Method for production of diethylene triamine and other linear polyethylene polyamines

FIELD: organic chemistry.

SUBSTANCE: target products is produced by ethylene diamine transamination. Reaction is carried out at 135-180°C at pressure of 5-40 MPa in presence of hydrogen and catalyst particles containing 26-65 wt.% of metallic nickel on porous carrier.

EFFECT: high ethylene diamine conversion ratio and high selectivity in relate to target acyclic polyethylene polyamines under advantageous reaction conditions.

10 cl, 2 tbl, 1 ex

 

The technical field to which the invention relates.

The invention relates to a method for Diethylenetriamine and higher polyethylenepolyamines by transamination of Ethylenediamine. The method is characterized by a high degree of conversion of ethylene diamine and high selectivity of the formation of the acyclic polyethylenepolyamines, such as Diethylenetriamine. Cyclic amines such as piperazine, produced little.

The level of technology

The most desirable products upon receipt of ethyleneamines are acyclic, preferably linear ethylenamine containing primary and secondary amino groups. Ethylenamine containing heterocycles are of less interest for the industry. Thus, in U.S. patent 4568746 described a method of obtaining a composition amines containing a high ratio of Diethylenetriamine to piperazine, by transamination of Ethylenediamine in the presence of Nickel, cobalt or rhodium catalyst at a temperature of 170-210°and under a pressure of 7 MPa (1000 psi). Specifically described catalysts are Raney Nickel and Raney cobalt with the size of the catalyst particles 20-60 μm, rhodium supported on alumina, Ni/Re/B deposited on silicon dioxide, and Ni/Zr supported on kieselguhr. Catalysts of the type Raney Nickel or Raney cobalt is inconvenient in operation, the AK they are fragile and difficult to handle. In addition, the small particle size makes it inappropriate to continuous operation, and hinders the removal of the catalyst from the reaction mixture. On the other hand, the catalyst containing the medium, allow to obtain a relatively high yield of piperazine.

In U.S. patent 5410086 also disclosed a method of regulating the ratio Diethylenetriamine to the piperazine when transaminasemia Ethylenediamine in the presence of hydrogen and a hydrogenating catalyst, by controlling the hydrogen concentration in the liquid reaction phase. Preferred hydrogenation catalysts are catalyst of the Raney Nickel and Raney cobalt or Nickel/rhenium/boric catalyst.

In the working examples disclosed method transamination of Ethylenediamine, and the process is carried out in a tubular reactor loaded with a catalyst containing about 6.2 wt.% Nickel, 4.4 wt.% rhenium and 1.8 wt.% boron on the media.

In addition, in the United Kingdom patent 1508460 describes a method for Diethylenetriamine by transamination of ethylenimine in the presence of a catalyst containing at least one transition metal of group VIII of the Periodic table of the elements at a temperature of from 100 to 150°C, and the process is carried out until the degree of conversion of 70% or less. Preferably the catalyst is at least 20% of the volume of the reaction zone and the reaction time is from 5 to 10 hours.

A common problem of these methods transamination of Ethylenediamine with the formation of Diethylenetriamine and higher polyethylenepolyamines is the fact that at moderate temperatures and pressures they lead to the formation of too much a relative amount of cyclic ethyleneamines, such as piperazine, and/or that the degree of conversion of ethylene diamine is too low. Thus, a need exists for improvement of the method of obtaining a high degree of conversion of ethylene diamine and at the same time obtain the desired ratio between the target acyclic polyethylenepolyamine and cyclic polyethylenepolyamines under favorable reaction conditions.

