CN106311166A - Method for preparing adsorbent used for purification of acetylisovaleryltylosin tartrate - Google Patents
Method for preparing adsorbent used for purification of acetylisovaleryltylosin tartrate Download PDFInfo
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- CN106311166A CN106311166A CN201610691175.0A CN201610691175A CN106311166A CN 106311166 A CN106311166 A CN 106311166A CN 201610691175 A CN201610691175 A CN 201610691175A CN 106311166 A CN106311166 A CN 106311166A
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- ether
- thousand rhzomorph
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/08—Vinylidene chloride
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Abstract
The invention provides a method for preparing an adsorbent used for purification of acetylisovaleryltylosin tartrate. The method comprises the following steps: dispersing a certain amount of vinylidene chloride in water, adding 3-(4-iodo-phenyl)-1-(4'-boryl-phenyl)-proply-2-ketene, 2-(allyloxymethyl)-18-crown-6-ether, ammonium persulfate, polyvinyl alcohol, 2-acrylylamino-2-methyl-1-propanesulfonic acid, 5-norbornene-2-carboxylic acid-2-tetrahydropyrane ester and 10-alkenylhendecyloxytrimethylsilane, heating, carrying out a reaction at a proper temperature, filtering the product, and drying, so as to obtain the adsorbent used for purification of acetylisovaleryltylosin tartrate.
Description
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the preparation method of a kind of safe ten thousand rhzomorph purification adsorbents.
Background technology
Safe ten thousand rhzomorphs are the abbreviations of tartaric acid acetylisovaleryl tylosin, tartaric acid acetylisovaleryl tylosin
(Aivlosin Tartrate is called for short AIV), is the macrolide antibiotics of a new generation. general English name:
Acetylisovalery tylosin.AIV be on the basis of tylosin through biofermentation semi-synthetic and obtain a kind of big
Cyclic lactone class poultry special antibiotic .AIV has opposing activity to many gram positive bacterias and some negative bacterium, embrace include former
Body, vibrio, spirillum and big virus, to Mycoplasma gallisepticum, pig popularity pneumonia, pig bloody dysentery etc. has the curative effect of uniqueness.
CN104610403A discloses a kind of new method utilizing safe ten thousand rhzomorphs of purified on silica, and the method is with post layer by layer
Analysis silica gel is separating medium, with following substances composition mixed liquor as eluent, safe ten thousand rhzomorph crude products are purified: 1) oil
Ether；2) ethyl acetate and/or butyl acetate；With 3) diethylamine, one or many in triethylamine and N, N-diisopropyl ethyl amine
Kind, safe ten thousand rhzomorph crude products are purified, and by rotary evaporation to obtain safe ten thousand rhzomorphs of high-purity.
CN105030801A discloses the preparation method of a kind of safe ten thousand rhzomorph preparations, and wherein, this preparation method includes: (1)
Be added to the water dissolving by wall material, is configured to binder solution, this wall material be ratio be polylactic acid and the arabic gum of 1:1；(2)
Safe ten thousand rhzomorph heartwoods are added in this binder solution, mix homogeneously, make mixture；And (3) are by preparation in this step (2)
Mixture be spray-dried, be prepared as this safe ten thousand rhzomorph preparations.
Existing safe ten thousand rhzomorph purification techniques, the adsorbent effect scarcely using adsorbent or employing is poor, leads
The purity causing safe ten thousand rhzomorph products has bigger restriction.
Summary of the invention
It is an object of the invention to: providing the preparation method of a kind of safe ten thousand rhzomorph purification adsorbents, it can apply to Thailand
In ten thousand rhzomorph purifications, its adsorption rate is fast, and adsorbing contaminant amount is big, so applying the Thailand ten thousand rhzomorph product that this adsorbent produces
Purity is high.It is characterized in that preparation process includes:
A certain amount of vinylidene chloride is distributed in water, adds 3-(the iodo-phenyl of 4-)-1-(4 '-boryl-benzene in following ratio
Base)-propyl-2-ketenes, 2-(allyloxy methyl)-18-crown-6-ether, Ammonium persulfate. and polyvinyl alcohol, 2-acrylamido-2-
Methyl isophthalic acid-propane sulfonic acid, 5-norborene-2-carboxylic acid-2-tetrahydropyrans ester, 10-thiazolinyl hendecane epoxide trimethyl silane, rise
Temperature, at 80-120 DEG C, reacts 6-16 hour, and product filters, and dries, i.e. obtains safe ten thousand rhzomorph purification adsorbents.
