CN104292076A - Production method of butenediol diacetate - Google Patents
Production method of butenediol diacetate Download PDFInfo
- Publication number
- CN104292076A CN104292076A CN201410531814.8A CN201410531814A CN104292076A CN 104292076 A CN104292076 A CN 104292076A CN 201410531814 A CN201410531814 A CN 201410531814A CN 104292076 A CN104292076 A CN 104292076A
- Authority
- CN
- China
- Prior art keywords
- butylene glycol
- acetic acid
- butenediol
- production
- glycol esters
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/095—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of organic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a production method of butenediol diacetate, which comprises the following steps: carrying out catalytic hydrolysis by using butenediol diacetate, water and a catalyst in an intermittent reaction kettle, wherein the mole ratio of the butenediol diacetate to the water is (1:12)-(1:24.5); in the process of reaction, keeping a system at normal pressure and room temperature; and continuously stir, and slowly feeding trace oxygen-nitrogen mixed gas, wherein the oxygen-nitrogen ratio of the oxygen-nitrogen mixed gas is 1:8, and the feeding speed is 20-35 ml/min.m<3>. According to the invention, butenediol is greenly synthesized by hydrolyzing mixed preparations such as sodium hydrogen sulfate and sodium acetate at normal pressure and room temperature, so that less reaction wastes are produced, and easily disposed, less polymers are produced, butenediol diacetate is synthesized in one step, and the method is good in operating condition, low in production cost, less in investment of production, and high in product conversion rate, and therefore, the method has good production convenience.
Description
Technical field
The present invention relates to a kind of production method of two acetic acid butylene glycol esters.
Background technology
Two acetic acid butylene glycol esters are the key intermediates producing BDO suitability for industrialized production, and its product butylene glycol directly processed can be used for the multiple technologies fields such as medication chemistry.Original butylene glycol often adopts the addition of acetylene formaldehyde, adopts selective catalytic hydrogenation, obtains target product butylene glycol.Owing to adopting acetylene method process for processing, therefore this production line environmental pollution is large, and waste is many, is more and more unfavorable for the demand of the present green environment of China, the manufacture technology finding a kind of convenient cheapness, particularly eco-friendly butylene glycol becomes one of focus of our concern.
Adopt 2-butylene method process for processing 1, the production technology scheme of 4-butyleneglycol, there is environmental friendliness, production technology is reliable and secure, low in investment cost, the prices of raw and semifnished materials are competitive, becoming people and accelerating 1,4-butyleneglycol industrial structure change adjusts, and particularly opens up the industrial technology scheme of Chinese's independent development.
Mainly divinyl and acetic acid, oxygen chemical combination obtain in the source of two acetic acid butylene glycol esters, report is rarely had to the hydrolysis of diacetate butylene glycol both at home and abroad, this is mainly because two acetic acid butylene glycols are acid or aqueous conditions hydrolysis all can exist some polymkeric substance or etherification product, impurity in products is higher, the follow-up refining difficulty of crude product is larger, for addressing these problems, develop new technology for hydrolyzing and method for hydrolysis, the two acetic acid butylene glycol Ester hydrolysis problems that solve just seem particularly important.
Summary of the invention
The technology of the present invention is the deficiency in order to solve background technology, provides a kind of two acetic acid butylene glycol Ester hydrolysis production technology synthetic methods of improvement, thoroughly to solve all technical problems occurred in original acetic ester hydrolysis production process.
The object of the invention is to realize as follows: a kind of production method of two acetic acid butylene glycol esters, comprises the following steps:
A, two acetic acid butylene glycol esters, water, catalyst is utilized to be hydrolyzed, adopt batch reactor, the wherein mol ratio 1:12-1:24.5 of two acetic acid butylene glycol esters and water, holder series normal temperature normal pressure in reaction process, Keep agitation, and slowly pass into trace oxygen nitrogen mixed gas, wherein oxygen nitrogen is than being 1:8, passes into speed 20-35ml/min.m3;
The system that catalyzes and synthesizes in B, steps A is:
The blended solid of sodium pyrosulfate and sodium-acetate, wherein sodium pyrosulfate and sodium-acetate mol ratio are 1:4-1:8;
Further prioritization scheme is, the production method of above-mentioned a kind of two acetic acid butylene glycol esters, adopts the catalyzer described in step B, and consumption, to add acetic ester quality, 3-6%, reacts 3-5 hour.
Advantage of the present invention: the present invention adopts mixed preparation sodium pyrosulfate and sodium-acetate, under normal temperature and pressure conditions, hydrolysis green syt butylene glycol, reaction waste is few, and be easy to process, polymkeric substance is few, one-step synthesis, and operational condition is good, low production cost, investment of production is few, and product yield is high, has good production convenience.
