CN103483407B - A kind of Matachrom extractive crystallization double solvent and extractive crystallization method - Google Patents
A kind of Matachrom extractive crystallization double solvent and extractive crystallization method Download PDFInfo
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- CN103483407B CN103483407B CN201310468714.0A CN201310468714A CN103483407B CN 103483407 B CN103483407 B CN 103483407B CN 201310468714 A CN201310468714 A CN 201310468714A CN 103483407 B CN103483407 B CN 103483407B
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Abstract
The present invention relates to a kind of Matachrom extractive crystallization double solvent and extractive crystallization method, this double solvent is mixed by the benzene homologue of C6 ~ 12 alkane of 20% ~ 80% and C8 ~ 10 of 20% ~ 80%.Double solvent of the present invention solubleness in water is extremely low, can reduce the loss in extraction process; Density is little, extracts and return the emulsification of extraction process little, is easy to be separated; Cheap, the production cost of Matachrom can be reduced; The two kinds of solvent stabilities selected are high, can remove residue in solvent by acid, alkali and oxide treatment, and carry out distillation process without the need to consuming a large amount of steam, the solvent after process can reuse.Undertaken extracting and returning extraction by solvent of the present invention, realize the technique of the Matachrom of crystallization in aqueous phase, Matachrom quality is significantly better than the Matachrom of solvent phase crystallization, and in Matachrom of the present invention, Erythromycin A reaches between 84 ~ 86%.
Description
Technical field
The invention belongs to technical field of biological fermentation, particularly relate to a kind of Matachrom extractive crystallization double solvent and extractive crystallization method.
Background technology
Erythromycin is a class macrolide antibiotics, mainly comprises 6 kinds of components such as Erythromycin A, berythromycin, Erythromycin C, Erythromycin D, Erythromycin E and ErF, wherein the strongest with the antibacterial activity of Erythromycin A.Matachrom is a class macrolide antibiotics, is the thiocyanate-of erythromycin.Matachrom is veterinary drug, for the infection of gram-positive microorganism and mycoplasma; More as initial feed for the synthesis of macrolide antibiotics such as erythromycin, Roxithromycin, Azythromycin, clarithromycins.At present, the preparation of Matachrom mainly adopts two membrane process and extraction process, the solvent that wherein extraction process uses is mostly N-BUTYL ACETATE or the solvent containing N-BUTYL ACETATE, in N-BUTYL ACETATE water, solubleness reaches 1%, in extraction process, solvent loss is large, not only increase production cost, and a large amount of N-BUTYL ACETATEs enter waste water be difficult to process.
Summary of the invention
Object of the present invention is just the defect overcoming above-mentioned prior art, and provide a kind of solubleness low, solvent loss is little, and cost is low, is convenient to the Matachrom extractive crystallization double solvent processed;
Another object of the present invention is to provide the extractive crystallization method utilizing above-mentioned double solvent to carry out Matachrom.
Technical scheme taked for achieving the above object is:
A kind of Matachrom extractive crystallization double solvent, it is characterized in that being mixed by the benzene homologue of C6 ~ 12 alkane of 20% ~ 80% and C8 ~ 10 of 20% ~ 80%.
Described C6 ~ 12 alkane comprises straight-chain paraffin and naphthenic hydrocarbon, comprises hexanaphthene, normal hexane, heptane, octane, nonane, decane, undecane, dodecane.Benzene homologue is dimethylbenzene, partially triphen, isopropyl benzene etc.
A kind of Matachrom extractive crystallization method, it is characterized in that its processing step is: first adopt the double solvent mixed by the benzene homologue of C6 ~ 12 alkane of 10% ~ 90% and C8 ~ 10 of 10% ~ 90% to extract erythromycin filtrate, static separating obtained double solvent extraction liquid dewaters through saturated NaCl solution, activated carbon decolorizing, after filtration, add pure water, and then strip with acetum, in stripping solution, stream adds ammonium thiocyanate solution and carries out crystallization, and rear separation, drip washing, drying obtain Matachrom.
The volume ratio of described erythromycin filtrate and double solvent is 10:1 ~ 5.
Described extraction conditions is: extraction temperature 30 ~ 40 DEG C, extraction pH10.0 ~ 11.0.
Described reextraction condition is: acetum concentration is 10 ~ 20%, reextraction temperature 15 ~ 40 DEG C, pH4.5 ~ 5.5.
Described ammonium thiocyanate concentration of polymer solution is 10% ~ 50%, and its consumption adds 2.4 ~ 4ml ammonium thiocyanate solution according to every 100ml strip liquor stream, and stream adds 1.5 ~ 3.5 hours time.
Described used double solvent is first the process of the hydrochloric acid soln of 1 ~ 10% by concentration, and divide Xiang Houzai concentration of anhydrating to be 1 ~ 10% buck process, finally use 0.1 ~ 1% hydrogen peroxide to process, the solvent after process can reuse.
