CN110777442A - 衣康酸胍基苯乙烯共聚消毒纤维制备方法 - Google Patents
衣康酸胍基苯乙烯共聚消毒纤维制备方法 Download PDFInfo
- Publication number
- CN110777442A CN110777442A CN201911076950.1A CN201911076950A CN110777442A CN 110777442 A CN110777442 A CN 110777442A CN 201911076950 A CN201911076950 A CN 201911076950A CN 110777442 A CN110777442 A CN 110777442A
- Authority
- CN
- China
- Prior art keywords
- itaconic acid
- fiber
- disinfection
- styrene
- preparation
- 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.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 53
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000004659 sterilization and disinfection Methods 0.000 title claims abstract description 32
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 title claims abstract description 16
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- -1 itaconic acid guanidine hydrochloride Chemical compound 0.000 claims abstract description 20
- 230000001954 sterilising effect Effects 0.000 claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- 229920001577 copolymer Polymers 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012024 dehydrating agents Substances 0.000 claims description 5
- 229960000789 guanidine hydrochloride Drugs 0.000 claims description 5
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 3
- 238000001891 gel spinning Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000645 desinfectant Substances 0.000 abstract description 7
- 239000003242 anti bacterial agent Substances 0.000 abstract description 6
- 241000588724 Escherichia coli Species 0.000 abstract description 4
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 4
- 230000005923 long-lasting effect Effects 0.000 abstract description 3
- 231100000956 nontoxicity Toxicity 0.000 abstract description 3
- 241000589562 Brucella Species 0.000 abstract description 2
- 241000222122 Candida albicans Species 0.000 abstract description 2
- 230000009471 action Effects 0.000 abstract description 2
- 229940095731 candida albicans Drugs 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000004040 coloring Methods 0.000 abstract description 2
- 239000003651 drinking water Substances 0.000 abstract description 2
- 235000020188 drinking water Nutrition 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000002147 killing effect Effects 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 26
- 230000003385 bacteriostatic effect Effects 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 229940079593 drug Drugs 0.000 description 5
