MX2009007443A - Process for the manufacture of alkanolamine mixtures of low diethanolamine content. - Google Patents

Abstract

Described is a process for producing an ethanolamine mixture of low diethanolamine content, the process comprising a first ethoxylation reaction using aqueous ammonia and an excess of ethylene oxide, also including the elimination of the residual water and ammonia, and a second ethoxylation reaction performed over the product obtained from the first ethoxylation. The product thus obtained has a high content of TEA and an important amount of amine glycol ether which, along with the ethanolamines generate a composition that is useful for the manufacture of softeners, as an intermediary for the manufacture of detergents and it is widely used in the cosmetic industry. As an alternative, the ethoxylation stage may be applied over a pure ethanolamine or a mixture thereof, and obtain a product with properties similar to those products obtained from ammonia and ethylene oxide.

Description

MANUFACTURE OF ALCANOLAMINE MIXTURES DIETANOLAMINE CONTENT FIELD OF THE INVENTION The present invention relates to the production of alkanolamines and, in particular, to a mixture of ethanolamines and glycol a, which is very useful in fabrics, softeners for textiles and in ethics.

BACKGROUND OF THE INVENTION Ethanolamines, as for example tanolamin, or by-products of the same wide range of applications in the area of detectors, cosmetics, emulsifiers, etc.

Many of the processes for obtaining this state of the art, starting from the reaction of ethylene and ammonia, focus on reaching some ethanolamine in particular, ethoxylated byproducts and obtaining products with or of purity.

In this context, ethanolamines have been found in the product of the relative amounts of oxide of iaco. Various processes have been designed for the performance of some ethanolamine in particular, patents US 4,847,418 and US 5,545,757 to raise an excess of ammonia to obtain a pro- portion containing a greater proportion of MEA and / or Another modification on the reaction before making a first addition of the Crude ucto comprising mainly DEA and reacting the raw product again with ene at temperatures of 110 to 180 ° C to obtain TEA, DEA and secondary components, in TEA enido is 80%. Finally, it was rectified with phosphorous acid or hypophosphorous p-tanolamin with a purity greater than 99%.

Another process for obtaining ASD with a high za is described in patent US 6,683,217. It is a continuous process in which the amide and ammonia are reacted, then the unreacted ammonia is separated from inua; and finally s roducto to successive distillations until obtaining purity.

US Pat. No. 6,846,959 describes a process for alkanolamines using an Nolamines are removed from the bottom of the column erior processing and purification.

So far, the art documents? This is the obtaining of the ethanolamines with 0 of purity or the obtaining of mezlamines with some predominant species.

The present invention provides a mixture of alkanolamines with low content of amine, wherein the resulting mixture has as chemical intermediary the use of detergents such as lauryl sul-tanolamine and triethanol-lauryl ether sulfate textile-type triethanolamine methyl sulfate . In the cosmetics industry, use in the formation of emulsions and com to control the pH of products such anolamin, which makes it suitable to be useful formulations without exceeding the limits. Other benefits of the product here are that it has an extremely high APHA color number which is very appreciated by the formulators to have a freezing point lower than the 21 ° C aration which presents the Trietanoam as an advantage for storage and storage. Therefore, it simplifies important ways required for its use.

TIV0S: (1) Providing a process to promote a mixture of ethanolamines and other amine subproducts that together are useful. olamines practically colorless, easy to industrially pulverize. 4) Provide a process for obtaining ethanolamines with a low anolamin content, where the obtained mixture is to be used in different formulations without exceeding maximums allowed by the FDA and the Euro Union.

Other objects of the invention will be to depart from the following description.

SUMMARY OF THE INVENTION According to the present invention, a process for producing a melamine with a low content of diethanolamine, reaction of ethylene oxide and ammonia is proposed. The cam performed in an ethoxylator reactor in which The use of textile softeners of the methyl triethanolamine type, fatty acid detergents, triethanolamine-containing detergents or lauryl ether sulpholamine, and for use in the resulting cosmetic industry has an APHA color number and a freezing point below that facilitates storage and storage. handling, to compar 21 ° C that presents the Trietanoamina 99%.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a diagram of the reactor used in the invention.

