Controllable preparation method for silica-gel chromatographic filler
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A silica gel chromatography, silica gel technology, applied in chemical instruments and methods, other chemical processes, etc., to avoid the use of organic reagents
Inactive Publication Date: 2016-11-09
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF2 Cites 2 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
However, so far there is no solvent-free method for
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0028] N - Preparation of Methylimidazole Silica Gel Chromatography Packing (Sil-MIm)
[0029] Steps:
[0030] ① First weigh 0.5 g of silica gel and 0.04 g of CPTMS into a 25 mL round bottom flask, and then add 10 mL of bonded monomer MIm into it;
[0031] ② The mixture of silica gel, silane reagent CPTMS and bonded monomer MIm in a certain proportion was reacted for 48 h at 120 °C under magnetic stirring;
[0032] ③ After the reaction, the prepared chromatographic material was washed several times with a small amount of methanol and then with a large amount of water, and then dried in a vacuum oven for 12 h.
Embodiment 2
[0034] N - Preparation of Methylimidazole Silica Gel Chromatography Packing (Sil-MIm)
[0035] Steps:
[0036] ① First weigh 0.5 g of silica gel and 0.06 g of CPTMS into a 25 mL round bottom flask, and then add 10 mL of bonded monomer MIm into it;
[0037] ② The mixture of silica gel, silane reagent CPTMS and bonded monomer MIm in a certain proportion was reacted under magnetic stirring at 60 °C for 48 h;
[0038] ③ After the reaction, the prepared chromatographic material was washed several times with a small amount of methanol and then with a large amount of water, and then dried in a vacuum oven for 12 h.
Embodiment 3
[0040] N - Preparation of Methylimidazole Silica Gel Chromatography Packing (Sil-MIm)
[0041] Steps:
[0042] ① First weigh 1.0 g of silica gel and 0.04 g of CPTMS into a 25 mL round bottom flask, and then add 10 mL of bonded monomer MIm into it;
[0043] ② The mixture of silica gel, silane reagent CPTMS and bonded monomer MIm in a certain proportion was reacted for 48 h at 120 °C under magnetic stirring;
[0044] ③ After the reaction, the prepared chromatographic material was washed several times with a small amount of methanol and then with a large amount of water, and then dried in a vacuum oven for 6 h.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
PUM
Login to view more
Abstract
The invention discloses a controllable preparation method for silica-gel chromatographic filler. The method comprises the specific steps: adding an MIm (N-methylimidazole) functional monomer into silica gel (SiO2) and CPTMS (3-chloropropyl trimethoxy silane), carrying out a reaction for 12 to 48 hours at the temperature of 60 DEG C to 150 DEG C with stirring, then, carrying out washing sequentially by methanol and water, and carrying out drying, thereby obtaining N-methylimidazole modified silica-gel chromatographic filler, wherein the mass ratio of the silica gel to the CPTMS is 0.5: (0.02 to 0.5); the mass/volume ratio of the silica gel to the MIm functional monomer is (0.5 to 2.5)g: (10 to 50)mL. According to the method, the amount of bonding of the functional monomer is controlled through strictly controlling the charging rate of the silica gel to the silane reagent; meanwhile, the excessive added functional monomer is a reactant and is also a dispersant, so that additional organic solvent is not required to be added; the functional monomer can be reused, so that the requirements of green chemistry are fully met.
Description
technical field [0001] The invention relates to a method for the controllable preparation of silica gel chromatographic packing, specifically a method for preparing by adding silica gel and silane reagents in the case of far excessive functional monomers N - A solvent-free method of methylimidazole-modified silica gel chromatography media (Sil-MIm). Background technique [0002] There are many solvent-free preparation methods, such as: ultrasonic assistance, microwave radiation, ultra-low temperature synthesis and so on. These methods have been successfully applied to many research fields. However, so far there is no solvent-free method for the preparation of chromatographic stationary phases. Contents of the invention [0003] The object of the present invention is to provide a controllable preparation method of a solvent-free, controllably bonded silica gel chromatographic filler. [0004] A controllable preparation method of silica gel chromatographic packing is cha...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to view more
IPC IPC(8): B01J20/286B01J20/30
CPCB01J20/286
Inventor 邱洪灯刘后梅
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
Login to view more 
Login to view more