CN105237426A - Method for controlling chain type ferrous glycine complex crystal size and uniformity - Google Patents
Method for controlling chain type ferrous glycine complex crystal size and uniformity Download PDFInfo
- Publication number
- CN105237426A CN105237426A CN201510770356.8A CN201510770356A CN105237426A CN 105237426 A CN105237426 A CN 105237426A CN 201510770356 A CN201510770356 A CN 201510770356A CN 105237426 A CN105237426 A CN 105237426A
- Authority
- CN
- China
- Prior art keywords
- chain type
- ferrous glycine
- grain size
- glycine
- uniformity coefficient
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for controlling chain type ferrous glycine complex crystal size and uniformity. The method comprises the main steps that during hydro-thermal synthesis of a chain type ferrous glycine complex, the feeding solid-to-liquid ratio is 1.5-2.5; after hydro-thermal synthesis, the crystallization temperature is controlled to range from 30 DEG C to 50 DEG C, a fine-granule product with the size being smaller than 100 micrometers and the weight accounting for 2-5% that of the raw material glycine is added, and the proper cooling rate of 0.5-5 DEG C/min and the proper stirring rate of 200-700 rpm are controlled, so that the chain type ferrous glycine complex is cooled to the temperature of 25 DEG C for separation by crystallization. The method has the advantages that the existing simple ferrous glycine complex synthesis technology is utilized, no special vacuum circulation equipment or crystallization technology is needed, the crystal size and uniformity of the ferrous glycine complex are effectively improved, the fine powder product consumption is decreased, the production efficiency is high, the cost is low, and the crystallization technology is simple.
Description
Technical field
The invention belongs to third generation microelement feed addictive-chain type glycosides propylhomoserin ferrous complex preparing technical field, be specifically related to a kind of method controlling chain type complex of ferrous glycine grain size number and uniformity coefficient.
Background technology
Water-soluble chain type glycosides propylhomoserin ferrous complex, be in recent years development faster the third generation trace element iron feed additive.It for main raw material with ferrous sulfate, glycine, controls mol ratio and is about 1:1, at 60 DEG C-80 DEG C, be uniformly mixed Hydrothermal Synthesis 0.5-1h, is cooled to certain temperature direct crystallization to separate out product.Its production technique is simple, yield is high, cost is lower.
But water-soluble chain type glycosides propylhomoserin ferrous complex is cooled to certain temperature, direct crystallization separates out product, when plant-scale operation, grain size number is smaller, and particle size distribution is wide, bring difficulty to the size classification of dry rear product, screening, define more fine powder product.Adopt vacuum cycle crystallizer, effectively can improve grain size number and the uniformity coefficient of water-soluble chain type glycosides propylhomoserin ferrous complex, but it not only increases facility investment and running cost, and increase the complicacy of technique.
If do not adopt vacuum cycle crystallizer, to the water-soluble chain type glycosides propylhomoserin ferrous complex product of short run, after Hydrothermal Synthesis, do not stir and directly Slow cooling crystallization, the grain fineness number of gained is large.But industrial scale is produced, does not stir and directly Slow cooling crystallization, not only make production efficiency low because temperature fall time is long; and because of at the bottom of mass crystallization thing sedimentary deposit tank; primary crystallization granularity is large, and grain fineness number diminishes with the prolongation of temperature fall time, and particle size uniformity is poor.
Therefore, do not adopting under vacuum cycle crystallizer prerequisite, seeking a kind of low cost simple method effectively improving chain type complex of ferrous glycine grain size number and uniformity coefficient, imperative.
Summary of the invention
The object of the present invention is to provide and a kind ofly do not adopted under vacuum cycle crystallizer prerequisite, the low cost simple method of grain size number and uniformity coefficient when effectively can improve industrial scale production chain type complex of ferrous glycine.
Object of the present invention is achieved in the following ways:
A kind of method controlling chain type complex of ferrous glycine grain size number and uniformity coefficient, the solid-to-liquid ratio that feeds intake of chain type complex of ferrous glycine Hydrothermal Synthesis is 1.0-3, after Hydrothermal Synthesis completes, the temperature controlling to add crystal seed is 30-50 DEG C, then adds to account for certain particle size range (choosing the crystal seed of required particle size range according to the product requirement) fine particle product that raw material glycine weight 2-5% is less than 100 μm and make crystal seed; After adding crystal seed, to control rate of temperature fall be 0.5 DEG C/min-5 DEG C/min, and control stir speed (S.S.) 200rpm-700rpm simultaneously, make complex of ferrous glycine be cooled to 25 DEG C of crystallizations.