Disclosure of inventions

The inventors found that the above aims can be achieved by implementing the method of transamination in mild conditions to conduct the reaction in the presence of a catalyst containing a large number of metallic Nickel on a porous oxide carrier. According to the present invention Diethylenetriamine and higher acyclic polyethylenepolyamine result of transamination of Ethylenediamine at a temperature of 135-180°C, preferably 150-165°C, under a pressure of from 5 to 40 MPa, preferably from 8 to 35 MPa, in the presence of hydrogen and catalyst particles, the content of asego lasts 26 to 65%, preferably 30-65 wt.% metallic Nickel on a porous oxide carrier, preferably containing aluminum oxide, silicon dioxide, or a mixture. Specified transamination can be conducted periodically, but preferred is a continuous process. At a temperature of from 145 to 165°and the degree of conversion of ethylene diamine of 4 to 30% with a high selectivity can be obtained acyclic polyethylenepolyamine. So, when the degree of conversion of 10% weight ratio of acyclic polyethylenepolyamine and cyclic ethylenimine in the reaction mixture can be higher than 20:1, and when the degree of conversion of 15% above 15:1. The corresponding ratio obtained in the working examples of U.S. patent 5410086 are much smaller.

The catalytically active portion of the catalyst according to the present invention includes a significant amount of metallic Nickel deposited on a porous oxide carrier. In addition, the catalyst may additionally contain a catalytically effective metals that are usually used in amination processes, such as cobalt, iron, copper, palladium, or mixtures thereof. These metals may be present as metals in a total amount from 0.1 to 12 wt.% from the amount of metallic Nickel. Usually Nickel and any additional metals are the answer to the public for the catalytic effect when transaminasemia.

In addition, the catalytic effect may be enhanced due to the presence of small amounts of other metal, in order to achieve improved selectivity for the desired products. These promoters may be present as metals in a total amount from 0.1 to 15 wt.% from the amount of metallic Nickel. Examples of suitable promoters are calcium, magnesium, strontium, lithium, sodium, potassium, barium, cesium, tungsten, iron, ruthenium, zinc, uranium, titanium, rhodium, palladium, platinum, iridium, osmium, silver, gold, molybdenum, rhenium, cadmium, lead, rubidium, boron and manganese. So, for example, rhenium has a significant positive effect on the selectivity and degree of conversion, whereas ruthenium has the tendency to decrease the degree of conversion, but greatly increases the selectivity for acyclic polyethylenepolyamines.

Examples of suitable porous oxide carriers are silica or various forms of alumina, such as alpha-, Delta-, theta - and gamma-form, or mixtures thereof. Preferably, the content of aluminum oxide is at least 25% by weight of the carrier. In addition, the carrier may contain small amounts of other oxide materials, such as titanium dioxide, magnesium oxide and zirconium dioxide. Particularly preferred are the aluminum oxide is or combinations of aluminum oxide along with silicon dioxide, containing at least 25 wt.% aluminum oxide. The internal surface area of the carrier may vary from 20 to 1000 square meters per gram of the carrier, preferably from 40 to 400 m2/, Typically the carrier is 30-74% of total weight of the catalyst. In preferred embodiments the embodiment of the invention the transamination catalyst contains Nickel promoted with ruthenium, rhenium, palladium or platinum on a porous carrier containing alumina or alumina in combination with silicon dioxide. The catalytically active surface of the catalyst is usually from 10 to 70 square meters per gram of catalyst. Typically, the catalyst has a particle size that at least 80%, preferably at least 95 wt.%, have a size between 0.1 and 10 mm, preferably between 0.2 and 5 mm

The transamination catalyst can be obtained by initial co-precipitation of Nickel salts and salts of any additional and/or promoting metals, such as nitrate salts, granular media according to the invention in an alkaline solution or by impregnation of a granular carrier salts of metals. In addition to nitrate salts most commonly used salts are the acetate, acetylacetonate, ammoniumsulfate, borate, bromide, carbonate, chloride, chromite, citrate, cyanide, 2-ethylhexanoate, fluorine is d, formate, hydroxide, hydroxyacetate, iodide, methoxide, 2-methoxyethoxy, nitrosylchloride, nitrosylated, octanoate, oxalate, perchlorate, phosphate, sulpham, sulfate, and tetrafluoroborate. Sediment and impregnated substance respectively washed with deionized water, pressed into the form or extruded. Then, the resulting granules can be dried in air followed by calcination in air at a temperature in the range of 200-1200°usually in the range of 300-500°C, depending on the temperature of decomposition of the salts used, as these salts are transformed into oxides. Finally, metal oxides reduced to metals in the presence of hydrogen at a temperature of 150-600°C, depending on the nature of metal oxides, until it reaches the desired degree of recovery. When the catalyst contains two or more metals, you can use the United way of deposition and impregnation. Suitable methods of preparation of the catalyst is additionally described in M.V.Twigg, J.T.Richardson, Appl. Catal. A 190 (2000) 61-72, E. Kis et al., Polyhedron 17, 1 (1998) 27-34; A.Baiker, W.Richarz, Syn. Comm. 8 (1) (1978) 27-32.

