CN107513014A - 一种水杨酸碘络合物、制备方法及应用 - Google Patents
一种水杨酸碘络合物、制备方法及应用 Download PDFInfo
- Publication number
- CN107513014A CN107513014A CN201610447691.9A CN201610447691A CN107513014A CN 107513014 A CN107513014 A CN 107513014A CN 201610447691 A CN201610447691 A CN 201610447691A CN 107513014 A CN107513014 A CN 107513014A
- Authority
- CN
- China
- Prior art keywords
- salicylic acid
- iodine
- complex compound
- preparation
- iodine complex
- 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
- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
- ZVVHPYOYQRQSJH-UHFFFAOYSA-N [I].OC(=O)C1=CC=CC=C1O Chemical compound [I].OC(=O)C1=CC=CC=C1O ZVVHPYOYQRQSJH-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims abstract description 56
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011630 iodine Substances 0.000 claims abstract description 32
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 32
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229960004889 salicylic acid Drugs 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008139 complexing agent Substances 0.000 claims abstract description 6
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical group II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000007800 oxidant agent Substances 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- 239000012046 mixed solvent Substances 0.000 claims description 12
- 239000000645 desinfectant Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 5
- 206010012735 Diarrhoea Diseases 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 230000001954 sterilising effect Effects 0.000 abstract description 11
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000006978 adaptation Effects 0.000 abstract 1
- 238000009374 poultry farming Methods 0.000 abstract 1
- 239000012043 crude product Substances 0.000 description 20
- 239000000843 powder Substances 0.000 description 19
- 241000894006 Bacteria Species 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 12
- 239000000725 suspension Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 238000001816 cooling Methods 0.000 description 10
- 239000013078 crystal Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 9
- 229940093930 potassium iodate Drugs 0.000 description 9
- 235000006666 potassium iodate Nutrition 0.000 description 9
- 239000001230 potassium iodate Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 241000588724 Escherichia coli Species 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- HEILIGJNYTWOHU-UHFFFAOYSA-N ethanol 2-hydroxybenzoic acid Chemical compound CCO.OC(=O)C1=CC=CC=C1O HEILIGJNYTWOHU-UHFFFAOYSA-N 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- RTKIYNMVFMVABJ-UHFFFAOYSA-L thimerosal Chemical compound [Na+].CC[Hg]SC1=CC=CC=C1C([O-])=O RTKIYNMVFMVABJ-UHFFFAOYSA-L 0.000 description 5
