CN109794172A - A kind of preparation method of the antibacterial hollow-fibre membrane for blood purification - Google Patents
A kind of preparation method of the antibacterial hollow-fibre membrane for blood purification Download PDFInfo
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- CN109794172A CN109794172A CN201910071151.9A CN201910071151A CN109794172A CN 109794172 A CN109794172 A CN 109794172A CN 201910071151 A CN201910071151 A CN 201910071151A CN 109794172 A CN109794172 A CN 109794172A
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- fibre membrane
- calcium
- mesoporous silicon
- silver
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- 239000012528 membrane Substances 0.000 title claims abstract description 91
- 239000000835 fiber Substances 0.000 title claims abstract description 89
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 49
- 239000008280 blood Substances 0.000 title claims abstract description 26
- 210000004369 blood Anatomy 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 106
- 239000010703 silicon Substances 0.000 claims abstract description 106
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 97
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229940072056 alginate Drugs 0.000 claims abstract description 55
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 55
- 229920000615 alginic acid Polymers 0.000 claims abstract description 55
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011575 calcium Substances 0.000 claims abstract description 45
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 45
- 239000004332 silver Substances 0.000 claims abstract description 36
- 229910052709 silver Inorganic materials 0.000 claims abstract description 35
- 238000005266 casting Methods 0.000 claims abstract description 32
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002166 wet spinning Methods 0.000 claims abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 179
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 96
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 74
- 239000007864 aqueous solution Substances 0.000 claims description 65
- 239000000243 solution Substances 0.000 claims description 49
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000004695 Polyether sulfone Substances 0.000 claims description 30
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 27
- 235000010413 sodium alginate Nutrition 0.000 claims description 27
- 239000000661 sodium alginate Substances 0.000 claims description 27
- 229940005550 sodium alginate Drugs 0.000 claims description 27
- 229920006393 polyether sulfone Polymers 0.000 claims description 26
- 239000000725 suspension Substances 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 18
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 17
- 229940113088 dimethylacetamide Drugs 0.000 claims description 17
- 238000009987 spinning Methods 0.000 claims description 14
- 239000007863 gel particle Substances 0.000 claims description 11
- -1 Ether sulfone Chemical class 0.000 claims description 10
- 159000000007 calcium salts Chemical class 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 239000004088 foaming agent Substances 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 1
- 150000004040 pyrrolidinones Chemical class 0.000 claims 1
- 238000009938 salting Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 238000001631 haemodialysis Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 11
- 239000003053 toxin Substances 0.000 abstract description 10
- 231100000765 toxin Toxicity 0.000 abstract description 10
- 108700012359 toxins Proteins 0.000 abstract description 10
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 150000003384 small molecules Chemical class 0.000 abstract description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 16
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 description 16
- 238000002791 soaking Methods 0.000 description 14
- 238000005406 washing Methods 0.000 description 13
- 230000010355 oscillation Effects 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- 239000007787 solid Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 239000002808 molecular sieve Substances 0.000 description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 11
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 235000010410 calcium alginate Nutrition 0.000 description 9
- 239000000648 calcium alginate Substances 0.000 description 9
- 229960002681 calcium alginate Drugs 0.000 description 9
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 9
- 229930003779 Vitamin B12 Natural products 0.000 description 8
- 230000008081 blood perfusion Effects 0.000 description 8
- 239000004202 carbamide Substances 0.000 description 8
- FDJOLVPMNUYSCM-WZHZPDAFSA-L cobalt(3+);[(2r,3s,4r,5s)-5-(5,6-dimethylbenzimidazol-1-yl)-4-hydroxy-2-(hydroxymethyl)oxolan-3-yl] [(2r)-1-[3-[(1r,2r,3r,4z,7s,9z,12s,13s,14z,17s,18s,19r)-2,13,18-tris(2-amino-2-oxoethyl)-7,12,17-tris(3-amino-3-oxopropyl)-3,5,8,8,13,15,18,19-octamethyl-2 Chemical compound [Co+3].N#[C-].N([C@@H]([C@]1(C)[N-]\C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C(\C)/C1=N/C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C\C1=N\C([C@H](C1(C)C)CCC(N)=O)=C/1C)[C@@H]2CC(N)=O)=C\1[C@]2(C)CCC(=O)NC[C@@H](C)OP([O-])(=O)O[C@H]1[C@@H](O)[C@@H](N2C3=CC(C)=C(C)C=C3N=C2)O[C@@H]1CO FDJOLVPMNUYSCM-WZHZPDAFSA-L 0.000 description 8
- 229940109239 creatinine Drugs 0.000 description 8
- 229940045136 urea Drugs 0.000 description 8
- 239000002441 uremic toxin Substances 0.000 description 8
- 239000011715 vitamin B12 Substances 0.000 description 8
- 235000019163 vitamin B12 Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 150000003457 sulfones Chemical class 0.000 description 6
- 208000037157 Azotemia Diseases 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 208000009852 uremia Diseases 0.000 description 5
