CN105503640A - Efficient preparation method of salicylamide - Google Patents
Efficient preparation method of salicylamide Download PDFInfo
- Publication number
- CN105503640A CN105503640A CN201511012668.9A CN201511012668A CN105503640A CN 105503640 A CN105503640 A CN 105503640A CN 201511012668 A CN201511012668 A CN 201511012668A CN 105503640 A CN105503640 A CN 105503640A
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- ionized water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0201—Oxygen-containing compounds
- B01J31/0204—Ethers
-
- 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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/40—Substitution reactions at carbon centres, e.g. C-C or C-X, i.e. carbon-hetero atom, cross-coupling, C-H activation or ring-opening reactions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to an efficient preparation method of salicylamide. The preparation method comprises the following steps: (1) weighing raw materials, wherein the raw materials comprise the following components in parts by weight: 35-50 parts of salicylic acid, 10-20 parts of liquid ammonia, 100-200 parts of ionized water and 5-10 parts of catalyst; (2) uniformly mixing the 35-50 parts of salicylic acid, the 10-20 parts of liquid ammonia and 10-20 parts of ionized water, and heating at the temperature of 85-110 DEG C to obtain an ammonization solution; (3) adding the 12-22 parts of catalyst into the ammonization solution, and performing dehydration treatment for 2-4 hours to obtain a primary product; (4) uniformly mixing the residual ionized water and the primary product by stirring to obtain a secondary product, adding the secondary product into a centrifugal machine to perform centrifuging, removing supernate, and drying precipitate to obtain the salicylamide. The method for preparing the salicylamide has the advantages of low cost and prevention of pollution.
Description
Technical field
The present invention relates to field of fine chemical, especially a kind of preparation method of efficient salicylic amide.
Background technology
Salicylic amide, chemical name is neck hydroxybenzamide, is the reliable antipyretic throe medicine of curative effect.Clinically for having a headache and fever, the disease such as arthrodynia and rheumatism; Meanwhile, it is again a kind of important fine-chemical intermediate, is widely used in the fields such as medicine, agricultural chemicals, spices, fuel, additive synthesis.The ammonification of water at normal temperature poplar acid amides, puts ionized water, opens stirring in Whitfield's ointment, and logical ammonia ammoniacal liquor, make Whitfield's ointment ammonification be salicylic amide, preparation method's cost of existing salicylic amide is increased, and complex process, easily causes environmental pollution.
Summary of the invention
The object of the invention is the preparation method in order to provide a kind of efficient salicylic amide, use the method prepare salicylic amide cost low, not easily pollute.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for efficient salicylic amide, its preparation method is as follows:
(1) take starting material, described raw-material moiety is counted by weight: Whitfield's ointment 35-50 part, liquefied ammonia 10-20 part, ionized water 100-120 part, catalyzer 5-10 part;
(2), after Whitfield's ointment 35-50 part, liquefied ammonia 10-20 part, ionized water 10-20 part being mixed, heat at the temperature of 85-110 DEG C, obtain ammoniated solution;
(3) add in ammoniated solution catalyzer 12-22 part carry out processed 2-4h after Primary product;
(4) ionized water of surplus is added in Primary product carry out mix and blend and obtain secondary species, secondary species is added carry out in whizzer centrifugal, abandoning supernatant, throw out is carried out drying salicylic amide.
The preparation method of above-mentioned a kind of efficient salicylic amide, wherein, described catalyzer is one or more the combination of phospho-molybdic acid, trimethylbenzene, vinyltrimethoxy silane, zinc phosphate and ammonium chloride emphasis.
Beneficial effect of the present invention is:
The invention solves and use wintergreen oil to prepare the high cost problem of salicylic amide for raw material, adopt catalyzer, ammoniated solution dehydration is obtained salicylic amide, and catalyzer is simple and easy to get, and cost is low, and production technique simplifies, three waste discharge less this.
Specific embodiment
Below by way of specific embodiment, the specific embodiment of the present invention is described in further detail.
Example one
A preparation method for efficient salicylic amide, its preparation method is as follows:
(1) take starting material, described raw-material moiety is counted by weight: Whitfield's ointment 42 parts, 15 parts, liquefied ammonia, ionized water 110 parts, catalyzer 7 parts;
(2), after Whitfield's ointment 42 parts, 15 parts, liquefied ammonia, ionized water 15 parts being mixed, heat at the temperature of 100 DEG C, obtain ammoniated solution;
(3) add in ammoniated solution phospho-molybdic acid 7 parts carry out processed 3h after Primary product;
(4) ionized water of 95 parts is added in Primary product carry out mix and blend and obtain secondary species, secondary species is added carry out in whizzer centrifugal, abandoning supernatant, throw out is carried out drying salicylic amide.