The way transamination can be advantageously carried out both in continuous and in periodic mode. In a continuous process hydrogen and Ethylenediamine miss accordingly, as the gas and liquid mixture under pressure through a stationary the th or fluidized bed of catalyst at the desired temperature. In the case of the solid catalyst, at least 80% of the catalyst particles, preferably at least 95% by weight of the catalyst particles have a size of from 0.5 to 10 mm, preferably from 1 to 5 mm In the fluidized bed, at least 80% of the catalyst particles, preferably at least 95% by weight of the catalyst particles have a size of from 0.1 to 2 mm, preferably from 0.2 to 1 mm, the resulting reaction mixture contains the transamination products, such as Diethylenetriamine, Triethylenetetramine and piperazine, unreacted Ethylenediamine, ammonia released in the process of transamination, and hydrogen. Usually this reaction mixture is treated, first separating low molecular weight compounds, hydrogen and ammonia from unreacted Ethylenediamine and various transamination products that are subjected to fractional distillation. Hydrogen and Ethylenediamine back in the process.

The presence of hydrogen in the process of transamination provides a high yield of the desired acyclic polyethylenepolyamines and suppresses or reduces the poisoning of the catalyst. Typically, the amount of hydrogen is 0.1 to 3 moles per 1 mole of ethylene diamine. It is desirable to maintain a significant portion of the hydrogen and ethylene diamine in the liquid phase. Thus, the pressure in the reactor will depend mainly on the reaction temperature, but also the and the number of hydrogen and ethylene diamine. Since the temperature is moderate, the pressure will also be reasonable and appropriate is between 5 and 40 MPa, preferably between 8 and 35 MPa, and the temperature is 135-185°C, preferably 145-165°C. Under these conditions the degree of conversion of ethylene diamine is satisfactory at high selectivity for linear polyethylenepolyamines.

The implementation of the invention

Example

The crate containing one of the catalysts according to table 1, placed in an autoclave equipped with a stirrer and a temperature controller. Then the autoclave rinsed with gaseous nitrogen and load it with 120 g of ethylene diamine. After closing the autoclave, it is injected hydrogen to a pressure of 30 bar, and with stirring the contents of the reactor are heated to the reaction temperature and maintained at this temperature for 4 hours, then the process stops, reducing the temperature of the reaction mixture. The reaction mixture is analyzing the content of Ethylenediamine (EDA), Diethylenetriamine (DETA), higher acyclic polyethylenepolyamines (VAP) and piperazinone joints (PIP). The results of transamination are given in table 2.

From these results it is evident that the catalysts according to the invention have a high activity already at 150°C. At a temperature of about 150-165°With the catalysts according to the obreteniyu have a high selectivity for the formation of Diethylenetriamine and polyethylenepolyamines, as well as providing a satisfactory degree of conversion. The presence of ruthenium additionally improves the selectivity, while the rhenium increases both selectivity and degree of conversion. At low temperature also reduces the pressure at which the hydrogen is present in the liquid phase. Experiments a and b are comparative tests in which there is an unsatisfactory combination of a low degree of conversion and low selectivity towards formation of acyclic compounds.

