CN104725232A - Preparation method of butyl paraben - Google Patents
Preparation method of butyl paraben Download PDFInfo
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- CN104725232A CN104725232A CN201310718323.XA CN201310718323A CN104725232A CN 104725232 A CN104725232 A CN 104725232A CN 201310718323 A CN201310718323 A CN 201310718323A CN 104725232 A CN104725232 A CN 104725232A
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- China
- Prior art keywords
- water
- preparation
- drying
- cooling
- butyl paraben
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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)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of butyl paraben, which comprises the following steps: 1. adding para-hydroxybenzoic acid, n-butanol and sodium bisulfate into a three-neck flask provided with a water separator, a thermometer and a reflux condensation tube, and heating under reflux for 5 hours; and 2. after the reaction finishes, discharging the water layer and n-butanol in the water separator, washing the crude product respectively with water, a sodium carbonate solution, a saturated saline solution, drying, distilling, recovering the n-butanol, cooling, adding water, shaking, cooling, precipitating a white product, carrying out vacuum filtration, and drying to obtain the finished product butyl paraben. By using the sodium bisulfate instead of the liquid sulfuric acid to catalyze the synthesis of butyl paraben, the preparation method is simple to operate, and has the advantages of accessible raw materials, no corrosiveness for equipment and no environment pollution. The sodium bisulfate is a green catalyst.
Description
Technical field
The present invention relates to a kind of preparation method of sanitas, be specifically related to a kind of preparation method of Tegosept B.
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, be widely used in the aspects such as daily use chemicals, medicine, food, feed and various industrial antisepsis, in parabens, the anti-corrosive antibacterial effect of butyl ester is the strongest.The synthesis of nipagin esters adopts P-hydroxybenzoic acid and butanols 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 preparation method of Tegosept B, replace fluid sulphuric acid to catalyze and synthesize nipagin esters with sodium pyrosulfate, simple to operate, raw material is easy to get, corrosion-free to equipment, environmentally safe, is a kind of green catalyst.
The preparation method of described Tegosept B, comprises the following steps:
One, in the there-necked flask that water trap, thermometer and reflux condensing tube are housed, P-hydroxybenzoic acid, propyl carbinol and sodium pyrosulfate is added, reflux 5h;
Two, react complete, release the propyl carbinol in water layer and water trap, by thick product respectively through water, sodium carbonate solution, saturated common salt water washing, distill after drying, reclaim propyl carbinol, add water after cooling and carry out shaking, cooling, separate out white products, again through suction filtration, drying, get product Tegosept B.
The preparation method of Tegosept B provided by the invention, its beneficial effect is, replace fluid sulphuric acid to catalyze and synthesize nipagin esters with sodium pyrosulfate, simple to operate, raw material is easy to get, corrosion-free to equipment, environmentally safe, is a kind of green catalyst.
Embodiment
Below in conjunction with an embodiment, the preparation method of Tegosept B provided by the invention is described in detail.
Embodiment
One, in the there-necked flask that water trap, thermometer and reflux condensing tube are housed, P-hydroxybenzoic acid, propyl carbinol and sodium pyrosulfate is added, reflux 5h;
Two, react complete, release the propyl carbinol in water layer and water trap, by thick product respectively through water, sodium carbonate solution, saturated common salt water washing, distill after drying, reclaim propyl carbinol, add water after cooling and carry out shaking, cooling, separate out white products, again through suction filtration, drying, get product Tegosept B.
Claims (1)
1. a preparation method for Tegosept B, is characterized in that: it comprises the following steps:
One, in the there-necked flask that water trap, thermometer and reflux condensing tube are housed, P-hydroxybenzoic acid, propyl carbinol and sodium pyrosulfate is added, reflux 5h;
Two, react complete, release the propyl carbinol in water layer and water trap, by thick product respectively through water, sodium carbonate solution, saturated common salt water washing, distill after drying, reclaim propyl carbinol, add water after cooling and carry out shaking, cooling, separate out white products, again through suction filtration, drying, get product Tegosept B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310718323.XA CN104725232A (en) | 2013-12-24 | 2013-12-24 | Preparation method of butyl paraben |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310718323.XA CN104725232A (en) | 2013-12-24 | 2013-12-24 | Preparation method of butyl paraben |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104725232A true CN104725232A (en) | 2015-06-24 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310718323.XA Pending CN104725232A (en) | 2013-12-24 | 2013-12-24 | Preparation method of butyl paraben |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104725232A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518671A (en) * | 2016-11-09 | 2017-03-22 | 山东益丰生化环保股份有限公司 | Preparation method of butylparaben |
-
2013
- 2013-12-24 CN CN201310718323.XA patent/CN104725232A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518671A (en) * | 2016-11-09 | 2017-03-22 | 山东益丰生化环保股份有限公司 | Preparation method of butylparaben |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150624 |
|
| WD01 | Invention patent application deemed withdrawn after publication |