CN105646291A - Method for separating and purifying creatine mother liquor - Google Patents

Method for separating and purifying creatine mother liquor Download PDF

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Publication number
CN105646291A
CN105646291A CN201510993439.3A CN201510993439A CN105646291A CN 105646291 A CN105646291 A CN 105646291A CN 201510993439 A CN201510993439 A CN 201510993439A CN 105646291 A CN105646291 A CN 105646291A
Authority
CN
China
Prior art keywords
mother liquor
flesh
acid
creatine
flesh acid
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
Application number
CN201510993439.3A
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Chinese (zh)
Inventor
陈文如
任举
王建峰
温建华
司双喜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JIANGSU YUANYANG PHARMACEUTICAL CO Ltd
Original Assignee
JIANGSU YUANYANG PHARMACEUTICAL CO Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by JIANGSU YUANYANG PHARMACEUTICAL CO Ltd filed Critical JIANGSU YUANYANG PHARMACEUTICAL CO Ltd
Priority to CN201510993439.3A priority Critical patent/CN105646291A/en
Publication of CN105646291A publication Critical patent/CN105646291A/en
Priority to PCT/CN2016/110959 priority patent/WO2017114226A1/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C277/00Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
    • C07C277/08Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C279/00Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
    • C07C279/04Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of guanidine groups bound to acyclic carbon atoms of a carbon skeleton
    • C07C279/14Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of guanidine groups bound to acyclic carbon atoms of a carbon skeleton being further substituted by carboxyl groups

Abstract

The invention discloses a method for separating and purifying a creatine mother liquor. The method is as below: sending a mother liquor after creatine synthesis by using a pump through a feeding tube to an electrodialyser for separation. The mother liquor contains 0.01-5% of creatine and 0.1-25% of an inorganic salt; the electrodialyser is equipped with an electrodialysis membrane; and the electrodialysis membrane has different permeability on creatine and inorganic salt. The method for separating and purifying a creatine mother liquor is simple, economical and safe, and achieves clean production.

Description

The purification method of a kind of flesh acid mother liquor
Technical field
The present invention relates to separation technology field, particularly relate to the purification method of a kind of flesh acid mother liquor.
Background technology
Flesh acid (Creatine) is white powder crystallization, and without smelly, mildly bitter flavor, molecular formula is C4H9N3O2, molecular weight (MolecularWeight) is 131.13, is dissolved in water, is slightly soluble in cold water, is insoluble to dehydrated alcohol, ether and acetone.
Flesh acid is a kind of amino acid derivative, is the natural nutrient being present in human body, and in human body, flesh acid is synthesized in liver, kidney, pancreas. The synthesis promoting nucleic acid, protein, the deposit of increase energy i (in vivo) material, the growth of promotion muscle, and delay fatigue and acceleration physical efficiency recovery are had important effect by flesh acid.
At present, the production of this product and application all being given enough attention both at home and abroad, report document is also more, and the route that foreign literature mentions synthesis flesh acid mainly contains following several:
1) calcyanide and sodium sarcosinate reactant aqueous solution directly generate flesh acid;
2) calcyanide reacts to obtain O-methyl-isourea hydrochloride with the methanol solution being saturated with dry hydrogen chloride gas, and O-methyl-isourea hydrochloride is obtained by reacting flesh acid again with sarkosine;
3) calcyanide and aqueous hydrochloric acid generate chlorine for first amidine muriate when leading to air, are then obtained by reacting flesh acid with sodium sarcosinate;
4) Mono Chloro Acetic Acid and first amine are obtained by reacting sodium sarcosinate or sarkosine potassium, then are obtained by reacting flesh acid with cyanamide;
5) generate S-methyl-isourea by raw material of thiocarbamide and methyl-sulfate, S-methyl-isourea again with sarkosine, sodium sarcosinate or sarkosine nak response to flesh acid.
6) urea and methyl-sulfate are obtained by reacting O-methyl-isourea methyl sulfate, need not be further purified, then are obtained by reacting flesh acid with sodium sarcosinate.
By comparing, which kind of method ineffective, the mother liquor of synthesis flesh acid all can have the existence of sodium salt and sylvite, owing to environmental protection pond requires that the salt of water inlet is lower, mother liquor not directly discharges, and mother liquor contains flesh acid and a large amount of salt, it is possible to while recycling mother liquor improve effects, reduce the pressure to environmental protection. Existing carry out desalination purification mother liquor by ion-exchange resin and concentrated method, but these method cost compares are big, and environment can be produced secondary pollution.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of simple and easy to do, economic, not only safety but also can realize the purification method of the flesh acid mother liquor of cleanly production.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is:
The purification method of a kind of flesh acid mother liquor is provided, the mother liquor after synthesis flesh acid is utilized pump delivered in electrodialyzer by liquid pushing tube and is separated;Containing massfraction in described mother liquor is the flesh acid of 0.01 ~ 5% and the inorganic salt of 0.1 ~ 25%; In described electrodialyzer, electrodialytic membranes being housed, described electrodialytic membranes is different with inorganic salt perviousness to flesh acid.
In a preferred embodiment of the present invention, described inorganic salt are sodium-chlor.
In a preferred embodiment of the present invention, the temperature of described mother liquor is 10 ~ 50 DEG C.
The invention has the beneficial effects as follows: the purification method of a kind of flesh acid mother liquor of the present invention, can minimizing energy consumption by a relatively large margin, the acid of flesh in flesh acid mother liquor is thoroughly separated with inorganic salt, and whole production process does not produce " three wastes ", production environment is good, the total recovery of product obviously increases, and quality product significantly improves, and is desirable environmental protection technique.
Embodiment
Below the better embodiment of the present invention is described in detail, so that advantages and features of the invention can be easier to be readily appreciated by one skilled in the art, thus protection scope of the present invention is made more explicit defining.
Embodiment 1: by containing massfraction be 0.8% flesh acid with the 500g flesh acid mother liquor of 25% sodium-chlor at 20 DEG C of temperature, pump is utilized to pass through liquid pushing tube, deliver in the electrodialyzer of in-built electrodialytic membranes, owing to electrodialytic membranes is different with the electric conductivity of inorganic salt to flesh acid, different by property, such that it is able to be thoroughly separated flesh acid and inorganic salt, adding appropriate water synergy in electrodialyzer, it be 24.5% sodium chloride aqueous solution and 98g massfraction is the flesh aqueous acid of 0.14% that final process obtains 479g massfraction.
Embodiment 2: by containing massfraction be 2% flesh acid with the 500g flesh acid mother liquor of 5% sodium-chlor at 20 DEG C of temperature, pump is utilized to pass through liquid pushing tube, deliver in the electrodialyzer of in-built electrodialytic membranes, add appropriate water, final process obtain 491g massfraction be 4.5% sodium chloride aqueous solution and 94g massfraction be 0.48% flesh aqueous acid.
Embodiment 3: by containing massfraction be 5% flesh acid with the 500g flesh acid mother liquor of 10% sodium-chlor at 20 DEG C of temperature, pump is utilized to pass through liquid pushing tube, deliver in the electrodialyzer of in-built electrodialytic membranes, add appropriate water, final process obtain 488g massfraction be 9.75% sodium chloride aqueous solution and 89g massfraction be 0.88% flesh aqueous acid.
The foregoing is only embodiments of the invention; not thereby the patent scope of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, all it is included in the scope of patent protection of the present invention with reason.

