CN107698455A - A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process - Google Patents
A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process Download PDFInfo
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- CN107698455A CN107698455A CN201710984917.3A CN201710984917A CN107698455A CN 107698455 A CN107698455 A CN 107698455A CN 201710984917 A CN201710984917 A CN 201710984917A CN 107698455 A CN107698455 A CN 107698455A
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- Prior art keywords
- mother liquor
- ferrous bisglycinate
- bisglycinate chelate
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- circulating mother
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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Abstract
The invention belongs to chemical technology field, and in particular to a kind of ferrous bisglycinate chelate and circulating mother liquor recovery process, according to 2CaF2+4HCl+H2SiO3=2CaCl2+SiF4↑+3H2O principle, a certain amount of CaF is taken respectively2And HCl, add CaF in the lower section of the container of kipp gas generator2, the top of container adds HCl, then toward mother liquor is slowly added into the spherical hopper of kipp gas generator, produces until without gas, then system is filtered, its filter residue is ferrous bisglycinate chelate product；Its filtrate is adjusted to its pH=4 with CaO, and its chemical equation is：H₂SO₄+CaO+H2O=CaSO4·2H2O ↓, 2Fe3++3CaO+3H2O=Fe(OH)3↓+3Ca2+, then system is filtered, its filtrate is to reclaim mother liquor.Present invention process solves the problems, such as that ferrous bisglycinate chelate is difficult to recovery, while make it that circulating mother liquor is reclaimed.Present invention process flow is simple, has promotional value.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of ferrous bisglycinate chelate and circulating mother liquor recovery process.
Background technology
Ferrous bisglycinate chelate [Fe (Gly) 2] is a kind of amino-acid chelate, and iron is hemoglobin, myoglobins, a variety of enzyme systems
Main Ingredients and Appearance, play nutrition, immune important function in vivo.Ferrous bisglycinate chelate is nutritional feed additive, in feed
In for preventing and treating animal anemia, obtain optimal immune level, healthy growth provides an efficient, safe and simple approach.With
Inorganic acid molysite is compared with organic acid molysite, and ferrous bisglycinate chelate has that stability is good, is easily absorbed, no iron taste, no gastrointestinal irritation,
Have no toxic side effect, the features such as bioavailability is high, be that latest generation mends iron additive, for livestock and poultry while iron and sweet ammonia can be supplemented
Acid, improve animal palatability.The production technology of ferrous glycine is to use FeSO4·7H2O synthesizes a kind of chelate, mistake with glycine
A small amount of unreacted FeSO is had in journey4.7H2O, because mother liquor pH value is acidity, ferrous iron easily occurs following reaction and is oxidized to
Ferric iron：4Fe2++O2+4H+=4Fe3++2H2O, the Fe substituted into through multiple circulating mother liquor ring mother liquor in production process3+It is accumulative more next
It is more, in addition, FeSO4·7H2Doped with Si in O raw materials, H is generated with free acid reaction2SiO3,The Fe contained in mother liquor3+And
H2SiO3There is detrimental effect to product.In a liquid, it is absinthe-green ferrous glycine network that mother liquor, which stands a period of time lower floor,
(chela）Compound is difficult to reclaim, if while mother liquor directly discharge, one wastes, and on the other hand causes environmental pollution, and mother liquor is through processing
It can recycle, therefore it is particularly important to study a kind of recovery process of mother liquor.
The content of the invention
It is an object of the present invention to solve the problems, such as that product is difficult to recovery to ferrous bisglycinate chelate in process of production, makes simultaneously
Obtain mother liquor to be reclaimed, cause the waste of resource.
To reach above-mentioned purpose, the technical solution adopted in the present invention is：
A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process, comprises the following steps：
（1）A certain amount of CaF is taken respectively2And HCl, add CaF in the lower section of the container of kipp gas generator2, the top of container adds
HCl, then toward mother liquor is slowly added into the spherical hopper of kipp gas generator, produced until without gas, it is learned reaction equation and is：
2CaF2+4HCl+H2SiO3=2CaCl2+SiF4↑+3H2O, obtain system 1；
（2）By step（1）Obtained system 1 is filtered, and collects its filter residue, as ferrous bisglycinate chelate, and its filtrate is adjusted with CaO
To its pH=4, system 2 is obtained, its chemical equation is：H2SO4+CaO+H2O=CaSO4·2H2O ↓, 2Fe3++3CaO+3H2O=Fe
(OH)3↓+3Ca2+, then system 2 is filtered, its filtrate is the circulating mother liquor reclaimed, and filter residue abandons it.
In the present invention, further instruction, step（1）Described in kipp gas generator container in the CaF that adds2With
HCl ratios are 1g：2.5-3ml.
In the present invention, further instruction, the CaF2Purity be >=98%.
In the present invention, further instruction, the concentration of the HCl is 36-38%.
