CN110038520A - A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] - Google Patents
A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] Download PDFInfo
- Publication number
- CN110038520A CN110038520A CN201910180695.9A CN201910180695A CN110038520A CN 110038520 A CN110038520 A CN 110038520A CN 201910180695 A CN201910180695 A CN 201910180695A CN 110038520 A CN110038520 A CN 110038520A
- Authority
- CN
- China
- Prior art keywords
- soybean fiber
- cup
- adsorbent
- aromatic modified
- stirring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
Abstract
The invention discloses a kind of preparation methods of the aromatic modified soybean fiber adsorbent of cup [8], which is characterized in that pre-processes soybean fiber 2mol/L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution, obtains pretreated soybean azelon；Using propane diamine and urea to pretreated soybean azelon amination, amination soybean fiber is obtained；Then, methanol: 64 ~ 68%, thionyl chloride: 15 ~ 18%, tert-butyl-calix [8] aromatic hydrocarbons: 4 ~ 8%, stirring and dissolving, add amination soybean fiber: 10 ~ 12%, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, after cooling, it is washed with deionized to neutrality, it is separated by solid-liquid separation, it is dry, obtain the aromatic modified soybean fiber adsorbent of cup [8].The adsorbent has very high adsorption capacity to pyrrole Luo Hong, has specificity with specifically, at low cost, high mechanical strength can be Reusability 10 times or more, and adsorbent can be easily separated.
Description
Technical field
The present invention relates to a kind of preparation method of modified magnetic biological adsorption agent, in particular to a kind of cup [8] is aromatic modified
The preparation method of soybean fiber adsorbent and the application being enriched with to pyrrole Luo Hong adsorbing separation, belong to environment and chemical technology is led
Domain.
Background technique
Pyrrole Luo Hong, molecular formula are C17H19ClN2It is red that RNA is presented in O, pyrrole Luo Hong, is usually used in detecting point of RNA in cell
Cloth, basic dye, different colours can be presented in it in conjunction with intracellular DNA, RNA respectively.It is often used with together with methyl green and is
Methyl green-pyronin, when methyl green and pyronin are as mixed dye, methyl green is aobvious in conjunction with DNA selective in chromatin
Show green or blue；Pyronin is displayed in red with the RNA selective binding in kernel, cytoplasm.Its reason may be two kinds of dyes
There is Competition in the mixing dye liquor of material, while two kinds of nucleic acid molecules are all polymers, and its extent of polymerization is different.Methyl
Green is presented in conjunction with green DNA easily high with extent of polymerization.And red is then presented in pyronin in conjunction with the lower RNA of extent of polymerization
(but the DNA of depolymerization can also be combined with pyronin and red is presented).That is RNA is big to pyronin affinity, is dyed to red, and DNA
It is big to methyl green affinity, be dyed to green, the purification of dyestuff, separation, in removal ambient water dyestuff all have it is highly important
Meaning.
Calixarenes generally refers to the macrocyclic compound being made of methylene-bridged phenol units, nineteen forty-two gold gram
(Zinke, Austria) synthesis for the first time obtains, and is known as cup by ancient odd (C.D.Gutscht, the U.S.) due to its structure is as a wineglass
Aromatic hydrocarbons.Most of calixarenes fusing point is higher, at 250 DEG C or more.It is several there are commonly the solubility very little in solvent
It is not soluble in water.There is calixarenes " cavity " of adjustable section to be named as cup [n] aromatic hydrocarbons according to phenol units number.
More typically cup [4] aromatic hydrocarbons, cup [6] aromatic hydrocarbons and cup [8] aromatic hydrocarbons.It is a kind of more adaptation extensively compared with cyclodextrin, crown ether
The analogue enztme of property, the third generation host compound referred to as after crown ether and cyclodextrin.Therefore, based on cup [n] aromatic hydrocarbons
Molecular capsule research molecular recognition, the fractionation of optically active substance, the trapping of compound with separate, catalyst and function
Before will all there be wide application in the fields such as nano material, the absorption of various drugs or desorption, self-assembled structures and oversubscription fructification
Scape and development potentiality.Calixarenes is directly used in calixarenes in solvent extraction and is lost, while also to use toxic organic solvent, makes
At environmental pollution, it is unfavorable for operating, the application is linked to calixarenes as active group on biological skeleton, overcomes above-mentioned lack
Point.