Aforesaid method controls the solid-to-liquid ratio that feeds intake and is preferably 1.5-2.5.
The temperature that aforesaid method controls to add crystal seed is preferably 30 DEG C-45 DEG C.
Aforesaid method preferably adds the fine particle product being less than certain particle size range of 100 μm accounting for raw material glycine weight 3% and makes crystal seed.
Aforesaid method controls rate of temperature fall and is preferably 1 DEG C/min-3 DEG C/min.
Aforesaid method controls stir speed (S.S.) and is preferably 300rpm-700rpm.
In aforesaid method, reinforced solid-to-liquid ratio affects recrystallization temperature or degree of supersaturation, thus impact adds the temperature (see accompanying drawing 1) of crystal seed.Under a certain solid-to-liquid ratio condition, the temperature adding crystal seed is not suitable for, even if add crystal seed, crystal seed dissolves, and with not add crystal seed the same, grain size number and uniformity coefficient are also bad; Cross low temperature and add crystal seed, separated out a large amount of crystal, grain size number and uniformity coefficient are also bad, so the present invention controls reinforced solid-to-liquid ratio and add seeding temperature, preferably to control reinforced solid-to-liquid ratio be 1.5-2.5 and the temperature controlling to add crystal seed is 30 DEG C-50 DEG C.
In aforesaid method, rate of temperature fall is also a very important parameter.Along with the increase of rate of temperature fall, grain size number and the uniformity coefficient of chain type complex of ferrous glycine are deteriorated gradually, but during lower than certain value, on grain size number and uniformity coefficient impact little (see accompanying drawing 2).So the constant rate of temperature fall of the present invention be 0.5 DEG C/min-5 DEG C/min.
In aforesaid method, after controlling reinforced solid-to-liquid ratio, adding seeding temperature and rate of temperature fall, add crystal seed crystallisation by cooling, grain size number and the uniformity coefficient of chain type complex of ferrous glycine are deteriorated with the increase of stir speed (S.S.), but exceed certain stir speed (S.S.), grain size number and uniformity coefficient improve with the increase of stir speed (S.S.) (see accompanying drawing 3).Illustrating that surperficial crystallization reaction speed is fast, is not main controlling factor, and the accumulation and sediment of crystallisate, to stir the damage of crystal and the diffusive migration of feed liquid be main influence factor.Low stirring velocity damage crystallisate, and the deposition of crystallisate affects diffusion mass transfer, grain size number and uniformity coefficient increase with stir speed (S.S.) and are deteriorated; And although high stirring velocity damages crystallisate, damage is tending towards constant, and high stirring velocity accelerates diffusion mass transfer simultaneously, makes grain size number and uniformity coefficient improve with the increase of high stirring velocity on the contrary.Control stir speed (S.S.) is 200rpm-700rpm, to obtain grain size number and the uniformity coefficient of optimized chain type complex of ferrous glycine.
Method of the present invention is contriver studying the kinetics of crystallization of complex of ferrous glycine, grain size number and uniformity coefficient and solid-to-liquid ratio, on the basis of the relation such as temperature, rate of temperature fall, stir speed (S.S.) when adding crystal seed, exploration a kind of low cost simple method controlling complex of ferrous glycine grain size number and uniformity coefficient out.
Advantage of the present invention is: (1) need not change the existing synthesis technique of complex of ferrous glycine, by optimal control solid-to-liquid ratio, add seeding temperature, rate of temperature fall and stir speed (S.S.) etc., effectively optimize and improve grain size number and the uniformity coefficient of complex of ferrous glycine; (2) obtain relatively evenly and the larger crystal grain of particle, make dry after the size classification of product, screening easier, reduce fine particle product amount; (3) technique is simple, production efficiency is high, cost is low, vacuum crystallizing equipment that need not be special and crystallization processes.(4) industrial scale be particularly suitable for without independent loops crystallizer is produced.
Accompanying drawing illustrates:
Fig. 1 adds seeding temperature and the relation curve of the solid-to-liquid ratio that feeds intake;
Fig. 2 is the relation curve of cooling rate and granularity;
Fig. 3 is the relation curve of stir speed (S.S.) and granularity.
