CN106310234A - Application of bovine lactoferrin and hydrolysate or enzymatic hydrolysate in medicine for treating gynecological diseases - Google Patents
Application of bovine lactoferrin and hydrolysate or enzymatic hydrolysate in medicine for treating gynecological diseases Download PDFInfo
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Abstract
The invention discloses application of bovine lactoferrin and hydrolysate or enzymatic hydrolysate in a medicine for treating gynecological diseases. The bovine lactoferrin is protein which is separated and extracted from milk, bovine coloctrum or bovine whey protein and has biological activity; the hydrolysate or the enzymatic hydrolysate is lactoferricin. According to the application disclosed by the invention, by adding the bovine lactoferrin and the enzymatic hydrolysate lactoferricin thereof in the medicine for treating gynecological diseases, the bovine lactoferrin and hydrolysate or enzymatic hydrolysate have the advantages of high medicine solubility, quick effect, definite curative effect and the like in gynecological local application. Compared with a suppository, the bovine lactoferrin and hydrolysate or enzymatic hydrolysate are higher in dissolving speed and better in absorption. Experiments prove that effervescent tablets prepared by the invention have a remarkable bacteriostatic action on gonococcus, staphylococcus aureus, escherichia coli, candida albicans and microsporum gypseum, so the effervescent tablets have better curative effects on gynecological inflammation caused by the germs.
Description
Technical field
The present invention relates to Bovine Lactoferrin applied technical field, specifically a kind of Bovine Lactoferrin and hydrolysis or zymolyte exist
Application in gynecological's medicine.
Background technology
Epidemiological study shows: female internal vulva illness remain the main commonly encountered diseases of female friend and frequently-occurring disease it
One.China's relevant information investigation display, women of child-bearing age's gynaecopathia sickness rate is more than 70%.Paper reference net is with phase before 40 years
Ratio, the ovarian tumors rate of China women adds 33%, and the sickness rate of endometriosis rises to more than 15%.Many female
The premature ovarian failure of property is also advanced by 5～10 years, in 40～the women of 55 years old, has the women of nearly half to occur in that climacteric in advance
Symptom.In the pick test that substantial amounts of door exanthema is suffered from, all can detect several or even tens kinds of pathogenic bacterium, antibacterial and virus are described
It it is one of the pathogenesis of these illness.Gynecological inflammation and women beauty treatment have inherence cause effect relation, can cause series skin,
The cosmetic problem of the aspects such as body, such as pale or sallow complexion, skin splash, appearance are wan and sallow, emaciated physique or obesity, body odor
Deng.The medicine for the treatment of and method are numerous the most many, but, due to the particularity of illness, it requires the medicine intending selecting
The bacteriostasis and sterilization effect of existing wide spectrum, does not has again the side effect of synthetic antibiotic to cause affected part microenvironment and degenerate, the most protected and
Repair the effect of mucosa, there is no again sense of discomfort.It is thus desirable to provide a kind of medicine meeting above-mentioned requirements.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of Bovine Lactoferrin and zymolyte thereof answering in gynecologic medicine
With, Bovine Lactoferrin and zymolyte thereof the gynecological's medicine bactericidal effect prepared is good, itself and there is endocrine regulation and beauty treatment
Effect of skin care.
Bovine Lactoferrin and hydrolysis thereof or zymolyte application in preparation gynecological medicine, described hydrolysis or zymolyte be newborn
Ferrum element.
Further, described Bovine Lactoferrin refers to the tool of separation and Extraction from milk, cattle colostrums or milk albumin
Bioactive albumen.
Further, described Bovine Lactoferrin is the Bovine Lactoferrin extracted from the milk that normal milk cattle secretes, or
From the Bovine Lactoferrin through vaccinating or extract milk that milk cattle after genetic modification is produced.
Further, described breast ferrum element molecular weight is between 3700-5000Da.
