CN113735729A - Production process of feed-grade ferrous glutamate - Google Patents
Production process of feed-grade ferrous glutamate Download PDFInfo
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- CN113735729A CN113735729A CN202110884222.4A CN202110884222A CN113735729A CN 113735729 A CN113735729 A CN 113735729A CN 202110884222 A CN202110884222 A CN 202110884222A CN 113735729 A CN113735729 A CN 113735729A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C229/76—Metal complexes of amino carboxylic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
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Abstract
The invention relates to the technical field of ferrous glutamate production, and particularly discloses a production process of feed-grade ferrous glutamate. The process has low energy consumption, is green and environment-friendly, does not generate substances polluting the environment, and can ensure that all indexes such as product content, heavy metal and the like can meet the quality requirements of feed-grade ferrous glutamate; 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.
Description
Technical Field
The invention relates to the technical field of ferrous glutamate production, in particular to a production process of feed-grade ferrous glutamate.
Background
The trace elements are essential nutrients for animal growth and reproduction, mainly including copper, iron, manganese, zinc, cobalt, chromium, etc. and participate in a series of digestion, physiological and biological synthesis processes. At present, most of the inorganic trace elements such as ferrous sulfate are used in production practice, but the use of the inorganic trace elements has the following defects: firstly, the bioavailability is low, animals can only utilize 2-10% of the addition of inorganic trace elements generally, most of the inorganic trace elements are discharged out of the body, so that environmental pollution is caused, in addition, ionic metal elements are easily influenced by phytic acid, oxalic acid and cellulose in intestinal tracts, the absorption rate is further reduced, and meanwhile, the biological value is influenced by the antagonism among the elements; secondly, the inorganic trace elements can react with lipid and vitamins to accelerate the oxidation of fat and vitamins and are unfavorable for the growth and development of animals; thirdly, high-dose microelements (especially copper, zinc or iron and the like) generate a large amount of free radicals in the process of small intestine absorption and tissue utilization to cause circulating chain reaction, peroxide (such as hydrogen peroxide and the like) can be generated once in each circulation, the peroxide can cause peroxidation damage to DNA, RNA, mitochondrial membranes, endoplasmic reticulum membranes, cell membranes and the like, the integrity of the intestinal cell membranes is seriously damaged, intestinal villi is withered, cracked and dropped, the depth of crypts is increased, the number of absorption cells is reduced, the number of secretory cells is increased, the nutrition absorption capacity is reduced, the intestinal tract repair function is weakened, the growth of animals is hindered, the feed utilization rate is reduced, the disease resistance and the stress resistance are reduced, and the meat quality is reduced.
The organic trace element refers to a compound formed by combining trace elements and organic ligands through covalent bonds and ionic bonds, the organic ligands usually comprise proteins, small peptides, amino acids, organic acids such as gluconic acid and fumaric acid, polysaccharide derivatives and the like, and the stability coefficient of a chelate or complex formed by the amino acid serving as a ligand and a metal is favorable for absorption, transportation and utilization of the trace elements in the organic trace element. Amino acids reported as organic trace element ligands of feed include glycine, methionine, zinc hydroxy methionine, lysine and the like, but organic trace elements of different amino acid ligands have different physicochemical properties, particularly water solubility and acid resistance. If the water solubility is too high, the metal ions in the organic trace elements are separated from the ligands and exist in an ionic state in the presence of water, so that the water solubility is not different from that of the inorganic trace elements. In addition, due to the specific digestion and absorption process of animals, all feeds must be treated by the stomach firstly and then enter the intestinal tract to be digested and absorbed, and the pH value of chyme in the stomach is generally 3-4 as the stomach of the animals meets the digestion environment of pepsin, so that the organic trace elements are required to have strong acid resistance, and the metal ions can be ensured to enter the intestinal tract in an organic form and then be absorbed by the organism.
The application effect of the ferrous glutamate serving as the animal growth promoting feed additive is that the ferrous glutamate has low water solubility, strong acid resistance and high bioavailability, and the ferrous glutamate serving as the animal growth promoting feed additive has higher safety compared with other iron sources such as ferrous sulfate.
However, the existing production process for synthesizing ferrous glutamate is only limited to laboratory synthesis and is difficult to be applied to actual production, so that a production process of feed-grade ferrous glutamate is provided.
