Method of preparing neodymium-carboxylate component of diene hydrocarbon polymerization catalyst

FIELD: polymerization catalysts.

SUBSTANCE: invention, in particular, relates to synthetic rubber production and can be use in petrochemical industry. Invention proposes reaction of neodymium oxide or salt with C8-C20-carboxylic acid at acid-to-neodymium molar ratio between 2.2:1 and 5.0:1 in solvent and in presence of halogen-containing acid and/or Lewis acid at continuous stirring. Reaction proceeds directly upon dispersing and continuous renewal of reaction surface, milling surface ranging from 0.055 to 5.0 m2 per 1 L reaction mixture volume. Above-mentioned dispersing and continuous renewal of reaction surface are performed both consecutively and simultaneously for 1.0-3.0 h and, if necessary, reaction mixture is recycled. When consecutively carrying out both processes, dispersing is effected until conversion 75-85% is attained, after which reaction of neodymium oxide or salt is completed at continuous renewal of reaction surface during 0.5-1.0 h.

EFFECT: increased conversion of neodymium oxide or salt to 100% and reduced losses of raw materials and power.

8 cl, 1 dwg, 11 ex

 

The invention relates to a technology for catalyst components for the polymerization of diene hydrocarbons upon receipt of synthetic rubber and can be used in the petrochemical industry.

A method of obtaining metallocarborane catalyst components for the polymerization of conjugated dienes, synthesized by the interaction of aqueous solutions of nitrates of the metals with carboxylic acid dissolved in the hydrocarbons under the action of ammonia or amines, for example, processing of neodymium nitrate organic acid, followed by removal of water by azeotropic dehydration receive readingabout component for the synthesis of the catalyst for polymerization of conjugated dienes [U.S. Pat. U.S. No. 5220045].

The disadvantage of this method, despite 80-90% yields of the target product, is the need to use expensive enamelled equipment because of the very high acidity of the reaction medium, the presence of stage water washing of the obtained catalyst component and the high unit costs of the nitrates of metals and amines used to neutralize the environment.

In addition, readingabout have oligomeric or polymeric structure, the result of which contain some amount of water, salts and bases, which reduce the activity of the component of catalysis is ora, and catalyst for polymerization of conjugated dienes.

The closest in technical essence to the present method of obtaining readingabout compounds used as a component of catalyst for the polymerization of diene hydrocarbons, is the method of receiving notimportant used as the metal component in the coordination of the catalytic system and obtained by passing the stages of formation of a dispersion of neodymium oxide in an organic solvent selected from the group of aliphatic, cycloaliphatic solvents or their mixtures at a temperature of 20-100°interaction With oxide of neodymium with neodecanoic acid in the presence of hydrogen chloride in aqueous solution at a molar ratio neodecanoate acid: neodymium oxide from 6:1 to 15:1, the deposition of products of interaction and separation of the resulting notimportant with subsequent keeping it under nitrogen and direction on preparation of a catalyst for polymerization of diene hydrocarbons [U.S. Pat. U.S. No. 6482906 B1 from 16.05.2000].

The disadvantage of this method of obtaining notimportant is significant variation in the yield of the target product from 83 to 100% depending on the process temperature interaction of neodymium oxide and neodata new acids and a high content of neodecanoic is islote component of the catalyst, caused by a large excess neodecanoic acid relative to the neodymium oxide. This contributes to the high unit costs of the main raw materials for the production component of the catalyst, and the use of a component of a catalyst for the synthesis of the catalyst for polymerization of diene hydrocarbons will reduce the activity of the polymerization process and the quality of degassing and drying of rubber, increasing energy consumption.

In addition, the use of very dilute aqueous solutions of hydrochloric acid increases acidic waste and the need for expensive corrosion-resistant equipment.

The aim of the invention is to increase the yield of the target product and the efficiency of use of raw materials and energy resources.