Further, described treatment medicine for gynecopathy refers to for treating vulval ulcer, inflammation, red and swollen or rotten to the corn
Medicine and for cleaning the medicine of vagina.
A kind of gynaecological applications applying Bovine Lactoferrin and zymolyte thereof given below, it is effervescent tablet, including following group
Point:
Bovine Lactoferrin or breast ferrum element 4-10
Flos Lonicerae extract 60-120
Herba Taraxaci extract 40-100
Sodium bicarbonate 100-500
Citric acid 60-150
Sodium lauryl sulphate 2-10
Microcrystalline Cellulose 60-130
Ethanol 8-20ml
Magnesium stearate 3-15
Dried starch 200-500
Described Bovine Lactoferrin be saturation be the low ferrum saturation lactoferrin of 5-8%.
Above-mentioned effervescent tablet preparation method is:
(1), Flos Lonicerae, Herba Taraxaci are decocted 2 times by 8-10 times of weight water respectively, each 2 hours, united extraction liquid, filters dense
It is reduced to do, thus respectively obtains Flos Lonicerae extract, Herba Taraxaci extract；
(2), by low ferrum saturation lactoferrin or breast ferrum element, sodium bicarbonate, citric acid, sodium lauryl sulphate, crystallite fibre
Dimension element, ethanol, magnesium stearate, dried starch and Flos Lonicerae extract, Herba Taraxaci extract mix, tabletting and get final product.
The preparation process of described low ferrum saturation lactoferrin is:
1st step, uses cation exchange resin that the lactoferrin in Lac Bovis seu Bubali is adsorbed, resolved；Described resolving is to adopt
With two grades of parsings, the first order resolves the saline solution parsing being to use 1～2.5%, and desorbed solution is lactoperoxidase pheron, discards；
The second level resolves the saline solution parsing being to use 3.5～7%, and desorbed solution is sent into the 2nd step and processed；Described saline solution refer to sodium salt,
Potassium salt or calcium salt soln；
2nd step, the desorbed solution obtaining the 1st step uses separation film to concentrate；Described separation film is that molecular cut off exists
The ultrafilter membrane of 1000～30K；
3rd step, the concentrated solution that the 2nd step obtains uses insoluble Fe3+Chelating resin adsorbs, then uses separation film to concentration
Liquid concentrates；Need during described adsorption operations in concentrated solution, add acetic acid, acetate and citrate, prepare its absorption
In environment, citrate concentration is 0.1mol/L ~ 0.5mol/L, and regulates pH to 5.0～6.7；Described separation film is to retain point
Son measures the ultrafilter membrane 1000～30K；
Further, the concentrated solution that the 2nd described step obtains, can be again through a weak-type cation before sending into the 3rd step
The absorption of resin, solution echo the concentration of ultrafilter membrane；Described weak-type cationic resin refers to CM resin.
Described insoluble Fe3+Chelating resin refers to D403 chelating resin；In the 3rd described step, the adsorption time of resin
20～120 minutes, during absorption, rotating speed of agitator speed was 20～150rpm, and adsorption temp is at 3～30 DEG C.
In described 1st step, the preparation process of cation exchange resin is:
1st step, takes 10g chloracetylated polystyrene-divinylbenzene microspheres carrier PS-acyl-Cl, adds 60ml oxolane
Swelling 12 h, add 40ml methanol, then according to weight ratio PS-acyl-Cl: ethylenediamine: sodium bicarbonate is 1:8:0.7, depends on
Secondary addition ethylenediamine and sodium bicarbonate, be at 80 DEG C stirring reaction 24h, after reaction terminates, poured into by product in sand core funnel,
Being washed till neutrality with distilled water, methanol filter wash is dried under vacuum to constant weight 3 times, obtains cross-linking EDA microsphere supported；
2nd step, claims 60g to take crosslinking EDA microsphere supported, is placed in three-neck flask, after adding swelling 12 h of dimethylformamide, add
Enter 2-acrylamido-2-methyl propane sulfonic acid 16g, N-butoxy methyl acrylamide 3g, acrylic acid double cyclopentenyl ester,
K2CO35g, tetrabutyl ammonium bromide 12g, under stirring in the oil bath of uniform temperature back flow reaction, reaction terminate after by product
It is transferred in sintered filter funnel, with distilled water diafiltration to neutral after cleaning 4 times with the HC1 of 5wt%, finally drains after methanol filter wash,
It is dried under vacuum to constant weight, obtains cation exchange resin.
