CN104607162B - A kind of cation exchange mosaic type crystalline substance glue separating medium and preparation method thereof - Google Patents
A kind of cation exchange mosaic type crystalline substance glue separating medium and preparation method thereof Download PDFInfo
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- CN104607162B CN104607162B CN201510019873.1A CN201510019873A CN104607162B CN 104607162 B CN104607162 B CN 104607162B CN 201510019873 A CN201510019873 A CN 201510019873A CN 104607162 B CN104607162 B CN 104607162B
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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
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
- B01J20/285—Porous sorbents based on polymers
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/44—Materials comprising a mixture of organic materials
- B01J2220/445—Materials comprising a mixture of organic materials comprising a mixture of polymers
Abstract
The invention discloses a kind of cation exchange mosaic type crystalline substance glue separating medium and preparation method thereof.It is characterized in that described mosaic type crystal gel medium is the continuous bed medium of poly hydroxy ethyl acrylate of embedded cellulose microsphere, obtained through the propane sulfonic acid grafting and modifying of 2 acrylamido, 2 methyl 1,0.1~300 μm of its aperture, porosity 80~95%, with sulfonic group cation exchange functional group, to the mg/mL crystalline substance glue of adsorption capacity 1~5 of lysozyme model protein.The aperture of mosaic type crystal gel medium provided by the invention possesses diffusion mass transfer absorption aperture and the multilevel hole of convective mass transfer super big hole from sub-micron and micron dimension, improve crystal gel medium specific surface area and chemical modification after adsorption site；It is very stable under isolating environment meanwhile the host material biocompatibility of described crystal gel medium is excellent, repeat and utilize, there is good security, had broad application prospects in bio-chemistry separation field.
Description
Technical field
The invention belongs to chemical separating media technology field, and in particular to a kind of cation exchange mosaic type crystalline substance glue separation is situated between
Matter and preparation method thereof.
Background technology
Crystal gel medium is a kind of new chromatography medium occurred in recent years, has size in its medium skeleton from several micro-
Rice arrives hundreds of microns of super large hole, it is allowed to which microbial cell or cell fragment pass through, therefore, suitable for from microbial fermentation
Quickly divide in liquid, cell culture fluid, blood and complex biological feed liquid fluid such as whey, cow's milk containing other solid phase impurity
From large biological molecule material.Its separation process step is few, and mass transfer of the large biological molecule in brilliant glue column is rapid, and separation is time-consuming
Short, separative efficiency is good, there is important application prospect in bio-separation field.
Although domestic and foreign scholars have been successfully prepared the crystal gel medium of different series, existing crystal gel medium hole chi
Very little size is concentrated mainly on a few micrometers to about 100~200 microns, and specific surface area is smaller, and hole level is single, adsorption site compared with
It is few so that the adsorption capacity and separating effect of crystal gel medium all do not give full play to.But by conventional crystallization pore and to gather
Close the crystal gel medium that reaction coupling process prepares multistage secondary aperture, then it is relatively difficult.Meanwhile with cation exchange functional group
The brilliant compound crystal gel medium of glue mosaic type does not have document report then.
The content of the invention
It is brilliant present invention aims at a kind of cation exchange mosaic type is provided for the above-mentioned problems in the prior art
Glue separating medium and preparation method thereof.
A kind of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that described mosaic type crystal gel medium
For continuous bed medium, there is multilevel hole of the aperture from sub-micron and micron dimension, the mosaic type crystal gel medium is embedded with
Brilliant glue microballoon, and band is just like formula（Ⅰ）Shown sulfonic group cation exchange functional group：
（Ⅰ）
A kind of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that described mosaic type crystal gel medium
Matrix using embedded cellulose microsphere poly hydroxy ethyl acrylate crystalline substance gel matrix.
A kind of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that described mosaic type crystal gel medium
The aperture of multilevel hole is 0.1~300 μm, porosity 80~95%, and the adsorption capacity to lysozyme model protein is 1~5
Mg/mL crystalline substance glue.