Soybean fiber belongs to aftergrowth azelon, using food grade soyabean protein powder as raw material, utilizes biology
Engineering technology extracts the globulin in albumen powder, by adding functional aid, is grafted, altogether with high polymers such as itrile group, hydroxyls
Poly-, blending, is made certain density protein spinning solution, changes protein steric structure, forms through wet spinning.It has
Soft feel as cashmere, the sub-dued lustre as silk are praised better than the excellent performances such as the warmth retention property of cotton and good skin-friendly
For " health and comfort fiber of new century " and " the good fabric that skin is liked ".Soybean fiber outer layer is essentially all albumen
Matter, containing a variety of amino acid needed by human, soybean fiber has carboxyl abundant, amino groups, it is easy to will live
Property group connection on.Soybean fiber is with relative density is low, specific strength is high, large specific surface area, light-weight, good penetrability
The advantages that, usual specific surface area is bigger, hole is more, the site of surface link functional group is abundanter, the active group chained
More, the adsorption capacity of the more adsorbents of active group is bigger, and adsorption capacity is stronger.
Summary of the invention
An object of the present invention is to provide a kind of preparation method of aromatic modified soybean fiber adsorbent of cup [8],
Another object is that aromatic modified soybean fiber adsorbent the separating to pyrrole Luo Hong of a kind of cup [8] obtained.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8], which is characterized in that this method have with
Lower processing step:
(1) soybean fiber pre-processes: soybean fiber being crushed, partial size is between 1.5 ~ 2.5mm, with 2mol/L sulfuric acid
In 1.0mol/L ammonium persulfate mixed solution, 4 ~ 6 h of soaking at room temperature, then 20min is boiled, after cooling, deionized water is used in filtering
Washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is added by following composition mass percentage concentration, deionized water: 74 ~
76%, propane diamine: 6 ~ 8%, urea: 6 ~ 8%, heating stirring dissolution, pretreated soybean azelon: 10 ~ 12%, the sum of each component
It is dry absolutely, to be washed with deionized, being separated by solid-liquid separation after cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h,
Obtain amination soybean fiber；
(3) preparation of the aromatic modified soybean fiber adsorbent of cup [8]: in the reactor, dense by following composition quality percentage
Degree is added, methanol: 64 ~ 68%, thionyl chloride: and 15 ~ 18%, tert-butyl-calix [8] aromatic hydrocarbons: 4 ~ 8%, stirring and dissolving adds amino
Change soybean fiber: 10 ~ 12%, the sum of each component is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, cooling
Afterwards, it is washed with deionized to neutrality, is separated by solid-liquid separation, it is dry, obtain the aromatic modified soybean fiber adsorbent of cup [8].
Soybean fiber as described in step (1) and 2mol/L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution are consolidated
Liquor ratio is between 1g:15 ~ 18mL.
Cup [8] aromatic modified soybean fiber adsorbent is applied in separation and concentration, feature are as follows: by the cup of preparation
[8] aromatic modified soybean fiber adsorbent impregnates 0.5 ~ 1h with deionized water, adsorbs by static method.
Cup [8] the aromatic modified soybean fiber adsorbent of preparation deionized water is impregnated into 0.5 ~ 1h, by dynamic method
Absorption.
Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1) the aromatic modified soybean fiber adsorbent of cup [8] that obtains of the present invention have good physical and chemical stability and
Excellent mechanical strength has big specific surface area, and adsorption capacity is big, reaches 198.25mg/g to pyrrole Luo Hong maximum adsorption capacity,
It is wear-resisting can Reusability number up to 10 times or more, the speed of absorption is fast, and absorption chooses, and desorption performance is good, can be wider
Soda acid within the scope of use.
(2) the aromatic modified soybean fiber adsorbent of cup [8] that the present invention obtains both had had the excellent of solid support material
Point also solves the losing issue in active group application, to rutin with very strong specificity and specifically.
(3) condition for crossing range request of synthesis is easy to control, and low energy consumption, easy to operate, is belonged to process for cleanly preparing, is easy to
Industrialized production is natural green product, biodegradable.
Specific embodiment
Embodiment 1
(1) soybean fiber pre-process: by 20g partial size between 1.5 ~ 2.5mm soybean fiber, with the 2mol/ of 320mL
In L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution, 5 h of soaking at room temperature, then boil 20min, after cooling, filtering, spend from
Sub- water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 150mL, propane diamine: 14g, urine
Element: 14g, heating stirring dissolution, pretreated soybean azelon: 22g, it is cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h
Afterwards, it is washed with deionized, is separated by solid-liquid separation, it is dry, obtain amination soybean fiber；
(3) it the preparation of the aromatic modified soybean fiber adsorbent of cup [8]: in the reactor, is separately added into, methanol: 168mL,
Thionyl chloride: 21mL, tert-butyl-calix [8] aromatic hydrocarbons: 14g, stirring and dissolving add amination soybean fiber: 20g, in 60
± 2 DEG C of constant temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain cup [8]
Aromatic modified soybean fiber adsorbent.
