CN103694121A - Novel synthetic process of tris (2-propylheptyl) trimellitate - Google Patents
Novel synthetic process of tris (2-propylheptyl) trimellitate Download PDFInfo
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- CN103694121A CN103694121A CN201310612434.2A CN201310612434A CN103694121A CN 103694121 A CN103694121 A CN 103694121A CN 201310612434 A CN201310612434 A CN 201310612434A CN 103694121 A CN103694121 A CN 103694121A
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- China
- Prior art keywords
- reaction
- enanthol
- trimellitic anhydride
- trimellitate
- heptanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a novel synthetic process of tris (2-propylheptyl) trimellitate. The process comprises the following steps: (1) taking raw materials according to a molar ratio of trimellitic anhydride to heptanol being 1:2.7-2.9, and taking a catalyst isopropyl titanate accounting for 0.3-0.35% of the total weight of trimellitic anhydride and heptanol; (2) taking raw materials according to a molar ratio of trimellitic anhydride to heptanol being 1:2.5-2.6, adding 80% of the catalyst into the reactor and heating for reaction; (3) continuing to heat the reaction materials to 200-220 DEG C, and adding the remaining heptanol and the catalyst isopropyl titanate into the reaction kettle for reaction; (4) decolorizing the reaction materials to obtain a crude product, and adding hydrogen peroxide accounting for 1-1.2 wt% of the whole reaction system in the decolorization process; and (5) conducting neutralization washing on the crude product with neutralization washing temperature at 105-110 DEG C, dealcoholizing and filtering to obtain a finished product of tris (2-propylheptyl) trimellitate. The process provided by the invention not only can reduce the production energy consumption but also can improve the color and grade of the finished product.
Description
Technical field
The invention belongs to organic chemical synthesis field, more specifically relate to the synthetic field of a kind of softening agent tri trimellitate (2-propyl group heptan) ester.
Background technology:
Tri trimellitate (2-propyl group heptan) ester is a kind of industrial softening agent with polyester plasticizer and monomer-plasticizer advantage.It has good plasticizing capacity, resistance to migration, water-fast extractable and thermostability, can be used as the heat-resisting and weather resistance softening agent of the various kinds of resin such as polyvinyl chloride, vinyl chloride copolymer, nitrocellulose, ethyl cellulose, be particularly useful for heat-resisting cable material, sheet material, sheet material, gasket etc. and require heat-resisting and durable goods.
In traditional explained hereafter, the index look of the tri trimellitate of producing (2-propyl group heptan) ester number is difficult to reach top grade product with resistivity, therefore, need to optimize existing production technique to obtain the more product of quality product level.
Summary of the invention:
For above-mentioned deficiency, the object of the present invention is to provide a kind of new production process that can improve tri trimellitate (the 2-propyl group heptan) ester of product grade.
The present invention is achieved by the following technical solutions.
A new synthesis process for tri trimellitate (2-propyl group heptan) ester, is characterized in that: processing step is,
(1) by trimellitic anhydride: the mol ratio of enanthol is that 1:2.7-2.9 gets raw material, gets catalyst Ti isopropyl propionate by the 0.3%-0.35% of inclined to one side acid anhydride and enanthol total mass;
(2), by trimellitic anhydride: the mol ratio of enanthol is that 1:2.5-2.6 gets raw material, get 80% of catalyzer and be fed in reactor, temperature reaction;
(3) reaction mass is warming up to 200-220 ℃, remaining enanthol and catalyst Ti isopropyl propionate are added to reaction kettle for reaction;
(4) material having reacted is decoloured process and obtain crude product, in bleaching process, add the hydrogen peroxide that total reaction system quality mark is 1%-1.2%;
(5) crude product is neutralized to washing, the temperature of neutralization washing is 105-110 ℃, after dealcoholysis, filtration, obtains finished product tri trimellitate (2-propyl group heptan) ester.
Beneficial effect: technique of the present invention adds the enanthol can fast reaction speed at twice, reduces the energy consumption of reaction; In bleaching process, add hydrogen peroxide, can improve the look number of tri trimellitate (2-propyl group heptan) ester, in and washing process in improve washing temperature, make like this product can reach the index of top grade product completely.