- 208000020832 chronic kidney disease Diseases 0.000 description 3
- 208000022831 chronic renal failure syndrome Diseases 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000008030 elimination Effects 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 210000003734 kidney Anatomy 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002560 therapeutic procedure Methods 0.000 description 3
- 206010061666 Autonomic neuropathy Diseases 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 208000001647 Renal Insufficiency Diseases 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 210000001367 artery Anatomy 0.000 description 2
- 208000026106 cerebrovascular disease Diseases 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 208000035850 clinical syndrome Diseases 0.000 description 2
- CVSVTCORWBXHQV-UHFFFAOYSA-N creatine Chemical compound NC(=[NH2+])N(C)CC([O-])=O CVSVTCORWBXHQV-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000002526 effect on cardiovascular system Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 201000006370 kidney failure Diseases 0.000 description 2
- 235000003715 nutritional status Nutrition 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- 208000017667 Chronic Disease Diseases 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002648 combination therapy Methods 0.000 description 1
- 238000007485 conventional hemodialysis Methods 0.000 description 1
- 229960003624 creatine Drugs 0.000 description 1
- 239000006046 creatine Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 239000000385 dialysis solution Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000000322 hemodialysis Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000003907 kidney function Effects 0.000 description 1
- 231100000518 lethal Toxicity 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 208000030159 metabolic disease Diseases 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Plant Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation methods of antibacterial hollow-fibre membrane for blood purification.The preparation method of this antibacterial hollow-fibre membrane is the following steps are included: 1) mesoporous silicon loads silver and calcium ion；2) preparation package carries off the alginate of sub- mesoporous silicon；3) casting solution is prepared；4) dry-jet wet spinning prepares antibacterial hollow-fibre membrane.Obtained this antibacterial hollow-fibre membrane is a kind of antibacterial hollow-fibre membrane that can be used for blood purification.The advantages that hollow-fibre membrane that the present invention is prepared is with high security, preparation manipulation is simple, at low cost, it can be applied to haemodialysis.The open porous structure of the hollow-fibre membrane that the present invention is prepared can be such that toxin is smoothly through, and selectively adsorb small molecule, middle molecule toxins, to achieve the effect that effectively to remove toxin.Meanwhile the releasable micro silver ion of mesoporous silicon for carrying silver, calcium achievees the effect that antibacterial into blood and dialyzate.
Description
Technical field
The present invention relates to a kind of tunica fibrosa, in particular to the preparation side of a kind of antibacterial hollow-fibre membrane for blood purification
Method.
Background technique
Chronic renal failure refers to that various kidney troubles lead to the gradual irreversibility decline of renal function, until function loses institute
Clinical syndrome composed by a series of symptoms of appearance and metabolic disorder.The chronic renal failure of terminal phase is uremia, and generation refers to
The shared clinical syndrome of the kidney trouble in various advanced stages is a series of clinics that chronic renal failure enters the appearance of terminal stage
Syndrome composed by showing, it is closely bound up with the retention of various uremic toxins in vivo.Kidney failure can accelerate artery congee
Sample hardening, once developing to artery occlusion, will cause a variety of diseases such as cardiovascular and cerebrovascular disease, kidney trouble, liver diseases.Its
In, cardiovascular and cerebrovascular disease is the lethal first cause of uremic patient.According to the statistics of the World Health Organization, every year about 17,000,000
People dies of this chronic disease, accounts for 30% or so of global total death toll.Uremia seriously threatens human health, with me
State's urbanization and industrialized continuous development, the increase of society and economic pressures, uremic patient group, China will be further
Expand.Also, with economic and science and technology development, requirement of the people to quality of life is also higher and higher, reaches to the attention of health
To unprecedented degree.The uremia blood purification therapy with auxiliary therapeutic action is developed, there is the huge market demand, it is preceding
Scape is very wide.
The currently existing uremic blood purification therapy of document report, more concern haemodialysis or haemodialysis and blood fill
Curative effect associated with stream.Though compared with the blood purifications therapy such as conventional hemodialysis, removing energy of the blood perfusion to uremic toxins
Power increases.But there is a problem of following: 1) electrolyte caused by blood perfusion can not solve in blood purification process, soda acid
Unbalance.So blood perfusion is generally combined with haemodialysis, electrolyte, acid are kept while reaching and efficiently removing toxin
Soda balance；2) simultaneously, after haemodialysis combination, cost is substantially improved blood perfusion, causes the bigger warp of patient and its family
Ji pressure；3) when blood absorbence lacks specificity to the absorption of uremic toxins, elimination effect is also undesirable.