DETAILED DESCRIPTION OF THE INVENTION The process is carried out in two stages, or toxilation starting from ethylene oxide and ammonium pure ethanolamine, or mixtures thereof, for a product with similar properties.

ROCESO OF OBTAINING MIXTURE OF ETHANOLAMINAS ONIACO AND ETHYLENE OXIDE 1: In an ethoxylator reactor (10) (verifiably inertized by nitrogen purging between 5 and 20 lb / in2 (34.474-137.895 to 35.0 parts of aqueous ammonium hydroxide ammonia entrainment of between 20 and 50%, at line ( 11) The ammonium hydroxide is agonized at a temperature between 40 and 80 ° C, preferably 50 and 65 ° C.

After heating, the ethylene ad starts through line (12) until c n2 (68,948 kPa) in the reactor (10), the heating starts to start to extract the ammonia so that the temperature remains below The crude product has the following weight (percentage by weight): Monoethanolamine (MEA): 0 - Diethanolamine (DEA): 0 - Triethanolamine (TEA): 45 - Ethanolamine glycolether (GEA): 5 - A 2: The crude containment ethoxylation reactor (10) obtained in step 1, is cooled to between 30-70 ° C and is again inerted at a pressure between about 5 and 5 474-344.74 kPa). The material is heated At this time the material is cooled to a temperature below 50 ° C.

The product thus obtained presents the typical solution given in percentage by weight: MEA 0 - 1% DEA 0 - 3.5% TEA 65 - 85% GEA 10 - 35% PLO 1 A 1 In a 14-liter ethanol reactor with a pressure of 10 lb / in2 of nitrogen, 3,548 kg of aqueous hydroxide were charged with a concentration of 31% ammoniacal ammonia. it led to emptiness and warming. The product was analyzed by gas chromatography to determine its composition. Table 1 shows four batches made under the icions.

TABLE 1 A 2 7,122 Kg of crude product were loaded lots B, C and D and the results are shown in TABLE 2 The final product has a number of co r to 10 Pt-Co and a lower freezing point ROCESO OF OBTAINING MIXTURE OF ETANOLAMINES The reaction conditions in this device are similar to those indicated in the first modality, as indicated below: (Ethanol reactant reactor (10) is added to the reactor (10) between 5 and 20 lb / in2 895 kPa), the raw material is stirred and the temperature is 50-50. 150 ° C, preferably between 60 grams ethylene oxide (12) maintaining a reactor (10) of between 50 lb / in2 (344.74 kPa n2 (1,034.2 kPa) to complete between 0.5 ml of ethylene per mole of ethanolamine, way pe 1.0 and 3.0 moles of ethylene oxide by olamine, and still more preferred, between 1.0 and 2 ethylene per mole of ethanolamine, At the end the aterial remains in digestion for 30 to 60 m and pressurized to 20 lb / in2 (137.90 kP rial was heated under agitation to a temper and the addition of 6,150 kg of oxide was started with the pressure less than 75 lb / in2 (517.11 k reaction ratio between 80 and 90 ° C. The temperature conditions were maintained for cooling afterwards, and gas chromatography results are shown in Table 3: TABLE 3 LOT E-l (% by weight) LOTE F-l (% in p MEA 0.2 0.34 DEA 0.80 0.74 TEA 76.42 80.23 GEA 22.58 18.69 The addition of 3.527 Kg of oxide with the pressure less than 75 lb / in2 (517.11 k reaction ratio between 100-120 ° C) was maintained under agitation until the temperature conditions were maintained. After cooling, the gas chromatography material is shown in Table 4: TABLE 4 resulting product has a number ion less than 75 lb / in2 (517.11 kPa) and the temperature between 120 - 150 ° C. At the end of the temperature conditions, the temperature was cooled by 30 minutes. The material was analogous of gases resulting in the composition of abla 5: TABLE 5 The resulting product has a number less than 10 Pt-Co and a freezing point in 10 ° C.