- 239000000126 substance Chemical class 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 230000000638 stimulation Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000249 desinfective effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- XREHTUHQSOFHEC-UHFFFAOYSA-N C=C(CC(=O)O)C(=O)O.C(=N)(N)N Chemical compound C=C(CC(=O)O)C(=O)O.C(=N)(N)N XREHTUHQSOFHEC-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 208000010201 Exanthema Diseases 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- DGCWMQUWINMIBY-UHFFFAOYSA-N diaminomethylideneazanium 2-methylidenebutanedioate Chemical compound C=C(CC(=O)[O-])C(=O)[O-].C(=[NH2+])(N)N.C(=[NH2+])(N)N DGCWMQUWINMIBY-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940000406 drug candidate Drugs 0.000 description 1
- 201000005884 exanthem Diseases 0.000 description 1
- 239000003777 experimental drug Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 125000002795 guanidino group Chemical group C(N)(=N)N* 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 231100000046 skin rash Toxicity 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000001550 time effect Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/42—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising cyclic compounds containing one carbon-to-carbon double bond in the side chain as major constituent
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/13—Amines
- A61K31/155—Amidines (), e.g. guanidine (H2N—C(=NH)—NH2), isourea (N=C(OH)—NH2), isothiourea (—N=C(SH)—NH2)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/10—Antimycotics
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/36—Amides or imides
- C08F222/38—Amides
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Animal Behavior & Ethology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Oncology (AREA)
- Communicable Diseases (AREA)
- Textile Engineering (AREA)
- Polymers & Plastics (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Epidemiology (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Artificial Filaments (AREA)
Abstract
本发明涉及一种衣康酸胍基苯乙烯共聚消毒纤维制备方法。制备方法如下：步骤1：衣康酸胍盐酸盐合成，步骤2：衣康酸胍基苯乙烯共聚纤维合成。本发明提供一种衣康酸胍基苯乙烯共聚消毒纤维制备方法。该纤维合成方法简便，杀菌、抑菌能力强。价格便宜。该消毒剂杀菌广谱，速效，持效杀菌能力长，安全无毒，环保。对布氏杆菌、大肠杆菌、金黄色葡萄球菌、白色念珠菌等有极强的杀灭作用，其稳定性也很好，有效期长达二年，且具有易于涂抹、渗透迅速、挥发快、不着色、易清洗等优点；可用于皮肤与创面消毒、手消毒、空气消毒、妇科及泌尿科消毒、饮用水消毒等，是一种新型、理想的便捷消毒剂。
Description
技术领域
本发明涉及消毒产品领域，具体地说是一种衣康酸胍基苯乙烯共聚消毒纤维制备方法。
背景技术
衣康酸曾被认为是生物技术手段生产的前12种生物化学物质之一。它在绿色化学领域的潜在应用是众多的。目前，衣康酸及其化学衍生物被认为是低工业相关性的利基化学品，具有活泼的化学性质，可进行自身间的聚合，也能与带有杀菌性的单体聚合成高分子化合物，然后进行纺丝，形成抗菌纤维。抗菌纤维中起作用的抗菌剂可以防止有害微生物对纤维本身的粘附,在附着在纤维上的时候就被抑制然后杀死,从而起到保护使用人员的作用。在人们的生产生活中不可避免地接触到各种病毒、细菌和真菌等微生物,这些微生物不仅污染环境,而且还导致许多疾病的产生,严重的威胁了人类的身心健康。抗菌性纤维作为一种新型的卫生保健纤维,它的开发以及应用完全符合市场需求,在人类日益关爱自身健康的环境下,将具有良好的市场开发应用前景。
抗菌纤维一般可以分为天然抗菌纤维和人工抗菌纤维两大类。天然抗菌纤维是指天然纤维本身就具有抗菌性，例如甲壳素纤维,竹原纤维、麻纤维等这类本身就具有抗菌效果的天然纤维，天然抗菌纤维生产工艺复杂、产品耐热性差；人工抗菌纤维是采用物理的或化学的方法将抗菌剂引入纤维表面及内部,一般包括以下几种方法:共混纺丝法、复合纺丝法、接枝改性法、离子交换法、湿纺法和后整理法。人工抗菌纤维的抗菌剂包括有机金属化合物、氯代酚以及硫化合物类等强抗菌性化学物质，其中部分抗菌剂纺织成抗菌纤维会破坏人体细胞组织，从而引起皮肤炎症、皮肤斑疹，也有部分有机金属化合物抗菌剂纺织成抗菌纤维穿在身上不舒适。