Table 1

Catalysts transamination
Experience No.Media, wt.%Nickel, wt.%Other metals, wt.%The active surface of the catalyst, m2/gCatalyst
Size mmThe quantity g
1Aluminum oxide, 10055-311,610,2
2Aluminum oxide, 10055-311,69,1
3Aluminum oxide, 10047-143,2 10,2
4Aluminum oxide, 10047-143,210,0
5Aluminum oxide, 10047-143,210,0
6Aluminum oxide, 50/

Silicon dioxide, 50
60-351,210,2
7Aluminum oxide, 50/

Silicon dioxide, 50
60-351,210,3
8Aluminum oxide, 50/

Silicon dioxide, 50
60-351,2the 10.1
9Silicon dioxide, 10038-321,210,2
10Aluminum oxide, 10033-84,810,2
11Aluminum oxide, 10033-84,810,8
12Aluminum oxide, 50/

Silicon dioxide, 50
600,75 EN*1>351,29,8
13 Aluminum oxide, 50/

Silicon dioxide, 50
600,75 EN*1>351,28,7
14Aluminum oxide, 50/

Silicon dioxide, 50
604,5 EN*1>3b1,28,6
15Aluminum oxide, 50/

Silicon dioxide, 50
600,75 Re*2>351,28,0
16Aluminum oxide, 50/

Silicon dioxide, 50
600,75 EN*3>351,2
AndAluminum oxide, 10016-64,87,2
InSilicon dioxide, 10015-103,27,4
*1impregnation with ruthenium chloride
*2impregnation of ammonium perrhenate
*3the impregnation nitrosylation ruthenium

Table 2

The results of transamination
Experience No.Temperature is, °The degree of transformation, ED, %The transamination products, wt.%The weight ratio*
PIPDEATH metalWAP
116027,311,871,616,47,5
215511,37,584,67,612,3
317038,415,862,621,35,3
416220,49,178,6to 12.010,0
516015,0a 4.987,77,219,5
61509,1a 3.9to 92.13,724,3
715215,16,086,77,1the 15.6
816038,015,165,119,6the 15.6
917023,816,0to 59.624,15,2
10170 52,320,625,953,2the 3.8
1115013,812,163,124,57,3
1217042,714,563,321,85,9
13150of 5.42,295,91,144,5
141503,51,597,30,064,1
1515015,45,884,314,516,1
1615011,24,089,26,323,6
And1705,532,8588,32,0
In1702,828,566,43,72,5
* (DETA+VAP)/PIP

1. The method of obtaining Diethylenetriamine and other linear polyethylenepolyamines by transamination of Ethylenediamine, characterized in that the reaction is carried out at a temperature of 135-180°under the pressure of 5-40 MPa, in the presence of water is ode and of the catalyst particles, containing from 26 to 65 wt.% metallic Nickel on a porous oxide carrier.

2. The method according to claim 1, characterized in that the reaction temperature is 145-165°C.

3. The method according to claim 1 or 2, characterized in that the medium contains aluminum oxide, silicon dioxide, or a mixture containing aluminum oxide and silicon dioxide, and the catalyst contains from 30 to 65 wt.% metallic Nickel.

4. The method according to claim 3, characterized in that the carrier is an alumina or a mixture of aluminum oxide and silicon dioxide containing at least 25 wt.% aluminum oxide.

5. The method according to any one of claims 1 to 4, characterized in that the catalyst has a particle size that at least 80 wt.% particles have a size of from 0.1 to 10 mm

6. The method according to any one of claims 1 to 5, characterized in that in addition to metallic Nickel catalyst also contains, as metals, cobalt, iron, copper, palladium, or mixtures thereof in a total amount from 0.1 to 12 wt.% in the calculation of the amount of metallic Nickel.

7. The method according to any one of claims 1 to 5, characterized in that the catalyst also contains a metal selected from the group consisting of calcium, magnesium, strontium, lithium, sodium, potassium, barium, cesium, tungsten, iron, ruthenium, zinc, uranium, titanium, rhodium, palladium, platinum, iridium, osmium, silver, gold, molybdenum, rhenium, cadmium, lead, rubidium, boron, Morgans is or their mixture in a total amount of metal from 0.1 to 15 wt.% in the calculation of the amount of metallic Nickel.

8. The method according to claim 7, characterized in that the metal is rhenium, ruthenium, palladium or platinum.

9. The method according to any one of claims 1 to 8, characterized in that the method is a continuous process.

10. The method according to claim 9, wherein the amination is carried out in a tubular reactor containing a fixed catalyst bed.



 

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