Claims (1)

1. CLAIMS 1. A process of manufacturing an amine olamines and glycol ethers from ene and ammonia, the process is characterized by the following steps: a) Feed an ethereal reactor inert with nitrogen and pressurized, with ammonium hydroxide; b) Submit the ammonium hydroxide to agitation; c) Add ethylene oxide to the reactor orción of 2 to 3 moles of oxide for each mole of hmonium; d) Keep the reagents under condition until completing the dual oxide reaction; h) Add again ethylene oxide at a ratio that varies between 0.5 and 2.0 moles of ethylene per mole of crude product; i) Keep the reagents under condition for the time necessary to complete the ethylene oxide and thus obtain a m amine and amine glycol ethers with a cont oolamine less than or equal to 3.5% by weight. 2. The process according to claim 1, step (a) the reactor is kept pressurized imediately 34,474 kPa and 137,895 kPa. 3. The process according to claim 1, step (a) the reactor is kept pressurized 4. The process according to claim 1, ammonium hydroxide solution which is added in - 7. The process according to claim 1, while the addition of the ethylene oxide in the pasion is maintained below 827.37 kPa. 8. The process according to claim 3, step (d) the reaction time is between coughs. 9. The process according to claim 1, step (e) removal of the residual ammonia at a pressure lower than 68,948 kPa and at a temperature of 150 ° C. 10. The process according to claim 1, resulting from the first ethoxylation of the composition given in percentage by weight: MEA: 0 - 7% DEA: 0 - 20% TEA: 45 - 85% 14. The process according to claim e in step (g) and the temperature is found ° C. 15. The process according to claim 1, step (g) the reactor is kept presure 344.74 kPa and at a temperature of 85 ° 16. The process according to claim 1, step (h) the pressure is between 344.7 and 4.20 kPa. 17. The process according to claim 1, step (h) the pressure is 413.69 kPa. 18. The process according to claim 1, step (i) the reaction is carried out for a period ranging from 30 to 60 minutes. 19. The process according to claim 1, step (i) the temperature varies from 60 to 90 ° C. "" 22. The process according to claim 1, final product has a color number APHA me or. 23. The process according to claim 1, final product has a freezing point at 10 ° C. 24. A product obtained from n any of claims 1 to 23. 25. The use of the product obtained to that claimed in claims 1 to 23 sentence of a softening composition of triethanolamine fatty acid texturyl sulfate 26. The use of the product obtained to that claimed in claims 1 to 23 of detergents such as lauryl sulfolane or laurel ether sulfate of triethanolamine In any proportion, the process is characterized by the following steps: (a) Feed a reactor in an inert state with nitrogen, with olamine (s); (b) Pressurize the reactor and heat the a of step (a); (c) Add to the reactor between 0.5 and 5 ethylene, per mole of ethanolamine; (d) Keep the reagents under condition for the time necessary to complete the ethylene reaction; (e) Cool the material and thus obtain an amine tanolamines and glycol ethers with a continolamine equal to or less than 3.5% by weight. 29. The process according to the claim 32. The process according to claim e in step (b) the raw material is heated to 80-90 ° C. 33. The process according to claim e in step (c) is added between 1 and 3 moles of ene per mole of ethanolamine. 34. The process according to claim e in step (c) is added between 1 and 2 moles of ene per mole of ethanolamine. 35. The process according to claim e in step (c) the pressure is maintained between 5.74 kPa) and 150 lb / in2 (1.034.2 kPa). 36. The process according to claim e in step (c) the pressure is less than 517.11 kP 37. The process according to claim e in step (d) the reaction is carried out "- 40. The process according to the claim and the product has a freezing point at 10 ° C. 41. A product obtained from n any of claims 23 to 40. 42. The use of the product obtained in accordance with claims 23 to 40, sentence of a softening composition of triethanolamine fatty acid texturyl sulfate 43. The use of the product obtained in accordance with claims 23 to 40, sentence of detergents such as lauryl sulfolane or triethanolamine laurel ether sulfate 44. The use of the product obtained for this purpose according to claims 23 to 40, sentence of cosmetic formulations.