Disclosure of Invention
The invention aims to provide a production process of feed-grade ferrous 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 ferrous 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 iron, and controlling the molar ratio of the total iron 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 ferrous glutamate product in a cooling crystallization mode;
(5) obtaining solid-phase ferrous 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 ferrous glutamate by drying, controlling the surface moisture to be 0-1%, and screening to remove large-particle products to obtain qualified products.
Preferably, the iron in step (2) is ferrous sulfate or ferric hydroxide.
Feed-grade ferrous glutamate production equipment comprises a reaction kettle, wherein the reaction kettle provides a reaction space for feed-grade ferrous glutamate preparation, a delay injector is arranged at the upper end of the reaction kettle and slowly inputs ferric sulfate or ferric hydroxide into the reaction kettle, a crystallizer is arranged at the lower end of the reaction kettle, connecting rings are symmetrically arranged on the inner side wall of the crystallizer, filter screens are connected onto the connecting rings and are convenient to hang in the crystallizer, the filter screens are in a bag shape and are used for containing materials after reaction in the reaction kettle, an auxiliary separation assembly is arranged at the lower side of each filter screen and comprises a vibration plate, a connecting plate is fixedly connected to the lower end of the vibration plate, a first connecting column is fixedly connected to the lower end of the connecting plate, a second connecting column is fixedly connected to the bottom wall of the crystallizer and corresponds to the first connecting column, first spliced pole with be provided with the spring between the second spliced pole, the tip of first spliced pole insert in the spring, the connecting plate is right the spring plays limiting displacement, the interior material warp of reation kettle the filter screen filters the back liquid phase part and falls into the bottom of crystallizer, simultaneously material whereabouts in-process in the reation kettle can be beaten the vibration board, the vibration board receives to hit and hits the hitting reach the reaction force of spring and vibration drive material vibration on the filter screen, supplementary solid-liquid further separation, the crystallizer with be connected with the connecting pipe between the reation kettle, the connecting pipe be used for to transmission in the reation kettle mother liquor in the crystallizer.
Preferably, the buffer injector is a piston injector, the piston injector is fixedly penetrated through the upper wall of the reaction kettle, the ferrous sulfate or ferric hydroxide solution is input into the buffer injector to push the piston, and the buffer injector slowly injects the ferrous sulfate or ferric hydroxide solution into the reaction kettle.
Preferably, the outer side wall of the slow injector is fixedly connected with a limiting ring, the limiting ring is in contact with the upper wall of the reaction kettle, and the arrangement of the limiting ring further fixes the slow injector.
Preferably, the vibration board is the arc, and the arc is upwards protruding, protruding department with the bottom of filter screen contacts, and the arc is easily liquid phase part along its whereabouts more, and arc and pocket form the filter screen corresponds mutually, and its vibration top moves the filter screen drives the filter screen vibration, liquid phase part in the further filtering resultant.
The invention has the beneficial effects that: the preparation method comprises the steps of adopting a wet synthesis process, adopting ferrous sulfate or ferric hydroxide to react with glutamic acid in a solution, controlling the reaction temperature and the reaction time to obtain a solution of ferrous glutamate, cooling and crystallizing to obtain a ferrous glutamate product, drying, removing surface moisture, screening, and removing a large-particle product to obtain the feed-grade ferrous glutamate. The process has low energy consumption, is green and environment-friendly, does not generate substances polluting the environment, and can ensure that all indexes such as product content, heavy metal and the like can meet the quality requirements of feed-grade ferrous glutamate; 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 an enlarged view taken at A in FIG. 1 according to the present invention;
fig. 3 is a front view of the main structure of the present invention.
Wherein: 1-reaction kettle, 2-slow injector, 3-crystallizing tank, 4-connecting ring, 5-filter screen, 6-auxiliary separating component, 601-vibrating plate, 602-connecting plate, 603-first connecting column, 604-second connecting column, 605-spring, 7-connecting tube and 8-spacing 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. 1-3:
(1) adding deionized water and feed-grade glutamic acid into the reaction kettle 1;
(2) slowly inputting ferric sulfate into the reaction kettle 1 through a buffer injector 2, wherein the molar ratio of the total iron 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 ferrous glutamate chelate;
(4) stopping heating, opening an outlet valve of the reaction kettle 1, enabling a liquid phase part of materials in the reaction kettle 1 to fall into the bottom of the crystallization tank 3 after the materials are filtered by the filter screen 5, reducing the temperature in the crystallization tank 4 to 25 ℃ to obtain a ferrous glutamate product, striking the vibration plate 601 in the falling process of the materials in the reaction kettle 1, and vibrating the vibration plate 601 by the striking and the reaction force of the spring 605 to drive the materials on the filter screen 5 to vibrate to assist the further separation of solid and liquid; the mother liquor in the crystallization tank 3 is transferred into the reaction kettle 1 through the connecting pipe 7 to continue to react by the operation of the pump body;
(5) and (3) drying the solid phase by using a drying oven, removing the surface moisture of the solid-phase ferrous glutamate to make the surface moisture of the solid-phase ferrous glutamate be 0-1%, and screening to remove large-particle products to obtain qualified products.
