CN105642322A - 一种合成水杨酰胺的催化剂及其制备方法 - Google Patents
一种合成水杨酰胺的催化剂及其制备方法 Download PDFInfo
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- CN105642322A CN105642322A CN201511013515.6A CN201511013515A CN105642322A CN 105642322 A CN105642322 A CN 105642322A CN 201511013515 A CN201511013515 A CN 201511013515A CN 105642322 A CN105642322 A CN 105642322A
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- catalyst
- salicylamide
- sodium hydroxide
- dihydrogen phosphate
- lithium oxide
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- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- SKZKKFZAGNVIMN-UHFFFAOYSA-N Salicilamide Chemical compound NC(=O)C1=CC=CC=C1O SKZKKFZAGNVIMN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229960000581 salicylamide Drugs 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 21
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001947 lithium oxide Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- MFXMOUUKFMDYLM-UHFFFAOYSA-L zinc;dihydrogen phosphate Chemical compound [Zn+2].OP(O)([O-])=O.OP(O)([O-])=O MFXMOUUKFMDYLM-UHFFFAOYSA-L 0.000 claims description 16
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 3
- MFXMOUUKFMDYLM-UHFFFAOYSA-H zinc;diphosphate Chemical compound [Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O MFXMOUUKFMDYLM-UHFFFAOYSA-H 0.000 abstract 2
- 239000000047 product Substances 0.000 description 7
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 6
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 3
- 229960004889 salicylic acid Drugs 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XEKFWVITKOJGIB-UHFFFAOYSA-N 2-hydroxybenzamide Chemical compound NC(=O)C1=CC=CC=C1O.NC(=O)C1=CC=CC=C1O XEKFWVITKOJGIB-UHFFFAOYSA-N 0.000 description 1
- 208000006820 Arthralgia Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 239000003907 antipyretic analgesic agent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229960001047 methyl salicylate Drugs 0.000 description 1
- 239000003750 molluscacide Substances 0.000 description 1
- 230000002013 molluscicidal effect Effects 0.000 description 1
- 208000004296 neuralgia Diseases 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1808—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with zinc, cadmium or mercury
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/10—Preparation of carboxylic acid amides from compounds not provided for in groups C07C231/02 - C07C231/08
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
本发明提供了一种合成水杨酰胺的催化剂,该催化剂由磷酸二氢锌、氧化锂和氢氧化钠组成,磷酸二氢锌:氧化锂:氢氧化钠为1-1.5:0.3-0.8:1-2,按重量比计,该催化剂性能重复性好,有利于工业化;易于分离,有利于产品的分离纯化;大大提高了水杨酰胺的提纯率及产品纯度,另外,提供了该催化剂的制备方法,该方法操作方便,工艺简单。
Description
技术领域
本发明属于一种催化剂,特别涉及一种合成水杨酰胺的催化剂,属于水杨酰胺的技术领域。
背景技术
水杨酰胺(salicylamide,结构式为2-(HO)C6H4CONH2)学名为2-羟基苯甲酰胺(2-Hydroxylbenzamide),是一种非常重要的有机合成中间体,是合成其许多重要衍生物(如杀螺剂硝苯柳胺,镇痛止热药邻乙氧基苯甲酰胺等)的原料,广泛应用于医药、香料、染料,橡胶助剂等诸多领域。水杨酰胺不仅是一个重要的精细化工中间体,而且也是一种被广泛接受和大量使用的解热镇痛药,用于发热头痛,神经痛,关节痛及活动性风湿症等,具有很好的疗效。