Claims (3)

1. the purification method of a flesh acid mother liquor, it is characterised in that, the mother liquor after synthesis flesh acid is utilized pump delivered in electrodialyzer by liquid pushing tube and is separated; Containing massfraction in described mother liquor is the flesh acid of 0.01 ~ 5% and the inorganic salt of 0.1 ~ 25%; In described electrodialyzer, electrodialytic membranes being housed, described electrodialytic membranes is different with inorganic salt perviousness to flesh acid.
2. the purification method of flesh acid mother liquor according to claim 1, it is characterised in that, described inorganic salt are sodium-chlor.
3. the purification method of flesh acid mother liquor according to claim 1, it is characterised in that, the temperature of described mother liquor is 10 ~ 50 DEG C.
CN201510993439.3A 2015-12-28 2015-12-28 Method for separating and purifying creatine mother liquor Pending CN105646291A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201510993439.3A CN105646291A (en) 2015-12-28 2015-12-28 Method for separating and purifying creatine mother liquor
PCT/CN2016/110959 WO2017114226A1 (en) 2015-12-28 2016-12-20 Method for separating and purifying creatine mother liquor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510993439.3A CN105646291A (en) 2015-12-28 2015-12-28 Method for separating and purifying creatine mother liquor

Publications (1)

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CN105646291A true CN105646291A (en) 2016-06-08

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WO (1) WO2017114226A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017114226A1 (en) * 2015-12-28 2017-07-06 江苏远洋药业股份有限公司 Method for separating and purifying creatine mother liquor

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114591203B (en) * 2022-02-15 2024-03-29 上海奥萝拉医药科技有限公司 Preparation method of high-purity creatine

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101415672A (en) * 2006-04-06 2009-04-22 澳泽化学特罗斯特贝格有限公司 Process for preparing creatine, creatine monohydrate or guanidinoacetic acid
CN101967106A (en) * 2010-09-01 2011-02-09 河北宏源化工有限公司 Method for treating L-p-hydroxyphenylglycine desalting mother liquor by adopting bipolar membrane electrodialysis technology
CN103664665A (en) * 2013-12-13 2014-03-26 天津天成制药有限公司 Solid sodium sarcosine preparation method
CN104744280A (en) * 2015-04-07 2015-07-01 湖北锡太化工有限公司 Method of preparing sarcosine by bipolar membrane electrodialysis process

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105646291A (en) * 2015-12-28 2016-06-08 江苏远洋药业股份有限公司 Method for separating and purifying creatine mother liquor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101415672A (en) * 2006-04-06 2009-04-22 澳泽化学特罗斯特贝格有限公司 Process for preparing creatine, creatine monohydrate or guanidinoacetic acid
CN101967106A (en) * 2010-09-01 2011-02-09 河北宏源化工有限公司 Method for treating L-p-hydroxyphenylglycine desalting mother liquor by adopting bipolar membrane electrodialysis technology
CN103664665A (en) * 2013-12-13 2014-03-26 天津天成制药有限公司 Solid sodium sarcosine preparation method
CN104744280A (en) * 2015-04-07 2015-07-01 湖北锡太化工有限公司 Method of preparing sarcosine by bipolar membrane electrodialysis process

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
汪耀明等: "电渗析技术清洁分离纯化肌氨酸", 《化工学报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017114226A1 (en) * 2015-12-28 2017-07-06 江苏远洋药业股份有限公司 Method for separating and purifying creatine mother liquor

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Application publication date: 20160608