CN108864362A - A kind of large scale is uniformly dispersed the preparation method of type crystalline substance matrix material - Google Patents
A kind of large scale is uniformly dispersed the preparation method of type crystalline substance matrix material Download PDFInfo
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- CN108864362A CN108864362A CN201810478779.6A CN201810478779A CN108864362A CN 108864362 A CN108864362 A CN 108864362A CN 201810478779 A CN201810478779 A CN 201810478779A CN 108864362 A CN108864362 A CN 108864362A
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/24—Homopolymers or copolymers of amides or imides
- C08L33/26—Homopolymers or copolymers of acrylamide or methacrylamide
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Abstract
It is uniformly dispersed the preparation method of type crystalline substance matrix material the present invention relates to a kind of large scale, belongs to brilliant glue material technical field.Technical solution of the present invention in electrolyte by adding modified material triglyceride, through triglyceride during polymerization prepares brilliant glue, as dispersing agent, by the presence and increase chain length of the structure of the fatty acid chain on its molecule the flocculation of particle can reduced, strong adsorption occurs for the group and particle surface generated due to electrolyte mixing with triglyceride, to force hydrocarbon chain to rest in the solvent neighbouring with particle surface, mutual alienation, to provide spatial stability for particle, to be effectively improved the uniformity coefficient in polyacrylamide crystalline substance matrix material polymerization process.
Description
Technical field
It is uniformly dispersed the preparation method of type crystalline substance matrix material the present invention relates to a kind of large scale, belongs to brilliant glue material technology
Field.
Background technique
Separating medium, that is, crystal gel medium of crystal glue chromatography isolation technics is a kind of special continuous bed medium of monoblock type, it
Skeleton and pore structure and conventional continuous bed it is different, it is also different from the resulting gel of typical polymerization reaction.Inside crystal gel medium
With size up to a few micrometers of super large holes interconnected to hundreds of microns, microbial cell, the cell in material liquid can be made
The solid particles such as fragment pass through, and realize and operate with the analogous high flow rate of expansion bed.In addition to this, crystal gel medium also has
Elasticity and very strong restorability well, can Reusability.The preparation of polymer crystalline substance glue usually follows three steps (1) and contains
Prepared by the mixed solution of monomer/performed polymer, crosslinking agent and initiator, (2) low temperature gelation, and (3) thaw.When containing the groups such as monomer
The solution divided is chilled to solvent crystallization temperature hereinafter, partial solvent molecule forms crystallization, and the components such as monomer are concentrated in one
Non-frozen liquid phase micro-area；Polymerization/gelation reaction occurs at low temperature for high concentration monomer, generates cross-linked polymer phase；Reaction knot
Beam, space occupied by solvent crystal grain form perforation hole after thawing.
Crystal gel medium possesses size up to a few micrometers to hundreds of microns because of it and mutually interconnects as a kind of novel separating medium
Logical super large hole, therefore be suitable under high flow velocities directly handling the biological raw material liquid containing solid particle, biology may be implemented
The fast separating and purifying of macromolecular.The crystal gel medium small volume having been commercialized at present, single-column are difficult to larger suitable for treating capacity
Occasion.If major diameter, large volume, high-throughput whole crystal gel medium can be prepared, this problem will be can effectively solve.But due to crystalline substance
The preparation of glue medium is the complex process that a solvent crystallization is coupled with monomer polymerization, and diabatic process includes crystallization exotherm and gathers
Heat release two parts are closed, if its size is larger, in the Unsteady Heat Transfer process for macroscopically showing as mobile phase boundray, are caused in it
Portion generates more apparent Temperature Distribution difference, and the inhomogeneities of Temperature Distribution can then directly result in crystal gel medium internal structure
Unevenly, performance declines.This is also where preparing the difficulty of large scale entirety crystal gel medium, so how to prepare a kind of with excellent
The large scale crystalline substance glue material of different uniform performance is necessary.
