CN107098809A - A kind of method for purification of high-purity sodium salicylate - Google Patents
A kind of method for purification of high-purity sodium salicylate Download PDFInfo
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- CN107098809A CN107098809A CN201710340145.XA CN201710340145A CN107098809A CN 107098809 A CN107098809 A CN 107098809A CN 201710340145 A CN201710340145 A CN 201710340145A CN 107098809 A CN107098809 A CN 107098809A
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- sodium salicylate
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- filtrate
- purity sodium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method for purification of high-purity sodium salicylate, its step is：(1) in 5000 milliliters of brown glass flasks with backflow and agitating device, it is 96% ethanol and raw material sodium salicylate and activated carbon to add volume parts, is stirred at reflux in 80~85 DEG C of heating water baths after 2 hours, is cooled to 50~60 DEG C, filtering, activated carbon is added in gained filtrate, then is heated to reflux 2 hours in 80~85 DEG C of water-baths, 50~60 DEG C are cooled to, first filtered with G4 glass filters, filtrate is collected, is then filtered again with polytetrafluoroethylene filter, filtrate is collected；(2) in brown glass flask of the filtrate injection with condensation reception device (1) above-mentioned steps collected, concentration is heated in 90~95 DEG C of water-baths to steam etoh solvent and reclaim, and when recovered solvent amount reaches 2000 milliliters, stops concentration, being cooled in room temperature, flask has mass crystallization；(3) fractional crystallization, collects mother liquor, and the crystallization separated obtains pure white high-purity sodium salicylate finished product after being dried in vacuo in 50 DEG C.
Description
Technical field
The invention belongs to chemical reagent field, especially a kind of method for purification of high-purity sodium salicylate.
Background technology
Recently as electronics, the innovation and development in each field such as new energy, new material, medication chemistry, to the chemistry on basis
Product purity requirement more and more higher, traditional technical grade chemicals can not meet the requirement of current innovative technology.Develop high-purity
Fine chemistry industry unit product turns into the important opportunity that chemicals production enterprise transformation is upgraded.
High-purity sodium salicylate is analyzed in biological medicine, chemical synthesis, nuclear material, has important use in terms of metallurgy.At present,
Document report, and the sodium salicylate purification of practical application mainly use traditional aqueous solution recrystallization means.Due to water
The light sensitivity of poplar acid sodium, oxidizable, very big etc. characteristic of solubility in water is obtained with traditional aqueous solution recrystallization method for purification
Yellow or pink can be all carried in various degree to product, and unstable product quality, yield low consumption is big.
The content of the invention
It is an object of the invention to overcome prior art deficiency there is provided a kind of steady quality, the high high-purity salicylic acid of yield
The method for purification of sodium.
The technical solution adopted by the present invention is：
A kind of method for purification of high-purity sodium salicylate, its step is：
(1) in 5000 milliliters of brown glass flasks with backflow and agitating device, addition volume parts are 96% ethanol
With raw material sodium salicylate and activated carbon, it is stirred at reflux in 80~85 DEG C of heating water baths after 2 hours, is cooled to 50~60 DEG C, use
G4 glass filters are filtered, and activated carbon is added in gained filtrate, then are heated to reflux 2 hours in 80~85 DEG C of water-baths, are cooled to
50~60 DEG C, first filtered with G4 glass filters, collect filtrate, then filtered again with polytetrafluoroethylene filter, collect filtrate；
(2) in brown glass flask of the filtrate injection with condensation reception device (1) above-mentioned steps collected, in 90~95
Heating concentration steams etoh solvent and reclaimed in DEG C water-bath, when recovered solvent amount reaches 2000 milliliters, stops concentration, cooling
To room temperature, there is mass crystallization in flask；
(3) fractional crystallization, collects mother liquor, and mother liquor is reusable.The crystallization separated is obtained after being dried in vacuo in 50 DEG C
Pure white high-purity sodium salicylate finished product.
Moreover, it is described (1) to be (3) area be 20 square metres, door and window dress dark-brown glass lucifuge, with 90 watts of low-pressure sodium lamps
Carried out in the operation room of illumination.
Moreover, step (1) in, the sodium salicylate and volume parts are that the amount ratio of 96% ethanol is 5:27(Kg/L).
Moreover, step (1) in, the amount ratio of the sodium salicylate and activated carbon is 100:1.
Moreover, step (1) in, the apertures of the G4 glass filters is 3~4 microns.
Moreover, step (1) in, the polytetrafluoroethylene filter aperture be 0.1 micron.