In existing disclosed document, CN104258829A discloses serium inorganic phosphorus adsorbent and preparation method thereof, fills for blood
The adsorption column of stream；CN102335465A discloses treatment uremia blood perfusion device；CN101307149A discloses a kind of medical
The preparation method of adsorbing agent carrier；(the observation of curative effect and shield of a variety of blood purification combination therapy Uremic complications such as Fang Guilian
Reason, Anhui medicine, 2013,17,43-345) it discloses to high flux hemodialysis, hemodiafiltration, renal failure
The elimination effect of uremic toxins is compared；It is quick it is equal (different blood purification modes uremic toxins are removed and
The therapeutic evaluation of autonomic neuropathy, Guangdong medicine, 2010,22,2943-2945) have studied haemodialysis, hemodiafiltration
With haemodialysis joint blood perfusion to uremic toxins' removing and to the influential effect of autonomic neuropathy；Duan Shengdong is (different
For dialyzing method to maintenance dialysis patient's uremia Dusuqing except the influence of effect and nutritional status, practical clinical medicine is miscellaneous
Will, 2015,19,26-29) haemodialysis, hemodiafiltration, haemodialysis joint blood perfusion are had studied to uremic toxins
The influence of elimination effect and nutritional status.But the above blood purification method is mostly that Blood index or haemodialysis and blood perfusion join
With, it is difficult to solve the problems, such as that pH, electrolyte acid-base balance or treatment cost are higher.
Summary of the invention
Of the existing technology in order to overcome the problems, such as, the purpose of the present invention is to provide a kind of antibacterials for blood purification
The preparation method of hollow-fibre membrane.
The preparation method is that first carrying out the loading of silver ion and calcium ion to mesoporous silicon, alginate is then used
It is tentatively wrapped up, while dispersing the mesoporous silicon for carrying silver, calcium in Polymer Solution and forming casting solution；It is squirted by dry
Method spining technology carries out curing molding in sodium alginate aqueous solution and ionic calcium soln.
In order to achieve the above purpose, the technical solution used in the present invention is:
A kind of preparation method of antibacterial hollow-fibre membrane, comprising the following steps:
1) mesoporous silicon loads silver and calcium ion: dispersing mesoporous silicon in the solution of silver salt and calcium salt, resulting suspension
It is dry, obtain the mesoporous silicon for carrying silver, calcium；
2) preparation package carries off the alginate of sub- mesoporous silicon: dispersing alginate solution for the mesoporous silicon for carrying silver, calcium
In, gel particle is obtained, is sieved, the alginate that package carries off sub- mesoporous silicon is obtained；
3) it prepares casting solution: alginate, pore-foaming agent and solvent that polyether sulfone, package carry off sub- mesoporous silicon being mixed, taken off
Bubble, obtains casting solution；
4) dry-jet wet spinning prepares antibacterial hollow-fibre membrane: casting solution being sprayed through spinning head, in certain core liquid stream
It sequentially enters under speed and air section distance condition and is shaped in alginate solution and calcium salt soln, obtain antibacterial hollow-fibre membrane.
Preferably, in the preparation method step 1) of this antibacterial hollow-fibre membrane, the solution of mesoporous silicon and silver salt and calcium salt
Amount ratio is 1g:(60~100) mL.
Preferably, in the preparation method step 1) of this antibacterial hollow-fibre membrane, the solution of silver salt and calcium salt is to contain nitre
The aqueous solution of sour silver and calcium nitrate；Wherein, the mass concentration of silver nitrate is 2.5%~5%, and the mass concentration of calcium nitrate is
2.5%~5%.
Preferably, in the preparation method step 1) of this antibacterial hollow-fibre membrane, specifically under normal pressure, mesoporous silicon is surpassed
Sound is scattered in silver nitrate and calcium nitrate aqueous solution, obtains suspension in oscillation on shaking table, vacuumizes, repeat 3~5 times.
Preferably, in the preparation method step 1) of this antibacterial hollow-fibre membrane, the dry mode of suspension is that freezing is dry
It is dry.
Preferably, in the preparation method step 2) of this antibacterial hollow-fibre membrane, the mesoporous silicon and alginate of silver, calcium are carried
The amount ratio of solution is 1g:(80~200) mL.
Preferably, in the preparation method step 2) of this antibacterial hollow-fibre membrane, alginate solution is that mass concentration is
2.5%~5% sodium alginate aqueous solution.
Preferably, in the preparation method step 2) of this antibacterial hollow-fibre membrane, be sieved for 800 mesh~1200 mesh molecules
Sieve；It is further preferred that sieving was 1000 mesh molecular sieves.After the sieving of step 2), particle under collection screen, as package are carried
The alginate of ion mesoporous silicon.