- 229940033663 thimerosal Drugs 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 244000063299 Bacillus subtilis Species 0.000 description 3
- 235000014469 Bacillus subtilis Nutrition 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 208000003251 Pruritus Diseases 0.000 description 2
- 230000000202 analgesic effect Effects 0.000 description 2
- 239000002260 anti-inflammatory agent Substances 0.000 description 2
- 230000001741 anti-phlogistic effect Effects 0.000 description 2
- 230000003260 anti-sepsis Effects 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000007803 itching Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 239000001888 Peptone Substances 0.000 description 1
- 108010080698 Peptones Proteins 0.000 description 1
- 240000000203 Salix gracilistyla Species 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 241000385540 bacterium 10 Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 244000144987 brood Species 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 230000026045 iodination Effects 0.000 description 1
- 238000006192 iodination reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 235000019319 peptone Nutrition 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/363—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
-
- 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
- A01N59/12—Iodine, e.g. iodophors; Compounds 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
- A61K31/60—Salicylic acid; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/18—Iodine; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C65/00—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
- C07C65/01—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups containing hydroxy or O-metal groups
- C07C65/03—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups containing hydroxy or O-metal groups monocyclic and having all hydroxy or O-metal groups bound to the ring
- C07C65/05—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups containing hydroxy or O-metal groups monocyclic and having all hydroxy or O-metal groups bound to the ring o-Hydroxy carboxylic acids
- C07C65/10—Salicylic acid
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F13/00—Compounds containing elements of Groups 7 or 17 of the Periodic Table
- C07F13/005—Compounds without a metal-carbon linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Animal Behavior & Ethology (AREA)