Embodiment
Be intended to further illustrate the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1:
With ferrous sulfate, glycine for main raw material, control batching mol ratio and be about 1:1, feed in raw material and admittedly tuck in than being 1.5, at 60 DEG C-80 DEG C, be uniformly mixed Hydrothermal Synthesis 0.5-1h.After being cooled to 34 DEG C, the fine particle product adding 3% makes crystal seed, and control stir speed (S.S.) is 300rpm, and constant rate of temperature fall is 2.5 DEG C/min, cools to 25 DEG C, makes complex of ferrous glycine crystallization.Take dehydrated alcohol as dispersion agent, recording its mean particle size with laser particle size analyzer is 203 μm, and consistence is 1.09.
Embodiment 2:
With ferrous sulfate, glycine for main raw material, control batching mol ratio and be about 1:1, reinforced solid-to-liquid ratio is 2.5, at 60 DEG C-80 DEG C, is uniformly mixed Hydrothermal Synthesis 0.5-1h.Be cooled to 38 DEG C, the fine particle product adding 3% makes crystal seed, and control stir speed (S.S.) is 300rpm, and constant rate of temperature fall is 2.5 DEG C/min, cools to 25 DEG C, makes complex of ferrous glycine crystallization.Take dehydrated alcohol as dispersion agent, recording its mean particle size with laser particle size analyzer is 268 μm, and consistence is 1.19.
Embodiment 3:
With ferrous sulfate, glycine for main raw material, control batching mol ratio and be about 1:1, reinforced solid-to-liquid ratio is 2.5, at 60 DEG C-80 DEG C, is uniformly mixed Hydrothermal Synthesis 0.5-1h.Be cooled to 38 DEG C, the fine particle product adding 3% makes crystal seed, and control stir speed (S.S.) is 300rpm, and constant rate of temperature fall is 1.5 DEG C/min, cools to 25 DEG C, makes complex of ferrous glycine crystallization.Take dehydrated alcohol as dispersion agent, recording its mean particle size with laser particle size analyzer is 305 μm, and consistence is 1.26.
Embodiment 4:
With ferrous sulfate, glycine for main raw material, control batching mol ratio and be about 1:1, reinforced solid-to-liquid ratio is 2.0, at 60 DEG C-80 DEG C, is uniformly mixed Hydrothermal Synthesis 0.5-1h.Be cooled to 38 DEG C, the fine particle product adding 3% makes crystal seed, and control stir speed (S.S.) is 500rpm, and constant rate of temperature fall is 1.5 DEG C/min, cools to 25 DEG C, makes complex of ferrous glycine crystallization.Take dehydrated alcohol as dispersion agent, recording its mean particle size with laser particle size analyzer is 449 μm, and consistence is 1.59.
Claims (6)
1. one kind controls the method for chain type complex of ferrous glycine grain size number and uniformity coefficient, it is characterized in that, the solid-to-liquid ratio that feeds intake of chain type complex of ferrous glycine Hydrothermal Synthesis is 1.0-3, after Hydrothermal Synthesis completes, the temperature controlling to add crystal seed is 30-50 DEG C, then adds to account for the fine particle product that raw material glycine weight 2-5% is less than certain particle size range of 100 μm and make crystal seed; After adding crystal seed, to control rate of temperature fall be 0.5 DEG C/min-5 DEG C/min, and control stir speed (S.S.) 200rpm-700rpm simultaneously, make complex of ferrous glycine be cooled to 25 DEG C of crystallizations.
2. the method for control chain type complex of ferrous glycine grain size number according to claim 1 and uniformity coefficient, is characterized in that, controls the solid-to-liquid ratio that feeds intake and is preferably 1.5-2.5.
3. the method for control chain type complex of ferrous glycine grain size number according to claim 1 and uniformity coefficient, is characterized in that, the temperature controlling to add crystal seed is preferably 30 DEG C-45 DEG C.
4. the method for control chain type complex of ferrous glycine grain size number according to claim 1 and uniformity coefficient, is characterized in that, preferably adds the fine particle product being less than certain particle size range of 100 μm accounting for raw material glycine weight 3% and makes crystal seed.
5. the method for control chain type complex of ferrous glycine grain size number according to claim 1 and uniformity coefficient, is characterized in that, controls rate of temperature fall and is preferably 1 DEG C/min-3 DEG C/min.