Preferably, in the preparation method step 3) of this antibacterial hollow-fibre membrane, polyether sulfone, package carry off sub- mesoporous silicon
The amount ratio of alginate, pore-foaming agent and solvent is 1g:(0.01~0.05) g:(0.04~0.08) g:(0.5~1.5) mL.
Preferably, in the preparation method step 3) of this antibacterial hollow-fibre membrane, pore-foaming agent is polyvinylpyrrolidone, gathers
Ethylene glycol, polyvinyl alcohol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, ethylene glycol, glycerine, in diethylene glycol (DEG) at least
It is a kind of；It is further preferred that pore-foaming agent is at least one of polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol；Again into one
Step is preferred, and pore-foaming agent is polyvinylpyrrolidone；In some preferred embodiments of the present invention, polyvinylpyrrolidine
Ketone is selected from the polyvinylpyrrolidone of model K30.
Preferably, in the preparation method step 3) of this antibacterial hollow-fibre membrane, solvent is dimethyl acetamide, dimethyl
At least one of formamide, dimethyl sulfoxide, N-Methyl pyrrolidone, DMAC N,N' dimethyl acetamide；It is further preferred that molten
Agent is dimethyl acetamide or dimethylformamide.
Preferably, in the preparation method step 3) of this antibacterial hollow-fibre membrane, the mode of deaeration is standing and defoaming；Into one
Step is preferred, and the time of repose of standing and defoaming is 8h~12h, and dwell temperature is 10 DEG C~35 DEG C.
Preferably, in the preparation method step 4) of this antibacterial hollow-fibre membrane, the driving pressure of ejection be 0.08MPa~
0.5MPa。
Preferably, in the preparation method step 4) of this antibacterial hollow-fibre membrane, core flow velocity is 10mL/min~50mL/
min。
Preferably, in the preparation method step 4) of this antibacterial hollow-fibre membrane, air section distance is 0~20cm.
Preferably, in the preparation method step 4) of this antibacterial hollow-fibre membrane, core liquid is water.
In the preparation method step 4) of this antibacterial hollow-fibre membrane, alginate solution is the first solidification liquid；Preferably,
Alginate solution is that temperature is 50 DEG C~80 DEG C, and mass concentration is 5%~10% sodium alginate aqueous solution.
In the preparation method step 4) of this antibacterial hollow-fibre membrane, calcium salt soln is the second solidification liquid；Preferably, calcium salt
Solution is that temperature is 30 DEG C~70 DEG C, and mass concentration is 1%~4.5% calcium nitrate aqueous solution.
Preferably, the obtained membrane material of forming is soaking, dry in the air in the preparation method step 4) of this antibacterial hollow-fibre membrane
Dry-cure obtains finished product.
Preferably, in the preparation method step 4) of this antibacterial hollow-fibre membrane, impregnate for by membrane material through 70 DEG C~90
DEG C water soaking and washing for 24 hours~72h.
Preferably, it in the preparation method step 4) of this antibacterial hollow-fibre membrane, dries to dry in air.
A kind of antibacterial hollow-fibre membrane for blood purification, is made by above-mentioned preparation method.
The beneficial effects of the present invention are:
It the advantages that hollow-fibre membrane that the present invention is prepared is with high security, preparation manipulation is simple, at low cost, can answer
For haemodialysis.The open porous structure of the hollow-fibre membrane that the present invention is prepared can be such that toxin is smoothly through, and have choosing
Small molecule, middle molecule toxins are adsorbed to selecting property, to achieve the effect that effectively to remove toxin.Meanwhile the mesoporous silicon of load silver, calcium can
Micro silver ion is discharged into blood and dialyzate, achievees the effect that antibacterial.
Specifically, advantages of the present invention is as follows:
1) mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane that the present invention is prepared is constituted with polymer
Finger-like pore structure and sponge porous structure, permeability is strong, and mass transfer dynamics are fast.
2) mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane that the present invention is prepared is constituted with mesoporous silicon
Microcellular structure, can small molecule of the adsorption and diffusion to dialysis fluid side, middle molecule toxins in time, promote the clearance rate to toxin.
3) silver-colored, calcium containing carrying in mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane that the present invention is prepared
Mesoporous silicon, the calcium ion discharged in hollow-fibre membrane preparation process can assist the machinery of alginate in enhancing film basis material
Intensity.
4) silver-colored, calcium containing carrying in mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane that the present invention is prepared
Mesoporous silicon can discharge in time silver ion and reach antibacterial action.
5) mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane that the present invention is prepared, matrix are polyethers
Sulfone, alginate and mesoporous silicon, blood compatibility are good.
6) mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane that the present invention is prepared is to urea, creatinine and dimension
Raw element B12 has good cleaning performance, right to the clearance rate of creatinine up to 93.4% to the clearance rate of urea up to 95.2%
The clearance rate of vitamin B12 is up to 57.4%.
Specific embodiment
The contents of the present invention are described in further detail below by way of specific embodiment.Original used in embodiment
Material unless otherwise specified, can be obtained from routine business approach.
Embodiment 1
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 2.5% and concentration is 3.5%
Calcium nitrate aqueous solution.Under normal pressure, by 4.0g mesoporous silicon ultrasonic disperse in 400mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 4 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
3.5g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 350mL 3.0%, stirring at normal temperature 4h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
40g polyether sulfone, 0.57g package are carried to the alginate and 1.6g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 20mL dimethyl acetamide, then stands 9h at 10 DEG C, obtains casting solution.
Casting solution is sprayed under 0.2MPa driving through spinning head, 10mL/min core liquid (water) and 20cm air section away from
Sequentially entered under the conditions of 55 DEG C, 5.0% sodium alginate aqueous solution and 30 DEG C, 3.5% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 75 DEG C of water soaking and washing 54h, obtains mesoporous silicon/alginate/polyethers
Sulfone antibacterial hollow-fibre membrane.
Embodiment 2
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 2.5% and concentration is 5.0%
Calcium nitrate aqueous solution.Under normal pressure, by 5.0g mesoporous silicon ultrasonic disperse in 300mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 5 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
4.5g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 675mL 2.5%, stirring at normal temperature 4h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
60g polyether sulfone, 1.0g package are carried to the alginate and 3.6g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 30mL dimethyl acetamide, then stands 8h at 20 DEG C, obtains casting solution.
Casting solution is sprayed under 0.08MPa driving through spinning head, 40mL/min core liquid (water) and 0cm air section away from
Sequentially entered under the conditions of 50 DEG C, 8.0% sodium alginate aqueous solution and 40 DEG C, 1.0% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 70 DEG C of water soaking and washing 48h, obtains mesoporous silicon/alginate/polyethers
Sulfone antibacterial hollow-fibre membrane.
Embodiment 3
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 3.5% and concentration is 2.5%
Calcium nitrate aqueous solution.Under normal pressure, by 6.0g mesoporous silicon ultrasonic disperse in 360mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 3 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
5.0g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 750mL 5.0%, stirring at normal temperature 3h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
50g polyether sulfone, 2.5g package are carried to the alginate and 4.0g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 75mL dimethyl acetamide, then stands 9h at 35 DEG C, obtains casting solution.
Casting solution is sprayed under 0.5MPa driving through spinning head, 30mL/min core liquid (water) and 15cm air section away from
Sequentially entered under the conditions of 80 DEG C, 10.0% sodium alginate aqueous solution and 50 DEG C, 1.0% calcium nitrate aqueous solution in shape.
By solid hollow-fibre membrane through 70 DEG C water soaking and washing for 24 hours after, dry in air, obtain mesoporous silicon/alginate/poly-
Ether sulfone antibacterial hollow-fibre membrane.
Embodiment 4
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 4.0% and concentration is 3.0%
Calcium nitrate aqueous solution.Under normal pressure, by 6.0g mesoporous silicon ultrasonic disperse in 480mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 3 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
5.0g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 500mL 4.5%, stirring at normal temperature 3h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
40g polyether sulfone, 1.5g package are carried to the alginate and 3.2g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 60mL dimethyl acetamide, then stands 11h at 25 DEG C, obtains casting solution.
Casting solution is sprayed under 0.25MPa driving through spinning head, in the core liquid (water) and 10cm air section of 50mL/min
Sequentially entered under distance condition 65 DEG C, 7.0% sodium alginate aqueous solution and 35 DEG C, 1.5% calcium nitrate aqueous solution in shape.
It by solid hollow-fibre membrane after 90 DEG C of water soaking and washing 72h, dries in air, obtains mesoporous silicon/alginate/poly-
Ether sulfone antibacterial hollow-fibre membrane.
Embodiment 5
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 3.0% and concentration is 3.0%
Calcium nitrate aqueous solution.Under normal pressure, by 6.0g mesoporous silicon ultrasonic disperse in 480mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 3 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
5.0g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 400mL 3.5%, stirring at normal temperature 5h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
60g polyether sulfone, 2.25g package are carried to the alginate and 4.8g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 90mL dimethyl acetamide, then stands 10h at 20 DEG C, obtains casting solution.
Casting solution is sprayed under 0.1MPa driving through spinning head, 15mL/min core liquid (water) and 15cm air section away from
Sequentially entered under the conditions of 60 DEG C, 10.0% sodium alginate aqueous solution and 55 DEG C, 2.5% calcium nitrate aqueous solution in shape.