Bovine Lactoferrin is a kind of natural broad-spectrum antibiotic, has suppression to the pathogenic bacterium causing gynecological's sufferer and kills work
With.The hydrolysis of Bovine Lactoferrin or zymolyte breast ferrum element have more the antibacterial and sterilization effect of high two orders of magnitude than Bovine Lactoferrin
Really, and can effectively regulating intestinal canal flora movable, promote human metabolism, thus regulate human endocrine, reduce color
Speckle etc..Research shows, Bovine Lactoferrin is the most protected and repairs the effect of mucosa and the effect etc. of immunomodulating slow down aging.Cause
This selects Bovine Lactoferrin and hydrolysis thereof or zymolyte breast ferrum element to be desirable as the medicine for the treatment of gynecological diseases.
The present invention is by adding Bovine Lactoferrin and zymolyte breast ferrum element thereof in gynecologic medicine, in local application of gynecological
There is the advantages such as high, rapid-action, the determined curative effect of drug solubility.Compared with suppository, its dissolution velocity is faster than suppository, absorptance bolt
Agent is good.Experiment prove the effervescent tablet prepared of the present invention to gonococcus, staphylococcus aureus, colibacillus, Candida albicans,
Microsporon gypseum can have significant bacteriostasis, therefore has preferably treatment for above-mentioned germ gynecological inflammation
Effect.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
A kind of effervescent tablet treating gynaecopathia, its component is as follows:
Low ferrum saturation lactoferrin 6
Flos Lonicerae extract (solid content ＞ 80%) 100
Herba Taraxaci extract (solid content ＞ 80%) 80
Sodium bicarbonate 300
Citric acid 100
Sodium lauryl sulphate 4
Microcrystalline Cellulose 100
Ethanol 10ml
Magnesium stearate 6
Dried starch 294.
Effervescent tablet preparation method is as follows:
1, the preparation of low ferrum saturation lactoferrin: semi-skimmed milk 1890L, pH6.7, total protein is 3.38g/L, lactoferrin
Concentration is 126mg/L, and SPC70 resin is added agitator tank, adsorbs 80min, and stir speed (S.S.) is 60rpm, collects after adsorbing
Milk also uses RO water rinse resin, adds first order 100L 2.5%NaCl aqueous solution and desorbs 40min, speed of agitator 40rpm, receives
Collect with RO water wash after collected explanations or commentaries attached liquid；Add second level 100L 5.5%NaCl aqueous solution and desorb 40min, speed of agitator
40rpm, collects and collects resin 3 times with RO water wash after solving attached liquid.Desorbed solution and the second time RO leacheate of the second level merge
Collect 180L altogether, be transported in the micro-filtration membrane equipment of 0.1 μm carry out degerming, remove impurity；Device for ultrafiltration membrane by 30K molecular retention amount
Carrying out desalination and concentration, it is 20% that sampling detects its ferrum saturation；Lactoferrin dope is input to equipped with removing in CM resin container miscellaneous
Albumen, the device for ultrafiltration membrane collecting the lactoferrin solution continuation 10K molecular retention amount after having adsorbed foreign protein carries out desalination
Concentrate, a small amount of dope therein is carried out lyophilization gained pale pink dry powder.Powder moisture 3.0%, ash 1.1%, total egg
It is 96.3% in vain, ferrum saturation 20%；Again remaining lactoferrin dope is input to equipped with placing in D403 chelating resin tank
Row deferrization, add 0.1mol/L citrate, and Acetic acid-sodium acetate buffer adjust pH to 6.0, in addition stirring and adsorbing iron ion,
120 minutes resin absorption time, rotating speed of agitator speed 60rpm.Lactoferrin solution after collecting with absorption iron ion continues
Carry out desalination and concentration with the device for ultrafiltration membrane of 10K molecular retention amount, collect dope and carry out lyophilization gained pale pink dry powder.Powder
End water content 3.0%, ash 1.0%, total protein is 96.3%, ferrum saturation 7%.