6. the method for control chain type complex of ferrous glycine grain size number according to claim 1 and uniformity coefficient, is characterized in that, controls stir speed (S.S.) and is preferably 300rpm-700rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510770356.8A CN105237426A (en) | 2015-11-12 | 2015-11-12 | Method for controlling chain type ferrous glycine complex crystal size and uniformity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510770356.8A CN105237426A (en) | 2015-11-12 | 2015-11-12 | Method for controlling chain type ferrous glycine complex crystal size and uniformity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105237426A true CN105237426A (en) | 2016-01-13 |
Family
ID=55035299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510770356.8A Pending CN105237426A (en) | 2015-11-12 | 2015-11-12 | Method for controlling chain type ferrous glycine complex crystal size and uniformity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105237426A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178583A (en) * | 2016-09-20 | 2016-12-07 | 武汉科技大学 | The feedback of crystal product granularity during a kind of dilution crystallization |
| CN106397234A (en) * | 2016-09-05 | 2017-02-15 | 河北东华冀衡化工有限公司 | Preparation method of interfering ion-free ferrous glycinate |
| CN111777523A (en) * | 2020-06-08 | 2020-10-16 | 四川爱隆植物营养科技有限公司 | Preparation method of glycine iron chelate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467331A (en) * | 2013-09-26 | 2013-12-25 | 潍坊祥维斯化学品有限公司 | Iron glycine chelate crystal growth method |
-
2015
- 2015-11-12 CN CN201510770356.8A patent/CN105237426A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467331A (en) * | 2013-09-26 | 2013-12-25 | 潍坊祥维斯化学品有限公司 | Iron glycine chelate crystal growth method |
Non-Patent Citations (2)
| Title |
|---|
| 滕娇琴等: "饲料级甘氨酸亚铁的合成及分析方法", 《饲料与种植》 * |
| 许甲平: "甘氨酸铁螯合物结构式的验证分析", 《饲料工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397234A (en) * | 2016-09-05 | 2017-02-15 | 河北东华冀衡化工有限公司 | Preparation method of interfering ion-free ferrous glycinate |
| CN106178583A (en) * | 2016-09-20 | 2016-12-07 | 武汉科技大学 | The feedback of crystal product granularity during a kind of dilution crystallization |
| CN111777523A (en) * | 2020-06-08 | 2020-10-16 | 四川爱隆植物营养科技有限公司 | Preparation method of glycine iron chelate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105237426A (en) | Method for controlling chain type ferrous glycine complex crystal size and uniformity | |
| CN104192917B (en) | Nickel-cobalt sulfate continuous-crystallizing process | |
| CN106267880B (en) | The feedback of crystal product granularity in a kind of intermittent cooling crystallization process | |
| CN110054196B (en) | Method for preparing high-purity spherical instant boric acid by organic molecule induction | |
| CN104402023B (en) | A kind of production method improving carbonizatin method sodium bicarbonate product granularity | |
| CN103936632A (en) | Dicyandiamide continuous multistage crystallizing production process | |
| Ferguson et al. | Automated self seeding of batch crystallizations via plug flow seed generation | |
| CN102658148A (en) | Fischer-Tropsch synthesis iron-based catalyst and preparation method thereof | |
| Sander et al. | Pentaerythritol crystallization–Influence of the process conditions on the granulometric properties of crystals | |
| CN103910651B (en) | Iminodiacetonitrile continuous crystallisation technique | |
| CN105819471A (en) | Method for producing baking soda large in particle size | |
| EP2897903B1 (en) | Process for preparing crystalline ammonium sulfate product | |
| CN105985249A (en) | Method for recrystallizing TATB | |
| CN102553291B (en) | Cooling crystallization method | |
| CN109265355B (en) | Pentanediamine suberate salt and crystal thereof | |
| CN105753728A (en) | Medicinal L-valine dilution crystallization method | |
| CN111087295B (en) | Pentanediamine succinic acid terephthalic acid eutectic salt and preparation method thereof | |
| CN204412174U (en) | The special anchor gate stirrer of D-ribose crystallization | |
| CN205709871U (en) | A kind of device of hypergravity direct heat transfer method crystalline one ammonium | |
| CN202410227U (en) | Continuous type crystallizing system | |
| CN112429754A (en) | Large-particle magnesium sulfate cooling crystallization method and system | |
| CN205653182U (en) | Improve device of carbonization sodium bicarbonate granularity | |
| Siddique | Continuous crystallisation-case studies | |
| CN110776539A (en) | Method for controlling crystal size of maltitol | |
| CN105776162B (en) | A kind of method and device of the ammonium of hypergravity direct heat transfer method crystalline one |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160113 |
|
| RJ01 | Rejection of invention patent application after publication |