现在市场上使用的杀菌纤维主要有下面四种：
金属银物理混纺法。缺点：舒适度差，耐用度低。
含氯消毒液浸润法。缺点：抑菌时效短，副作用大。
金属离子明胶改性。缺点：法针对菌种范围小，改性条件苛刻。
纳米分散混熔法。缺点：工艺难度大，造价昂贵。
总之，市场上缺少高效、适用、方便的消毒纤维。
现在急需一种价格低廉、杀菌效果持久、对皮肤无刺激、无毒无副作用的抗菌纤维。
发明内容
本发明的目的是要提供一种成本低、对皮肤无刺激、高效杀菌、杀菌效果持久且价格低廉的衣康酸胍基苯乙烯共聚消毒纤维的制备方法。
本发明的技术方案是：
衣康酸胍基苯乙烯共聚消毒纤维制备方法，制备方法如下：
步骤1：衣康酸胍盐酸盐合成
在四颈瓶中，加入衣康酸、盐酸胍和浓硫酸脱水剂，加热135℃回流分水4小时，待反应时间3.5小时时停止加热，得到衣康酸胍盐酸盐，将产物放入烧杯中备用下一步聚合反应。
步骤2：衣康酸胍基苯乙烯共聚纤维合成：
在三颈瓶中加入衣康酸胍盐酸盐，苯乙烯，偶氮二异丁氰搅拌，加热到75℃，反应聚合1小时，将聚合产物趁热倒入烧杯中，采用干法湿纺制成纤维。
步骤1中所述衣康酸、盐酸胍和浓硫酸脱水剂重量比为130：95：2。
步骤2中衣康酸胍盐酸盐与苯乙烯的摩尔比为1：1-5。
本发明的有益效果:
1、本发明提供一种衣康酸胍基苯乙烯共聚消毒纤维制备方法。该纤维合成方法简便，杀菌、抑菌能力强。价格便宜。该消毒剂杀菌广谱，速效，持效杀菌能力长，安全无毒，环保。对布氏杆菌、大肠杆菌、金黄色葡萄球菌、白色念珠菌等有极强的杀灭作用，其稳定性也很好，有效期长达二年，且具有易于涂抹、渗透迅速、挥发快、不着色、易清洗等优点；可用于皮肤与创面消毒、手消毒、空气消毒、妇科及泌尿科消毒、饮用水消毒等，是一种新型、理想的便捷消毒剂。
2、本消毒剂起消毒作用的是胍基，是固定在纤维上，这样使用方便，而且清洗不掉，杀菌效果持久。
附图说明
图1为大肠杆菌抑菌检测图。
图2为金黄葡萄球菌药物的抑菌检测图。
具体实施方式
本发明的目的是要提供一种对皮肤无刺激、高效杀菌、杀菌效果持久且价格低廉的抗菌纤维的合成方法。消毒纤维合成分两步。具体合成路线如下：
合成路线
制备方法如下：
步骤1：衣康酸胍盐酸盐合成
安装好带有温度计、回流管、加料口和搅拌器的四颈瓶中，加入130克衣康酸、95克盐酸胍和2克浓硫酸脱水剂，加热135℃回流分水4小时，待反应时间3，5小时时停止加热。得到205克衣康酸胍盐酸盐(产率98％)将产物放入烧杯中备用下一步聚合反应。
步骤2：衣康酸胍基苯乙烯共聚纤维合成：
安装好带有温度计、滴液漏斗、搅拌器三颈瓶中加入20.3克衣康酸胍盐酸盐，10.4克苯乙烯，偶氮二异丁氰2克搅拌，加热到75℃，反应聚合1小时。将聚合产物趁热倒入烧杯中，攒足50克后采用干法湿纺制成纤维后，编制成抗菌纤维布，最后将纤维裁剪成口罩。
实施例2：
其它步骤都同上面叙述，只是步骤2中的衣康酸胍盐酸盐和苯乙烯用量摩尔比为1：1。
实施例3：
其它步骤都同上面叙述，只是步骤2中的衣康酸胍盐酸盐和苯乙烯用量摩尔比为1：5。
实施例5：
其它步骤都同上面叙述，只是步骤2中的衣康酸胍盐酸盐和苯乙烯用量摩尔比为1：3。
根据抗菌纤维用途不同改变苯乙烯和衣康酸胍盐酸盐的配比(如强度高则苯乙烯比例适当提高；抗菌效果好些则衣康酸胍盐酸盐比例高些)。
将衣康酸盐酸胍盐溶解在去离子水中做下面抑菌检测试验。
药物抑菌检测试验
实验药物：衣康酸胍基盐杀菌检测报告
实验菌种：大肠杆菌，金黄葡萄球菌
实验流程：
1.称取5克衣康酸胍盐酸盐加医药去离子水配置成1％溶液。
2.取实验菌种用培养基进行1：1000的浓度稀释，同时取三个96孔板。将稀释后的菌液加入96孔板的前七排，每排每孔加入量150微升，共加三个96板。
3.每个96板的前三排一孔依次再加入150微升稀释后的菌液，30微升药物。用排枪依次向后稀释，共稀释24个浓度梯度。孔板第七排为空白菌液对照。
4.孔板第八排各加150微升培养基，作空白对照。
5.所有试剂加入完毕，96孔板用封口膜封好，分别标注三种药物信息，放入37℃培养箱培养。
6.培养2h，4h，6h，8h，10h后用酶标仪检测并记录各孔菌液数据(检测波长为630nm)。
实验数据：
从图1和图2可以看出，抗菌纤维有抑菌效果，抑菌浓度为十个稀释梯度。
Claims (3)
1.衣康酸胍基苯乙烯共聚消毒纤维制备方法，其特征在于：
制备方法如下：
步骤1：衣康酸胍盐酸盐合成
在四颈瓶中，加入衣康酸、盐酸胍和浓硫酸脱水剂，加热135℃回流分水4小时，待反应时间3.5小时时停止加热，得到衣康酸胍盐酸盐，将产物放入烧杯中备用下一步聚合反应；
步骤2：衣康酸胍基苯乙烯共聚纤维合成：
在三颈瓶中加入衣康酸胍盐酸盐，苯乙烯，偶氮二异丁氰搅拌，加热到75℃，反应聚合1小时，将聚合产物趁热倒入烧杯中，采用干法湿纺制成纤维。
2.根据权利要求1所述的衣康酸胍基苯乙烯共聚消毒纤维制备方法，其特征在于：
步骤1中所述衣康酸、盐酸胍和浓硫酸脱水剂重量比为130：95：2。
3.根据权利要求1所述的衣康酸胍基苯乙烯共聚消毒纤维制备方法，其特征在于：
步骤2中衣康酸胍盐酸盐与苯乙烯的摩尔比为1：1-5。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911076950.1A CN110777442A (zh) | 2019-11-06 | 2019-11-06 | 衣康酸胍基苯乙烯共聚消毒纤维制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911076950.1A CN110777442A (zh) | 2019-11-06 | 2019-11-06 | 衣康酸胍基苯乙烯共聚消毒纤维制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110777442A true CN110777442A (zh) | 2020-02-11 |
Family
ID=69389634