- Wood Science & Technology (AREA)
- Epidemiology (AREA)
- Medicinal Chemistry (AREA)
- Environmental Sciences (AREA)
- Zoology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Inorganic Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
本发明属于化学领域,具体涉及一种水杨酸碘络合物、制备方法及应用,所述水杨酸碘络合物,络合剂为水杨酸,配位中心是碘分子。该制备方法以碘和水杨酸为原料,通过加入氧化剂作为催化剂,在一定温度下,反应一定时间,得到产品。该制备方法操作简单,绿色环保,易于实现工业化生产,具有重大经济效益和社会效益,本发明的水杨酸碘络合物,杀菌能力强、持效时间长高效稳定、安全无污染、快速杀菌与持久杀菌完美结合的优点,可广泛用于环境、水体、疫区、宠物医院、家禽养殖、畜牧业、水产养殖场等需要消毒、杀菌的场所,具有极强的推广意义。
Description
技术领域
本发明属于化学领域,具体涉及一种水杨酸碘络合物、制备方法及应用。
背景技术
随着人类对环保、食品安全等的重视,消毒剂的发展也在朝着高效与环保结合的方向发展,各类新型消毒剂涌现,近年出现的碘伏制剂因其高效、环保性能受到广泛关注。其杀菌机制是基于它的碘化作用以及对细胞外层的破坏作用。单质碘具有杀菌速度快的特点,但缺点是持效时间短、刺激性强。为了克服这些缺点,人们通常对单质碘的性质进一步改善。
而水杨酸具有防腐杀菌作用外,还有止痒消肿、止痛消炎等功能,常被用于络合剂,是医药工业重要的原料。为了改善消毒剂的性能,改善碘单质作为消毒剂的作用效果,提供一种复合性能好,持效时间长的碘络合物是十分重要的。
发明内容
本发明的目的在于提供一种复合性能好,持效时间长的水杨酸碘络合物。
为了解决上述技术问题,水杨酸碘络合物,络合剂为水杨酸,配位中心是碘分子。
具体地,所述水杨酸碘络合物的结构式为:
本发明还提供一种水杨酸碘络合物的制备方法,以碘和水杨酸为原料并溶于一定溶剂中,通过加入氧化剂作为催化剂,在一定温度下,反应一定时间,得到产品。
进一步地,还包括重结晶,进一步纯化,从而得到产品。
具体地,所述碘和水杨酸的摩尔比为1∶(1~2)。
作为优选,所述氧化剂为碘酸钾、高锰酸钾和重铬酸钾中的一种或多种。
作为优选,所述溶剂为水,或乙醇与水的混合物。
进一步地,所述反应时间为20min~2h;所述一定温度为室温至110℃。
作为优选,所述重结晶的溶剂为丙酮与冰醋酸以1∶1混合溶剂。
水杨酸碘络合物在消毒剂或治疗腹泻的试剂中的应用。
有益效果:
(1)本发明提出一种水杨酸碘络合物,其中络合剂为水杨酸,配位中心是碘分子。该络合物是以水杨酸为络合剂,水杨酸本身具有防腐杀菌作用外,还有止痒消肿、止痛消炎等功能,利用其作为络合剂,与碘形成络合物,复合性能好、杀菌能力强、持效时间长的水杨酸碘络合物,具有广泛的应用前景。
(2)本发明提供一种水杨酸碘络合物的制备方法,该制备方法操作简单,绿色环保,易于实现工业化生产,制备的水杨酸碘络合物杀菌能力强,复合性好,且无刺激性。
(3)本发明提供一种水杨酸碘络合物的制备方法,通过进一步重结晶,得到高纯度的产品。
(4)本发明提供一种水杨酸碘络合物的制备方法,通过控制碘和水杨酸的摩尔比制备出络合性能良好的水杨酸碘络合物产品。
(5)本发明提供一种水杨酸碘络合物的制备方法,通过控制,反应温度为室温至110℃,所述反应时间为20min~2h,有效制备提高反应速率和络合物性能。
(6)本发明提供一种水杨酸碘络合物的制备方法,通过控制反应溶剂,控制反应速率和反应效率,以及获得络合比不同的水杨酸碘络合物。
(7)本发明的水杨酸碘络合物,可广泛的应用于消毒剂或治疗腹泻。
具体实施方式
实施例1:
一种水杨酸碘络合物,该络合物的结构式为:
水杨酸碘络合物的制备方法:
在三颈烧瓶中,加入水杨酸,并加入水,缓慢加热至90℃,在搅拌条件下,逐渐加入碘粉、碘酸钾,反应20min,静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40℃真空干燥,得粉末状固体。
水杨酸碘络合物可作为消毒剂或治疗腹泻的试剂。
实施例2
在反应皿中,加入水杨酸,并加入乙醇,搅拌溶解;将碘粉加入水溶解,并将碘单质溶液加入上述水杨酸乙醇溶液中,并加入碘酸钾,室温下,反应20min,静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40℃真空干燥,得粉末状固体。
实施例3
在反应皿中,加入水杨酸,并加入乙醇,搅拌溶解;将碘粉加入水溶解,并将碘单质溶液加入上述水杨酸乙醇溶液中,并加入碘酸钾,室温下,反应1h,其中,水杨酸与碘粉的摩尔比为2∶1。乙醇与水的体积比为2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例4
在反应皿中,加入水杨酸,并加入乙醇,搅拌溶解;将碘粉加入水溶液溶解,并将碘单质溶液加入上述水杨酸乙醇溶液中,并加入碘酸钾,室温下,反应2h,其中,水杨酸与碘粉的摩尔比为1∶1。乙醇与水的体积比为2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例5
在反应皿中,加入水杨酸,并加入乙醇,搅拌溶解;将碘粉加入水溶液溶解,并将碘单质溶液加入上述水杨酸乙醇溶液中,并加入碘酸钾,室温下,反应30min,其中,水杨酸与碘粉的摩尔比为1.5∶1。乙醇与水的体积比为2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例6
在反应皿中,加入水杨酸,并加入乙醇,搅拌溶解;将碘粉加入水溶液溶解,并将碘单质溶液加入上述水杨酸乙醇溶液中,并加入碘酸钾,室温下,反应30min,其中,水杨酸与碘粉的摩尔比为1.2∶1。乙醇与水的体积比为2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例7