Example two
A preparation method for efficient salicylic amide, its preparation method is as follows:
(1) Kaolinite Preparation of Catalyst, counts by weight and phospho-molybdic acid 25 parts, trimethylbenzene 5 parts, vinyltrimethoxy silane 8 parts, zinc phosphate 0.5 part and ammonium chloride 3 parts is mixed to get catalyzer;
(2) take starting material, described raw-material moiety is counted by weight: Whitfield's ointment 35 parts, 10 parts, liquefied ammonia, ionized water 100 parts, catalyzer 5 parts;
(3), after Whitfield's ointment 35 parts, 10 parts, liquefied ammonia, ionized water 10 parts being mixed, heat at the temperature of 110 DEG C, obtain ammoniated solution;
(4) add in ammoniated solution catalyzer 5 parts carry out processed 2h after Primary product;
(5) 90 parts of ionized waters are added in Primary product carry out mix and blend and obtain secondary species, secondary species is added carry out in whizzer centrifugal, abandoning supernatant, throw out is carried out drying salicylic amide.
Example three
A preparation method for efficient salicylic amide, its preparation method is as follows:
(1) Kaolinite Preparation of Catalyst, counts by weight and phospho-molybdic acid 18 parts, trimethylbenzene 6 parts, vinyltrimethoxy silane 3 parts, zinc phosphate 2 parts and ammonium chloride 4 parts is mixed to get catalyzer;
(2) take starting material, described raw-material moiety is counted by weight: Whitfield's ointment 50 parts, 20 parts, liquefied ammonia, ionized water 120 parts, catalyzer 10 parts;
(3), after Whitfield's ointment 50 parts, 20 parts, liquefied ammonia, ionized water 20 parts being mixed, heat at the temperature of 85 DEG C, obtain ammoniated solution;
(4) add in ammoniated solution catalyzer 10 parts carry out processed 4h after Primary product;
(5) 100 parts of ionized waters are added in Primary product carry out mix and blend and obtain secondary species, secondary species is added carry out in whizzer centrifugal, abandoning supernatant, throw out is carried out drying salicylic amide.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments, and therefore, the present invention is not by the restriction of the present embodiment, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (2)
1. a preparation method for efficient salicylic amide, is characterized by, and its preparation method is as follows:
(1) take starting material, described raw-material moiety is counted by weight: Whitfield's ointment 35-50 part, liquefied ammonia 10-20 part, ionized water 100-120 part, catalyzer 5-10 part;
(2), after Whitfield's ointment 35-50 part, liquefied ammonia 10-20 part, ionized water 10-20 part being mixed, heat at the temperature of 85-110 DEG C, obtain ammoniated solution;
(3) add in ammoniated solution catalyzer 12-22 part carry out processed 2-4h after Primary product;
(4) ionized water of surplus is added in Primary product carry out mix and blend and obtain secondary species, secondary species is added carry out in whizzer centrifugal, abandoning supernatant, throw out is carried out drying salicylic amide.
2. the preparation method of a kind of efficient salicylic amide as claimed in claim 1, is characterized by, and described catalyzer is one or more the combination of phospho-molybdic acid, trimethylbenzene, vinyltrimethoxy silane, zinc phosphate and ammonium chloride emphasis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511012668.9A CN105503640A (en) | 2015-12-31 | 2015-12-31 | Efficient preparation method of salicylamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511012668.9A CN105503640A (en) | 2015-12-31 | 2015-12-31 | Efficient preparation method of salicylamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105503640A true CN105503640A (en) | 2016-04-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511012668.9A Pending CN105503640A (en) | 2015-12-31 | 2015-12-31 | Efficient preparation method of salicylamide |
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| CN (1) | CN105503640A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109513427A (en) * | 2018-11-19 | 2019-03-26 | 浙江海洋大学 | A kind of preparation method of straw base chromium ion adsorbent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891645A (en) * | 2010-07-27 | 2010-11-24 | 陕西科技大学 | Method for preparing salicylamide |
| CN102807504A (en) * | 2012-09-01 | 2012-12-05 | 罗梅 | Method for synthesizing salicylamide |
-
2015
- 2015-12-31 CN CN201511012668.9A patent/CN105503640A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891645A (en) * | 2010-07-27 | 2010-11-24 | 陕西科技大学 | Method for preparing salicylamide |
| CN102807504A (en) * | 2012-09-01 | 2012-12-05 | 罗梅 | Method for synthesizing salicylamide |
Non-Patent Citations (2)
| Title |
|---|
| 许华锋: "水杨酰胺合成工艺的改进研究", 《化学工业与工程技术》 * |
| 邢其毅等: "《基础有机化学》", 30 November 1993 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109513427A (en) * | 2018-11-19 | 2019-03-26 | 浙江海洋大学 | A kind of preparation method of straw base chromium ion adsorbent |
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Application publication date: 20160420 |