It by solid hollow-fibre membrane after 80 DEG C of water soaking and washing 36h, dries in air, obtains mesoporous silicon/alginate/poly-
Ether sulfone antibacterial hollow-fibre membrane.
Embodiment 6
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 3.0% and concentration is 2.5%
Calcium nitrate aqueous solution.Under normal pressure, by 5.0g mesoporous silicon ultrasonic disperse in 500mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 3 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
4.5g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 675mL 2.5%, stirring at normal temperature 3h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
50g polyether sulfone, 1.43g package are carried to the alginate and 2.0g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 50mL dimethyl acetamide, then stands 12h at 35 DEG C, obtains casting solution.
Casting solution is sprayed under 0.4MPa driving through spinning head, 20mL/min core liquid (water) and 15cm air section away from
Sequentially entered under the conditions of 75 DEG C, 7.0% sodium alginate aqueous solution and 55 DEG C, 1.5% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 90 DEG C of water soaking and washing 42h, obtains mesoporous silicon/alginate/polyethers
Sulfone antibacterial hollow-fibre membrane.
Embodiment 7
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 5.0% and concentration is 4.5%
Calcium nitrate aqueous solution.Under normal pressure, by 6.0g mesoporous silicon ultrasonic disperse in 600mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 5 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
5.0g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 1000mL 3.0%, stirring at normal temperature 4h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
60g polyether sulfone, 2.0g package are carried to the alginate and 2.4g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 60mL dimethyl acetamide, then stands 10h at 15 DEG C, obtains casting solution.
Casting solution is sprayed under 0.15MPa driving through spinning head, in the core liquid (water) and 10cm air section of 25mL/min
Sequentially entered under distance condition 80 DEG C, 6.0% sodium alginate aqueous solution and 60 DEG C, 4.5% calcium nitrate aqueous solution in shape.
It by solid hollow-fibre membrane after 80 DEG C of water soaking and washing 60h, dries in air, obtains mesoporous silicon/alginate/poly-
Ether sulfone antibacterial hollow-fibre membrane.
Embodiment 8
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 5.0% and concentration is 4.5%
Calcium nitrate aqueous solution.Under normal pressure, by 6.0g mesoporous silicon ultrasonic disperse in 600mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 4 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
3.5g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 700mL 4.0%, stirring at normal temperature 5h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
50g polyether sulfone, 0.71g package are carried to the alginate and 3.0g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 25mL dimethyl acetamide, then stands 12h at 30 DEG C, obtains casting solution.
Casting solution is sprayed under 0.45MPa driving through spinning head, 45mL/min core liquid (water) and 5cm air section away from
Sequentially entered under the conditions of 70 DEG C, 8.0% sodium alginate aqueous solution and 70 DEG C, 2.0% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 85 DEG C of water soaking and washing 42h, obtains mesoporous silicon/alginate/polyethers
Sulfone antibacterial hollow-fibre membrane.
Embodiment 9
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 4.5% and concentration is 5.0%
Calcium nitrate aqueous solution.Under normal pressure, by 5.0g mesoporous silicon ultrasonic disperse in 400mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 5 times；The suspension is freeze-dried, the mesoporous silicon for carrying silver, calcium is obtained.
4.5g is carried into silver-colored, calcium mesoporous silicon and is scattered in the sodium alginate aqueous solution of 900mL 3.5%, stirring at normal temperature 5h is obtained
It to gel particle, is screened using 1000 mesh molecular sieves, the particle under collection screen, obtains the mesoporous silicon that package carries silver, calcium
Alginate.
40g polyether sulfone, 1.0g package are carried to the alginate and 2.4g K30- polyvinylpyrrolidine of silver-colored, calcium mesoporous silicon
Ketone is dissolved in/is dispersed in 40mL dimethyl acetamide, then stands 8h at 25 DEG C, obtains casting solution.
Casting solution is sprayed under 0.2MPa driving through spinning head, 35mL/min core liquid (water) and 0cm air section away from
Sequentially entered under the conditions of 60 DEG C, 9.0% sodium alginate aqueous solution and 65 DEG C, 4.0% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 80 DEG C of water soaking and washing 66h, obtains mesoporous silicon/alginate/polyethers
Sulfone antibacterial hollow-fibre membrane.
Comparative example 1
Silver nitrate is dissolved in deionized water, obtains the silver nitrate aqueous solution that concentration is 4.5%.Under normal pressure, by 5.0g
Mesoporous silicon ultrasonic disperse obtains suspension in 400mL silver nitrate aqueous solution, in oscillation on shaking table, vacuumizes, is repeated 5 times；It should
Suspension is freeze-dried to obtain the mesoporous silicon for carrying silver.
