CN102249924A - Method for refining tri-n-hexyl trimellitate and refining agent used in method - Google Patents
Method for refining tri-n-hexyl trimellitate and refining agent used in method Download PDFInfo
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- CN102249924A CN102249924A CN2011102451242A CN201110245124A CN102249924A CN 102249924 A CN102249924 A CN 102249924A CN 2011102451242 A CN2011102451242 A CN 2011102451242A CN 201110245124 A CN201110245124 A CN 201110245124A CN 102249924 A CN102249924 A CN 102249924A
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Abstract
The invention relates to a method for refining tri-n-hexyl trimellitate and a refining agent used in the method. The refining agent comprises the following components: sodium carbonate, magnesium carbonate, activated carbon and magnesium sulfate, wherein the mass ratio of sodium carbonate to magnesium carbonate to activated carbon to magnesium sulfate is 0.5:1:2:1.5. The method for preparing the tri-n-hexyl trimellitate comprises the following refining steps: adding the refining agent in a tri-n-hexyl trimellitate crude product, stirring and refining for 1 hour, wherein the mass ratio of refining agent to trimellitic acid is (0.05-0.1):1; and filtering a mixed liquid after refining so as to obtain the tri-n-hexyl trimellitate finished product. In the preparation method, a high vacuum refining step is omitted when in production, and the investment of high vacuum pump equipment is avoided, thus saving equipment investment, reducing production cost and improving the market competitiveness of a product.
Description
Technical field;
The invention belongs to the organic compound preparation field, especially a kind of process for purification of tri n hexyl trimellitate and used finishing agent thereof.
Background technology;
In industrial production, in plastics industry and the war production, tri n hexyl trimellitate is as a kind of important organic compound and heat-resisting, and high temperature plasticizer has good electrical properties application more and more widely.The common production method of tri n hexyl trimellitate is the direct esterification reaction, the color that obtains product is for yellow, be difficult to sell as product, must carry out further making with extra care the refinement treatment that promptly reduces pressure step, the problem that this type of preparation method exists: 1, owing to need 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 tri n hexyl trimellitate process, 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.
Summary of the invention;
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of refining tri n hexyl trimellitate and used finishing agent thereof are provided, use the refining tri n hexyl trimellitate of finishing agent, can save facility investment, reduce cost, shorten the production time and can enhance productivity.
The technical scheme that realizes the object of the invention is as follows:
A kind of finishing agent that is used for refining tri n hexyl trimellitate is characterized in that its component and mass ratio are: yellow soda ash: magnesiumcarbonate: gac: sal epsom=0.5: 1: 2: 1.5.
A kind of method for preparing tri n hexyl trimellitate, comprise preparation tri n hexyl trimellitate crude product and refining two steps, it is characterized in that described purification step adopts finishing agent, in the crude product of tri n hexyl trimellitate, add finishing agent, the mass ratio of finishing agent and trimellitic acid is 0.05～0.1: 1, stirred refining one hour, the mixed solution after refining is filtered, obtain the tri n hexyl trimellitate finished product.
And the step of described preparation tri n hexyl trimellitate crude product is as follows:
(1) step of esterification: with trimellitic acid, n-hexyl alcohol, the vitriol oil, the mass ratio by 1: 2.56: 0.002～0.005 drops in the reactor, stirs, and micro-vacuum is heated to boiling reaction, keeps boiling reflux state separation moisture wherein;
(2) water-washing step: will add entry in the mixture after the esterification, the mass ratio of water and trimellitic acid is 0.8: 1, and after stirring, standing demix is removed water layer wherein;
(3) dealcoholysis step: the mixture dealcoholysis after will washing obtains the crude product tri n hexyl trimellitate.
Advantage of the present invention and beneficial effect are:
1. the preparation method of this tri n hexyl trimellitate is in purification step, use finishing agent (yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture), the product colour that obtains shoals, do not need the high vacuum refinement treatment promptly to can be used as product and sell, prepared quality product meets the technical requirements fully.This preparation method has saved the high vacuum purification step when producing, avoided the input of high-vacuum pump equipment, therefore, has saved facility investment, reduces production costs, and has improved the competitiveness of product in market.
2. the finishing agent that uses of the preparation method of this tri n hexyl trimellitate is yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture, have cheap, the characteristics that are easy to purchase.
3. the preparation method of this tri n hexyl trimellitate is easy to operate, and is simple, is convenient to realize suitability for industrialized production, enhances productivity.
4. the present invention uses finishing agent (yellow soda ash, magnesiumcarbonate, gac, sal epsom mixture) in process of production, guarantees quality product and prolonged storage stability.