This goal is achieved by the fact that in the proposed method of obtaining netinteractive component of catalyst for the polymerization of diene hydrocarbons by reacting the neodymium oxide or its salt with a carboxylic acid with 8 to 20 carbon atoms in the environment of the solvent is carried out in the presence of halogenated acids and/or Lewis acid under continuous stirring, interact oxide of neodymium or salts thereof, carboxylic acids and halogenated acids and/or Lewis acid in the environment of the solvent directly to the public in the processes of dispersion and the continuous renewal of the reaction surface, held under the surface of the milling 0,055-5.0 m21 l volume of the reaction mass; and the interaction of neodymium oxide or its salt is carried out at a molar ratio of carboxylic acid: neodymium from 3,3:of 1.0 to 5.0:1.0; processes of dispersion of neodymium oxide or salts thereof, carboxylic acids and halogenated acids and/or Lewis acid and the continuous renewal of the reaction surface carried out in sequence or simultaneously during 1,0-3,0 h, and if necessary, the reaction mass circulate; the sequential implementation of the processes of dispersion of the reaction mass and the continuous renewal of the reaction surface dispersion is carried out to achieve the conversion of 75-85%, then complete the interaction unreacted oxide neodymium or its salt with the continuous renewal of the reaction surface for 0.5-1.0 hours; synthesis catalyst component for the polymerization of diene hydrocarbons in the dispersion process is carried out, preferably, when the rotational speed of the stirrer 500-2000 min-1. The resumption of the reaction surface of neodymium oxide or its salt is carried out by means of bead, ball, disc mills, rotary-pulsation dispersant or other devices with a surface milling 0,055-5.0 m21 l volume of the reaction mass.

In contrast to the known method by implementing the process of obtaining a component of the catalyst when the dispersion products of interaction and continuous renewal of the reaction surface, decreasing the molar ratio of carboxylic acid: neodymium achieve reduction of specific consumption of raw materials and increase of output of readingabout, stabilize the content of the target product and carboxylic acids. Thanks to the continuous renewal of the reaction surface by the interaction of neodymium oxide or its salt with a carboxylic acid get readingabout with a very low content of unreacted carboxylic acids, salts, acids and water, than reach the high activity of the catalyst for polymerization of diene hydrocarbons. These help to increase the value of dry residue of the polymer solution and the reduction of energy consumption by obtaining a rubber.

In addition, increasing the purity of the catalyst component on the content of various impurities increase stabiles the ü the component of the catalyst and its shelf life, that is a very important factor in industrial conditions obtain diene polymers with a high content of CIS-1,4-units.

The proposed method for netinteractive component of catalyst for the polymerization of diene hydrocarbons is carried out, for example, shown in the drawing the schema as follows.

In the dissolver 1 line 2 serves the solvent, which is used as aliphatic, cycloaliphatic, aromatic hydrocarbons, mixtures thereof, halogenorganics connection, in particular hexane, cyclohexane, nefras, their mixtures, chlorobenzene. After filling dissolver solvent to the specified level include the stirrer 3 and begin heating dissolver hot circulation water supplied to the jacket 4 by line 5. Start downloading the neodymium oxide or its salt, which is served by lines 6 and 7, respectively. Halogenated acid and/or Lewis acid is served in the dissolver 1 pump 8 through line 9 in an aqueous solution, prepared in the apparatus 10. The water in the apparatus 10 is directed through line 11. If necessary, line 12 in the apparatus 10 is injected substances forming oxide of neodymium or its salts, carboxylic acid stable complexes, such as water, hydrogen chloride, acetylchloride, alkylphosphate, amines, acetylacetone. As salts of neodymium is used, for example, nitrate ambiguity of the mA, the neodymium chloride and its hydrates, neodymium perchlorate hydrate, neodymium sulfate hydrate, phosphate neodymium.

As the halogenated acid is used, for example, hydrogen chloride, hydrogen fluoride, and as Lewis acids are used, for example, aluminum chloride, neodymium chloride, chlorides of iron, chlorides of silicon, zinc, Nickel, tin, cobalt. The Lewis acid is also served in the apparatus 10 through line 13.

As carboxylic acids using carboxylic acid with 8 to 20 carbon atoms, served in the dissolver 1 through line 14. The molar ratio of carboxylic acid to the neodymium withstand equal(3,3-5,0): 1,0.

