CN102249923A - Method for refining tris(2-ethylhexyl)trimellitate and refining agent used thereby - Google Patents
Method for refining tris(2-ethylhexyl)trimellitate and refining agent used thereby Download PDFInfo
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- CN102249923A CN102249923A CN201110245063XA CN201110245063A CN102249923A CN 102249923 A CN102249923 A CN 102249923A CN 201110245063X A CN201110245063X A CN 201110245063XA CN 201110245063 A CN201110245063 A CN 201110245063A CN 102249923 A CN102249923 A CN 102249923A
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- CN
- China
- Prior art keywords
- ethylhexyl
- refining
- tri trimellitate
- trimellitate
- finishing agent
- 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.)
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 25
- 238000007670 refining Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 13
- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 title abstract 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000012043 crude product Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 11
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 9
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 claims description 18
- 238000005886 esterification reaction Methods 0.000 claims description 14
- 230000032050 esterification Effects 0.000 claims description 13
- 238000009835 boiling Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 8
- 229960001708 magnesium carbonate Drugs 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 235000017550 sodium carbonate Nutrition 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000001914 filtration Methods 0.000 abstract description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract 1
- 235000019341 magnesium sulphate Nutrition 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 6
- -1 2-Ethylhexyl Alcohols Chemical class 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for refining tris(2-ethylhexyl)trimellitate and a refining agent used thereby. The refining agent comprises components of sodium carbonate, magnesium carbonate, active carbon and magnesium sulfate in a mass ratio of 0.5:1:2:1.5. The method for refining the tris(2-ethylhexyl)trimellitate comprises the following steps of: adding the refining agent into a crude product of tris(2-ethylhexyl)trimellitate in a mass ratio of (0.05-0.1):1, stirring and refining for 1 hour, and filtering the refined mixed liquor to obtain the finished product of tris(2-ethylhexyl)trimellitate. In the preparation method, a step of refining in high vacuum is saved during production, and the input of high vacuum pump equipment is avoided, so the equipment investment is saved, the production cost is reduced and the market competitiveness of the product is improved.
Description
Technical field;
The invention belongs to the organic compound preparation field, especially a kind of process for purification of tri trimellitate 2-ethylhexyl and used finishing agent thereof.
Background technology;
In industrial production, in plastics industry and the war production, tri trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl and used finishing agent thereof are provided, use the refining tri trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl, comprise preparation tri trimellitate 2-ethylhexyl crude product and refining two steps, it is characterized in that described purification step adopts finishing agent, in the crude product of tri trimellitate 2-ethylhexyl, 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 tri trimellitate 2-ethylhexyl finished product.
And the step of described preparation tri trimellitate 2-ethylhexyl crude product is as follows:
(1) step of esterification: with trimellitic acid, 2-Ethylhexyl Alcohol, the vitriol oil, the mass ratio by 1: 2.76: 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 crude product tri trimellitate 2-ethylhexyl.
Advantage of the present invention and beneficial effect are:
1. the preparation method of this tri trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl 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, (200) 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, 276 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 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 crude product tri trimellitate 2-ethylhexyl.
(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 tri trimellitate 2-ethylhexyl finished product, this tri trimellitate 2-ethylhexyl content 99.0%, and color is less than No. 1 (iodine colorimetric).
Embodiment 2:
The preparation of finishing agent: with (60) g yellow soda ash, (120) g magnesiumcarbonate, (240) 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, 276 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 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 crude product tri trimellitate 2-ethylhexyl.
(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 tri trimellitate 2-ethylhexyl finished product, this tri trimellitate 2-ethylhexyl content 99.0%, and color is less than No. 1 (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, 276 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 crude product tri trimellitate 2-ethylhexyl.
(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 tri trimellitate 2-ethylhexyl finished product, this tri trimellitate 2-ethylhexyl content 99.0%, and color is less than No. 1 (iodine colorimetric).
Claims (3)
1. a finishing agent that is used for refining tri trimellitate 2-ethylhexyl 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 trimellitate 2-ethylhexyl, comprise preparation tri trimellitate 2-ethylhexyl crude product and refining two steps, it is characterized in that described purification step adopts finishing agent, in the crude product of tri trimellitate 2-ethylhexyl, 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 tri trimellitate 2-ethylhexyl finished product.
3. the method for a kind of refining tri trimellitate 2-ethylhexyl according to claim 2 is characterized in that the step of described preparation tri trimellitate 2-ethylhexyl crude product is as follows:
(1) step of esterification: with trimellitic acid, 2-Ethylhexyl Alcohol, the vitriol oil, the mass ratio by 1: 2.76: 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 crude product tri trimellitate 2-ethylhexyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110245063XA CN102249923A (en) | 2011-08-25 | 2011-08-25 | Method for refining tris(2-ethylhexyl)trimellitate and refining agent used thereby |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110245063XA CN102249923A (en) | 2011-08-25 | 2011-08-25 | Method for refining tris(2-ethylhexyl)trimellitate and refining agent used thereby |
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| Publication Number | Publication Date |
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| CN102249923A true CN102249923A (en) | 2011-11-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201110245063XA Pending CN102249923A (en) | 2011-08-25 | 2011-08-25 | Method for refining tris(2-ethylhexyl)trimellitate and refining agent used thereby |
Country Status (1)
| Country | Link |
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| CN (1) | CN102249923A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267908A (en) * | 2011-08-25 | 2011-12-07 | 天津市化学试剂研究所 | Method for refining trioctyl trimellitate and refining agent used thereby |
| 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 |
-
2011
- 2011-08-25 CN CN201110245063XA patent/CN102249923A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267908A (en) * | 2011-08-25 | 2011-12-07 | 天津市化学试剂研究所 | Method for refining trioctyl trimellitate and refining agent used thereby |
| 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 |
| CN102267908B (en) * | 2011-08-25 | 2014-03-26 | 天津市化学试剂研究所 | Method for refining trioctyl trimellitate and refining agent used thereby |
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Application publication date: 20111123 |