WO2014185872A4 - Dotp (di-octly terephthalate)production method - Google Patents
Dotp (di-octly terephthalate)production method Download PDFInfo
- Publication number
- WO2014185872A4 WO2014185872A4 PCT/TR2014/000096 TR2014000096W WO2014185872A4 WO 2014185872 A4 WO2014185872 A4 WO 2014185872A4 TR 2014000096 W TR2014000096 W TR 2014000096W WO 2014185872 A4 WO2014185872 A4 WO 2014185872A4
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- dotp
- tower
- alcohol
- production
- terephthalate
- Prior art date
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention is DOTP (Di octly terephthalate) production method at normal atmospheric pressure without using any inert gas by separating the water formed in the reaction by means of column in PVC plastic production industry.
Claims
AMENDED CLAIMS
received by the International Bureau on 19 November 2014 (19.1 1.2014)
WHAT IS CLAIMED IS
1. The present invention is a production method DOTP (Di-Octyl Terephthalate), and characterized in comprising the process steps in which;
tereftalatic acid (PTA) reacts with at least one alcohol and at least one catalyst in a reactor (10) in a pressureless operation open to the atmosphere, without using any inert gas,
the reactor (10) began to be heated with the heater,
when the reactor (10) temperature rises, excess alcohol and the water formed in the reaction begins to mobilize along the tower (90)
The water and the alcohol formed in the reaction is sent to the tower by small column (20) and the main column (30) which are the connection between reactor (10) and the tower (90); a d carrying alcohol, and water vapour to the tower in order to prevent foaming and pressure in the reactor (10),
Water condensed in the tower (90), and separated from alcohol due to difference of intensity (density of wate after reaction is 1 while the density of alcohol (2 ethyl hexanol) used is 0,833.) is collected at the bottom of the tower
(90), but alcohol stays on the surface of water, the totally water-free alcohol located in the tower return to the reactor (10) from column (40) and the spare line (50) carrying alcohol to the tower by means of heat exchangers,
Noncondenslng water or alcohol passes through the upper part of the tower (70), and collected in the collecting tank
the collection of the excess alcohol that cannot return through the spare line (50) and the column (AO) that carries the alcohol to the tower due to the pressure difference by the increase in the reaction temperature in the collecting tank (80),
Pumping into reactor (10) by spare line (50) once it reaches a certain level in collecting tank (80),
7
excess alcohol is taken under vacuum after the production,
resulting water content and acid number of the product is monitored and when the acid number falls below 0.1 mg / KOH, production is ended, crude product is washed with water, filtered and the production is ended,
DOTP produced by this method does not need to be washed with 2,5% NaOH and washed with water only,
after washing with water, it is sent directly to the filter without being processed with active carbon or bleaching earth.
2. A method of production OOTP (Di-Octy! Terephthalate) according to claim 1 , characterized in that when the reaction temperature reaches 190 C, the main column (30) is closed and production is continued only with the small column (20).
3. A method of production DOTP (Di-Octyl Terephthalate) according to claim 1. characterized in that the small column (20) is of 4" length, and the hitting point on the tower (9) is 300 cm higher than the bottom of the tower.
4. A method of production DOTP (Di-Octyl Terephthalate) according to claim 1 , characterized in that the main column (30) is of 6" lenght. and the hitting point on the tower (9) is 340 cm higher than the bottom of the tower,
5. A method of production DOTP (Di-Octyl Terephthalate) according to claim 1 , characterized in that the column (40) carrying alcohol to the tower is of 4" lenght, and 200 cm high from the bottom of the tower (90), and hitting the part of reactor (10) full of chemicals.
8. A method of production DOTP (Di-Octyl Terephthalate) according to claim 1 , characterized in that spare line (50) is of 2" lenght.
7. A method of production DOTP (Di-Octyl Terephthalate) according to claim 1 , characterized in that the colour of the product is at most 10 Ha^en and the excess alcohol does not turn yellow even if used hundred times by means of reaction realized in a pressureless operation open to the atmosphere, without using any inert gas.
8
8. A method of production DOTP (Di-Octyi Terephthalate) according to claim 1 , characterized in that carbon number of the alcohol used is at least 6 up to 10.
9. A method of production DOTP (Di-Octyi Terephthalate) according to claim 1. characterized in that PTA; alcohol molar ratio is 1 : 2.
10. A method of production DOTP (Di-Octyi Terephthalate) according to claim 9, characterized in that in production, the use of excess alcohol is 80% to 10%.