2, the preparation of extract: Flos Lonicerae, Herba Taraxaci are decocted 2 times by 8-10 times of weight water respectively, each 2 hours, closes
And extracting solution, filtering and concentrating is to dry, thus respectively obtains Flos Lonicerae extract, Herba Taraxaci extract.
3, remaining material is added in low ferrum saturation lactoferrin and extract, mixing, tabletting.
Embodiment 2
A kind of effervescent tablet treating gynaecopathia, its component is as follows:
Low ferrum saturation lactoferrin 9
Flos Lonicerae extract (solid content ＞ 80%) 90
Herba Taraxaci extract (solid content ＞ 80%) 90
Sodium bicarbonate 280
Citric acid 110
Sodium lauryl sulphate 7
Microcrystalline Cellulose 110
Ethanol 15ml
Magnesium stearate 9
Dried starch 280
Effervescent tablet preparation method is as follows:
1, the preparation of low ferrum saturation lactoferrin: semi-skimmed milk 1890L, pH6.7, total protein is 3.38g/L, lactoferrin
Concentration is 126mg/L, and SPC70 resin is added agitator tank, adsorbs 80min, and stir speed (S.S.) is 60rpm, collects after adsorbing
Milk also uses RO water rinse resin, adds first order 100L 2.5%NaCl aqueous solution and desorbs 40min, speed of agitator 40rpm, receives
Collect with RO water wash after collected explanations or commentaries attached liquid；Add second level 100L 5.5%NaCl aqueous solution and desorb 40min, speed of agitator
40rpm, collects and collects resin 3 times with RO water wash after solving attached liquid.Desorbed solution and the second time RO leacheate of the second level merge
Collect 180L altogether, be transported in the micro-filtration membrane equipment of 0.1 μm carry out degerming, remove impurity；Device for ultrafiltration membrane by 30K molecular retention amount
Carrying out desalination and concentration, it is 20% that sampling detects its ferrum saturation；Lactoferrin dope is input to equipped with removing in CM resin container miscellaneous
Albumen, the device for ultrafiltration membrane collecting the lactoferrin solution continuation 10K molecular retention amount after having adsorbed foreign protein carries out desalination
Concentrate, a small amount of dope therein is carried out lyophilization gained pale pink dry powder.Powder moisture 3.0%, ash 1.1%, total egg
It is 96.3% in vain, ferrum saturation 20%；Again remaining lactoferrin dope is input to equipped with placing in D403 chelating resin tank
Row deferrization, add 0.1mol/L citrate, and Acetic acid-sodium acetate buffer adjust pH to 6.0, in addition stirring and adsorbing iron ion,
120 minutes resin absorption time, rotating speed of agitator speed 60rpm.Lactoferrin solution after collecting with absorption iron ion continues
Carry out desalination and concentration with the device for ultrafiltration membrane of 10K molecular retention amount, collect dope and carry out lyophilization gained pale pink dry powder.Powder
End water content 3.0%, ash 1.0%, total protein is 96.3%, ferrum saturation 7%.
2, the preparation of extract: Flos Lonicerae, Herba Taraxaci are decocted 2 times by 8-10 times of weight water respectively, each 2 hours, closes
And extracting solution, filtering and concentrating is to dry, thus respectively obtains Flos Lonicerae extract, Herba Taraxaci extract.