Summary of the invention
The technical problems to be solved by the invention：It is uneven for dispersion inside existing large scale crystalline substance glue material, performance compared with
The problem of difference provides a kind of large scale and is uniformly dispersed the preparation method of type crystalline substance matrix material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
（1）In mass ratio 1:8, polyvinylidene fluoride-hexafluoropropene is added in 5% metabisulfite solution of mass fraction, is stirred
Mixed liquor is mixed to obtain, according to parts by weight, weighs 45~50 portions of mixed liquors, 10~15 parts of Diacrylates, 0.5 respectively
~1.0 parts of ammonium persulfates are stirred and heating water bath, and standing is cooled to room temperature, and collect reaction solution；
（2）It places reaction liquid into drying, standing at 75~85 DEG C to be cooled to room temperature, obtains gel modification liquid, in mass ratio 1:15, it will
Triglyceride is added in gel modification liquid, is stirred and is placed in homogenization in homogenizer, and mixing homogenizing fluid is obtained；
（3）Again according to parts by weight, 45~50 parts of acrylamide monomers, 25~30 parts of mixing homogenizing fluids, 5~10 parts are weighed respectively
N, N '-methylene-bisacrylamide and 2~3 parts of ammonium persulfates are placed in glass chromatography column, and program cooling is placed it in after sealing
Low temperature thermostat bath in, slow cooling, when temperature is down to -20 DEG C, stop cooling, insulation reaction；
（4）After the completion of Heat preservation, slow cooling stops cooling and insulation reaction after near -30 DEG C of temperature again, to
It after the completion of insulation reaction, places it in and stands at room temperature, filter and collect filter cake, washing, drying simultaneously collect to obtain dried object
The large scale is prepared into be uniformly dispersed type crystalline substance matrix material.
Step（3）The slow cooling is by 1 DEG C/min speed slow cooling.
Step（4）The slow cooling again is by 2 DEG C/min slow cooling.
Step（4）The washing is after being rinsed 3~5 times with 5% hydrochloric acid of mass fraction, then is rinsed with deionized water to washing
Liquid is washed to be in neutrality.
The present invention is compared with other methods, and advantageous effects are：
（1）Technical solution of the present invention uses polyvinylidene fluoride-hexafluoropropene to prepare modified electrolyte for raw material, passes through system
Standby gel electrolyte and acrylamide monomer is compound and its internal pore surface during preparing brilliant glue material is made to carry out chemistry
Modification, immobilized ion exchanging function group obtain a kind of embedded nanoparticle cationic ion exchange crystal gel medium, in ion exchange
In chromatography application, the absorption property of medium determines the efficiency isolated and purified, so the brilliant glue material of technical solution of the present invention preparation
Material has excellent grafting absorption property；
（2）Technical solution of the present invention passes through triglyceride by adding modified material triglyceride in electrolyte
During polymerization prepares brilliant glue, as dispersing agent, pass through the presence and increase chain length of the structure of the fatty acid chain on its molecule
The flocculation of particle, which can be made, to be reduced, and the group and particle surface generated due to electrolyte mixing with triglyceride occurs strong
Strong absorption, so that hydrocarbon chain is forced to rest in the solvent neighbouring with particle surface, mutual alienation, to provide sky for particle
Between stability, to be effectively improved the uniformity coefficient in polyacrylamide crystalline substance matrix material polymerization process.
Specific embodiment
In mass ratio 1:8, polyvinylidene fluoride-hexafluoropropene is added in 5% metabisulfite solution of mass fraction, is stirred
Mixed liquor is mixed to obtain, according to parts by weight, weighs 45~50 portions of mixed liquors, 10~15 parts of Diacrylates, 0.5 respectively
~1.0 parts of ammonium persulfates are placed in three-necked flask, then at 75~85 DEG C after 2~3h of heating water bath, standing is cooled to room temperature, and are received
Collection reaction solution is placed at 75~85 DEG C dry 1~2h, and standing is cooled to room temperature, and obtains gel modification liquid；In mass ratio 1:15, it will
Triglyceride is added in gel modification liquid, is stirred and is placed in 3~5h of homogenization in homogenizer, and mixing homogeneous is obtained
Liquid；Again according to parts by weight, 45~50 parts of acrylamide monomers, 25~30 parts of mixing homogenizing fluids, 5~10 parts of N are weighed respectively,
N '-methylene-bisacrylamide and 2~3 parts of ammonium persulfates are placed in glass chromatography column, and program cooling is placed it in after sealing
In low temperature thermostat bath, by 1 DEG C/min speed slow cooling, when temperature is down to -20 DEG C, stop cooling down, 2~3h of insulation reaction,
After the completion of Heat preservation, then press 2 DEG C/min slow cooling, after near -30 DEG C of temperature, stop cooling and insulation reaction 10~
12h places it in 1~2h of standing at room temperature, filter cake is filtered and collect, with 5% hydrochloric acid of mass fraction after the completion of insulation reaction
After rinsing 3~5 times, then after being rinsed to cleaning solution with deionized water and being in neutrality, vacuum freeze drying simultaneously collects to obtain dried object
The large scale is prepared into be uniformly dispersed type polyacrylamide base crystalline substance matrix material.
