CN107163176A - A kind of preparation method of macroporous absorbent resin - Google Patents
A kind of preparation method of macroporous absorbent resin Download PDFInfo
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- CN107163176A CN107163176A CN201710411666.XA CN201710411666A CN107163176A CN 107163176 A CN107163176 A CN 107163176A CN 201710411666 A CN201710411666 A CN 201710411666A CN 107163176 A CN107163176 A CN 107163176A
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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
- C08F212/00—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 an aromatic carbocyclic ring
- C08F212/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F212/36—Divinylbenzene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or 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 an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
Abstract
A kind of preparation method of macroporous absorbent resin, it is characterised in that including the steps：The preparation of monomer：The dilute benzene of diethyl, methacrylate, dibenzoyl peroxide are put into reactor by formula, are stirred at room temperature 25~30 minutes, pore-foaming agent hexamethylene is put into, is stirred at room temperature 25~30 minutes, the preparation of aqueous phase：Appropriate water is put into a kettle., powder salt is then put into, and stirring make it that salt solution is uniform.Gelatin is put into, methylene blue is stirred and heated to 55~60 DEG C, turn off stirring in advance, the amount of monomer prepared is pumped into reactor, empty stirring 10~15 minutes is not heated, aqueous phase is 55~60 DEG C at the beginning, and it is 40~45 DEG C or so to finish the temperature in monomer reaction kettle.After treating empty stirring 10~15 minutes, 68~70 DEG C are to slowly warm up to.Start to be incubated timing, after being incubated 4~5 hours, steam heating is to slowly warm up to 70~75 DEG C, is incubated 6~7 hours, is during which not related to stirring.
Description
Background technology
Macroporous absorbent resin is that a class is free of cation exchange groups and has the preparation of macroporous structure, with good
Macroreticular structure and larger specific surface area, can be 20 generation optionally through the organic matter in the physical absorption aqueous solution
Record the new organic polymer adsorbent that the grows up sixties.
Macroporous absorbent resin adsorption technology is used for wastewater treatment, medical industry, chemical industry, analytical chemistry, clinic earliest
The field such as calibrating and treatment, is widely used in the extracting and developing of Chinese herbal medicine effective ingredientses, purification work in China in recent years.
Compared with Chinese medicine preparation traditional handicraft, using the extract obtained small volume of macroporous absorbent resin technology, it is nonhygroscopic, external form is easily made
Various formulations attractive in appearance, are particularly suitable for use in granule, capsule and tablet, change the thick, black, big existing of traditional Chinese medicine compound preparation
As being conducive to the upgrading of Chinese medicine preparation formulation, promoting the development of modernization of cmm, State Administration of Traditional Chinese Medicine etc.
The 2002 ~ 2010 of unit consolidation issue《Medical science technical policy》Clearly propose：Chinese medicine dynamic countercurrent is developed to extract, surpass
The technologies such as critical extraction, prepared slices of Chinese crude drugs infiltration, macroreticular resin separation.
The macroporous absorbent resin for being used for stevioside extraction in current industrial production is generally AB-8, D101 model, and these are normal
That organic residue is high with resin generally existing, pretreatment difficulty is big, and particle diameter distribution is wide, inferior separating effect, the problems such as short life.
The content of the invention
It is an object of the invention to provide a kind of adsorption capacity, resistance tocrocking, selectivity it is stronger, the effect of recycling is more preferable
Macroporous absorbent resin preparation method.
The technical scheme is that：A kind of preparation method of macroporous absorbent resin, it is characterised in that including following step
Suddenly：
（1）The preparation of monomer：The dilute benzene of diethyl, methacrylate, dibenzoyl peroxide are put into reactor by formula, room temperature
Stirring 25~30 minutes, puts into pore-foaming agent hexamethylene, is stirred at room temperature 25~30 minutes；
（2）The preparation of aqueous phase：Appropriate water is put into a kettle., powder salt is then put into, and stirring make it that salt solution is uniform.Input is bright
Glue, methylene blue is stirred and heated to 55~60 DEG C, and stirring is turned off in advance；
（3）The amount of monomer prepared is pumped into reactor, empty stirring 10~15 minutes is not heated, aqueous phase is 55~60 at the beginning
DEG C, it is 40~45 DEG C or so to finish the temperature in monomer reaction kettle.After treating empty stirring 10~15 minutes, 68 are to slowly warm up to~
70℃.Start to be incubated timing, after being incubated 4~5 hours, steam heating is to slowly warm up to 70~75 DEG C, is incubated 6~7 hours, during which
It is not related to stirring；
（4）Wash greatly；
（5）Post processing, material for making clothes was carried out between water sieve, 16~50 mesh, finished product of packing.
