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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- CN
- China
- Prior art keywords
- tri
- refining
- hexyl trimellitate
- hexyl
- trimellitate
- 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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- MXHBQKVKHGQWRB-UHFFFAOYSA-N trihexyl benzene-1,2,4-tricarboxylate Chemical compound CCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCC)C(C(=O)OCCCCCC)=C1 MXHBQKVKHGQWRB-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000007670 refining Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- 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 abstract description 20
- 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 10
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 10
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 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
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 239000007788 liquid Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 abstract 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract 2
- 235000019341 magnesium sulphate Nutrition 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 description 6
- 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
- -1 n-hexyl alcohols Chemical class 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 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN102249924A true CN102249924A (en) | 2011-11-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102451242A Pending 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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| CN (1) | CN102249924A (en) |
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 |
-
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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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111123 |