The preparation method of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that the preparation method is such as
Under：With with ethylene linkage and sulfonic acid group can be anti-with the poly hydroxy ethyl acrylate mosaic type crystalline substance gel matrix of embedded cellulose microsphere
The monomer answered is grafted monomers, with Cu3+Solion is catalyst, the poly hydroxy ethyl acrylate to embedding cellulose microsphere
Mosaic type crystalline substance gel matrix carries out grafting and modifying, the immobilized sulfonic group cation exchange functional group in brilliant glue skeleton, obtains described
Cation exchange mosaic type crystal gel medium.
The preparation method of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that described grafted monomers
For 2- acrylamidos -2- methyl isophthalic acids-propane sulfonic acid, the grafted monomers are added in the form of 0.5~2 M monomer solutions,
The volumetric usage of the monomer solution is 3 ~ 5 times of mosaic type crystalline substance glue continuous bed dielectric matrix volume.
The preparation method of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that the catalyst Cu3+
Final concentration of 0.03~0.06M of solion, volumetric usage are 3 ~ 5 times of mosaic type crystalline substance glue continuous bed dielectric matrix volume.
The preparation method of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that the graft reaction
Temperature is 45~55 DEG C, and the reaction time is 0.5~4h.
The preparation method of described cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that described Cu3+Ion
Solution is K5[Cu(HIO6)2] solution or Na5[Cu(HIO6)2] solution.
By using above-mentioned technology, the present invention has the advantages that：
1）The host material of mosaic type crystal gel medium provided by the invention is wide variety of life in clinical and medical diagnosis
The good natural or polymeric material of thing compatibility, such as with ethylene linkage and sulfonic acid group can be with the poly- methyl-prop of embedded cellulose microsphere
Olefin(e) acid hydroxyl ethyl ester mosaic type crystalline substance gel matrix, its biocompatibility is excellent, very stable under isolating environment, repeats and utilizes, has
Good security；
2）Mosaic type crystalline substance glue fiber element provided by the invention is embedded in poly hydroxy ethyl acrylate in the form of porous microsphere
In, different from existing other cation exchange crystal gel mediums, it, which is formd, is provided simultaneously with diffusion mass transfer absorption aperture and to spreading
The multilevel hole of matter super big hole, improve crystal gel medium specific surface area and chemical modification after adsorption site；
3）The mosaic type crystalline substance glue separating medium of the present invention, its preparation method is simple and convenient to operate, suitable for being led in bio-chemistry separation
Domain is applied, and is had broad application prospects in bio-chemistry separation field.
Embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment 1
Na using 15.7mL concentration as 0.037M5[Cu(HIO6)2] solution is catalyst, take the mm of diameter 10,40 mm of height
Embedded cellulose microsphere poly hydroxy ethyl acrylate mosaic type crystalline substance gel matrix, its embedded cellulose crystalline substance glue microspherulite diameter
300~1900 μm, about 900 μm of average grain diameter, the mass ratio for accounting for brilliant gel matrix skeleton is 25%；It is 0.5 M with 15.7 mL concentration
2- acrylamidos -2- methyl isophthalic acids-propane sulfonic acid aqueous solution at 45 DEG C to brilliant gel matrix carry out the h of graft reaction 4, obtain
Poly hydroxy ethyl acrylate matrix and cellulose base cation exchange mosaic type crystal gel medium, its effective drainage porosity 84% are maximum
Porosity 95%, about 0.1~300 μm of aperture, to the mg/mL of adsorption capacity 1.10 of lysozyme model protein.
