CN102249911A - Preparation method of bis(2-ethylhexyl)sebacate - Google Patents
Preparation method of bis(2-ethylhexyl)sebacate Download PDFInfo
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- CN102249911A CN102249911A CN2011102230023A CN201110223002A CN102249911A CN 102249911 A CN102249911 A CN 102249911A CN 2011102230023 A CN2011102230023 A CN 2011102230023A CN 201110223002 A CN201110223002 A CN 201110223002A CN 102249911 A CN102249911 A CN 102249911A
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- herbaceous plants
- big flowers
- certain herbaceous
- flowers diacid
- ethylhexyl
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Abstract
The invention relates to a preparation method of bis(2-ethylhexyl)sebacate. In the method, the bis(2-ethylhexyl)sebacate product is obtained by esterification, washing, dealcoholization, refinement and filtration. According to the invention, a refining agent is added in the process of preparing bis(2-ethylhexyl)sebacate, so that the obtained product bis(2-ethylhexyl)sebacate is light in color, can be sold as a product in no need of high vacuum refinement and completely meets technical index requirements. The preparation method is convenient to achieve the industrial production and improve the production efficiency; the high vacuum refinement step is omitted during the production, and high vacuum pump equipment is not input, thereby saving equipment investment, reducing production cost and improving the market competitiveness of the product.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls.
Background technology
Certain herbaceous plants with big flowers diacid two 2-ethylhexyls are good low temperature softening agent of polyvinyl chloride, polystyrene, soluble cotton, ethyl cellulose.The plasticizing efficiency height can be given good low-temperature pliability of goods and photostabilization.But volatility is bigger, and water tolerance, resistance to migration and electrical insulating property are relatively poor.
In plastics industry and war production, certain herbaceous plants with big flowers diacid two 2-ethylhexyls have more and more widely application as a kind of important organic compound and cold resistant plasticizer.The common production method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls is direct esterification reactions, the color that obtains product is for yellow, be difficult to sell as product, must carry out further refining, the refinement treatment that promptly reduces pressure step, the problem that this type of preparation method exists: (1) is owing to needing to use expensive high-vacuum pump to realize in the decompression refinement treatment step, therefore, there is the problem that production unit is many, expense is high in this method, thereby is difficult to reduce cost; (2) because decompression refinement treatment step is to produce essential and very consuming time production stage in the certain herbaceous plants with big flowers diacid two 2-ethylhexyl processes, therefore, there is the problem that the production time is long, production efficiency is low in this method, is unfavorable for the raising of business economic benefit.
By retrieval, do not find the patent documentation relevant with this patent.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, the synthetic method of the certain herbaceous plants with big flowers diacid two 2-ethylhexyls that provide a kind of and can save facility investment, reduce cost, production efficiency are high.
The present invention realizes that the technical scheme of purpose is as follows:
A kind of preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls the steps include:
(1) esterification: with the certain herbaceous plants with big flowers diacid, 2-Ethylhexyl Alcohol, the vitriol oil drop in the reactor, under the micro-vacuum condition, stir, and are heated to boiling reaction, keep the boiling reflux state, after not having moisture to generate, stop heating, treat mixed solution naturally cooling in the still;
(2) washing: will add water in the mixture after the esterification, after stirring, standing demix is removed water layer wherein;
(3) dealcoholysis: the mixture after will washing, dealcoholysis obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl crude products;
(4) refining: as will to add finishing agent in the crude product after the dealcoholysis, stir 1～3h;
(5) filter: the mixed solution after will making with extra care filters, and obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl products,
Described finishing agent is that yellow soda ash, calcium oxide, magnesium oxide, gac, diatomite mix, and its weight ratio is a yellow soda ash: calcium oxide: magnesium oxide: gac: diatomite=0.2: 1: 1: 2: 1.
And the weight ratio of described certain herbaceous plants with big flowers diacid and finishing agent is 1: 0.003～0.008.
And, described certain herbaceous plants with big flowers diacid, 2-Ethylhexyl Alcohol, the weight ratio of the vitriol oil is the certain herbaceous plants with big flowers diacid: 2-Ethylhexyl Alcohol: the vitriol oil=1: 2.2: 0.002～0.005.
And the weight ratio of described certain herbaceous plants with big flowers diacid and water is 2: 1.
And described reactor is the encloses container that has agitator, heating unit and backwater condensing works.