The dispersion of neodymium oxide or its salt in dissolvere 1 in the environment of the solvent, carboxylic acid and initiator is carried out at a temperature of 50-85°preferably 55-70°when the rotational speed of the stirrer 100-3000 min-1preferably 500-2000 min-1If necessary, the dispersion process is carried out at the circulation of the reaction mass held by means of a pump 15, the feed of the reaction mass along the line 16 again in the dissolver 1.

Continuous renewal of the reaction surface, held by surface milling 0,055-5.0 m21 l volume, preferably at 0.5-1.5 m21 l volume, carried out by means of bead, ball, disc mills, rotary-pulsation dispersant and the other devices, ensuring the achievement of the specified surface milling unreacted oxide of neodymium or its salts in the process of interacting with a carboxylic acid, a halogen-containing acid and a Lewis acid and other initiators of the process.

Speed metania surface when milling is kept in the range 20-500 min-1.

The process of dispersion of neodymium oxide or salts thereof, carboxylic acids, halogenated acids and/or Lewis acid and the continuous renewal of the reaction surface carried out in sequence or simultaneously during 1,0-3,0 hours If necessary, the reaction mass circulate with multiplicity circulation from 1 to 10 h-1.

In contrast to the known method the implementation of the disperse and the continuous renewal of the reaction surface reach the intensification of the process of interaction of initial substances at the optimum temperature, precluding the formation of by-products and specific costs of the original substance is slightly higher than the costs calculated by stoichiometry. Through this process of obtaining netinteractive component of the catalyst interaction of neodymium oxide or its salt is carried out at a molar ratio of carboxylic acid: neodymium from 3,30:1 to 5.0:1.0 in. This allows achieving low carbon content to the slots in the component of the catalyst for polymerization of diene hydrocarbons, almost more than 2-3 times smaller than in the known method.

The sequential implementation of the processes of dispersion of the original substance reactions and continue the reaction surface of unreacted oxide of neodymium or its salts by milling the reaction mass after reaching 75-85% conversion of neodymium in netinteractive connection of the reaction mass from dissolver 1 pump 15 through line 16, then line 17 is sent to the device 18 and then through line 19 and 16 are returned to the dissolver 1. The reaction mass is subjected to the resumption of the reaction surface in the mill, the rotary pulse jet disperser, or other apparatus for 0.5-1.0 h, then the reaction mass display sucks on line 20 in the apparatus 21, which carry out the separation of the water layer, the output line 22 and the hydrocarbon layer is selected as the target product - neodammerung component of catalyst according to line 23.

While carrying out the processes of dispersion of neodymium oxide or salts thereof, carboxylic acids and/or Lewis acid and the continuous renewal of the reaction surface of unreacted oxide of neodymium or its salts duration of the interaction process is kept in the range of 1.0 to 3.0 h, and if necessary, the reaction mass to circulate.

In this case, the reaction is Assu from dissolver 1 pump 15 through line 16 and 17 are passed through the apparatus 18 and forth on lines 19 and 16 or line 24 of its return in the dissolver. These circuits perform using valves 25 and 26.

In contrast to the known method of obtaining netinteractive component of the catalyst of the proposed method provide the target product with a low content of salts and acids, which becomes possible due to the resumption of the reaction products surface interaction and more effective use.

Note that the device 18, which may use a rotary finger-taps type CPF or mixers with emitter type GARTH, the rotary pulse jet dispersers, disk mixers, ball or bead mill, if necessary, set before the pump 15 (not shown in the figure). In addition, the input and reaction water, and the solvent is optionally removed by evaporation in a rotary or conventional evaporators under vacuum at temperatures of 50-60°With (not specified).

Prepared readingabout component of the catalyst is fed to the polymerization of diene hydrocarbons, which are preferably used butadiene and isoprene.

The proposed method for netinteractive component of catalyst for the polymerization of diene hydrocarbons is illustrated by the following examples.

Example 1

Readingabout component of the catalyst p is liberizatsii diene hydrocarbons receive the proposed method.

