CN102408319A - Production process of p-hydroxyanisole - Google Patents
Production process of p-hydroxyanisole Download PDFInfo
- Publication number
- CN102408319A CN102408319A CN2010102874100A CN201010287410A CN102408319A CN 102408319 A CN102408319 A CN 102408319A CN 2010102874100 A CN2010102874100 A CN 2010102874100A CN 201010287410 A CN201010287410 A CN 201010287410A CN 102408319 A CN102408319 A CN 102408319A
- Authority
- CN
- China
- Prior art keywords
- production process
- sulfuric acid
- water
- hydroxyanisole
- mehq
- 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
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production process of p-hydroxyanisole. The production process mainly comprises the following four steps of: etherification; distillation; extraction; and depressurization and rectification, and is characterized in that the etherification procedure comprises the following steps of: sequentially adding sulfuric acid, water and methanol to a reaction kettle, and then evenly stirring; adding hydroquinone, heating to 50-55 DEG C and controlling the pressure at 0.1 to -0.2 Mpa for reacting for 6 hours; and then cooling to below 30 DEG C, slowly adding a sodium hydroxide solution with the concentration of 30%, neutralizing the solution until the pH value is 7, and finally filtering out sodium sulfate. In the production process, a methanol method is selected as a synthetic route; compared with the traditional dimethyl sulfate method, the methanol method has the advantages of high total yield up to 93%, high conversion rate up to 98%, low cost, high quality and the like; and in addition, the p-hydroxyanisole can be produced without season influence, thus enhancing market competitiveness.
Description
Technical field
The present invention relates to a kind of production technique of MEHQ, specifically is that a kind of production technique that adopts etherificate, distillation, extraction, rectification under vacuum four steps to form makes.
Background technology
MEHQ can be used for synthetic fine chemicals, as the stopper of vinyl-type plastic monomer, and ultraviolet inhibitor, dyestuff intermediate and be used for the inhibitor etc. of synthesised food, grease and makeup.At home and abroad all have than big market.
The physico-chemical property of this product and quality index
These article are white shape or wax shape xln, 52.5 ℃ of fusing points, and 243 ℃ of boiling points, specific density 1.55 is soluble in alcohol, ether, benzene and ETHYLE ACETATE, is slightly soluble in water, and these article are packed through interior lining paper bucket, are stored in shady and cool dry place.
Summary of the invention
Main task of the present invention is to provide a kind of production technique of MEHQ, specifically is that a kind of total yield can reach 93%, and transformation efficiency reaches the production technique of 98% MEHQ.
In order to solve above technical problem, the production technique of a kind of MEHQ of the present invention mainly is made up of etherificate, distillation, extraction, rectification under vacuum four steps; It is characterized in that: said etherificate operation is: with sulfuric acid, water, methyl alcohol add successively stir in the reaction kettle after, add Resorcinol, be warmed up to 50～55 ℃; Pressure-controlling is 0.1---0.2Mpa; Reacted 6 hours, and cooled to then below 30 ℃, slowly add 30% sodium hydroxide solution; The pH that neutralizes is 7, removes by filter sodium sulfate.
Further, said sulfuric acid: water: the volume ratio of methyl alcohol is: 1: 5---10: 2---5
Further, said sulfuric acid, water, methanol mixed solution: the volume ratio of Resorcinol is: 1: 0.2---0.5.
The invention has the advantages that: this synthetic route is selected the methyl alcohol method for use, and this method and traditional methyl-sulfate method relatively have the yield height, and cost is low, the quality advantages of higher; Total yield can reach 93%, and transformation efficiency reaches 98%.And produce the characteristics that do not receive seasonal effect, make this project have more the market competitiveness.
Embodiment
Embodiment
99% methyl alcohol 188.69kg; 98% sulfuric acid 204.8kg; Water 700kg; Add successively stir in the reaction kettle after, add 99% Resorcinol, 476.93kg; Be warmed up to 50～55 ℃, pressure-controlling is 0.1---and 0.2Mpa, reacted 6 hours; Cool to then below 30 ℃; The sodium hydroxide solution 544.23kg of slow adding 30%, the pH that neutralizes is 7, removes by filter sodium sulfate.99% finished product 500kg, MEHQ 495kg wherein, impurity 1.0kg, water 4kg.
Claims (3)
1. the production technique of a MEHQ mainly is made up of etherificate, distillation, extraction, rectification under vacuum four steps, and it is characterized in that: said etherificate operation is: with sulfuric acid, water, methyl alcohol add successively stir in the reaction kettle after; Add Resorcinol, be warmed up to 50～55 ℃, pressure-controlling is 0.1---0.2Mpa; Reacted 6 hours, and cooled to then below 30 ℃, slowly add 30% sodium hydroxide solution; The pH that neutralizes is 7, removes by filter sodium sulfate.