11. A method of producing DOTP (Di-Octyl Terephthalate) according to one of the preceding claims, characterized in that the reactor (10) has a structure having a simple stirrer and a heater which is controlled by a temperature control element,
12. A method of producing DOTP (Oi-Octyl Terephthalate) according to one of the preceding claims, characterized in that the tower (90) is open to the atmosphere through collecting tank (70) where escaping alcohol and water vapour are collected and pressure is normal atmospheric pressure.
13. A method of producing DOTP (Di-Octyl Terephthalate) according to one of the preceding claims, characterized in that the reaction temperature is between 170 "G and 220 °C.
14. A method of producing DOTP (Di-Octyl Terephthalate) according to one of the preceding claims, characterized in that the catalyst used is a catalyst selected from the group of TiPT (Titanium (IV) isopropoxide (97+%) (Tetraisopropyl titanate, tetrapropyl orthotitanate), "Π8Τ (Titanium (IV) n-butoxide (98+%) (Tetraisobuty! titanate), TNBT (Titanium (IV) n-butoxide (98+%) (Tetre n-butyl titanate), MSA ( ethanesulfonic acid), tin(ll) oxalate ( stannous oxalate ) ,
15. A method of producing DOTP (Di-Octyl Terephthalate) according to one of the preceding claims, characterized in that terephthalate (DOTP) esters ate used as a plasticizer.
9
16. A method of producing DOTP (Di-Octyl Terephthalate) according to one of the preceding claims, characterized in that the tower (90) comprises at least two and a maximum of 12 heat exchangers and at least 2 and no more than 12 rooms,
17. A method of production DOTP (Di-Octyl Terephthalate) according to claim 16, the mentioned exchangers are formed of 2 80 cm pipes approximately of 2" length, forming the rooms in the 100 cm free space between the two exchangers,
10
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2015149936A RU2015149936A (en) | 2013-05-13 | 2014-03-27 | METHOD FOR PRODUCING DIOKTILTEREPHTHALATE (DOTF) |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TR201305713 | 2013-05-13 | ||
| TR2013/05713 | 2013-05-13 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| WO2014185872A1 WO2014185872A1 (en) | 2014-11-20 |
| WO2014185872A4 true WO2014185872A4 (en) | 2015-01-08 |
Family
ID=51177119
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/TR2014/000096 WO2014185872A1 (en) | 2013-05-13 | 2014-03-27 | Dotp (di-octly terephthalate)production method |
Country Status (2)
| Country | Link |
|---|---|
| RU (1) | RU2015149936A (en) |
| WO (1) | WO2014185872A1 (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3351101A1 (en) | 2011-09-19 | 2018-07-25 | Fenwal, Inc. | Container for storing red blood cells |
| US10398625B2 (en) | 2013-03-13 | 2019-09-03 | Fenwal, Inc. | Medical containers with terephthalate plasticizer for storing red blood cell products |
| WO2015124236A1 (en) | 2014-02-20 | 2015-08-27 | Fresenius Hemocare Netherlands B.V. | Medical containers and system components with non-dehp plasticizers for storing red blood cell products, plasma and platelets |
| CN105001091A (en) * | 2015-08-31 | 2015-10-28 | 山东齐鲁增塑剂股份有限公司 | Esterification reaction process for plasticizer DOTP (dioctyl terephthalate) |
| CN105130804B (en) * | 2015-09-11 | 2017-03-01 | 山东成武易信环保科技有限公司 | The production method of environment-friendly plasticizer DOTP and production system |
| TWI624454B (en) * | 2017-06-19 | 2018-05-21 | Nanya Plastics Corp | Method for improving reaction efficiency of terephthalate plasticizer |
| CN109809988A (en) * | 2019-03-26 | 2019-05-28 | 山东同源环保新材料有限公司 | A kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7799942B2 (en) * | 2005-08-12 | 2010-09-21 | Eastman Chemical Company | Production of terephthalic acid di-esters |
| US7741509B2 (en) * | 2007-01-30 | 2010-06-22 | Eastman Chemical Company | Conversion of terephthalic acid to Di-n-butyl terephthalate |
-
2014
- 2014-03-27 RU RU2015149936A patent/RU2015149936A/en unknown
- 2014-03-27 WO PCT/TR2014/000096 patent/WO2014185872A1/en active Application Filing
Also Published As
| Publication number | Publication date |
|---|---|
| WO2014185872A1 (en) | 2014-11-20 |
| RU2015149936A (en) | 2017-06-19 |
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