CN105198761A - Crystal with high content of choline chloride and preparation method of crystal - Google Patents
Crystal with high content of choline chloride and preparation method of crystal Download PDFInfo
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- CN105198761A CN105198761A CN201510678547.1A CN201510678547A CN105198761A CN 105198761 A CN105198761 A CN 105198761A CN 201510678547 A CN201510678547 A CN 201510678547A CN 105198761 A CN105198761 A CN 105198761A
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Abstract
The invention relates to a crystal with high content of choline chloride and a preparation method of the crystal. The effective content of the choline chloride in the crystal is higher than 98%, and the content of moisture is lower than 0.5%. The crystal and the preparation method have the benefits as follows: the yield is increased, the investment cost and the energy consumption are reduced, exhaust gas emission caused by spray drying is reduced, besides, risks of mycotoxins, heavy metals and dust which are caused by other choline chloride agent forms are avoided, transportation is facilitated, and meanwhile, the quality of the choline chloride is guaranteed.
Description
Technical field
The present invention relates to a kind of high-content choline chloride crystal and preparation method thereof.
Background technology
Choline chloride 60, English name: cholinechloride, chemical name: choline chloride, chemical formula: C5H14NOCl, molecular weight is: 139.63, and it is white crystal, has strong water absorbability.Slightly have fishy smell and a salty bitter taste of tool.Soluble in water and alcohol, the aqueous solution almost in neutral, is insoluble to ether, sherwood oil, benzene and dithiocarbonic anhydride, unstable in basic solution.Fusing point 240 DEG C.Choline chloride aqueous solution agent storage temperature should lower than-12 DEG C.
Choline is a kind of water-soluble vitamins VB4, is present in fodder additives with the form of choline chloride 60.Choline can promote liver, the metabolism of fat of kidney; The basis of choline or body synthesis of acetyl choline, thus the transmission of the signal that affects the nerves.Choline is also one of the methyl source in body needed for methionine(Met) synthesis in addition.In much food, all contain natural choline, but its concentration is not enough to satisfied modern feed industry to the mushroom needs of animal.Therefore synthesis choline should be added to meet its needs in feed.Lack choline and can cause fatty liver, poor growth, laying rate reduces, and death such as to increase at the phenomenon.Choline chloride 60 is not only the mode of direct, the most most economical generally acknowledged supplementary choline, becomes the requisite additive of modern intensive animal productiong, and be today addition maximum, for the vitamins product that animal ratio is the highest.
Choline chloride 60 adopts epoxyethane method to produce, technique is as follows: Trimethylamine 99 and hydrochloric acid reaction 1:1 reaction with same mole, generate the trimethylamine hydrochloride of 54-57%, then the oxyethane of equimolar amount is added, generate crude product choline chloride 60, now choline chloride 60 becomes liquid, and content is about 65%, follow-uply to anhydrate, removal of impurities process, processing is to meet the need of market further.Existing market mainly contains four formulas: liquid choline chloride 60, in water, and effective content 70%-80%; Plant vector type choline chloride 60, effective content 50%-70%, choline chloride 60 is adsorbed in plant vector, and then carry out drying, moisture is lower than 4%; Silica supports type choline chloride 60, it is mixed by choline chloride 60 and silicon-dioxide, is generally the moisture of 15%-20%, content 50%; Choline chloride crystal, is formed by spraying dry, and content is higher than 96%, and moisture is lower than 0.5%.
Liquid choline chloride 60, due to the restriction of packaging means, is not easy to transport and uses, directly affecting international trade; Plant vector type choline chloride 60, owing to selecting plant vector, as corn cob meal, can bring the various carcinogenic mycotoxin that causes a disease such as aflatoxin, zearalenone, directly affect the health of feed quality and cultivated animals; Silica supports type choline chloride 60 due to fineness little, dust is large, easily block, and cost is high, there is the risk of Heavy Metal Pollution; Therefore the 4th kind of formula choline chloride crystal receives the concern of more and more client and likes, it had both been convenient to transport, various mycotoxin, heavy metal, dust equivalent risk are stopped again, it is optimal formulation, but the choline chloride crystal circulated in the market all adopts spray dried form to produce, there is the shortcomings such as energy consumption is high, facility investment is high, production capacity is low, dried tail gas discharge is many in which.