4.5g is carried into the sodium alginate aqueous solution that silver-colored mesoporous silicon is scattered in 900mL 3.5%, stirring at normal temperature 5h obtains gel
Shape particle is screened, the particle under collection screen using 1000 mesh molecular sieves, obtains the alginate that package carries silver-colored mesoporous silicon.
40g polyether sulfone, the alginate of the silver-colored mesoporous silicon of 1.0g package load and 2.4g K30- polyvinylpyrrolidone is molten
In/it is dispersed in 40mL dimethyl acetamide, 8h then is stood at 25 DEG C, obtains casting solution.
Casting solution is sprayed under 0.2MPa driving through spinning head, 35mL/min core liquid (water) and 0cm air section away from
Sequentially entered under the conditions of 60 DEG C, 9.0% sodium alginate aqueous solution and 65 DEG C, 4.0% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 80 DEG C of water soaking and washing 66h, obtains a kind of no sodium alginate and hands in advance
Mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane of connection package mesoporous silicon.
Comparative example 2
40g polyether sulfone and 2.4g K30- polyvinylpyrrolidone are dissolved in/are dispersed in 40mL dimethyl acetamide, then
8h is stood at 25 DEG C, obtains casting solution.
Casting solution is sprayed under 0.2MPa driving through spinning head, 35mL/min core liquid (water) and 0cm air section away from
Sequentially entered under the conditions of 60 DEG C, 9.0% sodium alginate aqueous solution and 65 DEG C, 4.0% calcium nitrate aqueous solution in shape.It will
Solid hollow-fibre membrane dries in air after 80 DEG C of water soaking and washing 66h, obtains a kind of alginate/polyether sulfone
Antibacterial hollow-fibre membrane.
Comparative example 3
Silver nitrate and calcium nitrate are dissolved in deionized water, obtaining silver nitrate that concentration is 4.5% and concentration is 5.0%
Calcium nitrate aqueous solution.Under normal pressure, by 5.0g mesoporous silicon ultrasonic disperse in 400mL silver nitrate and calcium nitrate aqueous solution, in shaking table
Upper oscillation obtains suspension, vacuumizes, is repeated 5 times；The suspension is freeze-dried to obtain the mesoporous silicon for carrying silver, calcium.
40g polyether sulfone, 1.0g are carried silver, the mesoporous silicon of calcium and 2.4g K30- polyvinylpyrrolidone to be dissolved in/be dispersed in
40mL dimethyl acetamide then stands 8h at 25 DEG C, obtains casting solution.
Casting solution is sprayed under 0.2MPa driving through spinning head, 35mL/min core liquid (water) and 0cm air section away from
Enter in 65 DEG C of aqueous solution under the conditions of and shapes.By solid hollow-fibre membrane after 80 DEG C of water soaking and washing 66h, in sky
It is dried in gas, obtains a kind of mesoporous silicon/polyether sulfone antibacterial hollow-fibre membrane.
Using test
The above-mentioned antibacterial hollow-fibre membrane being prepared is applied to blood purification, the specific method is as follows:
Doughnut is made in the antibacterial hollow-fibre membrane working process that embodiment 1-9 and comparative example 1~3 are prepared
Film haemodialyser, every dialyzer include about 4200 hollow-fibre membranes, effective length 190mm, and effective area is
0.6m2.Blood is the anticoagulant pig blood of sodium citrate, makes its urea concentration be about by outer addition urea, creatinine and vitamin B12
450ppm, creatine concentration are about 28ppm, and vitamin B12 concentration is about 678ppm.Three Duplicate Samples are arranged in each embodiment.Enter
Mouth flow control is 200mL/min, and medium, without any processing, comes back in medium bottle after dialyzer filters, and forms one
Circulating system, periodically sampling is detected.To after time point, each sample, sample preparation are simultaneously detected using kit, calculate urine
The concentration and clearance rate of element, creatinine and vitamin B12.Test result is as follows shown in table 1.
Clearance rate of the 1 antibacterial hollow-fibre membrane of table to urea, creatinine and vitamin B12
Test result shows antibacterial hollow-fibre membrane that embodiment 1-9 is prepared to urea, creatinine and vitamin B12
With good clearance rate.And with comparative example 1 (mesoporous silicon is not pre-loaded with calcium), comparative example 2 (without carry silver, calcium mesoporous silicon) and
The hollow-fibre membrane of comparative example 3 (being free of alginate) is compared, more excellent to the cleaning performance of urea, creatinine and vitamin B12.