In a heated flask of 1 l, equipped with a mechanical stirrer with speed 1500 h-1and fitting for the conclusion of the reaction mass, load 78,16 g of purified hexane and 23,36 g of neodymium oxide. Stir the mixture and bring the temperature up to 55°With injected 2.0 ml fuming hydrochloric acid concentration of 35 wt%, diluted in 10 ml of water. Type of 78.47 g neodecanoic acid. The reaction mass is circulated through the apparatus, filled beads with a size of 2 mm diameter and a length of 5 mm and a total volume of 100 ml with surface milling 5.0 m2/l volume. Speed metania surface can withstand 25 min-1. The time of reaction between the oxide of neodymium with neodecanoic acid with simultaneous dispersion of products of interaction and the resumption of the reaction surface in the process of milling the reaction mass with beads incubated 1 h Ratio of circulation of the reaction mass 5 h-1The molar ratio of neodecanoic acid to the neodymium of 3.32:1,0.

Received 90,3 g neodecanoate neodymium in the form of a purple solution containing neodecanoate neodymium 46,9 wt.% and 3.9 wt.% neodecanoic acid. The output neodecanoate neodymium 100%.

According to the method output neodecanoate neodymium was 94%, the content of neodecanoate neodymium in the solution component of the catalyst to 45.9 wt.%, the content of neodecanoic the second acid value of 4.76 wt.%. Temperature interaction 55°C, the duration of interaction 1 h Molar ratio neodecanoate acid to the neodymium in the known method was 3,32:1,0.

Examples 2-4

Readingabout component of the catalyst was prepared by the proposed method.

In laboratory dissolver with variator and stirrer speed 2250 min-1download 2 liters of chlorobenzene, 80,5 g of neodymium acetate and 172,5 g neodecanoic acid (versatool acid) After reaching 75-85% conversion of neodymium acetate, the reaction mass discharged and subjected to continuous renewal of the reaction surface by means of ball and ball mills, disc mixer. After treatment for 0.5 to 1.0 hours at speed metania surface milling 50 min-1the product is unloaded and subjected to evaporation of the solvent under vacuum of 30 mm Hg and a temperature of 57°C. Then determine the content of notimportant, neodecanoic acid and the output of notimportant. Chlorobenzene received normal or oxidative chlorination of benzene on the catalyst contains free soluble chlorine or hydrogen chloride in amounts sufficient to process them without special additives.

The solution notimportant containing 87,3-87,4 wt.% component catalyst poly is erinacei diene hydrocarbons washed from acetic acid and after settling, separation from water used for preparation of catalyst for polymerization of diene hydrocarbons. Get 228,0 g of the solution component catalyst containing 91,2 wt.% neodecanoate neodymium. Neodecanoate neodymium at a molar ratio neodecanoate acid: neodymium equal to 4:1, has the formula Nd H(C9H19COO)4in particular, when using neodymium acetate.

Example 5

Neodecanoate neodymium get on the proposed method. In a glass flask with a capacity of 150 ml download 0,202 g setevogo aluminum chloride, to 2.9 ml of 40%aqueous solution of diphenyloxide in toluene (d=0,93 g/ml)of 5.06 g of neodymium oxide and 20.8 g neodecanoic acid. The molar ratio of neodecanoate acid: neodymium is 4,013:1,0. This mixture is heated to 60°With pre-submitting a flask of 60 ml of a mixture of cyclohexane with neprasam. Include the stirrer speed 1250 min-1the process continued for 1 hour, then unload and stirred bead mill with surface milling 2.5 m2/l volume at the temperature of 50°s speed metania surface milling 75 min-1within 1 hour. After sludge discharged to 85.2 ml purple solution neodecanoate neodymium containing 24,77g of neodecanoate neodymium (33.3 wt.% in the solution). The output neodecanoate neodymium 100%.

In the known method get neodecanoate neodymium exit 92 wt% and containing a solution of 5.5 wt.% neodymium 8,48 wt.% neodecanoic acid and 0.24 wt.% water.