embodiment:
A production method for two acetic acid butylene glycol esters, comprises the following steps:
A, two acetic acid butylene glycol esters, water, catalyst is utilized to be hydrolyzed, adopt batch reactor, the wherein mol ratio 1:12-1:24.5 of two acetic acid butylene glycol esters and water, holder series normal temperature normal pressure in reaction process, Keep agitation, and slowly pass into trace oxygen nitrogen mixed gas, wherein oxygen nitrogen is than being 1:8, passes into speed 20-35ml/min.m3;
The system that catalyzes and synthesizes in B, steps A is:
The blended solid of sodium pyrosulfate and sodium-acetate, wherein sodium pyrosulfate and sodium-acetate mol ratio are 1:4-1:8; Adopt the catalyzer described in step B, consumption, to add acetic ester quality, 3-6%, reacts 3-5 hour.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. a production method for two acetic acid butylene glycol esters, comprises the following steps:
A, two acetic acid butylene glycol esters, water, catalyst is utilized to be hydrolyzed, adopt batch reactor, the wherein mol ratio 1:12-1:24.5 of two acetic acid butylene glycol esters and water, holder series normal temperature normal pressure in reaction process, Keep agitation, and slowly pass into trace oxygen nitrogen mixed gas, wherein oxygen nitrogen is than being 1:8, passes into speed 20-35ml/min.m3;
The system that catalyzes and synthesizes in B, steps A is:
The blended solid of sodium pyrosulfate and sodium-acetate, wherein sodium pyrosulfate and sodium-acetate mol ratio are 1:4-1:8.
2. the production method of a kind of two acetic acid butylene glycol esters according to claim 1, is characterized in that: adopt the catalyzer described in step B, and consumption, to add acetic ester quality, 3-6%, reacts 3-5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410531814.8A CN104292076A (en) | 2014-10-11 | 2014-10-11 | Production method of butenediol diacetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410531814.8A CN104292076A (en) | 2014-10-11 | 2014-10-11 | Production method of butenediol diacetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104292076A true CN104292076A (en) | 2015-01-21 |
Family
ID=52312069
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410531814.8A Pending CN104292076A (en) | 2014-10-11 | 2014-10-11 | Production method of butenediol diacetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104292076A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1368505A (en) * | 1972-01-03 | 1974-09-25 | Kuraray Co | Preparation of 1,4-diacyloxy-2-butene |
| US4062900A (en) * | 1975-08-07 | 1977-12-13 | Mitsubishi Chemical Industries Limited | Process for preparing butanediol and/or butenediol |
| GB1560694A (en) * | 1975-10-06 | 1980-02-06 | Mitsubishi Chem Ind | Process for producing butanediol or butenediol |
| CN102834370A (en) * | 2010-02-16 | 2012-12-19 | 株式会社Api | Method for producing 1-amino-1-alkoxycarbonyl-2-vinylcyclopropane |
-
2014
- 2014-10-11 CN CN201410531814.8A patent/CN104292076A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1368505A (en) * | 1972-01-03 | 1974-09-25 | Kuraray Co | Preparation of 1,4-diacyloxy-2-butene |
| US4062900A (en) * | 1975-08-07 | 1977-12-13 | Mitsubishi Chemical Industries Limited | Process for preparing butanediol and/or butenediol |
| GB1560694A (en) * | 1975-10-06 | 1980-02-06 | Mitsubishi Chem Ind | Process for producing butanediol or butenediol |
| CN102834370A (en) * | 2010-02-16 | 2012-12-19 | 株式会社Api | Method for producing 1-amino-1-alkoxycarbonyl-2-vinylcyclopropane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106349010B (en) | A method of producing cyclohexanol | |
| CN101092407B (en) | Method for preparing alpha - acetyl - gamma - butyrolactone | |
| CN110483268A (en) | A kind of method that heteropoly acid catalysis microcrystalline cellulose prepares levulic acid | |
| CN107814939B (en) | Method for synthesizing poly (ethylene glycol methyl phosphonate) by metal oxide catalysis | |
| CN104072565A (en) | High-yield simple preparation method of 17alpha-hydroxy progesterone | |
| WO2013023257A8 (en) | Oxidative catalytic process for the synthesis of lactic acid | |
| CN110833844A (en) | Application of cobalt carbonate in preparation of acetophenone by molecular oxygen solvent-free catalytic oxidation of ethylbenzene | |
| CN111825549B (en) | Synthesis method of n-butyl glycolate | |
| CN113509947A (en) | Catalyst for synthesizing p-methyl anisole and preparation method and application thereof | |
| CN105037083A (en) | Method for preparing butendiol diacetate | |
| CN104292076A (en) | Production method of butenediol diacetate | |
| CN105348319A (en) | Titanium butanediol and preparation method thereof | |
| CN104311404A (en) | Method for producing cinnamyl aldehyde | |
| CN104277027A (en) | Preparation method of (R)-propylene carbonate | |
| CN111233802B (en) | Preparation method of furoate | |
| CN109574843A (en) | The method for producing glyoxylic ester | |
| CN102731250A (en) | Method for synthesizing sec-butyl alcohol | |
| CN102643177B (en) | Preparation method of aromatic hydrofluoroethers | |
| CN112624915A (en) | Method for preparing 2, 5-dihydroxyterephthalic acid (DHTA) | |
| CN101230054A (en) | Preparation method of alpha-acetyl-gamma-butyrolactone | |
| CN102731335B (en) | A kind of post-treating method of oxalate hydrogenation liquid | |
| CN103232325A (en) | Method for preparing cyclohexanol from cyclohexene | |
| CN114539026B (en) | Method for synthesizing 1, 2-pentanediol by using ethanol and 1, 2-propanediol as raw materials | |
| CN106946697A (en) | A kind of method for synthesizing trioctyl trimellitate (TOTM) | |
| CN103506140B (en) | Lactic acid catalyst for synthesizing and synthetic method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150121 |