CN101914015B - Preparation and purification method of butyl stearate - Google Patents
Preparation and purification method of butyl stearate Download PDFInfo
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- CN101914015B CN101914015B CN 201010265387 CN201010265387A CN101914015B CN 101914015 B CN101914015 B CN 101914015B CN 201010265387 CN201010265387 CN 201010265387 CN 201010265387 A CN201010265387 A CN 201010265387A CN 101914015 B CN101914015 B CN 101914015B
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Abstract
The invention relates to preparation and a purification method of butyl stearate. The preparation comprises the following steps of: putting stearic acid, butanol and concentrated sulfuric acid into a reaction kettle in turn; stirring and simultaneously heating to boiling reaction; keeping a boiling reflux state and continuously separating water out of an oil-water separator till water is not generated; stopping heating to terminate esterification reaction; washing; distilling for removing a solvent; and refining to obtain liquid, namely the finished product of the butyl stearate. By saving a high-vacuum refining step in the production process, the preparation method has the advantages of avoiding using a high-vacuum pump, saving equipment investment, reducing production cost, shortening the whole production cycle, improving production efficiency, and contributing to the realization of industrial production of the whole scheme.
Description
Technical field
The invention belongs to field of lubricant, especially a kind of preparation of butyl stearate and process for purification.
Background technology
Especially in plastics industry is produced, butyl stearate has more and more widely as a kind of important organic compounds to be used, and in the transparent PVC goods, obtains general application as internal lubricant in industrial production.At present, the production method of butyl stearate is directly to carry out esterification, the follow-up purification step of not being correlated with, the color that obtains product is dark, is difficult to as production marketing, must further make with extra care, the refinement treatment that namely reduces pressure step, the problem that such preparation method exists is: 1, because the high-vacuum pump ability price of using in the decompression refinement treatment step is relatively high, virtually increased the cost of manufacturing enterprise, caused finished product to rise; 2, because decompression refinement treatment step is to produce in the butyl stearate process requisitely, and the needed time of this step is longer, with the whole production cycle elongate, production efficiency is low, is unfavorable for the raising of Business Economic Benefit.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the preparation method that a kind of facility investment is low, produce this locality, the butyl stearate that with short production cycle, production efficiency is high is provided.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation of butyl stearate and process for purification is characterized in that: step is as follows:
(1) step of esterification
In reactor, drop into successively stearic acid, butanols, the vitriol oil, under agitation be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops;
Wherein: stearic acid: propyl carbinol: the weight ratio of the vitriol oil is 1: 0.65: 0.001-0.005;
(2) water-washing step
Obtain after the esterification to such an extent that add entry in the mixed solution, after stirring, standing demix is removed water layer wherein, the mixture after obtaining washing;
Wherein: water and stearic weight ratio are 0.5: 1;
(3) distillation desolventizing step
With the mixture after the washing, distillation, residuum is the butyl stearate crude product;
(4) purification step
Add finishing agent in the butyl stearate crude product of step (3), mix 0.5-1.5 hour, filter, the liquid that obtains is the butyl stearate finished product;
Wherein, finishing agent is diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood weight ratio, by 1: 1: 5: mix at 1.5: 0.5;
Finishing agent and stearic weight ratio are 0.001-0.005: 1.
And described reactor is with heating unit, electricity stirring, thermometer water circulation condenser and water-and-oil separator.
Advantage of the present invention and positively effect are:
1, in the purification step of this preparation and process for purification, the finishing agent that uses is diatomite, magnesium hydroxide, gac, sal epsom, potassium carbonate mixtures, the butyl stearate crude product of preparing has been carried out further refining, product colour after refining shoals, do not need the high vacuum refinement treatment namely to can be used as product and sell, its quality meets the technical requirements fully.
2, this preparation method has saved the high vacuum purification step when producing, not only avoid the input of high-vacuum pump equipment, saved facility investment, reduced production costs, also shortened the cycle of whole production, enhance productivity, be convenient to make whole scheme to realize suitability for industrialized production.
3, the finishing agent that uses of the preparation method of this butyl stearate is the mixture of diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood, have cheap, the advantage that is easy to purchase.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A kind of preparation of butyl stearate and process for purification, step is as follows:
(1) step of esterification
To one with heating unit, electricity stirs, drop into successively stearic acid double centner, 65 kilograms in butanols, 0.1 kilogram of the vitriol oil in 200 liters of reactors of thermometer water circulation condenser and water-and-oil separator, under agitation be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops;
Wherein: stearic acid: propyl carbinol: the weight ratio of the vitriol oil is 1: 0.65: 0.001-0.005.
(2) water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein;
Wherein: water and stearic weight ratio are 0.5: 1.
(3) distillation desolventizing step
With the mixture after the washing, distillation removes excessive butanols, distillation temperature 110-120 ℃ and vacuum tightness 10 ± 2mmHg), and residuum is the butyl stearate crude product;
(4) purification step
In the butyl stearate crude product, add 0.1 kilogram of finishing agent (diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood), mix 1 hour, refined mixed solution is filtered, the liquid that obtains is the butyl stearate finished product, this butyl stearate content 99.5%, color is less than No. 3 (iodine colorimetric).
