CN106188376A - A kind of preparation method of colistin sulfate purification adsorbent - Google Patents
A kind of preparation method of colistin sulfate purification adsorbent Download PDFInfo
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- CN106188376A CN106188376A CN201610691194.3A CN201610691194A CN106188376A CN 106188376 A CN106188376 A CN 106188376A CN 201610691194 A CN201610691194 A CN 201610691194A CN 106188376 A CN106188376 A CN 106188376A
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- ethylene
- colistin sulfate
- purification adsorbent
- sulfate purification
- vinyl
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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
- 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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- Proteomics, Peptides & Aminoacids (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides the preparation method of a kind of colistin sulfate purification adsorbent: be distributed in water by a certain amount of vinylidene chloride, it is proportionally added into 5 norborene 1 methylcyclopentyl carboxylates, cyclopentadienyl group tetrahydroindenyl zirconium dichloride, Ammonium persulfate. and polyvinyl alcohol, 1 vinyl 3 1-Butyl-1H-imidazole tetrafluoroborate, VIPS ethylene three [(1 methyl ethylene) oxygen] silane, Ethylene Glycol Methyl vinyl ethers, heat up, react under preference temperature, product filters, dry, i.e. obtain colistin sulfate purification adsorbent.
Description
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the system of a kind of colistin sulfate purification adsorbent
Preparation Method.
Background technology
Colistin sulfate, have another name called colistin etc., white or near-white powder, odorless, bitter in the mouth have draw moist, soluble in water,
Being slightly soluble in methanol, ethanol, be practically insoluble in acetone, ether etc., free alkali is slightly soluble in water.Stablize in the range of PH3-7.5.Sulphuric acid
Colistin is produced by poly-viscosity bacillus, has stronger antibacterial action to gram negative bacteria, is used for treating gram negative bacteria and draws
The intestinal tract disease risen, as feed additive, and has obvious growth promoting function.Share preferably with sulfadiazine effect.
CN103073623B discloses the process for separation and purification of a kind of colistin sulfate, and the fermentation liquor that will produce is pre-
After process, enter continuous moving bed system；Continuous Moving Bed is provided with 30 resin columns, is divided into 3 functional areas；Wherein first district is
1-14 post, for adsorption zone；Renewing zone, second district is 15-24, parsing district of the 3rd district, for 25-30 post, uses multicolumn string
The mode of connection, feed liquid enters from 6-8 post, after 1 time adsorbs, then carries out 2 absorption at 9-11 post, and absorption terminates
Feed liquid and once wash material water mixing, enter 12-14 post finally adsorb；No. 30 posts are ER post, utilize product in pillar
The pure water in face ejects, and does not allow the water in post enter product；In this flow process, feed liquid is flowed by resin column ascending numerical direction, resin
The direction that post is successively decreased by resin column numeral rotates, and back action constantly circulates, produces continuously.
CN102718842B discloses a kind of sedimentation method and extracts the technique of colistin sulfate, comprises the following steps: (a) will
Fermentation liquid oxalic acid containing polymyxin E or concentrated sulphuric acid regulation pH value, filter through defecator；B () filtrate adds 0 metal
Chelating agent, inorganic flocculating agent, normal-temperature reaction 0.5-4.0h；The heating of (c) reactant liquor, cooling, sucking filtration；D () above-mentioned filtrate is molten with alkali
Liquid regulation pH value, solid-liquid separation obtains filter cake；Use sulfuric acid solution dissolving filter cake, obtain acidifying solution；Height it is separately added in acidifying solution
Potassium manganate and activated carbon, stir 0.5 ~ 2.0h, and sucking filtration obtains colistin sulfate liquid；E colistin sulfate liquid is centrifuged formula spray by ()
Mist is dried.
Existing colistin sulfate purifying technique has and repeats to adsorb often, operates complex, adsorbent speed
Degree causes the shortcoming that purity is low slowly, and product purity needs to improve.