Embodiment 2
(1) soybean fiber pre-process: by 50g partial size between 1.5 ~ 2.5mm soybean fiber, with the 2mol/ of 900mL
In L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution, 4 h of soaking at room temperature, then boil 20min, after cooling, filtering, spend from
Sub- water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 300mL, propane diamine: 24g, urine
Element: 32g, heating stirring dissolution, pretreated soybean azelon: 48g, it is cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h
Afterwards, it is washed with deionized, is separated by solid-liquid separation, it is dry, obtain amination soybean fiber；
(3) it the preparation of the aromatic modified soybean fiber adsorbent of cup [8]: in the reactor, is separately added into, methanol: 320mL,
Thionyl chloride: 40mL, tert-butyl-calix [8] aromatic hydrocarbons: 32g, stirring and dissolving add amination soybean fiber: 48g, in 60
± 2 DEG C of constant temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain cup [8]
Aromatic modified soybean fiber adsorbent.
Embodiment 3
(1) soybean fiber pre-process: by 40g partial size between 1.5 ~ 2.5mm soybean fiber, with the 2mol/ of 600mL
In L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution, 6 h of soaking at room temperature, then boil 20min, after cooling, filtering, spend from
Sub- water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 152mL, propane diamine: 16g, urine
Element: 12g, heating stirring dissolution, pretreated soybean azelon: 20g, it is cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h
Afterwards, it is washed with deionized, is separated by solid-liquid separation, it is dry, obtain amination soybean fiber；
(3) it the preparation of the aromatic modified soybean fiber adsorbent of cup [8]: in the reactor, is separately added into, methanol: 172mL,
Thionyl chloride: 18mL, tert-butyl-calix [8] aromatic hydrocarbons: 12g, stirring and dissolving add amination soybean fiber: 22g, in 60
± 2 DEG C of constant temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain cup [8]
Aromatic modified soybean fiber adsorbent.
Embodiment 4
(1) soybean fiber pre-process: by 50g partial size between 1.5 ~ 2.5mm soybean fiber, with the 2mol/ of 850mL
In L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution, 5.5 h of soaking at room temperature, then 20min is boiled, after cooling, filtering is spent
Ion water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 310mL, propane diamine: 24g, urine
Element: 24g, heating stirring dissolution, pretreated soybean azelon: 44g, it is cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h
Afterwards, it is washed with deionized, is separated by solid-liquid separation, it is dry, obtain amination soybean fiber；
(3) it the preparation of the aromatic modified soybean fiber adsorbent of cup [8]: in the reactor, is separately added into, methanol: 330mL,
Thionyl chloride: 11mL, tert-butyl-calix [8] aromatic hydrocarbons: 20g, stirring and dissolving add amination soybean fiber: 48g, in 60
± 2 DEG C of constant temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain cup [8]
Aromatic modified soybean fiber adsorbent.
Embodiment 5
Weigh 1.0g glasss [8] aromatic modified soybean fiber adsorbents be placed in 250mL stuffed conical flask impregnate 0.5 ~
1.0h, after filtration washing, it is in 100mg/L pyrrole Luo Hong standard solution, with diluted acid or the pH of alkali regulation system that 100mL concentration, which is added,
Value is 5.0 ~ 7.0, and 40 min of concussion absorption, take supernatant at room temperature, and the concentration of pyrrole Luo Hong is measured with spectrophotometry, according to
The concentration difference of pyrrole Luo Hong, calculates the aromatic modified soybean fiber adsorbent of cup [8] to pyrrole Luo Hong's in the solution of absorption front and back
Removal rate, the present invention obtained by the aromatic modified soybean fiber adsorbent of cup [8] all exist to the removal rate of pyrrole Luo Hong
95.82% or more, reach as high as 97.2%.The concentration of pyrrole Luo Hong standard solution is increased into 100mg/mL by same steps, is measured
Cup [8] aromatic modified soybean fiber adsorbent is 198.25mg/g to pyrrole Luo Hong adsorption capacity.
Claims (3)
1. a kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8], which is characterized in that this method has following
Processing step:
(1) soybean fiber pre-processes: soybean fiber being crushed, partial size is between 1.5 ~ 2.5mm, with 2mol/L sulfuric acid
In 1.0mol/L ammonium persulfate mixed solution, 4 ~ 6 h of soaking at room temperature, then 20min is boiled, after cooling, deionized water is used in filtering
Washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is added by following composition mass percentage concentration, deionized water: 74 ~
76%, propane diamine: 6 ~ 8%, urea: 6 ~ 8%, heating stirring dissolution, pretreated soybean azelon: 10 ~ 12%, the sum of each component
It is dry absolutely, to be washed with deionized, being separated by solid-liquid separation after cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h,
Obtain amination soybean fiber；
(3) preparation of the aromatic modified soybean fiber adsorbent of cup [8]: in the reactor, dense by following composition quality percentage
Degree is added, methanol: 64 ~ 68%, thionyl chloride: and 15 ~ 18%, tert-butyl-calix [8] aromatic hydrocarbons: 4 ~ 8%, stirring and dissolving adds amino
Change soybean fiber: 10 ~ 12%, the sum of each component is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, cooling
Afterwards, it is washed with deionized to neutrality, is separated by solid-liquid separation, it is dry, obtain the aromatic modified soybean fiber adsorbent of cup [8].