Matachrom extractive crystallization double solvent of the present invention has following technical superiority compared with N-BUTYL ACETATE:
The first, in water, solubleness is extremely low, is only 1 ‰, is 1/10th of N-BUTYL ACETATE, and thus in extraction process, loss reduces.
The second, density is little, extracts and return the emulsification of extraction process little, is easy to be separated.
Three, solvent is cheap, can reduce the production cost of Matachrom.
Four, two kinds of solvent stabilities selecting of the present invention are high, can remove residue in solvent by acid, alkali and oxide treatment, and carry out distillation process without the need to consuming a large amount of steam, the solvent after process can reuse.
5th: undertaken extracting and returning extraction by solvent of the present invention, realize the technique of the Matachrom of crystallization in aqueous phase, Matachrom quality is significantly better than the Matachrom of solvent phase crystallization, and in Matachrom of the present invention, Erythromycin A reaches between 84 ~ 86%.
Embodiment
The present invention is further described by following examples, and do not limit the present invention in any way, under the prerequisite not deviating from technical solution of the present invention, any change that those of ordinary skill in the art made for the present invention easily realize or change all will fall within claimed range of the present invention.
Embodiment 1
200ml(alkane 40%) decane and 300ml(benzene homologue 60%) isopropyl benzene mixing, join in 4000ml erythromycin filtrate, in filtrate, Erythromycin A concentration is 0.45%, add liquid caustic soda adjustment pH to 10.9,30 DEG C ~ 40 DEG C extractions, static separation obtains the double solvent extraction liquid that 500ml Erythromycin A concentration is 3.2%, erythromycin extraction liquid is after the dehydration of supersaturation NaCl solution, activated carbon decolorizing, filtration, add 500ml purified water and with 15% vinegar acid for adjusting pH to 4.9, staticly be separated 500ml returns extraction liquid, reextraction temperature controls at 15 DEG C ~ 40 DEG C.Return extract flow to add 10% ammonium thiocyanate 20ml(stream and add 1.5 ~ 3.5 hours time), complete crystallization, purified water drip washing after being separated, dry, obtain Matachrom 16.4g, moisture content 4.4%, the red middle Erythromycin A content 84.6% of sulphur.
Embodiment 2
200ml(alkane 40%) methylcyclohexane and 300ml(benzene homologue 60%) triphen mixing partially, join in 4000ml erythromycin filtrate, in filtrate, Erythromycin A concentration is 0.4%, add liquid caustic soda adjustment pH to 10.8,30 DEG C ~ 40 DEG C extractions, static separation obtains the double solvent extraction liquid that 500ml Erythromycin A concentration is 3.0%, erythromycin extraction liquid is after supersaturation NaCl dehydration, activated carbon decolorizing, filtration, add 500ml purified water and have 10% vinegar acid for adjusting pH to 4.8, staticly be separated 500ml returns extraction liquid, reextraction temperature controls at 15 DEG C ~ 40 DEG C.Return extract flow to add 20% ammonium thiocyanate 14ml(stream and add 1.5 ~ 3.5 hours time), complete crystallization, after being separated, purified water drip washing is dry, obtains Matachrom 15.8g, moisture content 4.6%, the red middle Erythromycin A content 84.9% of sulphur.
Embodiment 3
300ml(alkane 60%) nonane and 200ml(benzene homologue 40%) dimethylbenzene mixing, join in 4000ml erythromycin filtrate, in filtrate, Erythromycin A concentration is 0.35%, add liquid caustic soda adjustment pH to 10.5,30 DEG C ~ 40 DEG C extractions, static separation obtains the double solvent extraction liquid that 500ml Erythromycin A concentration is 2.8%, erythromycin extraction liquid, after supersaturation NaCl dehydration, activated carbon decolorizing, filtration, adds 500ml purified water and has 20% vinegar acid for adjusting pH to 5.3.Staticly be separated 500ml returns extraction liquid, reextraction temperature controls at 15 DEG C ~ 40 DEG C.Return extract flow to add 40% ammonium thiocyanate 12ml(stream and add 1.5 ~ 3.5 hours time), complete crystallization, after being separated, purified water drip washing is dry, obtains Matachrom 13.6g, moisture content 4.5%, the red middle Erythromycin A content 84.2% of sulphur.
Embodiment 4
100ml(alkane 20%) hexanaphthene and 400ml(benzene homologue 80%) butylbenzene mixing, join in 4000ml erythromycin filtrate, in filtrate, Erythromycin A concentration is 0.45%, add liquid caustic soda adjustment pH to 10.8,30 DEG C ~ 40 DEG C extractions, static separation obtains the double solvent extraction liquid that 500ml Erythromycin A concentration is 3.5%, and erythromycin extraction liquid, after supersaturation NaCl dehydration, activated carbon decolorizing, filtration, adds 500ml purified water and has 15% vinegar acid for adjusting pH to 5.3.Staticly be separated 500ml returns extraction liquid, reextraction temperature controls at 15 DEG C ~ 40 DEG C.Return extract flow to add 25% ammonium thiocyanate 14ml(stream and add 1.5 ~ 3.5 hours time), complete crystallization, after being separated, purified water drip washing is dry, obtains Matachrom 17.6g, moisture content 4.9%, the red middle Erythromycin A content 85.0% of sulphur.