3, remaining material is added in low ferrum saturation lactoferrin and extract, mixing, tabletting.
Embodiment 3
A kind of effervescent tablet treating gynaecopathia, its component is as follows:
Bovine Lactoferrin or breast ferrum element 4
Flos Lonicerae extract (solid content ＞ 80%) 60
Herba Taraxaci extract (solid content ＞ 80%) 50
Sodium bicarbonate 120
Citric acid 80
Sodium lauryl sulphate 4
Microcrystalline Cellulose 70
Ethanol 10ml
Magnesium stearate 5
Dried starch 200
Effervescent tablet preparation method is as follows:
1 is consistent with embodiment 2, differs only in, and is to be prepared into by following method by SPC70 resin replacement therein
To cation exchange resin:
1st step, takes 10g chloracetylated polystyrene-divinylbenzene microspheres carrier (PS-acyl-Cl), adds 60ml tetrahydrochysene furan
Mutter swelling 12 h, adds 40ml methanol, then according to weight ratio (PS-acyl-Cl): ethylenediamine (EDA): sodium bicarbonate is 1:
8:0.7, is sequentially added into ethylenediamine and sodium bicarbonate, is at 80 DEG C stirring reaction 24h, after reaction terminates, pours product into sand
In core funnel, being washed till neutrality with distilled water, methanol filter wash is dried under vacuum to constant weight 3 times, obtains cross-linking EDA microsphere supported；
2nd step, claims 60g to take crosslinking EDA microsphere supported, is placed in three-neck flask, after adding swelling 12 h of dimethylformamide, add
Enter 2-acrylamido-2-methyl propane sulfonic acid (AMPS) 16g, N-butoxy methyl acrylamide (NBMA) 3g, acrylic acid pair
Cyclopentenyl ester (DCPA), K2CO35g, tetrabutyl ammonium bromide (TBAB) 12g, reflux under stirring in the oil bath of uniform temperature
Reaction, product is transferred in sintered filter funnel after terminating by reaction, after cleaning 4 times with the HC1 of 5wt% with distilled water diafiltration extremely
Neutrality, finally drains after methanol filter wash, is dried under vacuum to constant weight, obtain cation exchange resin.
The technical specification of the low ferrum saturation lactoferrin finally given is: powder moisture 3.0%, ash 1.0%, total egg
It is 96.8% in vain, ferrum saturation 6%.
2 is consistent with embodiment 2.
3 is consistent with embodiment 2.
Embodiment 4
A kind of effervescent tablet treating gynaecopathia, its component is as follows:
Breast ferrum element 5
Flos Lonicerae extract (solid content ＞ 80%) 110
Herba Taraxaci extract (solid content ＞ 80%) 90
Sodium bicarbonate 400
Citric acid 150
Sodium lauryl sulphate 9
Microcrystalline Cellulose 120
Ethanol 18ml
Magnesium stearate 14
Dried starch 450
Effervescent tablet preparation method is as follows: with consistent with embodiment 2.
Effervescent tablet pharmacodynamics test in above-described embodiment:
One, the antiinflammatory action of this preparation
1, experiment material
1.1 medicines: this preparation (this preparation of following experiment is the present embodiment 2 gained preparation)；JIEERYIN: Sino-foreign joint venture
Chengdu En Weishixiang pharmaceutical Co. Ltd produces；Dimethylbenzene: Beijing Hua Wuchang produces
1.2 animals: extraordinary rex rabbit is bought from Jinan Jin Feng laboratory animal company limited.
2, experimental technique:
Take healthy male kind of rabbit 36, body weight 700-800g, be randomly divided into 3 groups: normal saline group, JIEERYIN group, this system
Agent group.