Summary of the invention
It is an object of the invention to: providing the preparation method of a kind of colistin sulfate purification adsorbent, it can apply to
In colistin sulfate purification, its adsorption rate is fast, and adsorbing contaminant amount is big, easy and simple to handle during application.It is characterized in that preparation
Step includes:
A certain amount of vinylidene chloride is distributed in water, adds 5-norborene-1-methylcyclopentyl carboxylate in following ratio,
Cyclopentadienyl group tetrahydroindenyl zirconium dichloride, Ammonium persulfate. and polyvinyl alcohol, 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate, VIPS
Ethylene three [(1-methyl ethylene) oxygen] silane, Ethylene Glycol Methyl vinyl ethers, heat up, at 80-120 DEG C, react 8-18 hour,
Product filters, and dries, i.e. obtains colistin sulfate purification adsorbent.
Ingredients weight parts
Vinylidene chloride 100
5-norborene-1-methylcyclopentyl carboxylate 1-5
Cyclopentadienyl group tetrahydroindenyl zirconium dichloride 0.1-0.5
Ammonium persulfate. 0.5-1.5
Polyvinyl alcohol 2-3
1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.2-0.8
VIPS ethylene three [(1-methyl ethylene) oxygen] silane 0.1-0.5
Ethylene Glycol Methyl vinyl ethers 0.5-1
Water 1000
Described 5-norborene-1-methylcyclopentyl carboxylate is commercially available prod, and such as Zhengzhou, this produces with Chemical Co., Ltd.
Product；Cyclopentadienyl group tetrahydroindenyl zirconium dichloride is commercially available prod, the product produced such as regent biochemical technology company limited of Shenzhen；
1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate is commercially available prod, public affairs as limited in Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences
The product that department produces；VIPS ethylene three [(1-methyl ethylene) oxygen] silane is commercially available prod, such as Zhangjiakou Ai Ke fine chemistry industry
The product that Co., Ltd produces；Ethylene Glycol Methyl vinyl ethers is commercially available prod, the liter scientific and technological limited public affairs of chemistry as farsighted in Shanghai
The product that department produces.
The product of the present invention has the advantages that
Introduce 5-norborene-1-methylcyclopentyl carboxylate, cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 1-vinyl-3-fourth
Base tetrafluoroborate, VIPS ethylene three [(1-methyl ethylene) oxygen] silane, as polymerization monomer, adsorbent has higher
Heat stability and chemical stability, specific surface area is high, and adsorption rate is fast, and the amount of adsorbing contaminant is big, thus colistin sulfate is pure
Degree improves.
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
In 2000L reactor, add 1000Kg water, 100Kg vinylidene chloride, 3Kg5-norborene-1-methylcyclopentyl carboxylic acid
Ester, 0.3Kg cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 1Kg Ammonium persulfate., 2.5Kg polyvinyl alcohol, 0.5Kg1-vinyl-3-butyl
Tetrafluoroborate, 0.3KgVIPS ethylene three [(1-methyl ethylene) oxygen] silane, 0.8Kg Ethylene Glycol Methyl vinyl ethers,
Being warming up to 100 DEG C, react 12h, product filters, and dries, i.e. obtains colistin sulfate purification adsorbent.
Embodiment 2
In 2000L reactor, add 1000Kg water, 100Kg vinylidene chloride, 1Kg5-norborene-1-methylcyclopentyl carboxylic acid
Ester, 0.1Kg cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 0.5Kg Ammonium persulfate., 2Kg polyvinyl alcohol, 0.2Kg1-vinyl-3-butyl
Tetrafluoroborate, 0.1KgVIPS ethylene three [(1-methyl ethylene) oxygen] silane, 0.5Kg Ethylene Glycol Methyl vinyl ethers,
Being warming up to 80 DEG C, react 8h, product filters, and dries, i.e. obtains colistin sulfate purification adsorbent.
Embodiment 3
In 2000L reactor, add 1000Kg water, 100Kg vinylidene chloride, 5Kg5-norborene-1-methylcyclopentyl carboxylic acid
Ester, 0.5Kg cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 1.5Kg Ammonium persulfate., 3Kg polyvinyl alcohol, 0.8Kg1-vinyl-3-butyl
Tetrafluoroborate, 0.5KgVIPS ethylene three [(1-methyl ethylene) oxygen] silane, 1Kg Ethylene Glycol Methyl vinyl ethers, rise
Temperature, to 120 DEG C, reacts 18h, and product filters, and dries, i.e. obtains colistin sulfate purification adsorbent.