Ingredients weight parts
Vinylidene chloride 100
3-(the iodo-phenyl of 4-)-1-(4 '-boryl-phenyl)-propyl-2-ketenes 0.01-0.1
2-(allyloxy methyl)-18-crown-6-ether 0.1-0.5
Ammonium persulfate. 2-3
Polyvinyl alcohol 1-2
2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid 0.01-0.1
5-norborene-2-carboxylic acid-2-tetrahydropyrans ester 0.01-0.1
10-thiazolinyl hendecane epoxide trimethyl silane 0.01-0.1
Water 1000
Described 3-(the iodo-phenyl of 4-)-1-(4 '-boryl-phenyl)-propyl-2-ketenes is commercially available prod, such as Beijing An Biqisheng
The product that thing Science and Technology Ltd. produces；2-(allyloxy methyl)-18-crown-6-ether is commercially available prod, chemistry as vast in Shanghai ancient cooking vessel
The product that Science and Technology Ltd. produces；2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid is commercially available prod, as biology is ground in Shanghai one
The product that Science and Technology Ltd. produces；5-norborene-2-carboxylic acid-2-tetrahydropyrans ester is commercially available prod, such as Alpha's chemical industry
The product that company limited produces；10-thiazolinyl hendecane epoxide trimethyl silane is commercially available prod, such as Shanghai Chu Qing new material science and technology
The product that company limited produces.
The product of the present invention has the advantages that
Introduce 3-(the iodo-phenyl of 4-)-1-(4 '-boryl-phenyl)-propyl-2-ketenes, 2-acrylamido-2-methyl isophthalic acid-the third
Sulfonic acid, phosphoenolpyruvate, 5-norborene-2-carboxylic acid-2-tetrahydropyrans ester, 10-thiazolinyl hendecane epoxide trimethyl silicane
Alkane, as polymerization monomer, adsorbent has higher heat stability and chemical stability, and specific surface area is high, and adsorption rate is fast, inhales
The amount of attached impurity is big, so the Thailand ten thousand rhzomorph product purity produced is higher.
Detailed description of the invention
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
100Kg polyvinyl alcohol, 1000Kg water, 0.05Kg3-(the iodo-phenyl of 4-)-1-(4 '-borine is added in 2000L reactor
Base-phenyl)-propyl-2-ketenes, 0.3Kg2-(allyloxy methyl)-18-crown-6-ether, 2.5Kg Ammonium persulfate., 1.5Kg polyethylene
Alcohol, 0.05Kg2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid, 0.05Kg5-norborene-2-carboxylic acid-2-tetrahydropyrans ester,
0.05Kg10-thiazolinyl hendecane epoxide trimethyl silane, is warming up to 100 DEG C, reacts 11h, and product filters, and dries, i.e. obtains Thailand
Ten thousand rhzomorph purification adsorbents.
Embodiment 2
100Kg polyvinyl alcohol, 1000Kg water, 0.01Kg3-(the iodo-phenyl of 4-)-1-(4 '-borine is added in 2000L reactor
Base-phenyl)-propyl-2-ketenes, 0.1Kg2-(allyloxy methyl)-18-crown-6-ether, 2Kg Ammonium persulfate., 1Kg polyvinyl alcohol,
0.01Kg2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid, 0.01Kg5-norborene-2-carboxylic acid-2-tetrahydropyrans ester,
0.01Kg10-thiazolinyl hendecane epoxide trimethyl silane, is warming up to 80 DEG C, reacts 6h, and product filters, and dries, and i.e. obtains safe ten thousand
Rhzomorph purification adsorbent.
Embodiment 3
100Kg polyvinyl alcohol, 1000Kg water, 0.1Kg3-(the iodo-phenyl of 4-)-1-(4 '-borine is added in 2000L reactor
Base-phenyl)-propyl-2-ketenes, 0.5Kg2-(allyloxy methyl)-18-crown-6-ether, 3Kg Ammonium persulfate., 2Kg polyvinyl alcohol,
0.1Kg2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid, 0.1Kg5-norborene-2-carboxylic acid-2-tetrahydropyrans ester,
0.1Kg10-thiazolinyl hendecane epoxide trimethyl silane, is warming up to 120 DEG C, reacts 16h, and product filters, and dries, and i.e. obtains safe ten thousand
Rhzomorph purification adsorbent.
Comparative example 1
Being added without 3-(the iodo-phenyl of 4-)-1-(4 '-boryl-phenyl)-propyl-2-ketenes, other conditions are with embodiment 1.
Comparative example 2
Being added without 2-(allyloxy methyl)-18-crown-6-ether, other conditions are with embodiment 1.
Comparative example 3
Being added without 2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid, other conditions are with embodiment 1.
Comparative example 4
Being added without 5-norborene-2-carboxylic acid-2-tetrahydropyrans ester, other conditions are with embodiment 1.
Comparative example 5
Being added without 10-thiazolinyl hendecane epoxide trimethyl silane, other conditions are with embodiment 1.
Comparative example 6
It is added without the adsorbent product that the present invention is produced, adsorbs with activated carbon.