Embodiment:
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
Get 1920 kilograms of trimellitic anhydride, 3248 kilograms of enanthol, 17.1 kilograms of isopropyl titanates are standby; First by 1920 kilograms of trimellitic anhydride, 2900 kilograms of enanthol, 13.7 kilograms of isopropyl titanates are fed in reactor, are warming up to 180-190 ℃ of reaction; React after 2 hours, continue to be warming up to 210 ℃, add isopropyl titanate to the reaction of remaining 348 kilograms of enanthol and 3.4 kilograms to finish; After reaction, must in reaction solution, add the gac of 52 kilograms and the hydrogen peroxide of 51.9 kilograms to decolour, after decolouring, obtain crude product; Crude product neutralizes washing, and the temperature of washing is controlled at 105 ℃, carries out dealcoholysis after washing, filters and obtains finished product tri trimellitate (2-propyl group heptan) ester.
Claims (1)
1. a new synthesis process for tri trimellitate (2-propyl group heptan) ester, is characterized in that: processing step is,
(1) by trimellitic anhydride: the mol ratio of enanthol is that 1:2.7-2.9 gets raw material, gets catalyst Ti isopropyl propionate by the 0.3%-0.35% of inclined to one side acid anhydride and enanthol total mass, standby;
(2) by trimellitic anhydride: the mol ratio of enanthol is that 1:2.5-2.6 gets raw material, get 80% of catalyzer and be fed in reactor, be warming up to 160-190 ℃ of reaction 2-3 hour;
(3) reaction mass is continued to be warming up to 200-220 ℃, remaining enanthol and catalyst Ti isopropyl propionate are added to reaction kettle for reaction;
(4) material having reacted is decoloured process and obtain crude product, in bleaching process, add the hydrogen peroxide that total reaction system quality mark is 1%-1.2%;
(5) crude product is neutralized to washing, the temperature of neutralization washing is 105-110 ℃, after dealcoholysis, filtration, obtains finished product tri trimellitate (2-propyl group heptan) ester.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310612434.2A CN103694121A (en) | 2013-11-28 | 2013-11-28 | Novel synthetic process of tris (2-propylheptyl) trimellitate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310612434.2A CN103694121A (en) | 2013-11-28 | 2013-11-28 | Novel synthetic process of tris (2-propylheptyl) trimellitate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103694121A true CN103694121A (en) | 2014-04-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310612434.2A Pending CN103694121A (en) | 2013-11-28 | 2013-11-28 | Novel synthetic process of tris (2-propylheptyl) trimellitate |
Country Status (1)
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| CN (1) | CN103694121A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107250098A (en) * | 2014-12-02 | 2017-10-13 | 埃默里油脂化学有限公司 | Ester plasticiser based on ethyl hexanol and propyl enanthol |
| CN107413383A (en) * | 2017-07-07 | 2017-12-01 | 江苏正丹化学工业股份有限公司 | The just pungent positive last of the ten Heavenly stems Lipase absobed catalyst of tri trimellitate and its application method |
| CN111574366A (en) * | 2020-06-22 | 2020-08-25 | 南通百川新材料有限公司 | Method for synthesizing triisodecyl trimellitate |
-
2013
- 2013-11-28 CN CN201310612434.2A patent/CN103694121A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107250098A (en) * | 2014-12-02 | 2017-10-13 | 埃默里油脂化学有限公司 | Ester plasticiser based on ethyl hexanol and propyl enanthol |
| CN107413383A (en) * | 2017-07-07 | 2017-12-01 | 江苏正丹化学工业股份有限公司 | The just pungent positive last of the ten Heavenly stems Lipase absobed catalyst of tri trimellitate and its application method |
| CN107413383B (en) * | 2017-07-07 | 2019-10-29 | 江苏正丹化学工业股份有限公司 | The just pungent positive last of the ten Heavenly stems Lipase absobed catalyst of tri trimellitate and its application method |
| CN111574366A (en) * | 2020-06-22 | 2020-08-25 | 南通百川新材料有限公司 | Method for synthesizing triisodecyl trimellitate |
| CN111574366B (en) * | 2020-06-22 | 2022-03-29 | 南通百川新材料有限公司 | Method for synthesizing triisodecyl trimellitate |
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Application publication date: 20140402 |