CN103435739A - Preparation method of temperature-sensitive type monolithic column - Google Patents
Preparation method of temperature-sensitive type monolithic column Download PDFInfo
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- CN103435739A CN103435739A CN2013103845467A CN201310384546A CN103435739A CN 103435739 A CN103435739 A CN 103435739A CN 2013103845467 A CN2013103845467 A CN 2013103845467A CN 201310384546 A CN201310384546 A CN 201310384546A CN 103435739 A CN103435739 A CN 103435739A
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Abstract
The invention relates to a preparation method of a temperature-sensitive type monolithic column, wherein the temperature-sensitive type monolithic column is obtained through polymerization reaction of acrylic acid and N-isopropyl acrylamide dissolved in a pore-foaming agent in one step. Compared with other temperature-sensitive type monolithic columns prepared through reaction such as surface grafting, the temperature-sensitive type monolithic column prepared by one step is simpler in preparation method and remarkably shorter in preparation time, so that the temperature-sensitive type monolithic column provided by the invention has very high application value in the field of adsorption separation of medicines and biomacromolecules.
Description
Technical field
The present invention relates to a kind of preparation method of temperature sensitive type integral post, soon vinylformic acid and NIPA are dissolved in pore-creating agent and obtain the temperature sensitive type integral post through the one-step polymerization reaction.
Background technology
Simply and not there is void volume between particle filled composite in the integral post preparation, with particles filled post, compares the separation efficiency with better perviousness and Geng Gao, can under lower back pressure, treat separate substance and efficiently separate fast.Therefore, its preparation and applied research have been become the focus in separating-purifying field.The class that Organic Polymer Monolithic Columns is most widely used in post as a whole has that the preparation method is simple, selection extensively, the advantage such as the pH range of application is wide, shown tempting application prospect in the separating-purifying field of biomacromolecule.NIPA is introduced to the Organic Polymer Monolithic Columns system and can make the temperature sensitive type integral post, when envrionment temperature changes near the LCST of NIPA, NIPA molecular chain form changes, the binding constant on guest molecule and integral post surface is undergone mutation, thereby realize the adsorption and desorption of molecule.This temperature sensitive type integral post has important using value in the compartment analysis field of the materials such as proteins and peptides.
The method for preparing at present the temperature sensitive type integral post mostly is the surface grafting method, after the first step reaction obtains Organic Polymer Monolithic Columns, by Surface grafting reaction, the NIPA molecule is received to the integral post bore surface again, thereby makes the temperature sensitive type integral post.The method preparation process is comparatively complicated.
Summary of the invention
The technical problem solved
For fear of the deficiencies in the prior art part, the present invention proposes a kind of preparation method of temperature sensitive type integral post.
Technical scheme
A kind of preparation method of temperature sensitive type integral post is characterized in that step is as follows:
Step 1: by methyl acrylic ester monomer, vinylformic acid, the NIPA aqueous solution, linking agent, pore-creating agent and initiator in mass ratio the ratio of 1～3 ﹕ 0.05～0.2 ﹕ 0.1～0.3 ﹕ 0.3～1.0 ﹕ 2～5 ﹕ 0.01～0.04 mix and make mixed solution under room temperature, wherein the massfraction of the NIPA aqueous solution is 5%～20%;
Step 2: mixed solution is poured in stainless steel void column pipe, sealed at both ends, be heated to 40～90 ℃ of initiated polymerizations, after completing, polyreaction obtains polymer column, and the reaction times is 24～48h;
Unreacted monomer, linking agent and pore-creating agent in the solvent extraction polymer column for step 3, obtain the temperature sensitive type polyalcohol integral pole.
Described methyl acrylic ester monomer is one or more any than mixing in methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate or glycidyl methacrylate.
Described linking agent is a kind of in Vinylstyrene or Ethylene glycol dimethacrylate or both is any than mixing.
Described pore-creating agent is one or more any than mixing in n-propyl alcohol, n-dodecanol, BDO or hexalin.
Described initiator is Diisopropyl azodicarboxylate or benzoyl peroxide.
Described solvent is acetone, methyl alcohol, ethanol or tetrahydrofuran (THF).
Beneficial effect
The preparation method of a kind of temperature sensitive type integral post that the present invention proposes, be dissolved in vinylformic acid and NIPA in pore-creating agent and obtain the temperature sensitive type integral post through the one-step polymerization reaction.It is more simple that the temperature sensitive type integral post prepared by this single stage method and other temperature sensitive type integral post by the reactions such as surface grafting preparations are compared the preparation method, preparation time obviously shortens, and it has very high using value at medicine and biomacromolecule fractionation by adsorption field.