Summary of the invention
The present invention is in order to make up the defect of prior art, provide a kind of raising production capacity, reduce cost of investment and energy consumption, decrease the exhaust emissions that spraying dry brings, and avoid the risk of mycotoxin that other choline chloride 60 formulations bring, heavy metal, dust, high-content choline chloride crystal of convenient transport and preparation method thereof.
The present invention is achieved through the following technical solutions:
A kind of high-content choline chloride crystal and preparation method thereof, in choline chloride crystal, the effective content of choline chloride 60 is more than 98%, within moisture 0.5%; Its preparation method comprises the steps: (1) sends the crude product choline chloride 60 adopting epoxyethane method to obtain into choline chloride 60 basin; (2) by crude product choline chloride 60 through decolorizing with activated carbon, flame filter press filter impurity elimination; (3) water white liquid choline chloride 60 is concentrated until crystal is separated out through negative pressure concentrating unit; (4) concentrated solution moves in secondary concentration device and proceeds to concentrate, until reach certain crystal amount, opens cooling circulating water cooling, separates out more crystal; (5) choline chloride 60 containing enough crystal is separated through centrifuge, sloughs moisture; (6) choline chloride crystal with a little moisture enters boiling drier, first cold wind blows away crystal top layer moisture, then anhydrates further with low temperature hot blast, then lowers the temperature with the cold wind after dehumidifying, content can be obtained and reach 98%, moisture lower than 0.5% choline chloride crystal.
Further, epoxyethane method is adopted to produce the crude product choline chloride 60 of gained, content 65%, moisture 35% in described step (1).
Further, the crude product choline chloride 60 in described step (2) pumps in the bleacher with stirring system, adds gac according to 1-5 ‰ adding proportion, mixing 10-20min, then utilize flame filter press to filter, retain gac and impurity, obtain the choline chloride 60 liquid of clear.
Further, above-mentioned gained choline chloride 60 concentrates through the distillation and concentration device with nahlock hole graphite heat exchanger and separator by described step (3), until crystal starts to separate out, obtains the concentrated solution of content 78%.
Further, concentrated solution heats up and continues to concentrate by described step (4) in the crystallizer with tubular heat exchange and vacuum system, crystal is separated out in a large number, wet and admittedly reach more than 50%, 4-7 DEG C of cooling circulating water is adopted to lower the temperature again, lower according to temperature, the principle that solubleness is less, make choline chloride crystal separate out further, wet and admittedly reach more than 70%.
Further, the crystal solution containing a large amount of crystal in described step (5) is carried out centrifugal through pulling bag lower discharging centrifuge, is retained by crystal, then wash by 4-7 DEG C of water at low temperature, remove plane of crystal impurity, just obtaining content can reach 98%, moisture lower than 1.5% choline chloride crystal.
Further, choline chloride crystal with a little moisture in described step (6) enters boiling drier, first blow away crystal top layer moisture with 30-40 DEG C of cold wind, anhydrate further with 90-110 DEG C of low temperature hot blast again, then lower the temperature with 40-60 DEG C of cold wind after dehumidifying, content can be obtained and reach 98%, moisture lower than 0.5% choline chloride crystal.
The invention has the beneficial effects as follows: the effective content of the choline chloride 60 adopting present method to prepare is more than 98%, within moisture 0.5%; Its preparation method not only increases production capacity, reduce cost of investment and energy consumption, decrease the exhaust emissions that spraying dry brings, and avoid the risk of mycotoxin that other choline chloride 60 formulations bring, heavy metal, dust, while convenient transport, ensure that the quality of choline chloride 60.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Accompanying drawing 1 is a kind of specific embodiment of the present invention.A kind of high-content choline chloride crystal of this invention and preparation method thereof, in choline chloride crystal, the effective content of choline chloride 60 is more than 98%, within moisture 0.5%; Its preparation method comprises the steps: (1) sends the crude product choline chloride 60 adopting epoxyethane method to obtain into choline chloride 60 basin; (2) by crude product choline chloride 60 through decolorizing with activated carbon, flame filter press filter impurity elimination; (3) water white liquid choline chloride 60 is concentrated until crystal is separated out through negative pressure concentrating unit; (4) concentrated solution moves in secondary concentration device and proceeds to concentrate, until reach certain crystal amount, opens cooling circulating water cooling, separates out more crystal; (5) choline chloride 60 containing enough crystal is separated through centrifuge, process of anhydrating; (6) choline chloride crystal with a little moisture enters boiling drier, and first cold wind blows away crystal top layer moisture, then anhydrates further with low temperature hot blast, then lower the temperature with the cold wind after dehumidifying, can obtain choline chloride crystal, content can reach 98%, and moisture is lower than 0.5%.