Advantage of the present invention and good effect are：
1. the present invention is to analyze pure chemistry reagent sodium salicylate as raw material, ethanol is solvent, the active carbon adsorption removal of impurity, warp
Cross dissolving, the activated carbon removal of impurity, filtering is concentrated and recycling design, is crystallized, separation, the step such as drying, finally it is pure white high-purity
Sodium salicylate, the particularly important is operationlocation should avoid sunlight from irradiating, and door and window uses dark-brown glass, and room lighting uses low pressure
Sodium vapor lamp, effectively prevent salicylic acid in course of reaction and changes colour, improve reaction efficiency.
2. by obtained product under the conditions of present invention process, white appearance purity is high, favorable reproducibility, steady quality, energy
The requirement of the high-end users such as scientific research institutions is met, to analyze pure chemistry reagent sodium salicylate as raw material, ethanol is solvent, activated carbon
The combination of adsorption-edulcoration matter provides good theoretical foundation for regent purification similar from now on.
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not limit
Qualitatively, it is impossible to which protection scope of the present invention is limited with this.
A kind of method for purification of high-purity sodium salicylate, its step is：
(1) in 5000 milliliters of brown glass flasks with backflow and agitating device, addition volume parts are 96% ethanol
2700 milliliters and 500 grams of raw material sodium salicylates and 5 grams of activated carbon, are stirred at reflux after 2 hours in 80~85 DEG C of heating water baths, cold
But to 50~60 DEG C, filtered with G4 glass filters (3~4 microns of aperture), 5 grams of activated carbon are added in gained filtrate, then 80
It is heated to reflux in~85 DEG C of water-baths 2 hours, is cooled to 50~60 DEG C, first filtered with G4 glass filters, collects filtrate, Ran Houzai
Filtered with 0.1 micron pore size polytetrafluoroethylene filter, collect filtrate；
(2) in brown glass flask of the filtrate injection with condensation reception device (1) above-mentioned steps collected, in 90~95
Heating concentration steams etoh solvent and reclaimed in DEG C water-bath, when recovered solvent amount reaches 2000 milliliters, stops concentration, cooling
To room temperature, there is mass crystallization in flask.
(3) fractional crystallization, collects mother liquor, and mother liquor is reusable.The crystallization separated is obtained after being dried in vacuo in 50 DEG C
Pure white high-purity sodium salicylate finished product.
It in area is 20 square metres that above steps, which is, and door and window dress dark-brown glass lucifuge is illuminated with 90 watts of low-pressure sodium lamps
Operation room in carry out.
Raw materials used sodium salicylate and activated carbon are analysis pure chemistry reagent in the present embodiment, and the ethanol of parts by volume 96% is
Pure absolute ethyl alcohol, which is analyzed, with chemical reagent adds what deionized water was voluntarily prepared.The Principles of Chemical Engineering of the present invention；Solvent is made of ethanol, it is living
Property carbon adsorption decolouring removal of impurities to sodium salicylate recrystallize purification.Operating environment lucifuge and specific illumination condition are to prevent water
Poplar acid sodium changes colour.
Although the preparation method and preparation process of the present invention have carried out illustration by preferred embodiments, person skilled can
Present invention is not being departed from, methods and techniques described herein is being modified or reconfigured in spirit and scope, is coming real
Now final technology of preparing.In particular, all similar replacements and change for a person skilled in the art
It is it will be apparent that they are considered as being included in spirit of the invention, scope and content.
Claims (6)
1. a kind of method for purification of high-purity sodium salicylate, it is characterised in that：Its step is：
(1) in 5000 milliliters of brown glass flasks with backflow and agitating device, it is 96% ethanol and original to add volume parts
Expect sodium salicylate and activated carbon, be stirred at reflux in 80~85 DEG C of heating water baths after 2 hours, be cooled to 50~60 DEG C, use G4 glass
Glass filter is filtered, and adds activated carbon in gained filtrate, then is heated to reflux 2 hours in 80~85 DEG C of water-baths, it is cooled to 50~
60 DEG C, first filtered with G4 glass filters, collect filtrate, then filtered again with polytetrafluoroethylene filter, collect filtrate；
(2) in brown glass flask of the filtrate injection with condensation reception device (1) above-mentioned steps collected, in 90~95 DEG C of water
Concentration is heated in bath to steam etoh solvent and reclaim, and when recovered solvent amount reaches 2000 milliliters, is stopped concentration, is cooled to room
There is mass crystallization in temperature, flask；
(3) fractional crystallization, collects mother liquor, and mother liquor is reusable.The crystallization separated obtains pure white after being dried in vacuo in 50 DEG C
High-purity sodium salicylate finished product.