The accompanying drawing explanation
Fig. 1: the stereoscan photograph of prepared temperature sensitive type integral post
Fig. 2: the graph of pore diameter distribution of prepared temperature sensitive type integral post.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1: the preparation of temperature sensitive type integral post
NIPA 0.02g is dissolved in 0.20g water, add 0.16g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 1.50g glycidyl methacrylate, 1.00g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 2: the preparation of temperature sensitive type integral post
NIPA 0.03g is dissolved in 0.20g water, add 0.16g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 1.50g glycidyl methacrylate, 1.00g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 3: the preparation of temperature sensitive type integral post
NIPA 0.01g is dissolved in 0.20g water, add 0.16g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 1.50g glycidyl methacrylate, 1.00g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 4: the preparation of temperature sensitive type integral post
NIPA 0.02g is dissolved in 0.20g water, add 0.20g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 1.50g glycidyl methacrylate, 1.00g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 5: the preparation of temperature sensitive type integral post
NIPA 0.02g is dissolved in 0.20g water, add 0.24g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 1.50g glycidyl methacrylate, 1.00g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 6: the preparation of temperature sensitive type integral post
NIPA 0.02g is dissolved in 0.20g water, add 0.16g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 2.00g glycidyl methacrylate, 0.80g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 7: the preparation of temperature sensitive type integral post
NIPA 0.02g is dissolved in 0.20g water, add 0.16g vinylformic acid, 1.20g n-propyl alcohol, 1.80g n-dodecanol, 1.50g glycidyl methacrylate, 1.00g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Embodiment 8: the preparation of temperature sensitive type integral post
NIPA 0.02g is dissolved in 0.20g water, add 0.16g vinylformic acid, 1.40g n-propyl alcohol, 1.40g n-dodecanol, 1.50g glycidyl methacrylate, 0.50g Ethylene glycol dimethacrylate and 24mg Diisopropyl azodicarboxylate to it again, ultrasonic it is mixed; The reactant mixed is injected to stainless steel void column pipe, and sealing is placed under 50 ℃ of water-baths reacts 24h; Reacted rear with methanol extraction wherein unreacted monomer, linking agent and pore-creating agent, obtained the temperature sensitive type integral post.
Claims (6)
1. the preparation method of a temperature sensitive type integral post is characterized in that step is as follows:
Step 1: by methyl acrylic ester monomer, vinylformic acid, the NIPA aqueous solution, linking agent, pore-creating agent and initiator in mass ratio the ratio of 1～3 ﹕ 0.05～0.2 ﹕ 0.1～0.3 ﹕ 0.3～1.0 ﹕ 2～5 ﹕ 0.01～0.04 mix and make mixed solution under room temperature, wherein the massfraction of the NIPA aqueous solution is 5%～20%;
Step 2: mixed solution is poured in stainless steel void column pipe, sealed at both ends, be heated to 40～90 ℃ of initiated polymerizations, after completing, polyreaction obtains polymer column, and the reaction times is 24～48h;
Unreacted monomer, linking agent and pore-creating agent in the solvent extraction polymer column for step 3, obtain the temperature sensitive type polyalcohol integral pole.
2. the preparation method of temperature sensitive type integral post according to claim 1 is characterized in that: described methyl acrylic ester monomer is one or more any than mixing in methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate or glycidyl methacrylate.
3. the preparation method of temperature sensitive type integral post according to claim 1 is characterized in that: described linking agent is a kind of in Vinylstyrene or Ethylene glycol dimethacrylate or both is any than mixing.
4. the preparation method of temperature sensitive type integral post according to claim 1 is characterized in that: described pore-creating agent is one or more any than mixing in n-propyl alcohol, n-dodecanol, BDO or hexalin.
5. the preparation method of temperature sensitive type integral post according to claim 1, it is characterized in that: described initiator is Diisopropyl azodicarboxylate or benzoyl peroxide.
6. the preparation method of temperature sensitive type integral post according to claim 1, it is characterized in that: described solvent is acetone, methyl alcohol, ethanol or tetrahydrofuran (THF).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474176A (en) * | 2017-07-31 | 2017-12-15 | 西北工业大学 | A kind of preparation method of surface hydrophilic and hydrophobic adjustable porous polyalcohol integral pole |
| CN107501460A (en) * | 2017-08-04 | 2017-12-22 | 西北工业大学 | A kind of preparation method of temperature sensitive type porous polymer integral post |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284892A (en) * | 2007-12-21 | 2008-10-15 | 北京科技大学 | Process for preparing monolithic material of hydrophilic polymers by frontal polymerization |
| CN102775564A (en) * | 2012-08-15 | 2012-11-14 | 西北工业大学 | Preparation method of temperature sensitive type monolithic column with chiral molecule recognition function |
| CN103242594A (en) * | 2013-05-14 | 2013-08-14 | 中国科学院长春应用化学研究所 | Polymer hydrogel microspheres and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284892A (en) * | 2007-12-21 | 2008-10-15 | 北京科技大学 | Process for preparing monolithic material of hydrophilic polymers by frontal polymerization |
| CN102775564A (en) * | 2012-08-15 | 2012-11-14 | 西北工业大学 | Preparation method of temperature sensitive type monolithic column with chiral molecule recognition function |
| CN103242594A (en) * | 2013-05-14 | 2013-08-14 | 中国科学院长春应用化学研究所 | Polymer hydrogel microspheres and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474176A (en) * | 2017-07-31 | 2017-12-15 | 西北工业大学 | A kind of preparation method of surface hydrophilic and hydrophobic adjustable porous polyalcohol integral pole |
| CN107474176B (en) * | 2017-07-31 | 2019-04-16 | 西北工业大学 | A kind of preparation method of surface hydrophilic and hydrophobic adjustable porous polyalcohol integral pole |
| CN107501460A (en) * | 2017-08-04 | 2017-12-22 | 西北工业大学 | A kind of preparation method of temperature sensitive type porous polymer integral post |
| CN107501460B (en) * | 2017-08-04 | 2019-04-19 | 西北工业大学 | A kind of preparation method of temperature sensitive type porous polymer integral post |
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Application publication date: 20131211 |