The preparation method of macroporous absorbent resin according to claim 1, it is characterised in that the step（1）Monomer
Feed intake and be formulated and be：
The dilute benzene of diethyl（Cross-linking monomer）, 120~130kg；Methacrylate（Monomer）, 9~10kg；Dibenzoyl peroxide（Urge
Agent）, 1~1.5kg；Hexamethylene（Pore-foaming agent）, 170~180kg.
It is preferred that, it is made up of following formula：
The dilute benzene of diethyl（Cross-linking monomer）, 122~128kg；Methacrylate（Monomer）, 9.2~9.8kg；Dibenzoyl peroxide
（Catalyst）, 1.1~1.4kg；Hexamethylene（Pore-foaming agent）, 175~178kg.
It is preferred that, it is made up of following formula：
The dilute benzene of diethyl（Cross-linking monomer）, 125~127kg；Methacrylate（Monomer）, 9.3~9.6kg；Dibenzoyl peroxide
（Catalyst）, 1.1~1.3kg；Hexamethylene（Pore-foaming agent）, 176~177kg.
The step（2）The proportion of salt solution be 1.12 to 1.2 between, 7~9kg of gelatin；Remaining is methylene blue.
The preparation method of macroporous absorbent resin according to claim 1, it is characterised in that the step（4）Heat
Coolant-temperature gage is 45~50 DEG C, and the time washed greatly every time is 10~15 minutes, by that analogy 4 to 5 times.
The step（5）Post processing concrete operations flow be：
（1）In material input reactor, discharge water and start distillation, distillation removes pore-foaming agent hexamethylene；
（2）In resin Archon input reactor, methanol is first pumped into, stirring is opened.Liquid caustic soda is pumped into again so that pH value is 7~8.Open
Beginning is warming up to 50~55 DEG C.Stirring is closed, constant temperature flows back 4~5 hours.Then methanol is drained；
（3）Into reactor, input reclaims methanol, puts into hydrochloric acid, and it is 3~4 to open stirring and adjusting pH value, is warming up to 50~55 DEG C, pass
It is stirred at reflux insulation 4~5 hours, then methanol is drained；
（4）Into reactor, input reclaims methanol, opens stirring and is warming up to 50~55 DEG C, is incubated 4~5 hours；
（5）New methanol is put into reactor, stirring is opened and is warming up to 50~55 DEG C, be incubated 4~5 hours；
（6）New ethanol is put into reactor, stirring is opened and is warming up between 50~55 DEG C, 4~5 hours are incubated；
（7）The methanol or ethanol of an above-mentioned step are drained, discharges water and boils to more than 100 DEG C, until no alcohol taste can blowing.
Step of the present invention（5）Resin end properties parameter be：
| Outward appearance | The opaque spherical particle of milky |
| Granularity（0.3 ~ 1.25mm of particle size range）/（%） | ≥95 |
| Water content/（%） | 70~85 |
| Wet true density/（g/ml） | 1.1~1.2 |
| Wet apparent density/（g/ml） | 0.6~0.7 |
| Than surface/（m2/g） | 490~530 |
| Average pore size/（nm） | 27~30 |
| Porosity/（%） | 42~46 |
| Pore volume/（ml/g） | 1.25~1.30 |
| Maximum operation (service) temperature/（℃） | 150 |
Macroporous absorbent resin suction-operated of the present invention is by it and adsorbed molecule（Adsorbate）Between Van der Waals
Gravitation, carries out physical absorption by huge ratio surface and works, therefore, big specific surface area, adsorption capacity is also stronger.
The water content of macroporous absorbent resin of the present invention, water content is higher, is more conducive to ion to spread, and water content is got over
Low, volume full exchange capacity is higher.
Beneficial effect produced by the present invention is：Macroporous absorbent resin prepared by the present invention, with absorption on the market
Resin is compared, and its adsorption capacity, resistance tocrocking, selectivity are stronger, and the effect of recycling is more preferable.The present invention is to equipment and raw material
Utilization rate it is high, be suitable for industrialized production.
Embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
Embodiment one
Fill three macroporous absorbent resins（200L）, labeled as 1#（STW-1）、2#（AB-8）、3#（D101）, high ethano is used after installing
Elution, is washed to after no alcohol taste, carries out soda acid acid（4%）Processing, is washed to standby after neutrality.The syrup feed liquid of high concentration is soaked,
Allow feed liquid to carry out supersaturated absorption by polymeric adsorbent, then washed with 2BV pure water, measure the volume of efflux.Entered with 1BV0.5%
Row alkali cleaning, is washed till neutrality with pure water afterwards.Desorbed, solution, which is sucked, uses Rotary Evaporators dealcoholysis, finally decolourizes, taken off with 70% ethanol
Spray dryer spray drying is used after the completion of color, stevioside crude product is produced.1#, 2#, 3# data see the table below：
| 1# | 2# | 3# | |
| Adsorbance/（Kg） | 16.6 | 14.8 | 11.8 |
| Desorption quantity/（Kg） | 16.7 | 14.9 | 12.0 |
| Solid gross mass/（Kg） | 17.1 | 15.2 | 12.4 |
| RA/（%） | 54.3 | 52.4 | 52.5 |
| Solids content general glycoside/（%） | 95.4 | 93.9 | 94.1 |
Embodiment two
1# after reuse（STW-1）、2#（AB-8）、3#（D101）Polymeric adsorbent（200L）, without processing, directly with high
Concentration syrup carries out supersaturated absorption, then is washed with 2BV pure water, measures the volume of efflux.Alkali cleaning is carried out with 1BV0.5%, it
Afterwards neutrality is washed till with pure water.Desorbed with 70% ethanol, solution, which is sucked, uses Rotary Evaporators dealcoholysis, finally decolourizes, is used after the completion of decolouring
Spray dryer spray drying, produces stevioside crude product.1#, 2#, 3# data see the table below：
| 1# | 2# | 3# | |
| Adsorbance/（Kg） | 16.1 | 13.0 | 10.1 |
| Desorption quantity/（Kg） | 16.5 | 12.9 | 11.0 |
| Solid gross mass/（Kg） | 16.5 | 13.0 | 12.5 |
| RA/（%） | 54.9 | 52.8 | 51.9 |
| Solids content general glycoside/（%） | 96.2 | 93.5 | 94.5 |
Embodiment three
1# after reuse（STW-1）、2#（AB-8）、3#（D101）Polymeric adsorbent（200L）, without processing, directly with high
Concentration syrup carries out supersaturated absorption, then is washed with 2BV pure water, measures the volume of efflux.Alkali cleaning is carried out with 1BV0.5%, it
Afterwards neutrality is washed till with pure water.Desorbed with 70% ethanol, solution, which is sucked, uses Rotary Evaporators dealcoholysis, finally decolourizes, is used after the completion of decolouring
Spray dryer spray drying, produces stevioside crude product.1#, 2#, 3#1#, 2#, 3# data see the table below：
| 1# | 2# | 3# | |
| Adsorbance/（Kg） | 15.3 | 10.7 | 9.2 |
| Desorption quantity/（Kg） | 15.5 | 11.0 | 9.5 |
| Solid gross mass/（Kg） | 15.6 | 10.9 | 9.8 |
| RA/（%） | 55.2 | 52.9 | 52.3 |
| Solids content general glycoside/（%） | 96.3 | 93.9 | 94.5 |
Claims (5)
1. a kind of preparation method of macroporous absorbent resin, it is characterised in that including the steps：
The preparation of monomer：The dilute benzene of diethyl, methacrylate, dibenzoyl peroxide are put into reactor by formula, room temperature is stirred
Mix 25~30 minutes, put into pore-foaming agent hexamethylene, be stirred at room temperature 25~30 minutes；
The preparation of aqueous phase：Appropriate water is put into a kettle., powder salt is then put into, and stirring make it that salt solution is uniform；
Gelatin is put into, methylene blue is stirred and heated to 55~60 DEG C, stirring is turned off in advance；
The amount of monomer prepared is pumped into reactor, empty stirring 10~15 minutes is not heated, aqueous phase is 55~60 DEG C at the beginning,
It is 40~45 DEG C or so to finish the temperature in monomer reaction kettle；
After treating empty stirring 10~15 minutes, 68~70 DEG C are to slowly warm up to；
Start to be incubated timing, after being incubated 4~5 hours, steam heating is to slowly warm up to 70~75 DEG C, is incubated 6~7 hours, during which
It is not related to stirring；
Wash greatly；
Post processing, material for making clothes was carried out between water sieve, 16~50 mesh, finished product of packing.