Embodiment 2
K using 9 mL concentration as 0.06M5[Cu(HIO6)2Solution is catalyst, takes the mm of diameter 10, highly 38 mm's is interior
Embedding cellulose microsphere poly hydroxy ethyl acrylate mosaic type crystalline substance gel matrix, its embedded cellulose crystalline substance glue microspherulite diameter 300~
1900 μm, about 900 μm of average grain diameter, the mass ratio for accounting for brilliant gel matrix skeleton is 25%；With the 2- propylene that 9 mL concentration are 2 M
Amide groups -2- methyl isophthalic acids-propane sulfonic acid aqueous solution carries out the h of graft reaction 0.5 at 55 DEG C to brilliant gel matrix, obtains poly- methyl
Hydroxy-ethyl acrylate matrix and cellulose base cation exchange mosaic type crystal gel medium, its effective drainage porosity 83 %, maximum pore
The % of rate 94, about 0.1~300 μm of pore size, to the mg/mL of saturated adsorption capacity 5 of lysozyme model protein.
Embodiment 3
K using 30 mL concentration as 0.04M5[Cu(HIO6)2Solution is catalyst, takes the mm of diameter 10, highly 52 mm's is interior
Embedding cellulose microsphere poly hydroxy ethyl acrylate mosaic type crystalline substance gel matrix, its embedded cellulose crystalline substance glue microspherulite diameter 300~
1900 μm, about 900 μm of average grain diameter, the mass ratio for accounting for brilliant gel matrix skeleton is 30%；With the 2- propylene that 20 mL concentration are 1 M
Amide groups -2- methyl isophthalic acids-propane sulfonic acid aqueous solution carries out the h of graft reaction 2 at 51 DEG C to brilliant gel matrix, obtains poly- methyl-prop
Olefin(e) acid hydroxyl ethyl ester matrix and cellulose base cation exchange mosaic type crystal gel medium, its effective drainage porosity 80%, maximum pore rate
94%, about 0.1~270 μm of pore size, to the mg/mL of adsorption capacity 3.4 of lysozyme model protein.
Embodiment 4
Na using 20 mL concentration as 0.03M5[Cu(HIO6)2] solution is catalyst, take the mm of diameter 10, height 40 mm
Embedded cellulose microsphere poly hydroxy ethyl acrylate mosaic type crystalline substance gel matrix, its embedded cellulose crystalline substance glue microspherulite diameter 300
~1900 μm, about 900 μm of average grain diameter, the mass ratio for accounting for brilliant gel matrix skeleton is 25%；With the 2- that 17 mL concentration are 0.5 M
Acrylamido -2- methyl isophthalic acids-propane sulfonic acid aqueous solution carries out the h of graft reaction 2 at 52 DEG C to brilliant gel matrix, obtains poly- first
Base hydroxy-ethyl acrylate matrix and cellulose base cation exchange mosaic type crystal gel medium, its effective drainage porosity 85%, maximum pore
Rate 95%, about 0.1~300 μm of aperture, to the mg/mL of adsorption capacity 1 of lysozyme model protein.
Embodiment 5
Na using 30 mL concentration as 0.04M5[Cu(HIO6)2] solution is catalyst, take the mm of diameter 10, height 50 mm
Embedded cellulose microsphere poly hydroxy ethyl acrylate mosaic type crystalline substance gel matrix, its embedded cellulose crystalline substance glue microspherulite diameter 300
~1900 μm, about 900 μm of average grain diameter, the mass ratio for accounting for brilliant gel matrix skeleton is 25%；With the 2- that 20 mL concentration are 1.8 M
Acrylamido -2- methyl isophthalic acids-propane sulfonic acid aqueous solution carries out the h of graft reaction 1.8 at 48 DEG C to brilliant gel matrix, is gathered
Hydroxyethyl methacrylate matrix and cellulose base cation exchange mosaic type crystal gel medium, its effective drainage porosity 85%, largest hole
Gap rate 95%, about 0.1~300 μm of aperture, to the mg/mL of adsorption capacity 3.6 of lysozyme model protein.