With dimethylbenzene 0.03ml/ only, before and after being applied to kind of rabbit auris dextra shell, two sides causes inflammation, and within 30 minutes, rear right auricular concha is distinguished again
It is coated with normal saline, JIEERYIN and this preparation (20% solution；3ml/kg), after 2 hours, de-cervical vertebra is put to death, and every rabbit is cut
Left and right two auricles, take off two auricles at ears symmetry with diameter 7mm card punch, weigh with analytical balance, subtract with auris dextra sheet
Going left auricle heavily for auris dextra swelling severe, and calculate inhibitory rate of intumesce respectively, each medicine group compares with matched group, the results are shown in Table 1:
3, experimental result
This preparation group, positive drug JIEERYIN matched group, the swelling that xylol leads to kind of the rabbit ear wide has obvious inhibiting effect, with
Matched group comparing difference has significance (P < 0.05).
Two, the bacteriostasis experiment of this preparation
(1) medicine
Sample: this preparation is effervescent tablet of the present invention by embodiment 1, is carried out bacteriostatic experiment with four kinds of variable concentrations, dense
Degree is respectively as follows: No. 1: 5%, No. 2: 10%, No. 3 15%, No. 4 20%；JIEERYIN (comparison is used).
Above medicine all makees bacteriostatic experiment with original content.
(2) experimental strain
Gonococcus niikita bacteria strain P-528-1 and the staphylococcus aureus of this teaching and research room preservation, colibacillus, Candida albicans
Bacterium, microsporon gypseum totally five kinds.
(3) experimental technique
Using cup-plate method, paper disk method is carried out simultaneously.Will above-mentioned five kinds of the most intensive streak inoculations of antibacterial train to corresponding flat board
Support on base, on each culture plate, then put two aseptic steel Oxford cups, in the cup of Oxford, be separately added into said medicine
Suspension 0.2ml is impregnated with same concentration medicinal liquid with the scraps of paper (after diameter 6mm autoclaving standby) simultaneously and is affixed on flat board,
Antibacterial culturing puts 37 DEG C of 24-48 hour observed results；Fungal culture puts 25 DEG C of one week observed results.
(4) result
Measure medicine bacteriostatic diameter (mm) around Oxford cup and the scraps of paper, the results are shown in Table 2.
Conclusion
Through the discriminatory analysis of experimental result, this preparation 1-4 sample is to gonococcus, staphylococcus aureus, colibacillus, white
Color candidiasis, microsporon gypseum bacteriostasis in addition to No. 1 sample, be superior to JIEERYIN.
Three, each embodiment Comparison of experiment results
Conclusion
Through the discriminatory analysis of experimental result, the present embodiment four is better than embodiment one, two, three.
Claims (9)
1. Bovine Lactoferrin and hydrolysis thereof or a zymolyte application in treatment medicine for gynecopathy, described hydrolysis or enzymolysis
Thing is breast ferrum element.
Application the most according to claim 1, it is characterised in that: described Bovine Lactoferrin refer to from milk, cattle colostrums or
The bioactive albumen of the tool of separation and Extraction in milk albumin.
Application the most according to claim 1, it is characterised in that: described Bovine Lactoferrin is the milk secreted from normal milk cattle
The Bovine Lactoferrin of middle extraction, or from the Lac Bovis seu Bubali ferrum through vaccinating or extract milk that milk cattle after genetic modification is produced
Albumen.
Application the most according to claim 1, it is characterised in that: described breast ferrum element molecular weight is between 3700-5000Da.
Application the most according to claim 1, it is characterised in that: described treatment medicine for gynecopathy refers to for treating pudendum
Ulcer, inflammation, red and swollen or rotten to the corn medicine and for cleaning the medicine of vagina.
Application the most according to claim 1, it is characterised in that one treats medicine for gynecopathy, dosage form is effervescent tablet, its
Including following component:
Bovine Lactoferrin or breast ferrum element 4-10
Flos Lonicerae extract 60-120
Herba Taraxaci extract 40-100
Sodium bicarbonate 100-500
Citric acid 60-150
Sodium lauryl sulphate 2-10
Microcrystalline Cellulose 60-130
Ethanol 8-20ml
Magnesium stearate 3-15
Dried starch 200-500
Described Bovine Lactoferrin be saturation be the low ferrum saturation lactoferrin of 5-8%.