2. the preparation method of macroporous absorbent resin according to claim 1, it is characterised in that the step（1）Monomer
Feed intake and be formulated and be：The dilute benzene of diethyl（Cross-linking monomer）, 120~130kg；Methacrylate（Monomer）, 9~10kg；Peroxidating two
Benzoyl（Catalyst）, 1~1.5kg；Hexamethylene（Pore-foaming agent）, 170~180kg.
3. the preparation method of macroporous absorbent resin according to claim 1, it is characterised in that：The step（2）Salt solution
Proportion be 1.12 to 1.2 between, 7~9kg of gelatin；Remaining is methylene blue.
4. the preparation method of macroporous absorbent resin according to claim 1, it is characterised in that the step（4）Hot water
Temperature is 45~50 DEG C, and the time washed greatly every time is 10~15 minutes, by that analogy 4 to 5 times.
5. the preparation method of macroporous absorbent resin according to claim 1, it is characterised in that the step（5）Rear place
Managing concrete operations flow is：
（1）In material input reactor, discharge water and start distillation, distillation removes pore-foaming agent hexamethylene；
（2）In resin Archon input reactor, methanol is first pumped into, stirring is opened；
Liquid caustic soda is pumped into again so that pH value is 7~8；
Start to warm up to 50~55 DEG C；
Stirring is closed, constant temperature flows back 4~5 hours；
Then methanol is drained；
（3）Into reactor, input reclaims methanol, puts into hydrochloric acid, and it is 3~4 to open stirring and adjusting pH value, is warming up to 50~55 DEG C, pass
It is stirred at reflux insulation 4~5 hours, then methanol is drained；
（4）Into reactor, input reclaims methanol, opens stirring and is warming up to 50~55 DEG C, is incubated 4~5 hours；
（5）New methanol is put into reactor, stirring is opened and is warming up to 50~55 DEG C, be incubated 4~5 hours；
（6）New ethanol is put into reactor, stirring is opened and is warming up between 50~55 DEG C, 4~5 hours are incubated；
（7）The methanol or ethanol of an above-mentioned step are drained, discharges water and boils to more than 100 DEG C, until no alcohol taste can blowing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109369852A (en) * | 2018-10-30 | 2019-02-22 | 扬州金珠树脂有限公司 | A kind of preparation method of nickel, cobalt, polluted by copper resin |
| CN109400660A (en) * | 2018-11-19 | 2019-03-01 | 江苏史蒂文生物科技有限公司 | The crocin standard items and preparation method thereof prepared from cape jasmine using new packing |
| CN111111261A (en) * | 2019-12-31 | 2020-05-08 | 高陵蓝晓科技新材料有限公司 | Chromatographic filler, preparation method and application thereof in separation and purification of chenodeoxycholic acid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369852A (en) * | 2018-10-30 | 2019-02-22 | 扬州金珠树脂有限公司 | A kind of preparation method of nickel, cobalt, polluted by copper resin |
| CN109369852B (en) * | 2018-10-30 | 2021-03-23 | 扬州金珠树脂有限公司 | Preparation method of nickel, cobalt and copper adsorption resin |
| CN109400660A (en) * | 2018-11-19 | 2019-03-01 | 江苏史蒂文生物科技有限公司 | The crocin standard items and preparation method thereof prepared from cape jasmine using new packing |
| CN109400660B (en) * | 2018-11-19 | 2021-11-09 | 江苏史蒂文生物科技有限公司 | Crocin standard prepared from fructus Gardeniae by using novel filler, and its preparation method |
| CN111111261A (en) * | 2019-12-31 | 2020-05-08 | 高陵蓝晓科技新材料有限公司 | Chromatographic filler, preparation method and application thereof in separation and purification of chenodeoxycholic acid |
| CN111111261B (en) * | 2019-12-31 | 2021-12-28 | 高陵蓝晓科技新材料有限公司 | Chromatographic filler, preparation method and application thereof in separation and purification of chenodeoxycholic acid |
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