the reaction kettle 1, transferring the materials into the crystallization tank 4 under the action of gravity, and introducing cold fluid into the cooling jacket 11 to reduce the temperature in the crystallization tank 4 to 30 ℃ to obtain a zinc glutamate product;

(5) pumping the mother liquor in the crystallization tank 4 back into the reaction kettle 1 along a third connecting pipe 8 for recycling through the work of a pump body, blowing crystals in the crystallization tank 4 into a drying box 9 through a positive pressure machine 5, passing through a second connecting pipe 6, filtering through a filter screen 7, and then entering the drying box 9;

(6) drying the crystal through a drying box 9, removing the surface moisture of the solid-phase zinc glutamate to 0-1%, opening a door of the drying box 9, taking out the product, and screening to remove large-particle products to obtain qualified products.

Wherein:

feed-grade zinc glutamate production equipment comprises a reaction kettle 1, wherein the reaction kettle 1 provides a reaction space for glutamic acid and zinc, the upper end of the reaction kettle 1 is provided with an opening, the opening part of the reaction kettle 1 is provided with a first sealing cover 2, the opening is an addition port of glutamic acid, a buffer injector 3 is further arranged beside the opening of the reaction kettle, the buffer injector 3 is used for slowly adding zinc into the reaction kettle 1, the lower end output port of the reaction kettle 1 is connected with the inlet port of a crystallization tank 4, materials can automatically enter the crystallization tank 4 under the action of gravity by opening the lower end output port valve of the reaction kettle 1, the output port of the crystallization tank 4 is connected with the inlet port of a drying box 9, the materials enter the crystallization tank 4 for crystallization after reaction in the reaction kettle, the crystallized parts enter the drying box 9 and are dried to obtain feed-grade zinc glutamate, and the equipment is matched with a zinc glutamate wet synthesis process, the preparation of feed-grade zinc glutamate is completed, complex operations such as ultrasound and the like are replaced, the equipment cost is low, the synthesis process is carried out in water, and no harmful byproducts are generated, so that the preparation of the zinc glutamate is environment-friendly, economic and efficient, and is suitable for industrial production.

Specifically, the slow injector 3 includes a slow injection pipe 301, the slow injection pipe 301 penetrates through the upper wall of the reaction kettle 1, the output end of the slow injection pipe 301 is a throat, the material in the slow injection pipe 301 is in a standing state under the action of no external force, the interior of the slow injection pipe 301 is slidably connected with a press plug 302, the press plug 302 can be used in a sliding manner by matching a slide block and a slide way, a strip-shaped slide way is arranged on the inner side wall of the slow injection pipe 301, the slide block is connected to the outer side wall of the press plug 302, so that the press plug 302 can stably move in the slow injection pipe 301, the opening at the upper end of the slow injection pipe 301 is detachably connected with a second sealing cover 303, the second sealing cover 303 penetrates through a first connecting pipe 304, the press plug 302 can move downwards to press zinc into the reaction kettle 1 by inputting positive pressure into the first connecting pipe 304, the second sealing cover 303 is opened, adding liquid zinc oxide into the slow injection pipe 301, closing the second closing cover 303, and starting an external press, wherein a proper pressure can be selected for input according to the requirement of the injection speed, the press plug 302 slowly moves downwards under the action of air pressure, the liquid zinc oxide in the slow injection pipe 301 is slowly added into the reaction kettle 1, and the glutamic acid and the zinc react more fully through slow addition.

Particularly, install positive press 5 on the lateral wall of crystallizer 4, crystallizer 4 with be connected with second connecting pipe 6 between the drying cabinet 9, be provided with filter screen 7 in the second connecting pipe 6, through positive press 5 work, can with crystal in the crystallizer 4 blows in the drying cabinet 9, the crystal is at the entering in-process, the process second connecting pipe 6 reaches filter screen 7, through filter screen 7 filter-pressing, the bold crystal becomes the fritter crystal and gets into in the drying cabinet 9, promote the finished product qualification rate.

Particularly, reation kettle 1 with be connected with third connecting pipe 8 between crystallizer 4, install the pump body on the third connecting pipe 8, will through pump body work mother liquor follows in crystallizer 4 third connecting pipe 8 is taken back extremely in reation kettle 1, mother liquor recycles, saves raw materials and does benefit to the environmental protection simultaneously.

Specifically, a reinforcing component is arranged outside the slow filling pipe 301, the reinforcing component includes a connecting ring 12, the connecting ring 12 is fixedly connected to the outer side wall of the slow filling pipe 301, a supporting rod 10 is connected between the connecting ring 12 and the upper wall of the reaction kettle 1, and the supporting rod 10 supports the connecting ring 12, so that the slow filling pipe 301 is stably connected to the upper wall of the reaction kettle 1.

Specifically, a cooling jacket 11 is provided outside the crystallization tank 4, and a cold fluid is introduced into the cooling jacket 11 to lower the temperature in the crystallization tank 4, thereby facilitating crystallization.

The feed grade zinc glutamate prepared in relation to examples 1-3 had the following physico-chemical properties:

	purity of the product%	Percentage of zinc in percent
			Example 1	98.5	97.9
Example 2	98.6	98.3
			Example 3	98.5	97.8

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.