Embodiment 4
The Thailand ten thousand thick product of rhzomorph of mass percent concentration about 85% is passed through and inhales equipped with 500g embodiment 1-3 and comparative example 1-6
The 1000L exchange column of attached dose of product, temperature 60 C, flow velocity 0.5BV/h, under the conditions of absorption purify, flow out by gas chromatographic detection
The weight/mass percentage composition of liquid, is shown in Table 1.
Table 1: the Thailand ten thousand rhzomorph product purity after the adsorbent product absorption that different process is produced.
| Numbering | Safe ten thousand rhzomorph purity (%) |
| Embodiment 1 | 96.8 |
| Embodiment 2 | 95.9 |
| Embodiment 3 | 97.3 |
| Comparative example 1 | 94.6 |
| Comparative example 2 | 95.1 |
| Comparative example 3 | 94.8 |
| Comparative example 4 | 95.2 |
| Comparative example 5 | 95.4 |
| Comparative example 6 | 92.1 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with the present invention it is
Basis, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, equivalent are replaced
Change or modification etc., be all covered by among protection scope of the present invention.
Claims (2)
1. a Thailand ten thousand rhzomorph purification adsorbent, it is characterised in that include following material component:
Ingredients weight parts
Vinylidene chloride 100
3-(the iodo-phenyl of 4-)-1-(4 '-boryl-phenyl)-propyl-2-ketenes 0.01-0.1
2-(allyloxy methyl)-18-crown-6-ether 0.1-0.5
Ammonium persulfate. 2-3
Polyvinyl alcohol 1-2
2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid 0.01-0.1
5-norborene-2-carboxylic acid-2-tetrahydropyrans ester 0.01-0.1
10-thiazolinyl hendecane epoxide trimethyl silane 0.01-0.1
Water 1000.
2. the preparation method of a Thailand ten thousand rhzomorph purification adsorbent, it is characterised in that comprise the following steps:
A certain amount of vinylidene chloride is distributed in water, be proportionally added into 3-(the iodo-phenyl of 4-)-1-(4 '-boryl-phenyl)-
Acrylate-2-ketenes, 2-(allyloxy methyl)-18-crown-6-ether, Ammonium persulfate. and polyvinyl alcohol, 2-acrylamido-2-first
Base-1-propane sulfonic acid, 5-norborene-2-carboxylic acid-2-tetrahydropyrans ester, 10-thiazolinyl hendecane epoxide trimethyl silane, heat up,
At 80-120 DEG C, reacting 6-16 hour, product filters, and dries, i.e. obtains safe ten thousand rhzomorph purification adsorbents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691175.0A CN106311166A (en) | 2016-08-21 | 2016-08-21 | Method for preparing adsorbent used for purification of acetylisovaleryltylosin tartrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691175.0A CN106311166A (en) | 2016-08-21 | 2016-08-21 | Method for preparing adsorbent used for purification of acetylisovaleryltylosin tartrate |
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| CN201610691175.0A Pending CN106311166A (en) | 2016-08-21 | 2016-08-21 | Method for preparing adsorbent used for purification of acetylisovaleryltylosin tartrate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755855A (en) * | 2014-01-06 | 2014-04-30 | 巨化集团技术中心 | Preparation method of spherical polyvinylidene chloride resin with micropore structures |
| CN104058370A (en) * | 2014-06-13 | 2014-09-24 | 王金明 | Method for purifying dimethyl dichlorosilane hydrolysis byproduct hydrochloric acid |
| CN105597711A (en) * | 2016-03-09 | 2016-05-25 | 张玲 | Preparation method of binary acid refined adsorbing material |
-
2016
- 2016-08-21 CN CN201610691175.0A patent/CN106311166A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755855A (en) * | 2014-01-06 | 2014-04-30 | 巨化集团技术中心 | Preparation method of spherical polyvinylidene chloride resin with micropore structures |
| CN104058370A (en) * | 2014-06-13 | 2014-09-24 | 王金明 | Method for purifying dimethyl dichlorosilane hydrolysis byproduct hydrochloric acid |
| CN105597711A (en) * | 2016-03-09 | 2016-05-25 | 张玲 | Preparation method of binary acid refined adsorbing material |
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Address after: 432000 Hubei city of Xiaogan province high tech Zone Qun Sheng Cun Nan Qu Bian min Lu 5 floor, room 91 Applicant after: Wang Qiyu Address before: 432000 Hubei city of Xiaogan province high tech Zone Danyang District Community Lisi mall two Room 201 Applicant before: Wang Qiyu |
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Address after: The new school district 322009 town Zhejiang city Yiwu province 5 Building 1 unit 201 room Applicant after: Wang Qiyu Address before: 432000 Hubei city of Xiaogan province high tech Zone Qun Sheng Cun Nan Qu Bian min Lu 5 floor, room 91 Applicant before: Wang Qiyu |
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Application publication date: 20170111 |