The present invention is prepared one kind and has antibacterial, toxin adsorption function and hydrophily more preferably hollow-fibre membrane, the system
Preparation Method is easy to operate.Gained mesoporous silicon/alginate/polyether sulfone antibacterial hollow-fibre membrane has open nano-micrometre more
Grade pore structure, hydrophily is good, can discharge silver ion carry out antibacterial while absorption remove uremic toxins, to urea,
The clearance rate of creatinine and vitamin B12 is high, is particularly suitable for the blood purification treatment of uremic patient.And the base of hollow-fibre membrane
Body material is polyether sulfone and alginate, has biological safety.
Finally, it should be noted that the above is only a preferred embodiment of the present invention, it is not intended to restrict the invention.For this
For the technical staff in field, the present invention can have various change and change, all within the spirits and principles of the present invention, done
Any modification, equivalent substitution, improvement and etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of antibacterial hollow-fibre membrane, it is characterised in that: the following steps are included:
1) mesoporous silicon loads silver and calcium ion: it disperses mesoporous silicon in the solution of silver salt and calcium salt, resulting suspension is dry,
Obtain carrying the mesoporous silicon of silver, calcium；
2) preparation package carries the alginate of the mesoporous silicon of silver-colored calcium: it disperses the mesoporous silicon for carrying silver, calcium in alginate solution,
Gel particle is obtained, is sieved, the alginate that package carries off sub- mesoporous silicon is obtained；
3) it prepares casting solution: alginate, pore-foaming agent and solvent that polyether sulfone, package carry off sub- mesoporous silicon being mixed, deaeration obtains
To casting solution；
4) dry-jet wet spinning prepares antibacterial hollow-fibre membrane: casting solution is sprayed through spinning head, in certain core flow velocity and
It sequentially enters under air section distance condition and is shaped in alginate solution and calcium salt soln, obtain antibacterial hollow-fibre membrane.
2. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 1, it is characterised in that: in step 1), be situated between
The solution usage ratio of hole silicon and silver salt and calcium salt is 1g:(60~100) mL.
3. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 2, it is characterised in that: in step 1), silver
The solution of salt and calcium salt is the aqueous solution containing silver nitrate and calcium nitrate；Wherein, the mass concentration of silver nitrate is 2.5%~5%,
The mass concentration of calcium nitrate is 2.5%~5%.
4. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 1, it is characterised in that: in step 2), carry
The amount ratio of silver, the mesoporous silicon of calcium and alginate solution is 1g:(80~200) mL.
5. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 4, it is characterised in that: in step 2), sea
Alginate soln is the sodium alginate aqueous solution that mass concentration is 2.5%~5%.
6. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 1, it is characterised in that: in step 3), gather
Ether sulfone, the amount ratio for wrapping up the alginate for carrying off sub- mesoporous silicon, pore-foaming agent and solvent are 1g:(0.01~0.05) g:(0.04
~0.08) g:(0.5~1.5) mL.
7. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 6, it is characterised in that: in step 3), cause
Hole agent is polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, second two
At least one of alcohol, glycerine, diethylene glycol (DEG)；Solvent is dimethyl acetamide, dimethylformamide, dimethyl sulfoxide, N- first
At least one of base pyrrolidones, DMAC N,N' dimethyl acetamide.
8. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 1, it is characterised in that: in step 4), spray
Driving pressure out is 0.08MPa~0.5MPa；Core flow velocity is 10mL/min~50mL/min, air section distance for 0~
20cm。
9. a kind of preparation method of antibacterial hollow-fibre membrane according to claim 8, it is characterised in that: in step 4), core
Liquid is water；Alginate solution is that temperature is 50 DEG C~80 DEG C, and mass concentration is 5%~10% sodium alginate aqueous solution；Calcium
Salting liquid is that temperature is 30 DEG C~70 DEG C, and mass concentration is 1%~4.5% calcium nitrate aqueous solution.
10. a kind of antibacterial hollow-fibre membrane for blood purification, it is characterised in that: be as described in any one of claim 1~9
Preparation method be made.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910071151.9A CN109794172B (en) | 2019-01-25 | 2019-01-25 | Preparation method of antibacterial hollow fiber membrane for blood purification |
| PCT/CN2019/104078 WO2020151228A1 (en) | 2019-01-25 | 2019-09-03 | Method for preparing antibacterial hollow fiber membrane for blood purification |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110743397A (en) * | 2019-11-26 | 2020-02-04 | 天津工业大学 | Preparation method of silver phosphate-containing calcium alginate antibacterial hydrogel filtering membrane |
| WO2020151228A1 (en) * | 2019-01-25 | 2020-07-30 | 广东省医疗器械研究所 | Method for preparing antibacterial hollow fiber membrane for blood purification |
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| CN109794172B (en) | 2021-05-14 |
| WO2020151228A1 (en) | 2020-07-30 |
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