The present invention has the advantage that compared with prior art：
Present invention process solves the problems, such as that ferrous bisglycinate chelate is difficult to recovery, while make it that circulating mother liquor is reclaimed.In mother liquor
Contain Fe3+And H2SiO3It can be occurred therewith using addition chemical reagent chemical anti-to the detrimental effect that has of product, the present invention
Should be so as to the method for removal, discarded filter residue is Fe (OH)3And CaSO4It is non-dangerous material, processing can be buried, will not be to environment
Pollute.In the technological process simultaneously, the pH of mother liquor is adjusted to 4, the outward appearance of the ferrous bisglycinate chelate of production is best.Work of the present invention
Skill flow is simple, has promotional value.
Embodiment
The invention provides a kind of ferrous bisglycinate chelate and circulating mother liquor recovery process is provided, to make the purpose of the present invention, skill
Art scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that tool described herein
Body embodiment only to explain the present invention, is not intended to limit the present invention.
Embodiment 1
A kind of ferrous bisglycinate chelate provided by the invention and circulating mother liquor recovery process are as follows：
A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process, comprises the following steps：
（1）A certain amount of CaF is taken respectively2And HCl, add CaF in the lower section of the container of kipp gas generator2, the top of container adds
HCl, then toward mother liquor is slowly added into the spherical hopper of kipp gas generator, produced until without gas, wherein, kipp gas generator
Lower section often adds 1gCaF2When, the amount that top adds HCl is 2.5ml, and its reaction equation is：2CaF2+4HCl+H2SiO3=2CaCl2
+SiF4↑+3H2O, obtain system 1；Wherein, the CaF2Purity be >=98%, the concentration of the HCl is 38%.
（2）By step（1）Obtained system 1 is filtered, and collects its filter residue, as ferrous bisglycinate chelate, and its filtrate uses CaO
Regulation obtains system 2, its chemical equation is to its pH=4：H2SO4+CaO+H2O=CaSO4·2H2O ↓, 2Fe3++3CaO+3H2O
=Fe(OH)3↓+3Ca2+, then system 2 is filtered, its filtrate is the circulating mother liquor reclaimed, and filter residue abandons it.
Embodiment 2
A kind of ferrous bisglycinate chelate provided by the invention and circulating mother liquor recovery process are as follows：
A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process, comprises the following steps：
（1）A certain amount of CaF is taken respectively2And HCl, add CaF in the lower section of the container of kipp gas generator2, the top of container adds
HCl, then toward mother liquor is slowly added into the spherical hopper of kipp gas generator, produced until without gas, wherein, kipp gas generator
Lower section often adds 1gCaF2When, the amount that top adds HCl is 2.8ml, and its reaction equation is：2CaF2+4HCl+H2SiO3=2CaCl2
+SiF4↑+3H2O, obtain system 1；Wherein, the CaF2Purity be >=98%, the concentration of the HCl is 37%.
（2）By step（1）Obtained system 1 is filtered, and collects its filter residue, as ferrous bisglycinate chelate, and its filtrate uses CaO
Regulation obtains system 2, its chemical equation is to its pH=4：H2SO4+CaO+H2O=CaSO4·2H2O ↓, 2Fe3++3CaO+3H2O
=Fe(OH)3↓+3Ca2+, then system 2 is filtered, its filtrate is the circulating mother liquor reclaimed, and filter residue abandons it.
Embodiment 3
A kind of ferrous bisglycinate chelate provided by the invention and circulating mother liquor recovery process are as follows：
A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process, comprises the following steps：
（1）A certain amount of CaF is taken respectively2And HCl, add CaF in the lower section of the container of kipp gas generator2, the top of container adds
HCl, then toward mother liquor is slowly added into the spherical hopper of kipp gas generator, produced until without gas, wherein, kipp gas generator
Lower section often adds 1gCaF2When, the amount that top adds HCl is 3ml, and its reaction equation is：2CaF2+4HCl+H2SiO3=2CaCl2+
SiF4↑+3H2O, obtain system 1；Wherein, the CaF2Purity be >=98%, the concentration of the HCl is 36%.
（2）By step（1）Obtained system 1 is filtered, and collects its filter residue, as ferrous bisglycinate chelate, and its filtrate uses CaO
Regulation obtains system 2, its chemical equation is to its pH=4：H2SO4+CaO+H2O=CaSO4·2H2O ↓, 2Fe3++3CaO+3H2O
=Fe(OH)3↓+3Ca2+, then system 2 is filtered, its filtrate is the circulating mother liquor reclaimed, and filter residue abandons it.
Described above is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, the equal change completed or modification change under the technical spirit suggested by all present invention, all should belong to
Cover the scope of the claims in the present invention.