Claims (6)
1. a kind of cation exchange mosaic type crystalline substance glue separating medium, it is characterised in that described mosaic type crystal gel medium is continuous bed
Medium, there is multilevel hole of the aperture from sub-micron and micron dimension, the mosaic type crystal gel medium is embedded with brilliant glue microballoon,
And band is just like formula（Ⅰ）Shown sulfonic group cation exchange functional group：
,
The matrix of described mosaic type crystal gel medium uses the poly hydroxy ethyl acrylate crystalline substance gel matrix of embedded cellulose microsphere,
The aperture of mosaic type crystal gel medium multilevel hole is 0.1~300 μm, porosity 80~95%, the suction to lysozyme model protein
Attached capacity is 1~5 mg/mL crystalline substance glue.
2. a kind of preparation method of cation exchange mosaic type crystalline substance glue separating medium according to claim 1, its feature exist
It is as follows in the preparation method：With with ethylene linkage and sulfonic acid group can be with the poly hydroxy ethyl acrylate of embedded cellulose microsphere
The monomer of mosaic type crystalline substance matrix qualitative response is grafted monomers, with Cu3+Solion is catalyst, and embedded cellulose microsphere is gathered
Hydroxyethyl methacrylate mosaic type crystalline substance gel matrix carries out grafting and modifying, the immobilized sulfonic group cation exchange work(in brilliant glue skeleton
Energy group, obtains described cation exchange mosaic type crystal gel medium.
3. the preparation method of cation exchange mosaic type crystalline substance glue separating medium according to claim 2, it is characterised in that institute
The grafted monomers stated are 2- acrylamidos -2- methyl isophthalic acids-propane sulfonic acid, and the grafted monomers are with 0.5~2 M monomer solutions
Form add, the volumetric usage of the monomer solution is 3 ~ 5 times of mosaic type crystalline substance glue continuous bed dielectric matrix volume.
4. the preparation method of cation exchange mosaic type crystalline substance glue separating medium according to claim 2, it is characterised in that institute
State catalyst Cu3+Final concentration of 0.03~0.06M of solion, volumetric usage are mosaic type crystalline substance glue continuous bed dielectric matrix body
Long-pending 3 ~ 5 times.
5. the preparation method of cation exchange mosaic type crystalline substance glue separating medium according to claim 2, it is characterised in that institute
The temperature for stating graft reaction is 45~55 DEG C, and the reaction time is 0.5~4h.
6. the preparation method of cation exchange mosaic type crystalline substance glue separating medium according to claim 2, it is characterised in that institute
The Cu stated3+Solion is K5[Cu(HIO6)2] solution or Na5[Cu(HIO6)2] solution.
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| CN106632860B (en) * | 2016-12-23 | 2019-05-24 | 浙江工业大学 | A kind of glucan base crystalline substance glue microballoon separating medium and preparation method thereof |
| CN107141403B (en) * | 2017-05-16 | 2019-01-25 | 齐鲁工业大学 | A kind of Cu2+Chelate the preparation method of polyhydroxypropyl methaciylate super-macroporous crystal gel medium |
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| US20030168629A1 (en) * | 2001-12-10 | 2003-09-11 | Lazar Warren G. | Reactive liquid polymer crosslinking agent and process for preparation |
| CN100413590C (en) * | 2006-07-12 | 2008-08-27 | 浙江工业大学 | Cation exchange type super macroporous continous bed crystal gel medium and its prepn. method |
| CN100574883C (en) * | 2007-06-29 | 2009-12-30 | 浙江工业大学 | A kind of cation-exchange crystal glue chromatography medium and preparation method thereof |
| CN103230784B (en) * | 2013-04-26 | 2015-01-28 | 浙江工业大学 | Composite continuous bed cryogel and preparation thereof, and application in separating IgG and albumin |
| CN103252218B (en) * | 2013-04-26 | 2015-08-05 | 浙江工业大学 | Hybrid overall crystal gel medium and preparation method thereof |
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