Application the most according to claim 6, it is characterised in that described effervescent tablet preparation method is:
(1), Flos Lonicerae, Herba Taraxaci are decocted 2 times by 8-10 times of weight water respectively, each 2 hours, united extraction liquid, filters dense
It is reduced to do, thus respectively obtains Flos Lonicerae extract, Herba Taraxaci extract；
(2), by low ferrum saturation lactoferrin or breast ferrum element, sodium bicarbonate, citric acid, sodium lauryl sulphate, crystallite fibre
Dimension element, ethanol, magnesium stearate, dried starch and Flos Lonicerae extract, Herba Taraxaci extract mix, tabletting and get final product.
8. according to the application described in claim 1-7, it is characterised in that the preparation process of described low ferrum saturation lactoferrin
For:
1st step, uses cation exchange resin that the lactoferrin in Lac Bovis seu Bubali is adsorbed, resolved；Described resolving is to adopt
With two grades of parsings, the first order resolves the saline solution parsing being to use 1～2.5%, and desorbed solution is lactoperoxidase pheron, discards；
The second level resolves the saline solution parsing being to use 3.5～7%, and desorbed solution is sent into the 2nd step and processed；Described saline solution refer to sodium salt,
Potassium salt or calcium salt soln；
2nd step, the desorbed solution obtaining the 1st step uses separation film to concentrate；Described separation film is that molecular cut off exists
The ultrafilter membrane of 1000～30K；
3rd step, the concentrated solution that the 2nd step obtains uses insoluble Fe3+Chelating resin adsorbs, then uses separation film to concentrated solution
Concentrate；Need during described adsorption operations in concentrated solution, add acetic acid, acetate and citrate, prepare its absorbing ring
In border, citrate concentration is 0.1mol/L ~ 0.5mol/L, and regulates pH to 5.0～6.7；Described separation film is to retain molecule
Measure the ultrafilter membrane 1000～30K；
Described insoluble Fe3+Chelating resin refers to D403 chelating resin；In the 3rd described step, the adsorption time 20 of resin～
120 minutes, during absorption, rotating speed of agitator speed was 20～150rpm, and adsorption temp is at 3～30 DEG C.
Application the most according to claim 8, it is characterised in that in described 1st step, the preparation process of cation exchange resin
For:
1st step, takes 10g chloracetylated polystyrene-divinylbenzene microspheres carrier PS-acyl-Cl, adds 60ml oxolane
Swelling 12 h, add 40ml methanol, then according to weight ratio PS-acyl-Cl: ethylenediamine: sodium bicarbonate is 1:8:0.7, depends on
Secondary addition ethylenediamine and sodium bicarbonate, be at 80 DEG C stirring reaction 24h, after reaction terminates, poured into by product in sand core funnel,
Being washed till neutrality with distilled water, methanol filter wash is dried under vacuum to constant weight 3 times, obtains cross-linking EDA microsphere supported；
2nd step, claims 60g to take crosslinking EDA microsphere supported, is placed in three-neck flask, after adding swelling 12 h of dimethylformamide, add
Enter 2-acrylamido-2-methyl propane sulfonic acid 16g, N-butoxy methyl acrylamide 3g, acrylic acid double cyclopentenyl ester,
K2CO35g, tetrabutyl ammonium bromide 12g, under stirring in the oil bath of uniform temperature back flow reaction, reaction terminate after by product
It is transferred in sintered filter funnel, with distilled water diafiltration to neutral after cleaning 4 times with the HC1 of 5wt%, finally drains after methanol filter wash,
It is dried under vacuum to constant weight, obtains cation exchange resin.
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Application publication date: 20170111 |