Claims (4)
1. a kind of ferrous bisglycinate chelate and circulating mother liquor recovery process, it is characterised in that comprise the following steps：
（1）A certain amount of CaF is taken respectively2And HCl, add CaF in the lower section of the container of kipp gas generator2, the top of container adds
HCl, then toward mother liquor is slowly added into the spherical hopper of kipp gas generator, produced until without gas, it is learned reaction equation and is：
2CaF2+4HCl+H2SiO3=2CaCl2+SiF4↑+3H2O, obtain system 1；
（2）By step（1）Obtained system 1 is filtered, and collects its filter residue, as ferrous bisglycinate chelate, and its filtrate is adjusted with CaO
To its pH=4, system 2 is obtained, its chemical equation is：H2SO4+CaO+H2O=CaSO4·2H2O ↓, 2Fe3++3CaO+3H2O=Fe
(OH)3↓+3Ca2+, then system 2 is filtered, its filtrate is the circulating mother liquor reclaimed, and filter residue abandons it.
2. a kind of ferrous bisglycinate chelate according to claim 1 and circulating mother liquor recovery process, it is characterised in that：Step（1）
Described in kipp gas generator container in the CaF that adds2It is 1g with HCl ratios：2.5-3ml.
3. a kind of ferrous bisglycinate chelate according to claim 1 and circulating mother liquor recovery process, it is characterised in that：The CaF2
Purity be >=98%.
4. a kind of ferrous bisglycinate chelate according to claim 1 and circulating mother liquor recovery process, it is characterised in that：The HCl
Concentration be 36-38%.
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| CN201710984917.3A CN107698455A (en) | 2017-10-20 | 2017-10-20 | A kind of ferrous bisglycinate chelate and circulating mother liquor recovery process |
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Citations (9)
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|---|---|---|---|---|
| US6407138B1 (en) * | 2000-10-11 | 2002-06-18 | Albion International, Inc. | Composition and method for preparing electrically neutral amino acid chelates free of interfering ions |
| CN101606715A (en) * | 2008-06-17 | 2009-12-23 | 浙江科技学院 | A kind of preparation method who disturbs anionic food-grade amino acid ferrous chelate compound that do not contain |
| CN101653199A (en) * | 2009-08-11 | 2010-02-24 | 化学工业（全国）饲料添加剂工程技术中心山东科技公司 | Preparation method of water-soluble feed additive ferrous glycine complex |
| EP2161075A1 (en) * | 2008-08-26 | 2010-03-10 | Pancosma Société Anonyme pour l'Industrie des Produits Biochimiques | Process and device for manufacturing organometallic complexes in powder form |
| CN103086901A (en) * | 2011-11-03 | 2013-05-08 | 青岛康地恩药业股份有限公司 | Preparation method of amino acid ferrous sulfate chelate |
| CN103492394A (en) * | 2011-02-17 | 2014-01-01 | Isf有限公司 | Process for preparing amino acid chelate compounds, amino acid chelate compounds and use of amino acid chelate compounds |
| CN105237425A (en) * | 2015-11-12 | 2016-01-13 | 中南大学 | Method for mother solution pretreatment and cyclic utilization in chain type ferrous glycine complex synthesis |
| CN106187797A (en) * | 2016-07-08 | 2016-12-07 | 仲恺农业工程学院 | A kind of preparation method of complex of ferrous glycine |
| CN107118115A (en) * | 2017-06-28 | 2017-09-01 | 北京博农利生物科技有限公司 | A kind of preparation method of Ferrous glycinate |
-
2017
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Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6407138B1 (en) * | 2000-10-11 | 2002-06-18 | Albion International, Inc. | Composition and method for preparing electrically neutral amino acid chelates free of interfering ions |
| CN101606715A (en) * | 2008-06-17 | 2009-12-23 | 浙江科技学院 | A kind of preparation method who disturbs anionic food-grade amino acid ferrous chelate compound that do not contain |
| EP2161075A1 (en) * | 2008-08-26 | 2010-03-10 | Pancosma Société Anonyme pour l'Industrie des Produits Biochimiques | Process and device for manufacturing organometallic complexes in powder form |
| CN101653199A (en) * | 2009-08-11 | 2010-02-24 | 化学工业（全国）饲料添加剂工程技术中心山东科技公司 | Preparation method of water-soluble feed additive ferrous glycine complex |
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| CN103086901A (en) * | 2011-11-03 | 2013-05-08 | 青岛康地恩药业股份有限公司 | Preparation method of amino acid ferrous sulfate chelate |
| CN105237425A (en) * | 2015-11-12 | 2016-01-13 | 中南大学 | Method for mother solution pretreatment and cyclic utilization in chain type ferrous glycine complex synthesis |
| CN106187797A (en) * | 2016-07-08 | 2016-12-07 | 仲恺农业工程学院 | A kind of preparation method of complex of ferrous glycine |
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Application publication date: 20180216 |