In mass ratio 1:8, polyvinylidene fluoride-hexafluoropropene is added in 5% metabisulfite solution of mass fraction, is stirred
Mixed liquor is mixed to obtain, according to parts by weight, weighs 45 portions of mixed liquors, 10 parts of Diacrylates, 0.5 part of persulfuric acid respectively
Ammonium is placed in three-necked flask, then at 75 DEG C after heating water bath 2h, standing is cooled to room temperature, and is collected reaction solution and is placed at 75 DEG C
Dry 2h, standing are cooled to room temperature, and obtain gel modification liquid；In mass ratio 1:15, triglyceride is added to gel modification liquid
In, it is stirred and is placed in homogenization 3h in homogenizer, obtain mixing homogenizing fluid；Again according to parts by weight, 45 parts are weighed respectively
Acrylamide monomer, 25 parts of mixing homogenizing fluids, 5 parts of N, N '-methylene-bisacrylamide and 2 parts of ammonium persulfates are placed in glass chromatography
It is placed it in column, after sealing in the low temperature thermostat bath of program cooling, by 1 DEG C/min speed slow cooling, is down to -20 to temperature
DEG C when, stop cooling, insulation reaction 2h, after the completion of Heat preservation, then press 2 DEG C/min slow cooling, near -30 DEG C to temperature
Afterwards, stop cooling and insulation reaction 10h is placed it in after the completion of insulation reaction and stood 1h at room temperature, filter and collect filter
Cake, after being rinsed 3 times with 5% hydrochloric acid of mass fraction, then after being rinsed to cleaning solution with deionized water and being in neutrality, vacuum freeze drying is simultaneously
Dried object is collected to obtain, the large scale can be prepared into and be uniformly dispersed type polyacrylamide base crystalline substance matrix material.
In mass ratio 1:8, polyvinylidene fluoride-hexafluoropropene is added in 5% metabisulfite solution of mass fraction, is stirred
Mixed liquor is mixed to obtain, according to parts by weight, weighs 47 portions of mixed liquors, 12 parts of Diacrylates, 0.7 part of persulfuric acid respectively
Ammonium is placed in three-necked flask, then at 77 DEG C after heating water bath 3h, standing is cooled to room temperature, and is collected reaction solution and is placed at 77 DEG C
Dry 2h, standing are cooled to room temperature, and obtain gel modification liquid；In mass ratio 1:15, triglyceride is added to gel modification liquid
In, it is stirred and is placed in homogenization 4h in homogenizer, obtain mixing homogenizing fluid；Again according to parts by weight, 47 parts are weighed respectively
Acrylamide monomer, 27 parts of mixing homogenizing fluids, 7 parts of N, N '-methylene-bisacrylamide and 2 parts of ammonium persulfates are placed in glass chromatography
It is placed it in column, after sealing in the low temperature thermostat bath of program cooling, by 1 DEG C/min speed slow cooling, is down to -20 to temperature
DEG C when, stop cooling, insulation reaction 2h, after the completion of Heat preservation, then press 2 DEG C/min slow cooling, near -30 DEG C to temperature
Afterwards, stop cooling and insulation reaction 11h is placed it in after the completion of insulation reaction and stood 2h at room temperature, filter and collect filter
Cake, after being rinsed 4 times with 5% hydrochloric acid of mass fraction, then after being rinsed to cleaning solution with deionized water and being in neutrality, vacuum freeze drying is simultaneously
Dried object is collected to obtain, the large scale can be prepared into and be uniformly dispersed type polyacrylamide base crystalline substance matrix material.
In mass ratio 1:8, polyvinylidene fluoride-hexafluoropropene is added in 5% metabisulfite solution of mass fraction, is stirred
Mixed liquor is mixed to obtain, according to parts by weight, weighs 50 portions of mixed liquors, 15 parts of Diacrylates, 1.0 parts of persulfuric acid respectively
Ammonium is placed in three-necked flask, then at 85 DEG C after heating water bath 3h, standing is cooled to room temperature, and is collected reaction solution and is placed at 85 DEG C
Dry 2h, standing are cooled to room temperature, and obtain gel modification liquid；In mass ratio 1:15, triglyceride is added to gel modification liquid
In, it is stirred and is placed in homogenization 5h in homogenizer, obtain mixing homogenizing fluid；Again according to parts by weight, 50 parts are weighed respectively
Acrylamide monomer, 30 parts of mixing homogenizing fluids, 10 parts of N, N '-methylene-bisacrylamide and 3 parts of ammonium persulfates are placed in glassy layer
It analyses in column, is placed it in after sealing in the low temperature thermostat bath of program cooling, by 1 DEG C/min speed slow cooling, be down to temperature-
At 20 DEG C, stop cooling, insulation reaction 3h after the completion of Heat preservation, then presses 2 DEG C/min slow cooling, to temperature near -30
After DEG C, stops cooling and insulation reaction 12h is placed it in after the completion of insulation reaction and stood 2h at room temperature, filter and collect filter
Cake, after being rinsed 5 times with 5% hydrochloric acid of mass fraction, then after being rinsed to cleaning solution with deionized water and being in neutrality, vacuum freeze drying is simultaneously
Dried object is collected to obtain, the large scale can be prepared into and be uniformly dispersed type polyacrylamide base crystalline substance matrix material.