Embodiment;
The present invention is further described below by specific embodiment; example of the present invention is illustrative; rather than it is determinate; therefore the present invention is not limited to the embodiment described in the embodiment; every other embodiments that drawn by those skilled in the art's technical scheme according to the present invention belong to the scope of protection of the invention equally.
Embodiment 1:
The preparation of finishing agent: with (50) g yellow soda ash, (100) g magnesiumcarbonate, (100) g gac, (150) g sal epsom mixes.
(1) step of esterification: have heating unit to one, electricity stirs, and drops into the trimellitic acid double centner successively in 500 liters of reactors of thermometer water circulation condenser and vacuum oil water separator, 256 kilograms of n-hexyl 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 250 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 the crude product tri n hexyl trimellitate.
(4) purification step: add 0.5 kilogram of finishing agent in the crude product after dealcoholysis, mixed 1 hour.
(5) filtration step: refined mixed solution is filtered, and the liquid that obtains is the tri n hexyl trimellitate finished product, this tri n hexyl trimellitate content 99.0%, and color is less than No. 2 (iodine colorimetric).
Embodiment 2:
The preparation of finishing agent: with (60) g yellow soda ash, (120) g magnesiumcarbonate, (120) g gac, (180) g sal epsom mixes.
(1) step of esterification: have heating unit to one, electricity stirs, and drops into the trimellitic acid double centner successively in 500 liters of reactors of thermometer water circulation condenser and vacuum oil water separator, 256 kilograms of n-hexyl 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 250 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 the crude product tri n hexyl trimellitate.
(4) purification step: add 0.6 kilogram of finishing agent in the crude product after dealcoholysis, mixed 1 hour.
(5) filtration step: refined mixed solution is filtered, and the liquid that obtains is the tri n hexyl trimellitate finished product, this tri n hexyl trimellitate content 99.0%, and color is less than No. 2 (iodine colorimetric).
Embodiment 3:
The preparation of finishing agent: with (70) g yellow soda ash, (140) g magnesiumcarbonate, (280) g gac, (210) g sal epsom mixes.
(1) step of esterification: have heating unit to one, electricity stirs, and drops into the trimellitic acid double centner successively in 500 liters of reactors of thermometer water circulation condenser and vacuum oil water separator, 256 kilograms of n-hexyl 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 the crude product tri n hexyl trimellitate.
(4) purification step: add 0.7 kilogram of finishing agent in the crude product after dealcoholysis, mixed 1 hour.
(5) filtration step: refined mixed solution is filtered, and the liquid that obtains is the tri n hexyl trimellitate finished product, this tri n hexyl trimellitate content 99.0%, and color is less than No. 2 (iodine colorimetric).
Claims (3)
1. a finishing agent that is used for refining tri n hexyl trimellitate is characterized in that its component and mass ratio are: yellow soda ash: magnesiumcarbonate: gac: sal epsom=0.5: 1: 2: 1.5.
2. method for preparing tri n hexyl trimellitate, comprise preparation tri n hexyl trimellitate crude product and refining two steps, it is characterized in that described purification step adopts finishing agent, in the crude product of tri n hexyl trimellitate, add finishing agent, the mass ratio of finishing agent and trimellitic acid is 0.05～0.1: 1, stirred refining one hour, the mixed solution after refining is filtered, obtain the tri n hexyl trimellitate finished product.
3. the method for a kind of refining tri n hexyl trimellitate according to claim 2 is characterized in that the step of described preparation tri n hexyl trimellitate crude product is as follows:
(1) step of esterification: with trimellitic acid, n-hexyl alcohol, the vitriol oil, the mass ratio by 1: 2.56: 0.002～0.005 drops in the reactor, stirs, and micro-vacuum is heated to boiling reaction, keeps boiling reflux state separation moisture wherein;
(2) water-washing step: will add entry in the mixture after the esterification, the mass ratio of water and trimellitic acid is 0.8: 1, and after stirring, standing demix is removed water layer wherein;
(3) dealcoholysis step: the mixture dealcoholysis after will washing obtains the crude product tri n hexyl trimellitate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102451242A CN102249924A (en) | 2011-08-25 | 2011-08-25 | Method for refining tri-n-hexyl trimellitate and refining agent used in method |
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| CN2011102451242A CN102249924A (en) | 2011-08-25 | 2011-08-25 | Method for refining tri-n-hexyl trimellitate and refining agent used in method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320972A (en) * | 2011-08-25 | 2012-01-18 | 天津市化学试剂研究所 | Method for refining trioctyl trimellate and refining agent used in refining |
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2011
- 2011-08-25 CN CN2011102451242A patent/CN102249924A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320972A (en) * | 2011-08-25 | 2012-01-18 | 天津市化学试剂研究所 | Method for refining trioctyl trimellate and refining agent used in refining |
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Application publication date: 20111123 |