CN104725235A - Preparation method of methyl paraben - Google Patents

Preparation method of methyl paraben Download PDF

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Publication number
CN104725235A
CN104725235A CN201310718495.7A CN201310718495A CN104725235A CN 104725235 A CN104725235 A CN 104725235A CN 201310718495 A CN201310718495 A CN 201310718495A CN 104725235 A CN104725235 A CN 104725235A
Authority
CN
China
Prior art keywords
preparation
aluminum sulfate
methyl paraben
tegosept
sulfate hydrate
Prior art date
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.)
Pending
Application number
CN201310718495.7A
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Chinese (zh)
Inventor
郝永明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao Xiuxian Foods Co Ltd
Original Assignee
Qingdao Xiuxian Foods Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Qingdao Xiuxian Foods Co Ltd filed Critical Qingdao Xiuxian Foods Co Ltd
Priority to CN201310718495.7A priority Critical patent/CN104725235A/en
Publication of CN104725235A publication Critical patent/CN104725235A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a preparation method of methyl paraben. The preparation method comprises the following steps: 1) adding methanol and p-hydroxybenzoic acid in the molar ratio of 35: 1, as well as aluminum sulfate hydrate into a high-pressure reaction kettle, stirring and heating to 130 DEG C and reacting for 3h; and 2) adding water after the reaction, heating to evaporate out unreacted methanol, dropping a sodium hydroxide solution into remaining liquid, cooling, precipitating solids, performing suction filtration, washing and drying to obtain white powder-like methyl paraben. According to the preparation method of methyl paraben provided by the invention, aluminum sulfate hydrate is used as a catalyst, and aluminum sulfate hydrate has high catalytic activity, simple operation, no equipment corrosion, low price, no toxicity and no environmental pollution, thereby being a green catalyst.

Description

The preparation method of Tegosept M
 
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 M.
 
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, wherein Tegosept M is strong fungicide.The synthesis of Tegosept M adopts P-hydroxybenzoic acid and methyl alcohol 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 M, be catalyzer with hydrazine aluminum sulfate, catalytic activity is high, simple to operate, corrosion-free to equipment, and cheap, nontoxic, environmentally safe, is a kind of green catalyst.
The preparation method of described Tegosept M, comprises the following steps:
One, in autoclave, add methyl alcohol and P-hydroxybenzoic acid that mol ratio is 35:1, hydrazine aluminum sulfate, is heated with stirring to 130 DEG C, reaction 3h;
Two, react complete, add water, heating steams unreacted methyl alcohol, drips sodium hydroxide solution in remaining liquid, and cooling separates out solid, suction filtration, washing, dry, obtains white powder Tegosept M.
The preparation method of Tegosept M provided by the invention, its beneficial effect is, be catalyzer with hydrazine aluminum sulfate, catalytic activity is high, simple to operate, corrosion-free to equipment, and cheap, nontoxic, environmentally safe, is a kind of green catalyst.
 
Embodiment
Below in conjunction with an embodiment, the preparation method of Tegosept M provided by the invention is described in detail.
 
Embodiment
One, in autoclave, add methyl alcohol and P-hydroxybenzoic acid that mol ratio is 35:1, hydrazine aluminum sulfate, is heated with stirring to 130 DEG C, reaction 3h;
Two, react complete, add water, heating steams unreacted methyl alcohol, drips sodium hydroxide solution in remaining liquid, and cooling separates out solid, suction filtration, washing, dry, obtains white powder Tegosept M.

Claims (1)

1. a preparation method for Tegosept M, is characterized in that: it comprises the following steps:
One, in autoclave, add methyl alcohol and P-hydroxybenzoic acid that mol ratio is 35:1, hydrazine aluminum sulfate, is heated with stirring to 130 DEG C, reaction 3h;
Two, react complete, add water, heating steams unreacted methyl alcohol, drips sodium hydroxide solution in remaining liquid, and cooling separates out solid, suction filtration, washing, dry, obtains white powder Tegosept M.
CN201310718495.7A 2013-12-24 2013-12-24 Preparation method of methyl paraben Pending CN104725235A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310718495.7A CN104725235A (en) 2013-12-24 2013-12-24 Preparation method of methyl paraben

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310718495.7A CN104725235A (en) 2013-12-24 2013-12-24 Preparation method of methyl paraben

Publications (1)

Publication Number Publication Date
CN104725235A true CN104725235A (en) 2015-06-24

Family

ID=53449719

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310718495.7A Pending CN104725235A (en) 2013-12-24 2013-12-24 Preparation method of methyl paraben

Country Status (1)

Country Link
CN (1) CN104725235A (en)

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C06 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20150624