Further, epoxyethane method is adopted to produce the crude product choline chloride 60 of gained, content 65%, moisture 35% in described step (1).
Further, the crude product choline chloride 60 in described step (2) pumps in the bleacher with stirring system, adds gac according to 1-5 ‰ adding proportion, mixing 10-20min, then utilize flame filter press to filter, retain gac and impurity, obtain the choline chloride 60 liquid of clear.
Further, above-mentioned gained choline chloride 60 concentrates through the distillation and concentration device with nahlock hole graphite heat exchanger and separator by described step (3), until crystal starts to separate out, obtains the concentrated solution of content 78%.
Further, concentrated solution heats up and continues to concentrate by described step (4) in the crystallizer with tubular heat exchange and vacuum system, crystal is separated out in a large number, wet and admittedly reach more than 50%, 4-7 DEG C of cooling circulating water is adopted to lower the temperature again, lower according to temperature, the principle that solubleness is less, make choline chloride crystal separate out further, wet and admittedly reach more than 70%.
Further, the crystal solution containing a large amount of crystal in described step (5) is carried out centrifugal through pulling bag lower discharging centrifuge, is retained by crystal, then wash by 4-7 DEG C of water at low temperature, remove plane of crystal impurity, just obtaining content can reach 98%, moisture lower than 1.5% choline chloride crystal.
Further, choline chloride crystal with a little moisture in described step (6) enters boiling drier, first blow away crystal top layer moisture with 30-40 DEG C of cold wind, anhydrate further with 90-110 DEG C of low temperature hot blast again, then lower the temperature with 40-60 DEG C of cold wind after dehumidifying, content can be obtained and reach 98%, moisture lower than 0.5% choline chloride crystal.
The present invention is not limited to above-mentioned embodiment, anyone should learn make under enlightenment of the present invention with the present invention, there is identical or close technical scheme, all fall within protection scope of the present invention.
The technology that the present invention does not describe in detail, shape, structure part are known technology.
Claims (8)
1. a high-content choline chloride crystal, is characterized in that, in choline chloride crystal, the effective content of choline chloride 60 is more than 98%, within moisture 0.5%.
2. the preparation method of a kind of high-content choline chloride crystal according to claim 1, is characterized in that: its preparation method comprises the steps: (1) sends the crude product choline chloride 60 adopting epoxyethane method to obtain into choline chloride 60 basin; (2) by crude product choline chloride 60 through decolorizing with activated carbon, flame filter press filter impurity elimination; (3) water white liquid choline chloride 60 is concentrated until crystal is separated out through negative pressure concentrating unit; (4) concentrated solution moves in secondary concentration device and proceeds to concentrate, until reach certain crystal amount, opens cooling circulating water cooling, separates out more crystal; (5) choline chloride 60 containing enough crystal is separated through centrifuge, process of anhydrating; (6) choline chloride crystal with a little moisture enters boiling drier, and first cold wind blows away crystal top layer moisture, then anhydrates further with low temperature hot blast, then lower the temperature with the cold wind after dehumidifying, can obtain choline chloride crystal, content can reach 98%, and moisture is lower than 0.5%.
3. the preparation method of a kind of high-content choline chloride crystal according to claim 2, is characterized in that: adopt epoxyethane method to produce the crude product choline chloride 60 of gained, content 65%, moisture 35% in described step (1).