Example 1,2,3 prepared by the present invention is tested for the property, specific test result is as follows shown in table table 1：
1 performance test table of table
As seen from the above table, brilliant gel matrix prepared by the present invention has the excellent performance that is uniformly dispersed.
Claims (4)
- The preparation method of type crystalline substance matrix material 1. a kind of large scale is uniformly dispersed, it is characterised in that specifically preparation step is：（1）In mass ratio 1:8, polyvinylidene fluoride-hexafluoropropene is added in 5% metabisulfite solution of mass fraction, is stirred Mixed liquor is mixed to obtain, according to parts by weight, weighs 45~50 portions of mixed liquors, 10~15 parts of Diacrylates, 0.5 respectively ~1.0 parts of ammonium persulfates are stirred and heating water bath, and standing is cooled to room temperature, and collect reaction solution；（2）It places reaction liquid into drying, standing at 75~85 DEG C to be cooled to room temperature, obtains gel modification liquid, in mass ratio 1:15, it will Triglyceride is added in gel modification liquid, is stirred and is placed in homogenization in homogenizer, and mixing homogenizing fluid is obtained；（3）Again according to parts by weight, 45~50 parts of acrylamide monomers, 25~30 parts of mixing homogenizing fluids, 5~10 parts are weighed respectively N, N '-methylene-bisacrylamide and 2~3 parts of ammonium persulfates are placed in glass chromatography column, and program cooling is placed it in after sealing Low temperature thermostat bath in, slow cooling, when temperature is down to -20 DEG C, stop cooling, insulation reaction；（4）After the completion of Heat preservation, slow cooling stops cooling and insulation reaction after near -30 DEG C of temperature again, to It after the completion of insulation reaction, places it in and stands at room temperature, filter and collect filter cake, washing, drying simultaneously collect to obtain dried object The large scale is prepared into be uniformly dispersed type crystalline substance matrix material.
- The preparation method of type crystalline substance matrix material 2. a kind of large scale according to claim 1 is uniformly dispersed, feature exist In：Step（3）The slow cooling is by 1 DEG C/min speed slow cooling.
- The preparation method of type crystalline substance matrix material 3. a kind of large scale according to claim 1 is uniformly dispersed, feature exist In：Step（4）The slow cooling again is by 2 DEG C/min slow cooling.
- The preparation method of type crystalline substance matrix material 4. a kind of large scale according to claim 1 is uniformly dispersed, feature exist In：Step（4）The washing is after being rinsed 3~5 times with 5% hydrochloric acid of mass fraction, then is rinsed to cleaning solution with deionized water It is in neutrality.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113234252A (en) * | 2021-06-07 | 2021-08-10 | 石河子大学 | Composite pore crystal glue medium and preparation method thereof |
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| CN1736579A (en) * | 2005-08-02 | 2006-02-22 | 浙江工业大学 | Super macroporous continuous bed crystalloid colloid medium and preparation process thereof |
| CN104177645A (en) * | 2014-08-14 | 2014-12-03 | 华南师范大学 | Preparation method of composite crystal adhesive |
| CN106009030A (en) * | 2016-06-26 | 2016-10-12 | 周荣 | Preparation method of large-sized polyacrylamide cryogel |
| CN107617426A (en) * | 2017-09-25 | 2018-01-23 | 常州市宇科不绣钢有限公司 | A kind of preparation method of high adsorption capacity crystalline substance glue microsphere particle |
| CN107868191A (en) * | 2017-11-06 | 2018-04-03 | 华南师范大学 | A kind of method of modifying of graphene |
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2018
- 2018-05-18 CN CN201810478779.6A patent/CN108864362A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736579A (en) * | 2005-08-02 | 2006-02-22 | 浙江工业大学 | Super macroporous continuous bed crystalloid colloid medium and preparation process thereof |
| CN104177645A (en) * | 2014-08-14 | 2014-12-03 | 华南师范大学 | Preparation method of composite crystal adhesive |
| CN106009030A (en) * | 2016-06-26 | 2016-10-12 | 周荣 | Preparation method of large-sized polyacrylamide cryogel |
| CN107617426A (en) * | 2017-09-25 | 2018-01-23 | 常州市宇科不绣钢有限公司 | A kind of preparation method of high adsorption capacity crystalline substance glue microsphere particle |
| CN107868191A (en) * | 2017-11-06 | 2018-04-03 | 华南师范大学 | A kind of method of modifying of graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113234252A (en) * | 2021-06-07 | 2021-08-10 | 石河子大学 | Composite pore crystal glue medium and preparation method thereof |
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