Example 2:
please refer to fig. 1-3:
(1) adding deionized water and feed-grade glutamic acid into the reaction kettle 1;
(2) slowly inputting ferric sulfate into the reaction kettle 1 through a buffer injector 2, wherein the molar ratio of the total iron 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 ferrous glutamate chelate;
(4) stopping heating, opening an outlet valve of the reaction kettle 1, enabling a liquid phase part of materials in the reaction kettle 1 to fall into the bottom of the crystallization tank 3 after the materials are filtered by the filter screen 5, reducing the temperature in the crystallization tank 4 to 28 ℃ to obtain a ferrous glutamate product, striking the vibration plate 601 in the falling process of the materials in the reaction kettle 1, and vibrating the vibration plate 601 by the striking and the reaction force of the spring 605 to drive the materials on the filter screen 5 to vibrate to assist the further separation of solid and liquid; the mother liquor in the crystallization tank 3 is transferred into the reaction kettle 1 through the connecting pipe 7 to continue to react by the operation of the pump body;
(5) and (3) drying the solid phase by using a drying oven, removing the surface moisture of the solid-phase ferrous glutamate to make the surface moisture of the solid-phase ferrous glutamate be 0-1%, and screening to remove large-particle products to obtain qualified products.
Example 3:
please refer to fig. 1-3:
(1) adding deionized water and feed-grade glutamic acid into the reaction kettle 1;
(2) slowly inputting ferric sulfate into the reaction kettle 1 through a buffer injector 2, wherein the molar ratio of the total iron 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 ferrous glutamate chelate;
(4) stopping heating, opening an outlet valve of the reaction kettle 1, enabling a liquid phase part of materials in the reaction kettle 1 to fall into the bottom of the crystallization tank 3 after the materials are filtered by the filter screen 5, reducing the temperature in the crystallization tank 4 to 30 ℃ to obtain a ferrous glutamate product, striking the vibration plate 601 in the falling process of the materials in the reaction kettle 1, and vibrating the vibration plate 601 by the striking and the reaction force of the spring 605 to drive the materials on the filter screen 5 to vibrate to assist the further separation of solid and liquid; the mother liquor in the crystallization tank 3 is transferred into the reaction kettle 1 through the connecting pipe 7 to continue to react by the operation of the pump body;
(5) and (3) drying the solid phase by using a drying oven, removing the surface moisture of the solid-phase ferrous glutamate to make the surface moisture of the solid-phase ferrous glutamate be 0-1%, and screening to remove large-particle products to obtain qualified products.
Wherein:
feed-grade ferrous glutamate production equipment comprises a reaction kettle 1, wherein the reaction kettle 1 provides a reaction space for feed-grade ferrous glutamate preparation, the upper end of the reaction kettle 1 is provided with a slow injector 2, the slow injector 2 slowly inputs ferric sulfate or ferric hydroxide into the reaction kettle 1, the lower end of the reaction kettle 1 is provided with a crystallizing tank 3, the inner side wall of the crystallizing tank 3 is symmetrically provided with a connecting ring 4, the connecting ring 4 is connected with a filter screen 5, the connecting ring 4 is convenient to hang the filter screen 5 in the crystallizing tank 3, the filter screen 5 is in a bag shape, the filter screen 5 is used for containing materials which are reacted in the reaction kettle 1, the lower side of the filter screen 5 is provided with an auxiliary separating component 6, the auxiliary separating component 6 comprises a vibrating plate 601, the lower end of the vibrating plate 601 is fixedly connected with a connecting plate 602, the lower end of the connecting plate 602 is fixedly connected with a first connecting column 603, a second connecting column 604 is fixedly connected to the bottom wall of the crystallizing tank 3 at a position corresponding to the first connecting column 603, a spring 605 is provided between the first connecting post 603 and the second connecting post 604, the end of the first connecting column 603 is inserted into the spring 605, the connecting plate 602 limits the spring 605, the liquid phase part of the materials in the reaction kettle 1 falls into the bottom of the crystallizing tank 3 after being filtered by the filter screen 5, meanwhile, the materials in the reaction kettle 1 hit the vibrating plate 601 in the falling process, the vibrating plate 601 is vibrated by the hitting and the reaction force of the spring 605 to drive the materials on the filter screen 5 to vibrate, so as to assist the further separation of solid and liquid, the crystallizer 3 with be connected with connecting pipe 7 between the reation kettle 1, connecting pipe 7 be used for to transmit in the reation kettle 1 the mother liquor in the crystallizer 3.
