CN104744259A - Method for synthesizing ethylparaben by catalysis of chitosan sulfate - Google Patents
Method for synthesizing ethylparaben by catalysis of chitosan sulfate Download PDFInfo
- Publication number
- CN104744259A CN104744259A CN201310722718.7A CN201310722718A CN104744259A CN 104744259 A CN104744259 A CN 104744259A CN 201310722718 A CN201310722718 A CN 201310722718A CN 104744259 A CN104744259 A CN 104744259A
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- CN
- China
- Prior art keywords
- chitosan sulfate
- ethylparaben
- ethyl
- water
- catalysis
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- 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.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a method for synthesizing ethylparaben by catalysis of chitosan sulfate, which comprises the following steps: 1)adding p-hydroxybenzoic acid, absolute ethyl alcohol, chitosan sulfate and a water carrying agent cyclohexane in a 3 mouth flask, heating and backflowing for water distribution; 2)completing esterification, stopping stirring, filtering while hot; and 3)distilling to obtain ethanol and cyclohexane, dumping the residue in cold water, after completely precipitating ethylparaben, performing pumping filtration and drying to obtain a crude product, and performing recrystallization by ethanol to obtain the refined product. According to the method provided in the invention, the chitosan sulfate is the novel solid acid salt catalyst, and has the advantages that catalytic activity is high, usage amount is little, selectivity is good, generation of side effect is reduced, product yield is high, post-treatment is simple and convenient, continuous catalysis performance is stable, equipment corrosion is prevented, waste liquid discharge is greatly reduced, no environment pollution is generated, and the method is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of sanitas, be specifically related to a kind of method that Chitosan Sulfate catalyzes and synthesizes ethyl p-hydroxybenzoate.
Background technology
Nipagin esters is also called para hydroxybenzene potassium acid esters, is the series of anticorrosion agent that purposes is the widest in the world, consumption is maximum, applying frequency is the highest at present.The advantages such as it has efficiently, low toxicity, spectrum, easily compatibility, are widely used in the aspects such as daily use chemicals, medicine, food, feed and various industrial antisepsis.The synthesis of ethyl p-hydroxybenzoate adopts P-hydroxybenzoic acid and ethanol directly to prepare under vitriol oil effect usually, but sulfuric acid has serious corrodibility, easily side reaction and contaminate environment occurs.
Summary of the invention
The object of the invention is to, provide a kind of Chitosan Sulfate to catalyze and synthesize the method for ethyl p-hydroxybenzoate, Chitosan Sulfate is a kind of solid acid salt catalyst of novelty, catalytic activity is high, and consumption is few, and selectivity is good, the generation of side reaction can be reduced, product yield is high, and aftertreatment is simple and convenient, continuous catalysis stable performance, prevent equipment corrosion, greatly reduce the discharge of waste liquid, environmentally safe, be applicable to suitability for industrialized production.
Described Chitosan Sulfate catalyzes and synthesizes the method for ethyl p-hydroxybenzoate, comprises the following steps:
One, in there-necked flask, add P-hydroxybenzoic acid, dehydrated alcohol, Chitosan Sulfate and water entrainer hexanaphthene, reflux divides water;
Two, esterification is complete, stops stirring, and filtered while hot reclaims catalyzer;
Three, steam ethanol and hexanaphthene, in residuum impouring cold water, after ethyl p-hydroxybenzoate is separated out completely, suction filtration is dry obtains crude product, obtains fine work with ethyl alcohol recrystallization.
Chitosan Sulfate provided by the invention catalyzes and synthesizes the method for ethyl p-hydroxybenzoate, and its beneficial effect is, Chitosan Sulfate is a kind of solid acid salt catalyst of novelty, catalytic activity is high, and consumption is few, and selectivity is good, the generation of side reaction can be reduced, product yield is high, and aftertreatment is simple and convenient, continuous catalysis stable performance, prevent equipment corrosion, greatly reduce the discharge of waste liquid, environmentally safe, be applicable to suitability for industrialized production.
Embodiment
Below in conjunction with an embodiment, method Chitosan Sulfate provided by the invention being catalyzed and synthesized to ethyl p-hydroxybenzoate is described in detail.
Embodiment
One, in there-necked flask, add P-hydroxybenzoic acid, dehydrated alcohol, Chitosan Sulfate and water entrainer hexanaphthene, reflux divides water;
Two, esterification is complete, stops stirring, and filtered while hot reclaims catalyzer;
Three, steam ethanol and hexanaphthene, in residuum impouring cold water, after ethyl p-hydroxybenzoate is separated out completely, suction filtration is dry obtains crude product, obtains fine work with ethyl alcohol recrystallization.
Claims (1)
1. Chitosan Sulfate catalyzes and synthesizes a method for ethyl p-hydroxybenzoate, it is characterized in that: it comprises the following steps:
One, in there-necked flask, add P-hydroxybenzoic acid, dehydrated alcohol, Chitosan Sulfate and water entrainer hexanaphthene, reflux divides water;
Two, esterification is complete, stops stirring, and filtered while hot reclaims catalyzer;
Three, steam ethanol and hexanaphthene, in residuum impouring cold water, after ethyl p-hydroxybenzoate is separated out completely, suction filtration is dry obtains crude product, obtains fine work with ethyl alcohol recrystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310722718.7A CN104744259A (en) | 2013-12-25 | 2013-12-25 | Method for synthesizing ethylparaben by catalysis of chitosan sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310722718.7A CN104744259A (en) | 2013-12-25 | 2013-12-25 | Method for synthesizing ethylparaben by catalysis of chitosan sulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104744259A true CN104744259A (en) | 2015-07-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310722718.7A Pending CN104744259A (en) | 2013-12-25 | 2013-12-25 | Method for synthesizing ethylparaben by catalysis of chitosan sulfate |
Country Status (1)
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| CN (1) | CN104744259A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970557A (en) * | 2019-03-26 | 2019-07-05 | 陕西科技大学 | A method of preparing paraben esters |
-
2013
- 2013-12-25 CN CN201310722718.7A patent/CN104744259A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970557A (en) * | 2019-03-26 | 2019-07-05 | 陕西科技大学 | A method of preparing paraben esters |
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Legal Events
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150701 |
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| WD01 | Invention patent application deemed withdrawn after publication |