Advantage of the present invention and positively effect are:
1, the present invention adds finishing agent (yellow soda ash, calcium oxide, magnesium oxide, gac, diatomite mixture) in preparation certain herbaceous plants with big flowers diacid two 2-ethylhexyl processes, make the product colour that obtains more shallow, do not need the high vacuum refinement treatment promptly to can be used as product and sell, and meet the technical requirements fully.
2, the finishing agent that uses among the present invention is calcium oxide, magnesium oxide, gac, diatomite mixture, have cheap, the characteristics that are easy to purchase, quality product and prolonged storage stability have been guaranteed simultaneously, the preparation method realizes simply, easy to operate, saved investment in production equipment, improved production efficiency.
3, the present invention is convenient to realize suitability for industrialized production, enhance productivity, owing to when producing, saved the high vacuum purification step, and the input of no high-vacuum pump equipment, thus facility investment saved, reduce production costs, improved the competitiveness of product in market.
Embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls the steps include:
(1) step of esterification: have heating unit, the electricity stirring to one, drop into certain herbaceous plants with big flowers diacid double centner successively in 300 liters of reactors of thermometer water circulation condenser and vacuum oil water separator, 160 kilograms of 2-Ethylhexyl Alcohols, 0.3 kilogram of the vitriol oil, under agitation, micro-vacuum is heated to boiling reaction simultaneously, keeps the boiling reflux state, constantly from water-and-oil separator, water sepn is gone out, after not having moisture to generate, stop heating, esterification stops.
(2) water-washing step: obtain to such an extent that add 50 kg water in the mixed solution after esterification, after stirring, standing demix is removed water layer wherein.
(3) dealcoholysis step: the mixture after will washing, dealcoholysis obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl crude products.
(4) purification step: add 0.5 kilogram of finishing agent (yellow soda ash, calcium oxide, magnesium oxide, gac, diatomite mixture were by 0.2: 1: 1: 2: 1 weight ratio mixes) in the crude product after dealcoholysis, mixed 1 hour.
(5) filtration step: refined mixed solution is filtered, and the liquid that obtains is certain herbaceous plants with big flowers diacid two 2-ethylhexyl finished products, these certain herbaceous plants with big flowers diacid two 2-ethylhexyl content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 2
A kind of preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls the steps include:
(1) step of esterification: have heating unit to one, electricity stirs, and drops into certain herbaceous plants with big flowers diacid double centner successively in 300 liters of reactors of thermometer water circulation condenser and water-and-oil separator, 160 kilograms of 2-Ethylhexyl Alcohols, 0.3 kilogram of the vitriol oil, under agitation, micro-vacuum, be heated to boiling reaction simultaneously, keep the boiling reflux state, constantly from water-and-oil separator, water sepn is gone out, after not having moisture to generate, stop heating, esterification stops.
(2) water-washing step: obtain to such an extent that add 50 kg water in the mixed solution after esterification, after stirring, standing demix is removed water layer wherein.
(3) dealcoholysis step: the mixture after will washing, dealcoholysis obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl crude products.
(4) purification step: add 0.6 kilogram of finishing agent (yellow soda ash, calcium oxide, magnesium oxide, gac, diatomite mixture were by 0.2: 1: 1: 2: 1 weight ratio mixes) in the crude product after dealcoholysis, mixed 1 hour.
(5) filtration step: refined mixed solution is filtered, and the liquid that obtains is certain herbaceous plants with big flowers diacid two 2-ethylhexyl finished products, these certain herbaceous plants with big flowers diacid two 2-ethylhexyl content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 3
A kind of preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls the steps include:
(1) step of esterification: have heating unit to one, electricity stirs, and drops into certain herbaceous plants with big flowers diacid double centner successively in 300 liters of reactors of thermometer water circulation condenser and water-and-oil separator, 160 kilograms of 2-Ethylhexyl Alcohols, 0.3 kilogram of the vitriol oil, under agitation, micro-vacuum, be heated to boiling reaction simultaneously, keep the boiling reflux state, constantly from water-and-oil separator, water sepn is gone out, after not having moisture to generate, stop heating, esterification stops.
(2) water-washing step: obtain to such an extent that add 50 kg water in the mixed solution after esterification, after stirring, standing demix is removed water layer wherein.
(3) dealcoholysis step: the mixture after will washing, dealcoholysis obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl crude products.