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911076950.1A Pending CN110777442A (zh) | 2019-11-06 | 2019-11-06 | 衣康酸胍基苯乙烯共聚消毒纤维制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110777442A (zh) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350022A (zh) * | 2000-10-19 | 2002-05-22 | 上海塑杰科技有限公司 | 一种多元胺与胍盐聚合物及其制备方法 |
| CN1445270A (zh) * | 2002-03-15 | 2003-10-01 | 上海塑杰科技有限公司 | 一种聚烯烃功能化母粒及其制备方法和应用 |
| JP2013147473A (ja) * | 2012-01-23 | 2013-08-01 | Japan Exlan Co Ltd | 抗ウイルス用粒子および該粒子を含有する製品 |
| CN105315459A (zh) * | 2014-10-29 | 2016-02-10 | 吉林云飞医药有限公司 | 一种聚己二酸基胍盐酸盐的制备方法 |
| CN109535418A (zh) * | 2018-10-10 | 2019-03-29 | 桂林新先立抗菌材料有限公司 | 一种抗菌织物材料及其制备方法 |
-
2019
- 2019-11-06 CN CN201911076950.1A patent/CN110777442A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350022A (zh) * | 2000-10-19 | 2002-05-22 | 上海塑杰科技有限公司 | 一种多元胺与胍盐聚合物及其制备方法 |
| CN1445270A (zh) * | 2002-03-15 | 2003-10-01 | 上海塑杰科技有限公司 | 一种聚烯烃功能化母粒及其制备方法和应用 |
| JP2013147473A (ja) * | 2012-01-23 | 2013-08-01 | Japan Exlan Co Ltd | 抗ウイルス用粒子および該粒子を含有する製品 |
| CN105315459A (zh) * | 2014-10-29 | 2016-02-10 | 吉林云飞医药有限公司 | 一种聚己二酸基胍盐酸盐的制备方法 |
| CN109535418A (zh) * | 2018-10-10 | 2019-03-29 | 桂林新先立抗菌材料有限公司 | 一种抗菌织物材料及其制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| 于太保等: "一种新型胍类高分子型抗菌剂的制备及抗菌性能表征", 《广东化工》 * |
| 张青山: "《有机合成反应基础》", 31 December 2004, 北京：高等教育出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100554296C (zh) | 可反应性高分子抗菌剂及其制备方法和应用 | |
| KR100752150B1 (ko) | 이미다졸륨 염을 갖는 광경화성 단량체, 상기 이미다졸륨염을 함유하는 항균성 광경화형 조성물 및 상기조성물로부터 제조되는 항균성 고분자 재료 | |
| CN101279219A (zh) | 双季铵盐阳离子表面活性剂及其制备方法与应用 | |
| CN105601778B (zh) | 一种含有季铵基团的环状卤胺类高分子抗菌剂及其制备方法和应用 | |
| CN101808514B (zh) | 生物活性苯胺共聚物 | |
| CN107531897A (zh) | 用于抗微生物应用的缩聚物 | |
| US20160100578A1 (en) | Anti-Microbial Polymer Incorporating a Quaternary Ammonium Group | |
| KR20200116134A (ko) | 분지형 폴리 (아미노산) 항균제 및 이의 용도 | |
| CN105820333A (zh) | 一种盐酸聚六亚甲基胍的制备方法 | |
| CN101747363A (zh) | 一种有机硅胍盐杀菌剂的制备方法 | |
| CN101810198B (zh) | 水杨酸碘消毒剂及其制备方法 | |
| CN107343506A (zh) | 一种有机磷酸锆抗菌剂 | |
| CN110105477A (zh) | 一种四苯基乙烯标记的响应性季铵盐化聚乙烯醇及制备与应用 | |
| CN106084203A (zh) | 一种水溶性嵌段聚季铵盐高分子材料及其制备方法 | |
| CN110028614A (zh) | 具有蛋白吸附功能的抗菌微纳米凝胶与纤维及其制备方法 | |
| Huang et al. | Preparation of grafted starch by IPDI coupling and its antibacterial properties | |
| CN107099031B (zh) | 一种耐高温改性聚六亚甲基胍及其制备方法和用途 | |
| CN110777442A (zh) | 衣康酸胍基苯乙烯共聚消毒纤维制备方法 | |
| CN105001198B (zh) | 含吡啶类季铵盐官能团的高分子杀菌消毒剂及其制备方法 | |
| CN105906664A (zh) | 季膦盐型抗菌单体及其制备方法 | |
| CN105557751A (zh) | 高分子生物有机碘及其制备方法、水产养殖疾病防治方法 | |
| Kubatova et al. | Evaluation of Effects of C60 fullerene and its derivatives on selected microorganisms | |
| CN111303413A (zh) | 一种四氢嘧啶基阳离子抗菌聚合物、其制备方法及应用 | |
| CN102690481B (zh) | 一种纳米溴化银聚合物复合抗菌剂及其制备方法 | |
| CN115894887A (zh) | 一种共聚季铵盐及其制备方法 |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200211 |
|
| RJ01 | Rejection of invention patent application after publication |