目前,合成水杨酰胺的方法主要有水杨酸氨化法和水杨酸甲酯氨化法。水杨酸氨化法是以水杨酸为原料,加入氨水在适当的条件氨基化,此方法合成的水杨酰胺提纯率低、成品纯度低,成品常常带粉红色泽,且提纯过程复杂。
发明内容
本发明所要解决的技术问题是提供一种合成水杨酰胺的催化剂,该催化剂性能重复性好,有利于工业化;易于分离,有利于产品的分离纯化;大大提高了水杨酰胺的提纯率及产品纯度,另外,提供了该催化剂的制备方法,该方法操作方便,工艺简单。
为了解决上述技术问题,本发明一种合成水杨酰胺的催化剂,由磷酸二氢锌、氧化锂和氢氧化钠组成,磷酸二氢锌:氧化锂:氢氧化钠为1-1.5:0.3-0.8:1-2,按重量比计。
上述的合成水杨酰胺的催化剂,由磷酸二氢锌、氧化锂和氢氧化钠组成,磷酸二氢锌:氧化锂:氢氧化钠为1:0.8:1,按重量比计。
上述的合成水杨酰胺的催化剂的制备方法,将磷酸二氢锌、氧化锂和氢氧化钠搅拌均匀,加入蒸馏水形成摩尔浓度为35%的溶液,将溶液放入反应釜中反应,反应过程中通过氨气,反应温度为180℃,反应时间为5小时,氨气流速为12m/s,反应后用蒸馏水洗涤至中性(pH=7),过滤,将所得的沉淀物在110℃下干燥1.5小时,再于270℃焙烧3小时制得催化剂,即可。
本发明与现有技术相比,有如下优点:
本发明性能重复性好,催化活性和稳定性高,有利于工业化;易于分离,有利于产品的分离纯化;大大提高了产品的提纯率及产品纯度。
具体实施方式
通过下述实施例可更详细地说明本发明。
实施例1
一种合成水杨酰胺的催化剂,将磷酸二氢锌、氧化锂和氢氧化钠搅拌均匀,加入蒸馏水形成摩尔浓度为35%的溶液,将溶液放入反应釜中反应,反应过程中通过氨气,反应温度为180℃,反应时间为5小时,氨气流速为12m/s,磷酸二氢锌:氧化锂:氢氧化钠为1:0.3:1,按重量比计,反应后用蒸馏水洗涤至中性(pH=7),过滤,将所得的沉淀物在110℃下干燥1.5小时,再于270℃焙烧3小时制得催化剂,即可。
实施例2
一种合成水杨酰胺的催化剂,将磷酸二氢锌、氧化锂和氢氧化钠搅拌均匀,加入蒸馏水形成摩尔浓度为35%的溶液,将溶液放入反应釜中反应,反应过程中通过氨气,反应温度为180℃,反应时间为5小时,氨气流速为12m/s,磷酸二氢锌:氧化锂:氢氧化钠为1:0.8:1,按重量比计,反应后用蒸馏水洗涤至中性(pH=7),过滤,将所得的沉淀物在110℃下干燥1.5小时,再于270℃焙烧3小时制得催化剂,即可。
实施例3
一种合成水杨酰胺的催化剂,将磷酸二氢锌、氧化锂和氢氧化钠搅拌均匀,加入蒸馏水形成摩尔浓度为35%的溶液,将溶液放入反应釜中反应,反应过程中通过氨气,反应温度为180℃,反应时间为5小时,氨气流速为12m/s,磷酸二氢锌:氧化锂:氢氧化钠为1.5:0.8:2,按重量比计,反应后用蒸馏水洗涤至中性(pH=7),过滤,将所得的沉淀物在110℃下干燥1.5小时,再于270℃焙烧3小时制得催化剂,即可。
尽管发明人已经对本发明的技术方案做了较为详细的阐述和列举,应当理解,对于本领域一个熟练的技术人员来说,对上述实施例作出修改和/或变通或者采用等同的替代方案是显然的,都不能脱离本发明精神的实质,本发明中出现的术语用于对本发明技术方案的阐述和理解,并不能构成对本发明的限制。
Claims (3)
1.一种合成水杨酰胺的催化剂,其特征在于,该催化剂由磷酸二氢锌、氧化锂和氢氧化钠组成,磷酸二氢锌:氧化锂:氢氧化钠为1-1.5:0.3-0.8:1-2,按重量比计。
2.如权利要求1所述的合成水杨酰胺的催化剂,其特征在于,该催化剂由磷酸二氢锌、氧化锂和氢氧化钠组成,磷酸二氢锌:氧化锂:氢氧化钠为1:0.8:1,按重量比计。
3.如权利要求1所述的合成水杨酰胺的催化剂的制备方法,其特征在于,将磷酸二氢锌、氧化锂和氢氧化钠搅拌均匀,加入蒸馏水形成摩尔浓度为35%的溶液,将溶液放入反应釜中反应,反应过程中通过氨气,反应温度为180℃,反应时间为5小时,氨气流速为12m/s,反应后用蒸馏水洗涤至中性(pH=7),过滤,将所得的沉淀物在110℃下干燥1.5小时,再于270℃焙烧3小时制得催化剂,即可。
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4701527A (en) * | 1983-12-05 | 1987-10-20 | Lever Brothers Company | Synthesis of salicylamides with improved reaction kinetics and improved effective yields |
CN101891645A (zh) * | 2010-07-27 | 2010-11-24 | 陕西科技大学 | 一种水杨酰胺的制备方法 |
CN102304061A (zh) * | 2011-07-05 | 2012-01-04 | 福建省胜达化工有限公司 | 一种水杨酰胺的制备方法 |
-
2015
- 2015-12-31 CN CN201511013515.6A patent/CN105642322A/zh active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4701527A (en) * | 1983-12-05 | 1987-10-20 | Lever Brothers Company | Synthesis of salicylamides with improved reaction kinetics and improved effective yields |
CN101891645A (zh) * | 2010-07-27 | 2010-11-24 | 陕西科技大学 | 一种水杨酰胺的制备方法 |
CN102304061A (zh) * | 2011-07-05 | 2012-01-04 | 福建省胜达化工有限公司 | 一种水杨酰胺的制备方法 |
Non-Patent Citations (2)
Title |
---|
THOMAS R.WARD ET AL.: "An Iron-Based Molecular Redox Switch as a Model for Iron Release from Enterobactin via the Salicylate Binding Mode", 《INORG.CHEM.》 * |
徐华峰,宋黎明,张凤霞: "水杨酰胺合成工艺的改进研究", 《化学工业与工程技术》 * |
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