CN108440332A - The recovery method of D-VB5 mother liquor of calcium - Google Patents
The recovery method of D-VB5 mother liquor of calcium Download PDFInfo
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- CN108440332A CN108440332A CN201810291698.5A CN201810291698A CN108440332A CN 108440332 A CN108440332 A CN 108440332A CN 201810291698 A CN201810291698 A CN 201810291698A CN 108440332 A CN108440332 A CN 108440332A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
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Abstract
The present invention relates to chemical production technical fields, and in particular to a kind of recovery method of D pantothenic acid mother liquor of calcium；By water vapour and D pantothenic acid mother liquor of calcium each lead into it is high-gravity rotating bed in, after atmospheric gas proposes processing, methanol gas and Liquid Residue are detached, the condensed reflux of methanol gas later obtains methanol, Liquid Residue moisturizing dissolves to obtain D calcium pantothenate aqueous solutions, it carries out decoloration and spray drying treatment successively to D calcium pantothenates aqueous solution again, obtains D calcium pantothenates；Recovery method provided by the invention is simple, using effect is apparent, methanol in product can be down to 0.1% or less, liquid is short in the revolving bed residence time, D calcium pantothenate invariance, it improves product quality and yield, atmospheric operation eliminates vacuum and the chilled brine circulatory system, reduces equipment investment and energy consumption, while also improving the rate of recovery of methanol.
Description
Technical field
The present invention relates to chemical production technical fields, and in particular to a kind of recovery method of D-VB5 mother liquor of calcium.
Background technology
D-VB5 calcium also known as vitamin B5.As the component part of coacetylase, the internal carbohydrate of D-VB5 calcium participation,
The metabolism of fat and protein is that human body and animal maintain the indispensable micro substance of normal physiological function, in medicine, food
And it is widely used in the fields such as beverage additive.
Currently, the process for producing D-VB5 calcium using chemical synthesis is as follows：D-pantoyl lactone and Beta-alanine calcium first
Alcoholic solution occurs acylation reaction and generates D-VB5 calcium, and D-VB5 calcium crystallizes precipitation, after separating treatment, gained in methanol solution
Contain 95% methanol and remaining D-VB5 calcium in mother liquor.For the methanol in recycling mother liquor, existing method is as follows：First by mother liquor
It is passed through in the reboiler of rectifying column, methyl alcohol vaporizing is made by heating, condensed reflux later obtains methanol.In fact, passing through essence
Tower is evaporated treated the methanol for still having about 10% in mother liquor, needs to enter atmospheric distillation tower through decompression and make further recycling.
Above-mentioned method for dealcoholized exists following insufficient：One is residence time of the mother liquor in reboiler is longer, high temperature causes
D-VB5 calcium decomposes, and product recovery rate is low；The second is decompression operation increases system viscosity, mass transfer rate is caused to reduce, recycled
The methanol for still having 0.3% in obtained D-VB5 calcium, impacts product quality；The third is complex process, cumbersome, essence
It is plate column or packed tower to evaporate device therefor, has the disadvantages such as volume is big, efficiency is low, of high cost, high energy consumption.
Invention content
The object of the present invention is to provide a kind of recovery method of D-VB5 mother liquor of calcium, this method is simple, reliable, at low cost,
It can realize the effective recycling of resource.
To achieve the above object, the technical solution adopted by the present invention is：A kind of recovery method of D-VB5 mother liquor of calcium, by water
Steam and D-VB5 mother liquor of calcium each lead into it is high-gravity rotating bed in, after atmospheric gas proposes processing, methanol gas and Liquid Residue obtain
To separation, the condensed reflux of methanol gas later obtains methanol, and Liquid Residue moisturizing dissolves to obtain D-VB5 calcium aqueous solution, then to D-
Calcium pantothenate aqueous solution carries out decoloration and spray drying treatment successively, obtains D-VB5 calcium.
In use, vapor and D-VB5 mother liquor of calcium are directly entered high-gravity rotating bed middle progress normal pressure air lift operation, this
Sample one is being to eliminate huge vacuum and the chilled brine circulatory system, significantly for traditional rectifying decompression operation
Reduce investment and the energy consumption of equipment, two being system mass-transfer efficiency higher under normal pressure, the rate of recovery and product matter of D-VB5 calcium
Amount is more preferable, and three being that stripping temperature is low, avoids the decomposition of D-VB5 calcium, further improves the rate of recovery of D-VB5 calcium.By
This is as it can be seen that modified technique economic benefit provided by the invention and obvious environment benefit, recovered obtained methanol and D-VB5 calcium
Purity is high, high-quality, can be used directly.