在三颈烧瓶中,加入水杨酸,并加入水,缓慢加热至100℃,在搅拌条件下,逐渐加入碘粉、碘酸钾,反应1h,其中,水杨酸与碘粉的摩尔比为1.2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例8
在三颈烧瓶中,加入水杨酸,并加入水,缓慢加热至110℃,在搅拌条件下,逐渐加入碘粉、碘酸钾,反应30min,其中,水杨酸与碘粉的摩尔比为2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例9
在三颈烧瓶中,加入水杨酸,并加入水,缓慢加热至95℃,在搅拌条件下,逐渐加入碘粉、高锰酸钾,反应2h,其中,水杨酸与碘粉的摩尔比为1∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
实施例10
在三颈烧瓶中,加入水杨酸,并加入水,缓慢加热至100℃,在搅拌条件下,逐渐加入碘粉、重铬酸钾,反应20min,其中,水杨酸与碘粉的摩尔比为1.2∶1。静置冷却后3000r/min离心2min,无水乙醇洗涤2次得到粗品。用丙酮与冰醋酸以1∶1混合溶剂对粗品进行重结晶,析出晶体,抽滤,于40e真空干燥,得粉末状固体。
杀菌试验
1材料和方法
1.1试验器材
试验菌株:大肠杆菌(8099)和金黄色葡萄球菌(ATCC6538),培养第6~8代;枯草杆菌黑色变种(ATCC9372),培养第4代,制备芽胞。
消毒液:将本申请实施例4-10所制得的粉末状水杨酸碘络合物用水配成混悬液。
1.2方法
1.2.1菌悬液的制备 取金黄色葡萄球菌(ATCC6538)和大肠杆菌(8099)24h新鲜培养物及枯草杆菌黑色变种(ATCC9372)芽胞悬液,用含10g/L蛋白胨磷酸盐缓冲液稀释配制成菌106-107个/ml菌悬液备用。
1.2.2中和剂选择试验 以大肠杆菌为代表。在25℃条件下,设平行6组试验,按悬液杀菌试验程序进行。①消毒液+菌悬液;②(消毒液+菌悬液)+中和剂;③中和剂+菌悬液;④(消毒液+中和剂)+菌悬液;⑤稀释液+菌悬液(正常菌对照);⑥稀释液+中和剂+培养基作为阴性对照。试验结果,以第1组不长菌或仅有极少数菌落生长;第2组有菌落生长,较第1组为多,但较第3、4、5组为少;第3、4、5组菌数相似,误差率≤10%;第6组无菌生长,为所选中和剂及其浓度适宜。试验重复3次。
1.2.3悬液杀菌试验
吸取0.5ml上述菌悬液于测试浓度的消毒剂溶液4.5ml内,置25℃水浴中作用5分钟;立即吸取上述菌药混合液1.0ml,加入9.0ml中和液中混合。中和10分钟后进行涂板活菌计数、计算杀菌率。
各实施例制得的水杨酸碘络合物混悬液的最低有效浓度试验结果见表1。
表1 测试结果
由表1可以看出,实施例4~10对大肠杆菌、金黄色葡萄球菌、枯草杆菌黑色变种的均起到杀菌效果,且实施例5对大肠杆菌的最低有效浓度为3%,对金黄色葡萄球菌的最低有效浓度为4%,对枯草杆菌黑色变种的最低有效浓度为5%,所需要的最低有效浓度最低,由此可以看出,实施例5提供的水杨酸碘络合物配制得到的消毒液杀菌效果最好。
显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (10)
1.一种水杨酸碘络合物,其特征在于,络合剂为水杨酸,配位中心是碘分子。
2.根据权利要求1所述的一种水杨酸碘络合物,其特征在于,结构式为:
3.一种水杨酸碘络合物的制备方法,其特征在于,以水杨酸和碘为原料并溶于一定溶剂中,通过加入氧化剂作为催化剂,在一定温度下,反应一定时间,得到产品。
4.根据权利要求3所述的水杨酸碘络合物的制备方法,其特征在于,还包括重结晶,从而得到产品。
5.根据权利要求3所述的水杨酸碘络合物的制备方法,其特征在于,碘和水杨酸的摩尔比为1∶(1~2)。
6.根据权利要求3所述的水杨酸碘络合物的制备方法,其特征在于,所述氧化剂为碘酸钾、高锰酸钾和重铬酸钾中的一种或多种。
7.根据权利要求3所述的水杨酸碘络合物的制备方法,其特征在于,所述溶剂为水,或乙醇与水的混合物。
8.根据权利要求4-7任一项所述的水杨酸碘络合物的制备方法,其特征在于,所述一定时间为20min~2h;所述一定温度为室温至110℃。
9.根据权利要求4所述的水杨酸碘络合物的制备方法,其特征在于,所述重结晶的溶剂为丙酮与冰醋酸以1∶1混合溶剂。
10.一种如权利要求1或2所述的水杨酸碘络合物在消毒剂或治疗腹泻的试剂中的应用。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610447691.9A CN107513014A (zh) | 2016-06-17 | 2016-06-17 | 一种水杨酸碘络合物、制备方法及应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610447691.9A CN107513014A (zh) | 2016-06-17 | 2016-06-17 | 一种水杨酸碘络合物、制备方法及应用 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN107513014A true CN107513014A (zh) | 2017-12-26 |
Family
ID=60720181
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610447691.9A Pending CN107513014A (zh) | 2016-06-17 | 2016-06-17 | 一种水杨酸碘络合物、制备方法及应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107513014A (zh) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1436557A (zh) * | 2002-02-03 | 2003-08-20 | 沈志强 | 一种杀菌药 |
EP1413293A1 (fr) * | 2002-10-24 | 2004-04-28 | Maria Yolanda Aliaga | Pommade conçue pour assurer la disparition des champignons |