Embodiment 5
400ml(alkane 80%) octane and 100ml(benzene homologue 20%) butylbenzene mixing, join in 4000ml erythromycin filtrate, in filtrate, Erythromycin A concentration is 0.43%, add liquid caustic soda adjustment pH to 10.5,30 DEG C ~ 40 DEG C extractions, static separation obtains the double solvent extraction liquid that 500ml Erythromycin A concentration is 3.2%, erythromycin extraction liquid, after supersaturation NaCl dehydration, activated carbon decolorizing, filtration, adds 500ml purified water and has 14% vinegar acid for adjusting pH to 5.3.Staticly be separated 500ml returns extraction liquid, reextraction temperature controls at 15 DEG C ~ 40 DEG C.Return extract flow to add 50% ammonium thiocyanate 14ml(stream and add 1.5 ~ 3.5 hours time), complete crystallization, after being separated, purified water drip washing is dry, obtains Matachrom 16.6g, moisture content 4.4%, the red middle Erythromycin A content 86.0% of sulphur.
Claims (6)
1. a Matachrom extractive crystallization method, it is characterized in that its processing step is: first adopt the double solvent mixed by the benzene homologue of C6 ~ 12 alkane of 10% ~ 90% and C8 ~ 10 of 10% ~ 90% to extract erythromycin filtrate, static separating obtained double solvent extraction liquid dewaters through saturated NaCl solution, activated carbon decolorizing, after filtration, add pure water, and then strip with acetum, in stripping solution, stream adds ammonium thiocyanate solution and carries out crystallization, and rear separation, drip washing, drying obtain Matachrom;
Described C6 ~ 12 alkane is decane, hexanaphthene, nonane or octane;
The benzene homologue of described C8 ~ 10 is dimethylbenzene, partially triphen or isopropyl benzene.
2. according to Matachrom extractive crystallization method according to claim 1, it is characterized in that: the volume ratio of described erythromycin filtrate and double solvent is 10:1 ~ 5.
3. according to Matachrom extractive crystallization method according to claim 1, it is characterized in that described extraction conditions is: extraction temperature 30 ~ 40 DEG C, extraction pH10.0 ~ 11.0.
4., according to Matachrom extractive crystallization method according to claim 1, it is characterized in that described reextraction condition is: acetum concentration is 10 ~ 20%, reextraction temperature 15 ~ 40 DEG C, pH4.5 ~ 5.5.
5. according to Matachrom extractive crystallization method according to claim 1, it is characterized in that described ammonium thiocyanate concentration of polymer solution is 10% ~ 50%, its consumption adds 2.4 ~ 4ml ammonium thiocyanate solution according to every 100ml strip liquor stream, and stream adds 1.5 ~ 3.5 hours time.
6. according to Matachrom extractive crystallization method according to claim 1, it is characterized in that: described used double solvent is first the process of the hydrochloric acid soln of 1 ~ 10% by concentration, Xiang Houzai concentration of anhydrating is divided to be 1 ~ 10% buck process, finally use 0.1 ~ 1% hydrogen peroxide to process, the solvent after process can reuse.
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| CN105777827A (en) * | 2014-12-15 | 2016-07-20 | 宁夏启元药业有限公司 | Extraction method of high-purity erythromycin E |
| CN105348340A (en) * | 2015-11-27 | 2016-02-24 | 宁夏启元药业有限公司 | Preparation method of erythromycin thiocyanate |
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| CN102858749A (en) * | 2010-04-20 | 2013-01-02 | 先正达参股股份有限公司 | Process for the preparation of pyrazole carboxylic acid amides |
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| FR1367842A (en) * | 1963-07-24 | 1964-07-24 | Pierrel Spa | Process for making a new water-soluble erythromycin salt |
| US3637654A (en) * | 1969-04-03 | 1972-01-25 | Abbott Lab | Purification of erythromycin thiocyanate |
| CN1050014A (en) * | 1989-07-18 | 1991-03-20 | 阿托化学公司 | Preparation 1, the method for two (4-the chloro-phenyl-)-trichloro-ethyl alcohol of 1- |
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| CN101133049A (en) * | 2005-03-03 | 2008-02-27 | 埃斯特维化学股份有限公司 | Process for the preparation of optically active derivatives of 2-(2-pyridylmethylsulfinyl)-benzimidazole via inclusion complex with 1,1'-binaphthalene-2, 2'diol |
| CN101624412A (en) * | 2008-07-10 | 2010-01-13 | 刘力 | Derivative of macrolides, method for preparing same and application thereof |
| CN102844306A (en) * | 2010-04-20 | 2012-12-26 | 先正达参股股份有限公司 | Process for preparation of pyrazole carboxylic acid amide |
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