Specific implementation mode
Technical solution disclosed by the invention is described further below by way of 4 embodiments：
Embodiment 1：D-VB5 mother liquor of calcium
(1) 1800kg absolute methanols are added into reaction vessel, 400kg Beta-alanines are added while stirring, add again later
Enter 160kg calcium oxide, 5kg activated carbon is added in insulation reaction 2 hours at 45 DEG C after reaction, first thick after stirring 0.5 hour
Filter, then secondary filter retain filtrate, obtain Beta-alanine calcium methanol solution；
(2) 580kgD- pantoic acid lactones are slowly added into Beta-alanine calcium methanol solution in 1 hour, then 25
Insulation reaction 3 hours at~35 DEG C, then it is cooled to 0-5 DEG C, and it is 5% to adjust reaction solution moisture, later at -5~-5 DEG C
Heat preservation crystallization 22 hours after crystallization completely, is separated by solid-liquid separation, obtains D-VB5 mother liquor of calcium；The D-VB5 mother liquor of calcium includes as follows
Ingredient：Water 4-6%, D-VB5 calcium 10-20%, surplus are methanol and inevitable impurity.
Embodiment 2：The recycling of D-VB5 mother liquor of calcium
D-VB5 mother liquor of calcium in Example 1, under the action of feed pump, by 2200L D-VB5s mother liquor of calcium and
The water vapour of 0.1MPa is passed through tri- layers of deflector type hypergravity rotations of BZ600-3P according to the volume flow rate of 1000L/h and 400L/h respectively
It in rotated bed, travels forward along baffling path, after atmospheric gas proposes processing, condensing reflux is carried out to obtained methanol gas and is handled
To methanol, the Liquid Residue obtained backward in isometric water be added be diluted dissolving, then adjusted with calcium hydroxide solution molten
Liquid PH to 7-8 obtains white D-VB5 calcium then by decoloration and spray drying treatment.
It recycles to obtain 1700kg methanol and 160kg white D-VB5 calcium by the method.
Sample detection is as a result as follows：G/C content 99.5% in methanol, the rate of recovery 95.6%, can be used directly.
D-VB5 calcium content 99.0%, 162 DEG C of fusing point, specific rotatory power [α] D23=+25.8 ° of (C=1, H2O), meet GB-T
7299-2006 D-VB5 standard calciums.
Embodiment 3：The recycling of D-VB5 mother liquor of calcium
Using the recovery method of embodiment 2,1690kg methanol and 158kgD- calcium pantothenates are obtained.
Sample detection is as a result as follows：G/C content 99.5% in methanol, the rate of recovery 93.8%, can be used directly.
D-VB5 calcium content 99.1%, 161 DEG C of fusing point, specific rotatory power [α] D23=+25.0 ° of (C=1, H2O), meet GB-T
7299-2006 D-VB5 standard calciums.
Comparative example 1：The recycling of D-VB5 mother liquor of calcium
It is disposably pumped into the reboiler of rectifying column, using steam by the D-VB5 calcium methanol mother liquor in Example 1
Indirectly heat, it is 80 DEG C or so to keep temperature in reboiler, and tower top temperature is 70 DEG C or so, and delivery temperature is less than 55 DEG C, tower top
Methanol steam through condensation, flow back, being cooled to 35~40 DEG C when be recycled to storage tank.The methanol solution of bottom of tower low concentration is through decompression
Make further recycling into atmospheric distillation tower, backward Liquid Residue (containing about 3-5% methanol) in that isometric water progress is added is dilute
Dissolving is released, then solution PH is adjusted to 7-8 with calcium hydroxide solution, then by decoloration and spray drying treatment, obtains D-VB5
Calcium.
It recycles to obtain 1200kg methanol and 192kg yellow-gray D-VB5 calcium powders by the method.
Sample detection is as a result as follows：Methanol G/C content 98.5%, the rate of recovery 66.7% cannot be used directly.