Wherein, finishing agent and stearic weight ratio are 0.001-0.005: 1
Finishing agent is diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood weight ratio, by 1: 1: 5: mix at 1.5: 0.5.
Embodiment 2
A kind of preparation of butyl stearate and process for purification, step is as follows:
(1) step of esterification
To one with heating unit, electricity stirs, drop into successively stearic acid double centner, 65 kilograms in butanols, 0.1 kilogram of the vitriol oil in 200 liters of reactors of thermometer water circulation condenser and water-and-oil separator, under agitation be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops;
(2) water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein;
(3) distillation desolventizing step
With the mixture after the washing, distillation removes excessive butanols, distillation temperature 110-120 ℃ and vacuum tightness 10 ± 2mmHg), and residuum is the butyl stearate crude product;
(4) purification step
In the butyl stearate crude product, add 0.2 kilogram of finishing agent (diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood), mix 1 hour, refined mixed solution is filtered, the liquid that obtains is the butyl stearate finished product, this butyl stearate content 99.5%, color is less than No. 3 (iodine colorimetric).
Embodiment 3
A kind of preparation of butyl stearate and process for purification, step is as follows:
(1) step of esterification
To one with heating unit, electricity stirs, drop into successively stearic acid double centner, 65 kilograms in butanols, 0.1 kilogram of the vitriol oil in 200 liters of reactors of thermometer water circulation condenser and water-and-oil separator, under agitation be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops;
(2) water-washing step
Obtain after the esterification to such an extent that add 50 kg water in the mixed solution, after stirring, standing demix is removed water layer wherein;
(3) distillation desolventizing step
With the mixture after the washing, distillation removes excessive butanols, distillation temperature 110-120 ℃ and vacuum tightness 10 ± 2mmHg), and residuum is the butyl stearate crude product;
(4) purification step
In the butyl stearate crude product, add 0.5 kilogram of finishing agent (diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood), mix 1 hour, refined mixed solution is filtered, the liquid that obtains is the butyl stearate finished product, this butyl stearate content 99.5%, color is less than No. 3 (iodine colorimetric).
Claims (2)
1. the preparation of a butyl stearate and process for purification, it is characterized in that: step is as follows:
⑴ step of esterification
In reactor, drop into successively stearic acid, butanols, the vitriol oil, under agitation be heated to simultaneously boiling reaction, keep the boiling reflux state, constantly from water-and-oil separator with moisture from going out, until after not having moisture to generate, stopped heating, esterification stops;
Wherein: stearic acid: propyl carbinol: the weight ratio of the vitriol oil is 1:0.65:0.001-0.005;
⑵ water-washing step
Obtain after the esterification to such an extent that add entry in the mixed solution, after stirring, standing demix is removed water layer wherein, the mixture after obtaining washing;
Wherein: water and stearic weight ratio are 0.5:1;
⑶ distillation desolventizing step
With the mixture after the washing, distillation, residuum is the butyl stearate crude product;
⑷ purification step
Add finishing agent in the butyl stearate crude product of step ⑶, mix 0.5-1.5 hour, filter, the liquid that obtains is the butyl stearate finished product;
Wherein, finishing agent is diatomite, magnesium hydroxide, gac, sal epsom, salt of wormwood weight ratio, mixes by 1:1:5:1.5:0.5;
Finishing agent and stearic weight ratio are 0.001-0.005:1.
2. the preparation of butyl stearate according to claim 1 and process for purification is characterized in that: described reactor with heating unit, electricity stir, thermometer water circulation condenser and water-and-oil separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010265387 CN101914015B (en) | 2010-08-28 | 2010-08-28 | Preparation and purification method of butyl stearate |
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| CN 201010265387 CN101914015B (en) | 2010-08-28 | 2010-08-28 | Preparation and purification method of butyl stearate |
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| CN101914015A CN101914015A (en) | 2010-12-15 |
| CN101914015B true CN101914015B (en) | 2013-10-23 |
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| CN102249911A (en) * | 2011-08-05 | 2011-11-23 | 天津市化学试剂研究所 | Preparation method of bis(2-ethylhexyl)sebacate |
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Non-Patent Citations (2)
| Title |
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| 酯类润滑剂硬脂酸丁酯合成的工艺改进;陈育知等;《南京师范大学学报》;20050630;54-57 * |
| 陈育知等.酯类润滑剂硬脂酸丁酯合成的工艺改进.《南京师范大学学报》.2005,54-57. |
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Address after: 300240 Tianjin Admiralty street Dongli District Xu Zhuangzi Patentee after: TIANJIN CHEMICAL REAGENT RESEARCH INSTITUTE CO., LTD. Address before: 300240 Tianjin Admiralty street Dongli District Xu Zhuangzi Patentee before: Tianjin chemical research institute |
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Granted publication date: 20131023 Termination date: 20160828 |