(4) (3) purification step: add 0.7 kilogram of finishing agent (yellow soda ash, calcium oxide, magnesium oxide, gac, diatomite mixture were by 0.2: 1: 1: 2: 1 weight ratio mixes) in the crude product after dealcoholysis, mixed 1 hour.
(5) filtration step: refined mixed solution is filtered, and the liquid that obtains is certain herbaceous plants with big flowers diacid two 2-ethylhexyl finished products, these certain herbaceous plants with big flowers diacid two 2-ethylhexyl content 99.5%, and color is less than No. 30 (platinum-cobalt colorimetric).
Claims (5)
1. the preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls the steps include:
(1) esterification: with the certain herbaceous plants with big flowers diacid, 2-Ethylhexyl Alcohol, the vitriol oil drop in the reactor, under the micro-vacuum condition, stir, and are heated to boiling reaction, keep the boiling reflux state, after not having moisture to generate, stop heating, treat mixed solution naturally cooling in the still;
(2) washing: will add water in the mixture after the esterification, after stirring, standing demix is removed water layer wherein;
(3) dealcoholysis: the mixture after will washing, dealcoholysis obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl crude products;
(4) refining: as will to add finishing agent in the crude product after the dealcoholysis, stir 1～3h;
(5) filter: the mixed solution after will making with extra care filters, and obtains certain herbaceous plants with big flowers diacid two 2-ethylhexyl products.
It is characterized in that: described finishing agent is that yellow soda ash, calcium oxide, magnesium oxide, gac, diatomite mix, and its weight ratio is a yellow soda ash: calcium oxide: magnesium oxide: gac: diatomite=0.2: 1: 1: 2: 1.
2. the preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls according to claim 1 is characterized in that: the weight ratio of described certain herbaceous plants with big flowers diacid and finishing agent is 1: 0.003～0.008.
3. the preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls according to claim 1 is characterized in that: described certain herbaceous plants with big flowers diacid, and 2-Ethylhexyl Alcohol, the weight ratio of the vitriol oil is the certain herbaceous plants with big flowers diacid: 2-Ethylhexyl Alcohol: the vitriol oil=1: 2.2: 0.002～0.005.
4. the preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls according to claim 1 is characterized in that: the weight ratio of described certain herbaceous plants with big flowers diacid and water is 2: 1.
5. the preparation method of certain herbaceous plants with big flowers diacid two 2-ethylhexyls according to claim 1 is characterized in that: described reactor is the encloses container that has agitator, heating unit and backwater condensing works.
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| CN2011102230023A CN102249911A (en) | 2011-08-05 | 2011-08-05 | Preparation method of bis(2-ethylhexyl)sebacate |
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| CN2011102230023A CN102249911A (en) | 2011-08-05 | 2011-08-05 | Preparation method of bis(2-ethylhexyl)sebacate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU443024A1 (en) * | 1972-03-20 | 1974-09-15 | Предприятие П/Я А-1788 | Method for producing carboxylic esters |
| CN1198783C (en) * | 2000-09-05 | 2005-04-27 | 奥克森诺奥勒芬化学股份有限公司 | Method for preparing carboxylic ester |
| CN101914018A (en) * | 2010-08-30 | 2010-12-15 | 天津市化学试剂研究所 | Method for preparing sebacic acid di-n-butyl ester |
| CN101914019A (en) * | 2010-08-30 | 2010-12-15 | 天津市化学试剂研究所 | Refining method of di-n-butyl sebacic acid |
| CN101914015A (en) * | 2010-08-28 | 2010-12-15 | 天津市化学试剂研究所 | Preparation and purification method of butyl stearate |
-
2011
- 2011-08-05 CN CN2011102230023A patent/CN102249911A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU443024A1 (en) * | 1972-03-20 | 1974-09-15 | Предприятие П/Я А-1788 | Method for producing carboxylic esters |
| CN1198783C (en) * | 2000-09-05 | 2005-04-27 | 奥克森诺奥勒芬化学股份有限公司 | Method for preparing carboxylic ester |
| CN101914015A (en) * | 2010-08-28 | 2010-12-15 | 天津市化学试剂研究所 | Preparation and purification method of butyl stearate |
| CN101914018A (en) * | 2010-08-30 | 2010-12-15 | 天津市化学试剂研究所 | Method for preparing sebacic acid di-n-butyl ester |
| CN101914019A (en) * | 2010-08-30 | 2010-12-15 | 天津市化学试剂研究所 | Refining method of di-n-butyl sebacic acid |
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Application publication date: 20111123 |