2. the production technique of a kind of MEHQ according to claim 1, it is characterized in that: said sulfuric acid: water: the volume ratio of methyl alcohol is: 1: 5---10: 2---5.
3. the production technique of a kind of MEHQ according to claim 1, it is characterized in that: said sulfuric acid, water, methanol mixed solution: the volume ratio of Resorcinol is: 1: 0.2---0.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102874100A CN102408319A (en) | 2010-09-20 | 2010-09-20 | Production process of p-hydroxyanisole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102874100A CN102408319A (en) | 2010-09-20 | 2010-09-20 | Production process of p-hydroxyanisole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102408319A true CN102408319A (en) | 2012-04-11 |
Family
ID=45910712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102874100A Pending CN102408319A (en) | 2010-09-20 | 2010-09-20 | Production process of p-hydroxyanisole |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102408319A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104292082A (en) * | 2014-09-05 | 2015-01-21 | 中国科学院青岛生物能源与过程研究所 | Preparation method for hydroquinone monoether compound |
| CN107694762A (en) * | 2017-11-10 | 2018-02-16 | 中南大学 | A kind of composition and method for floating of the flotation collecting rutile from ore |
| CN108314609A (en) * | 2018-01-03 | 2018-07-24 | 兄弟科技股份有限公司 | A kind of synthetic method of butylated hydroxy anisole |
-
2010
- 2010-09-20 CN CN2010102874100A patent/CN102408319A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104292082A (en) * | 2014-09-05 | 2015-01-21 | 中国科学院青岛生物能源与过程研究所 | Preparation method for hydroquinone monoether compound |
| CN107694762A (en) * | 2017-11-10 | 2018-02-16 | 中南大学 | A kind of composition and method for floating of the flotation collecting rutile from ore |
| CN107694762B (en) * | 2017-11-10 | 2019-07-02 | 中南大学 | A kind of composition and method for floating of the flotation collecting rutile from ore |
| CN108314609A (en) * | 2018-01-03 | 2018-07-24 | 兄弟科技股份有限公司 | A kind of synthetic method of butylated hydroxy anisole |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105236798A (en) | Preparation method of naphthalene-series water reducing agent | |
| CN106674244A (en) | Preparation method of cineole | |
| CN102408319A (en) | Production process of p-hydroxyanisole | |
| CN105237338A (en) | System and method for continuously synthesizing high-purity 3-chloro-1,2-propylene glycol | |
| CN102976897A (en) | Method for purifying tetrafluoro propanol | |
| CN103804125A (en) | Method for preparing policosanol through insect wax pressure reduction method | |
| CN115947915A (en) | Preparation method of vegetable oil-based polyurethane resin | |
| CN102515613A (en) | Method for preparing naphthalene based superplasticizer by using refined naphthalene by-product 90 naphthalene | |
| CN103304411B (en) | Preparation method of malonic ester | |
| CN103145562B (en) | N-ethyl aniline preparation method | |
| CN103721749B (en) | Avoid composite catalyst and the application thereof of fouling in production of biodiesel | |
| CN105985215A (en) | Cracking system for preparing high-purity isobutene from propylene glycol tert-butyl ether | |
| CN105732312B (en) | A kind of overcritical Hydrogenation of sec-Butyl Acetate for sec-butyl alcohol co-producing ethanol method | |
| CN101712599A (en) | Method for preparing allyl pentaerythritol | |
| CN204589030U (en) | A kind of cracking system utilizing propylene glycol t-butyl ether high purity iso-butylene | |
| CN113563155B (en) | Bromopropene synthesis method | |
| CN101712596A (en) | Method for preparing trimethylolpropane allyl ether | |
| CN102888282B (en) | Low-energy consumption production process for biodiesel | |
| CN101607903A (en) | A kind of preparation method of methoxyethyl acrylate | |
| CN102206143B (en) | Preparation method for intermediate product 2-naphthyl methyl ether of 6-methoxy-2-acetonaphthone | |
| CN110857270B (en) | High-content conjugated linoleic acid triglyceride and preparation method thereof | |
| CN106279562B (en) | A kind of synthesis technology of polycarboxylate water-reducer | |
| CN101712598A (en) | Method for preparing trimethylolpropane allyl ether | |
| CN112812026A (en) | Method for producing N, N-diethylamino isopropanol | |
| CN109053378A (en) | A method of preparing dihydromyrcenol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120411 |