D-VB5 calcium content 85.6%, specific rotatory power [α] D23=+19.2 ° of (C=1, H2O), it cannot be satisfied GB-T 7299-
2006 D-VB5 standard calciums.
Claims (6)
1. a kind of recovery method of D-VB5 mother liquor of calcium, which is characterized in that each lead into water vapour and D-VB5 mother liquor of calcium super
In gravity revolving bed, after atmospheric gas proposes processing, methanol gas and Liquid Residue are detached, later the condensed reflux of methanol gas
Methanol is obtained, Liquid Residue moisturizing dissolves to obtain D-VB5 calcium aqueous solution, then D-VB5 calcium aqueous solution is decolourized and sprayed successively
Mist is dried, and obtains D-VB5 calcium.
2. the recovery method of D-VB5 mother liquor of calcium according to claim 1, which is characterized in that the D-VB5 mother liquor of calcium packet
Include following ingredient：Water 4-6%, D-VB5 calcium 10-20%, surplus are methanol and inevitable impurity.
3. the recovery method of D-VB5 mother liquor of calcium according to claim 1, which is characterized in that the Liquid Residue and water it is mixed
It is 1 to close mass ratio:0.5-1.5.
4. the recovery method of D-VB5 mother liquor of calcium according to claim 3, which is characterized in that the Liquid Residue and water it is mixed
It is 1 to close mass ratio:0.8-1.2.
5. the recovery method of D-VB5 mother liquor of calcium according to claim 1, which is characterized in that the D-VB5 calcium aqueous solution
It is 6-10 to be first adjusted to PH with PH conditioning agents, then carries out decoloration and spray drying treatment.
6. the recovery method of D-VB5 mother liquor of calcium according to claim 5, which is characterized in that the PH conditioning agents are selected from hydrogen
One kind in sodium hydroxide solution, potassium hydroxide solution and calcium hydroxide solution.
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| CN201810291698.5A CN108440332A (en) | 2018-03-30 | 2018-03-30 | The recovery method of D-VB5 mother liquor of calcium |
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| CN201810291698.5A CN108440332A (en) | 2018-03-30 | 2018-03-30 | The recovery method of D-VB5 mother liquor of calcium |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110845307A (en) * | 2019-11-28 | 2020-02-28 | 安徽泰格生物科技有限公司 | Method for recovering D-calcium pantothenate mother liquor |
| CN111410614A (en) * | 2020-05-14 | 2020-07-14 | 吴江 | Full-synthesis environment-friendly process of D-calcium pantothenate |
| CN113214046A (en) * | 2020-12-04 | 2021-08-06 | 安徽华恒生物科技股份有限公司 | Method for recycling D-calcium pantothenate mother liquor |
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| BE673670A (en) * | 1964-12-14 | |||
| CN1492934A (en) * | 2001-02-21 | 2004-04-28 | �����ɷ� | Method for producing D-pantothenic acid and/or salt thereof as additive for animal feesdstuffs |
| CN101514156A (en) * | 2009-03-27 | 2009-08-26 | 浙江车头制药有限公司 | Method for recycling naproxen resolution solvent, resolving agent and by-product by overgravitational field |
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2018
- 2018-03-30 CN CN201810291698.5A patent/CN108440332A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE673670A (en) * | 1964-12-14 | |||
| CN1492934A (en) * | 2001-02-21 | 2004-04-28 | �����ɷ� | Method for producing D-pantothenic acid and/or salt thereof as additive for animal feesdstuffs |
| CN101514156A (en) * | 2009-03-27 | 2009-08-26 | 浙江车头制药有限公司 | Method for recycling naproxen resolution solvent, resolving agent and by-product by overgravitational field |
Non-Patent Citations (1)
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| 王广全,等: "超重力精馏技术及其产业化应用", 《现代化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110845307A (en) * | 2019-11-28 | 2020-02-28 | 安徽泰格生物科技有限公司 | Method for recovering D-calcium pantothenate mother liquor |
| CN111410614A (en) * | 2020-05-14 | 2020-07-14 | 吴江 | Full-synthesis environment-friendly process of D-calcium pantothenate |
| CN113214046A (en) * | 2020-12-04 | 2021-08-06 | 安徽华恒生物科技股份有限公司 | Method for recycling D-calcium pantothenate mother liquor |
| CN113214046B (en) * | 2020-12-04 | 2023-07-28 | 安徽华恒生物科技股份有限公司 | Method for recycling D-calcium pantothenate mother liquor |
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Application publication date: 20180824 |