CN1834087A (zh) * | 2005-03-17 | 2006-09-20 | 曾雄飞 | 有机碘络合物 |
CN101810198A (zh) * | 2010-05-06 | 2010-08-25 | 佛山市正典生物技术有限公司 | 水杨酸碘消毒剂及其制备方法 |
RU2538699C1 (ru) * | 2013-11-29 | 2015-01-10 | Закрытое акционерное общество "ФИРН М" (ЗАО "ФИРН М") | Фармацевтическая композиция для лечения людей, страдающих ксеростомией |
CN105557752A (zh) * | 2016-03-03 | 2016-05-11 | 佛山市正典生物技术有限公司 | 一种水杨酸碘泡沫型消毒剂及其制备方法 |
-
2016
- 2016-06-17 CN CN201610447691.9A patent/CN107513014A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1436557A (zh) * | 2002-02-03 | 2003-08-20 | 沈志强 | 一种杀菌药 |
EP1413293A1 (fr) * | 2002-10-24 | 2004-04-28 | Maria Yolanda Aliaga | Pommade conçue pour assurer la disparition des champignons |
CN1834087A (zh) * | 2005-03-17 | 2006-09-20 | 曾雄飞 | 有机碘络合物 |
CN101810198A (zh) * | 2010-05-06 | 2010-08-25 | 佛山市正典生物技术有限公司 | 水杨酸碘消毒剂及其制备方法 |
RU2538699C1 (ru) * | 2013-11-29 | 2015-01-10 | Закрытое акционерное общество "ФИРН М" (ЗАО "ФИРН М") | Фармацевтическая композиция для лечения людей, страдающих ксеростомией |
CN105557752A (zh) * | 2016-03-03 | 2016-05-11 | 佛山市正典生物技术有限公司 | 一种水杨酸碘泡沫型消毒剂及其制备方法 |
Non-Patent Citations (2)
Title |
---|
赵文艳 等31: "复方碘酊中的碘和水杨酸的配伍变化", 《江西医药》 * |
邝煜宏: "水杨酸碘搽剂含量测定的实验", 《现代食品与药品杂志》 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104013573B (zh) | 有效碘含量为5-12%的液体聚维酮碘 | |
CN103975949A (zh) | 一种壳聚糖碘液及其制备方法 | |
CN102550602A (zh) | 一种高含碘控释型消毒杀菌剂 | |
CN103059006B (zh) | 具有抗菌活性的白杨素-1,2,3-三氮唑类化合物及其制备方法 | |
CN113693080A (zh) | 一种石墨烯离子杀毒抗菌液及其制备方法 | |
CN107043432A (zh) | 一种两性羧甲基壳聚糖胍盐衍生物及其制备方法 | |
CN113367157A (zh) | 一种花状银/木质素复合抗菌颗粒的制备方法 | |
CN101161070A (zh) | 双链季铵盐复合邻苯二甲醛消毒剂 | |
CN109221104A (zh) | 一种含银碳点、制备方法及其应用 | |
CN107513014A (zh) | 一种水杨酸碘络合物、制备方法及应用 | |
CN108513987A (zh) | 一种用于室内杀菌的卤胺聚合物改性活性炭及其制备方法 | |
CN102516265B (zh) | 噻二唑喹啉类有机铜化合物及其制备方法、制剂及在防治农业植物病害中的用途 | |
CN102453256B (zh) | 一种制备具水溶性及生物可分解性抗菌剂的方法 | |
CN102846489B (zh) | 一种盐酸聚六亚甲基胍碘药浴液及其制备方法 | |
CN108863909A (zh) | 一类新型卤胺结构化合物及其制备方法和抗菌领域应用 | |
CN115304528A (zh) | 一种可降解的双子季铵盐及其制备方法、杀菌剂 | |
CN103113251A (zh) | N,n-对苯羧基羟苯基甲基季铵盐及其制备方法 | |
CN112889818A (zh) | 一种复合季铵盐消毒剂泡腾片的制造方法 | |
CN102516267B (zh) | 噻唑类有机铜化合物及其制备方法、制剂和用途 | |
CN107501078A (zh) | 一种枸橼酸碘络合物及其制备方法 | |
CN106719811B (zh) | 水产用自增稠型高含量碘伏溶液及其制备方法 | |
CN105669973A (zh) | 一种具抑菌活性的化合物及其制备和应用 | |
CN105348269B (zh) | 一种含喹喔啉和咔唑结构单元的衍生物及其应用 | |
CN116903557B (zh) | 一种复合杀菌混合物及其制备方法 | |
CN102206191B (zh) | 1,4-双(4-氨基-5-巯基-1,2,4-三唑)苯及其制备方法和用途 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
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 | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171226 |