Specifically, the slow injector 2 is a piston injector, the piston injector is fixedly penetrated through the upper wall of the reaction kettle 1, the ferrous sulfate or ferric hydroxide solution is input into the slow injector 2 to push the piston, and the slow injector 2 slowly injects the ferrous sulfate or ferric hydroxide solution into the reaction kettle 1.
Particularly, fixedly connected with spacing ring 8 on the lateral wall of slowly annotating ware 2, spacing ring 8 with reation kettle 1's upper wall contacts, setting up of spacing ring 8 is further to slowly annotate ware 2 plays the fixed action.
Particularly, vibration board 601 is the arc, and the arc is upwards protruding, protruding department with the bottom of filter screen 5 contacts, and the arc is easy liquid phase part more and follows its whereabouts, and arc and pocket form filter screen 5 corresponds mutually, and its vibration top moves filter screen 5 drives filter screen 5 vibrates, liquid phase part in the further filtering resultant.
The feed grade ferrous glutamate physicochemical properties prepared in relation to examples 1-3 are as follows:
| purity of the product% | Yield in terms of iron% | |
| Example 1 | 98.8 | 97.6 |
| Example 2 | 98.8 | 97.5 |
| Example 3 | 98.7 | 97.6 |
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.
Claims (6)
1. The production process of feed-grade ferrous glutamate is characterized by comprising the following steps: 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 iron, and controlling the molar ratio of the total iron 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 ferrous glutamate product in a cooling crystallization mode;
(5) obtaining solid-phase ferrous 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 ferrous glutamate by drying, controlling the surface moisture to be 0-1%, and screening to remove large-particle products to obtain qualified products.
2. The process for producing feed-grade ferrous glutamate according to claim 1, wherein: in the step (2), the iron is ferrous sulfate or ferrous hydroxide.
3. Production facility of feed level ferrous glutamate, its characterized in that: including reation kettle (1), the upper end of reation kettle (1) is provided with slowly annotating ware (2), slowly annotate ware (2) with ferric sulfate or ferric hydroxide slowly input extremely in reation kettle (1), the lower extreme of reation kettle (1) is provided with crystallizer (3), the symmetry is provided with go-between (4) on crystallizer (3) inside wall, be connected with filter screen (5) on go-between (4), filter screen (5) are the pocket form, the downside of filter screen (5) is provided with supplementary separator assembly (6), supplementary separator assembly (6) include vibration board (601), the lower extreme fixedly connected with connecting plate (602) of vibration board (601), the lower extreme fixedly connected with first spliced pole (603) of connecting plate (602), on the diapire of crystallizer (3) and with the corresponding position department fixedly connected with second spliced pole (604) of first spliced pole (603), first spliced pole (603) with be provided with spring (605) between second spliced pole (604), material warp in reation kettle (1) filter back liquid phase part falls into the bottom of crystallizer (3), simultaneously material whereabouts in-process can be hit in reation kettle (1) vibration board (601), vibration board (601) vibration drives material vibration on filter screen (5), supplementary solid-liquid further separation, crystallizer (3) with be connected with connecting pipe (7) between reation kettle (1), connecting pipe (7) be used for to transmission in reation kettle (1) mother liquor in the crystallizer (3).
4. The feed-grade ferrous glutamate production facility of claim 3, wherein: the slow injector (2) is a piston type injector which fixedly penetrates through the upper wall of the reaction kettle (1).
5. The feed-grade ferrous glutamate production facility of claim 4, wherein: fixedly connected with spacing ring (8) on the lateral wall of slowly annotating ware (2), spacing ring (8) with reation kettle (1) the upper wall contacts mutually.
6. The feed-grade ferrous glutamate production facility according to any one of claims 3-5, wherein: the vibrating plate (601) is an arc-shaped plate, the arc-shaped plate protrudes upwards, and the protruding part is in contact with the bottom end of the filter screen (5).
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