2. the method for purification of high-purity sodium salicylate according to claim 1, it is characterised in that：It is described (1) to being (3)
It it is 20 square metres in area, door and window fills dark-brown glass lucifuge, is carried out in the operation room illuminated with 90 watts of low-pressure sodium lamps.
3. the method for purification of high-purity sodium salicylate according to claim 1, it is characterised in that：Step (1) in, it is described
Sodium salicylate is 5 with the amount ratio that volume parts are 96% ethanol:27(Kg/L).
4. the method for purification of high-purity sodium salicylate according to claim 1, it is characterised in that：Step (1) in, it is described
The amount ratio of sodium salicylate and activated carbon is 100:1.
5. the method for purification of high-purity sodium salicylate according to claim 1, it is characterised in that：Step (1) in, it is described
The aperture of G4 glass filters is 3~4 microns.
6. the method for purification of high-purity sodium salicylate according to claim 1, it is characterised in that：Step (1) in, it is described
Polytetrafluoroethylene filter aperture is 0.1 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710340145.XA CN107098809A (en) | 2017-05-15 | 2017-05-15 | A kind of method for purification of high-purity sodium salicylate |
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| CN201710340145.XA CN107098809A (en) | 2017-05-15 | 2017-05-15 | A kind of method for purification of high-purity sodium salicylate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483250A (en) * | 2019-09-05 | 2019-11-22 | 青岛科技大学 | A kind of recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing process |
| CN110642707A (en) * | 2019-10-22 | 2020-01-03 | 成都市科隆化学品有限公司 | Purification production method of low-cost environment-friendly sodium salicylate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1755362A (en) * | 1923-04-06 | 1930-04-22 | Dow Chemical Co | Method of making sodium salicylates |
| GB353921A (en) * | 1930-04-29 | 1931-07-29 | Graesser Monsanto Chemical Wor | Improvements in and relating to the production and purification of salicylic acid or?-cresotinic acid or their salts |
| EP0224420B1 (en) * | 1985-10-29 | 1990-03-21 | Rhone-Poulenc Chimie | Process for the separation and purification of salicylic acid |
| CN101143817A (en) * | 2007-10-09 | 2008-03-19 | 山东新华隆信化工有限公司 | Method for producing salicylic acid by refining salicylic acid solution |
| CN105418402A (en) * | 2015-11-30 | 2016-03-23 | 山东新华制药股份有限公司 | Production technology of salicylic acid |
-
2017
- 2017-05-15 CN CN201710340145.XA patent/CN107098809A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1755362A (en) * | 1923-04-06 | 1930-04-22 | Dow Chemical Co | Method of making sodium salicylates |
| GB353921A (en) * | 1930-04-29 | 1931-07-29 | Graesser Monsanto Chemical Wor | Improvements in and relating to the production and purification of salicylic acid or?-cresotinic acid or their salts |
| EP0224420B1 (en) * | 1985-10-29 | 1990-03-21 | Rhone-Poulenc Chimie | Process for the separation and purification of salicylic acid |
| CN101143817A (en) * | 2007-10-09 | 2008-03-19 | 山东新华隆信化工有限公司 | Method for producing salicylic acid by refining salicylic acid solution |
| CN105418402A (en) * | 2015-11-30 | 2016-03-23 | 山东新华制药股份有限公司 | Production technology of salicylic acid |
Non-Patent Citations (5)
| Title |
|---|
| 何铁林 主编: "《水处理化学品手册》", 31 May 2000, 化学工业出版社 * |
| 吴崇珍等: "水杨酸生产工艺的改进研究", 《河南科学》 * |
| 广东工业大学精细化工教研室 编: "《精细化工生产技术及应用》", 31 August 1995, 广东科技出版社 * |
| 罗明生 主编: "《药剂辅助大全》", 31 January 2006, 四川科学技术出版社 * |
| 赵士寿主编: "《药剂学选论》", 30 April 1963, 上海科学技术出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483250A (en) * | 2019-09-05 | 2019-11-22 | 青岛科技大学 | A kind of recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing process |
| CN110642707A (en) * | 2019-10-22 | 2020-01-03 | 成都市科隆化学品有限公司 | Purification production method of low-cost environment-friendly sodium salicylate |
| CN110642707B (en) * | 2019-10-22 | 2022-04-19 | 成都市科隆化学品有限公司 | Purification production method of low-cost environment-friendly sodium salicylate |
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Application publication date: 20170829 |