4. the preparation method of a kind of high-content choline chloride crystal according to claim 2, it is characterized in that: the crude product choline chloride 60 in described step (2) pumps in the bleacher with stirring system, gac is added according to 1-5 ‰ adding proportion, mixing 10-20min, then flame filter press is utilized to filter, retain gac and impurity, obtain the choline chloride 60 liquid of clear.
5. the preparation method of a kind of high-content choline chloride crystal according to claim 2, it is characterized in that: above-mentioned gained choline chloride 60 concentrates through the distillation and concentration device with nahlock hole graphite heat exchanger and separator by described step (3), until crystal starts to separate out, obtain the concentrated solution of content 78%.
6. the preparation method of a kind of high-content choline chloride crystal according to claim 2, it is characterized in that: concentrated solution heats up and continues to concentrate by described step (4) in the crystallizer with tubular heat exchange and vacuum system, crystal is separated out in a large number, wet and admittedly reach more than 50%, 4-7 DEG C of cooling circulating water is adopted to lower the temperature again, lower according to temperature, the principle that solubleness is less, make choline chloride crystal separate out further, wet and admittedly reach more than 70%.
7. the preparation method of a kind of high-content choline chloride crystal according to claim 2, it is characterized in that: the crystal solution containing a large amount of crystal in described step (5) is carried out centrifugal through pulling bag lower discharging centrifuge, crystal is retained, then wash by 4-7 DEG C of water at low temperature, remove plane of crystal impurity, just obtain content and can reach 98%, moisture lower than 1.5% choline chloride crystal.
8. the preparation method of a kind of high-content choline chloride crystal according to claim 2, it is characterized in that: the choline chloride crystal with a little moisture in described step (6) enters boiling drier, first blow away crystal top layer moisture with 30-40 DEG C of cold wind, anhydrate further with 90-110 DEG C of low temperature hot blast again, then lower the temperature with 40-60 DEG C of cold wind after dehumidifying, content can be obtained and reach 98%, moisture lower than 0.5% choline chloride crystal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510678547.1A CN105198761A (en) | 2015-10-20 | 2015-10-20 | Crystal with high content of choline chloride and preparation method of crystal |
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| CN201510678547.1A CN105198761A (en) | 2015-10-20 | 2015-10-20 | Crystal with high content of choline chloride and preparation method of crystal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056629A (en) * | 2017-04-27 | 2017-08-18 | 河北科技大学 | A kind of preparation method of anhydrous halogenation choline and its derivative monocrystalline |
| CN108610359A (en) * | 2018-04-21 | 2018-10-02 | 山东奥博生物科技有限公司 | The preparation method of phosphoryl chloride choline calcium salt |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691333A (en) * | 2009-10-21 | 2010-04-07 | 山东恩贝科技有限公司 | Production technology for choline chloride |
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2015
- 2015-10-20 CN CN201510678547.1A patent/CN105198761A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691333A (en) * | 2009-10-21 | 2010-04-07 | 山东恩贝科技有限公司 | Production technology for choline chloride |
Non-Patent Citations (2)
| Title |
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| 张雅清等: "禽畜良好饲料添加剂", 《辽宁化工》 * |
| 田恒水等: "氯化胆碱合成新工艺", 《现代化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056629A (en) * | 2017-04-27 | 2017-08-18 | 河北科技大学 | A kind of preparation method of anhydrous halogenation choline and its derivative monocrystalline |
| WO2018195956A1 (en) * | 2017-04-27 | 2018-11-01 | 河北科技大学 | Method for preparing single crystal of anhydrous halogenated choline or derivative thereof |
| CN107056629B (en) * | 2017-04-27 | 2019-04-30 | 河北科技大学 | A kind of preparation method of anhydrous halogenation choline and its derivative monocrystalline |
| US10626079B2 (en) | 2017-04-27 | 2020-04-21 | Hebei University Of Science And Technology | Method for preparing single crystal of anhydrous halogenated choline or derivative thereof |
| CN108610359A (en) * | 2018-04-21 | 2018-10-02 | 山东奥博生物科技有限公司 | The preparation method of phosphoryl chloride choline calcium salt |
| CN108610359B (en) * | 2018-04-21 | 2020-05-29 | 山东奥博生物科技有限公司 | Preparation method of phosphorylcholine chloride calcium salt |
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Application publication date: 20151230 |