2. a kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] according to claim 1, special
Sign is, soybean fiber as described in step (1) and 2mol/L sulfuric acid and 1.0mol/L ammonium persulfate mixed solution are consolidated
Liquor ratio is between 1g:15 ~ 18mL.
3. a kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] according to claim 1 is made
The standby aromatic modified soybean fiber adsorbent of cup [8].
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910180695.9A CN110038520A (en) | 2019-03-11 | 2019-03-11 | A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910180695.9A CN110038520A (en) | 2019-03-11 | 2019-03-11 | A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110038520A true CN110038520A (en) | 2019-07-23 |
Family
ID=67274600
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910180695.9A Withdrawn CN110038520A (en) | 2019-03-11 | 2019-03-11 | A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110038520A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920469A (en) * | 2014-05-06 | 2014-07-16 | 济南大学 | Preparation method of citric acid silk adsorbent |
| CN106311187A (en) * | 2016-09-07 | 2017-01-11 | 济南大学 | Preparation method of melamine-modified magnetic coconut root-bark adsorbent |
-
2019
- 2019-03-11 CN CN201910180695.9A patent/CN110038520A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920469A (en) * | 2014-05-06 | 2014-07-16 | 济南大学 | Preparation method of citric acid silk adsorbent |
| CN106311187A (en) * | 2016-09-07 | 2017-01-11 | 济南大学 | Preparation method of melamine-modified magnetic coconut root-bark adsorbent |
Non-Patent Citations (1)
| Title |
|---|
| 魏静 等: "杯[4]芳烃-β-环糊精席夫碱的合成及其对碱性品红的吸附", 《石油化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103469362B (en) | Porous polyethyleneimine and chitosan blend fiber and preparation method and applications thereof | |
| CN104744702B (en) | Bovine serum albumin molecular imprinted polymer on surface and preparation method thereof | |
| CN103756002B (en) | A kind of porous magnetic spherex and preparation method thereof | |
| CN105019142B (en) | A kind of preparation method of the micro-nano PET of high pore volume | |
| CN101829549B (en) | Uniform-hole amine resin and preparation and application method thereof | |
| CN105968215B (en) | A kind of application of the method for nano-cellulose grafted amino group acid in terms of ultrafiltration membrane | |
| CN105195099B (en) | A kind of preparation method of the modified macroporous GAG adsorbent of beta cyclodextrin | |
| CN110396146A (en) | The preparation method of phenyl boric acid modified magnetic beta cyclo dextrin polymer and its application of Selective Separation shikimic acid | |
| CN103538306A (en) | Preparation method of antibacterial mildewproof silk wallpaper | |
| CN110394163A (en) | The preparation method of phenyl boric acid modified magnetic chitosan and its application of Selective Separation shikimic acid | |
| CN108452781A (en) | The preparation method of core-shell magnetic gamma-cyclodextrin polymer composites and application | |
| CN106046256A (en) | Method for preparing geniposide molecularly imprinted polymer magnetic microspheres | |
| CN106478577B (en) | A kind of process for separation and purification of flavanones and its analogue | |
| CN104248984B (en) | The preparation method of spherical diatomite mesoporous composite material and loaded catalyst and its preparation method and application and ethyl acetate | |
| Yao et al. | Application of cellulose to chromatographic media: Cellulose dissolution, and media fabrication and derivatization | |
| CN105771923A (en) | Melamine sponge /alginic acid composite type adsorbing material and preparation method thereof | |
| CN110038520A (en) | A kind of preparation method of the aromatic modified soybean fiber adsorbent of cup [8] | |
| CN102140121B (en) | A kind of tower draws the preparation method of industrial tannic acid | |
| CN107936551A (en) | A kind of composite membrane based on bamboo and wood hemicellulose/γ polyglutamic acids and its preparation method and application | |
| CN110038521A (en) | A kind of preparation method of the porous protein gel adsorbent of calixarenes modified magnetic | |
| WO2010060254A1 (en) | High selectivity hydrogen bonding polymeric adsorbent and its application on the separation and purification of effective constituents from ginkgo extract | |
| CN108543524B (en) | A kind of preparation method of the modified banana fiber adsorbent of diethylenetriamines | |
| CN106831803B (en) | Preparation method and application of benzophenanthridine alkaloid molecularly imprinted magnetic microspheres | |
| CN106092717A (en) | A kind of method that novel solid extracting agent synchronizes enrichment desalination to bovine serum albumin | |
| CN110141605A (en) | A kind of preparation method of snowpoppy total alkaloid nanoparticle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190723 |