Comparative example 1
Being added without 5-norborene-1-methylcyclopentyl carboxylate, other conditions are with embodiment 1.
Comparative example 2
Being added without cyclopentadienyl group tetrahydroindenyl zirconium dichloride, other conditions are with embodiment 1.
Comparative example 3
Being added without 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate, other conditions are with embodiment 1.
Comparative example 4
Being added without VIPS ethylene three [(1-methyl ethylene) oxygen] silane, other conditions are with embodiment 1.
Comparative example 5
Being added without Ethylene Glycol Methyl vinyl ethers, other conditions are with embodiment 1.
Comparative example 6
It is added without the adsorbent product that this patent produces, adsorbs with activated carbon.
Embodiment 4
The colistin sulfate crude product solution of purity about 75% is passed through the suction made equipped with 500g embodiment 1-3 and comparative example 1-6
In the 1000mL exchange column of attached dose of product, temperature 50 C, flow velocity 1BV/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 colistin sulfate purity after the colistin sulfate adsorbent purification that different process is produced.
| Numbering | Colistin sulfate purity (%) |
| Embodiment 1 | 86.7 |
| Embodiment 2 | 85.3 |
| Embodiment 3 | 87.9 |
| Comparative example 1 | 83.7 |
| Comparative example 2 | 84.2 |
| Comparative example 3 | 84.6 |
| Comparative example 4 | 84.5 |
| Comparative example 5 | 84.8 |
| Comparative example 6 | 80.2 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with this
Based on bright, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (2)
1. a colistin sulfate purification adsorbent, it is characterised in that include following material component:
Ingredients weight parts
Vinylidene chloride 100
5-norborene-1-methylcyclopentyl carboxylate 1-5
Cyclopentadienyl group tetrahydroindenyl zirconium dichloride 0.1-0.5
Ammonium persulfate. 0.5-1.5
Polyvinyl alcohol 2-3
1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.2-0.8
VIPS ethylene three [(1-methyl ethylene) oxygen] silane 0.1-0.5
Water 1000.
2. the preparation method of a colistin sulfate purification adsorbent, it is characterised in that comprise the following steps:
By weight, 100 parts of vinylidene chlorides are distributed in 1000 parts of water, add 1-5 part 5-norborene-1-methyl ring penta
Yl carboxylic acid ester, 0.1-0.5 part cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 0.5-1.5 part Ammonium persulfate. and 2-3 part polyvinyl alcohol,
0.2-0.8 part 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate, 0.1-0.5 part VIPS ethylene three [(1-methyl ethylene) oxygen]
Silane, 0.5-1 part Ethylene Glycol Methyl vinyl ethers, heat up, at 80-120 DEG C, react 8-18 hour, product filters, and dries, i.e.
Obtain colistin sulfate purification adsorbent.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691194.3A CN106188376A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of colistin sulfate purification adsorbent |
| CN201710382962.1A CN107022003A (en) | 2016-08-21 | 2017-05-26 | A kind of preparation method of colistin sulfate scarvenger |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691194.3A CN106188376A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of colistin sulfate purification adsorbent |
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| CN106188376A true CN106188376A (en) | 2016-12-07 |
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| CN201610691194.3A Withdrawn CN106188376A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of colistin sulfate purification adsorbent |
| CN201710382962.1A Withdrawn CN107022003A (en) | 2016-08-21 | 2017-05-26 | A kind of preparation method of colistin sulfate scarvenger |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710382962.1A Withdrawn CN107022003A (en) | 2016-08-21 | 2017-05-26 | A kind of preparation method of colistin sulfate scarvenger |
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| CN108554391A (en) * | 2017-12-08 | 2018-09-21 | 孝感市锐思新材科技有限公司 | One kind three（Trimethyl silane）The preparation method of borate polymeric material |
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| CN105597711B (en) * | 2016-03-09 | 2018-11-23 | 徐州鸿丰高分子材料有限公司 | A kind of preparation method of the adsorbent material of binary acid treating |
| CN105859938A (en) * | 2016-06-13 | 2016-08-17 | 王金明 | Preparation of cobalt adsorbent |
| CN105833854A (en) * | 2016-06-13 | 2016-08-10 | 王金明 | Preparation method of purified vanadium adsorption material |
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2016
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Application publication date: 20161207 |