Example 6

In a metal reactor with a stirrer with a capacity of 250 ml download 0,922 g setevogo aluminum chloride dissolved in 10 ml of water (pH of the solution 2,87 at 20°C), 80 ml of hexane and 11,68 g of neodymium oxide. The mixture was stirred at a rotational speed of the stirrer 1500 h-1and add 45 g neodecanoic acid.

The molar ratio of neodecanoate acid: neodymium is 3,76:1,0. The interaction is carried out for 1.5 hours at 55°C. Upload 122 ml (120,4 g) purple solution neodecanoate neodymium, which is placed in a ball mill with a surface milling 0,13 m2/l volume and subjected to the resumption of the reaction surface at a speed of Oltenia surface milling 35 min-1at a temperature of 50°C for 1 hour. The output neodecanoate neodymium 100%, the content of neodecanoate neodymium in a solution of 37.9 wt.%, neodecanoic acid - 7,65 wt.% and 10,69 wt.% water.

After settling and separation from water get to 108.8 g of the solution of neodecanoate neodymium containing 41,95 wt.% neodecanoate neodymium, 8,46 wt% neodecanoic acid and 0.28 wt.% water.

In the known method output neodecanoate neodymium amounted to 92 wt.%. Component of the catalyst contained 8,02 wt.% neodymium 11,58 wt.% free neodecanoic acid and 0.33 wt.% water.

Example 7

In a metal reactor with a capacity of 1 l load 23,36 g is xida neodymium, 180 ml of a mixture of cyclohexane with neprasam, 83,0 g neodecanoic acid, 10 ml, 0.88 mol/l solution of silicon tetrachloride in a mixture of cyclohexane with neprasam. Include the stirrer rotation speed 3000 min-1. Interaction in the process of dispersion spend 2 hours at a temperature of 50°C. the Molar ratio of neodecanoate acid: neodymium is 3,468:1,0. Then the reaction mass is unloaded and placed in a rotary pulse jet disperser with surface milling 1.5 m2/l reaction volume and speed metania surface milling 100 min-1. The resumption of the reaction surface is performed for 0.5 h at 50°C. Unload product in the amount of 290 ml. Output neodecanoate neodymium 100%of its content in the solution was 35.3 wt.%, the content of free neodecanoic acid of 4.05 wt.%.

Example 8

In a metal reactor with a stirrer with a capacity of 150 ml download 5.31g oxide of neodymium, 0,226 g setevogo aluminium chloride, of 0.182 g of acetylacetone and 19.6 g neodecanoic acid and 110 ml of a mixture of cyclohexane with neprasam. Begin the dispersion of the initial substances and carry out the process of interaction with the rotational speed of the agitator 2000 min-1and a temperature of 50°for 2.5 hours Unload 111,1 g of the reaction mass, which is treated in the mill surface milling 2.5 m2/l of volume at speed metania surface milling 75 mi the -1at a temperature of 50°C for 0.5 hours

The output neodecanoate neodymium 100 wt.%. The molar ratio of neodecanoate acid: neodymium equal to 3.58:1,0. The content of neodecanoate neodymium in solution 18,67 wt.%, free neodecanoic acid to 3.06 wt.%.

Example 9

In a round bottom flask with a capacity of 100 ml with a stirrer speed of 500 min-1enter 80 ml of chlorobenzene, 3.2 g of neodermata and 5.8 g of 2-ethylhexanol acid. This mixture is dispersed for 2.5 hours at a temperature of 70°With, then unload in a bead mill with surface milling 2.5 m2/l volume and the process of interaction with the resumption of the reaction surface at a speed of Oltenia surface milling 75 min-1for 0.5 h at a temperature of 50°C. Unload the product and after loading into a vacuum evaporator the solvent is distilled off at 50°and a vacuum of 10 mm RT. Art. Obtain 7.2 g of the neodymium carboxylate. The yield of 94.5 wt.% due to insufficient dosing 2-ethylhexanoic acid (molar ratio of 2-ethylhexanoate acid: neodymium is 3,732:1,0). The neodymium carboxylate of the formula Nd H(C8H15COO)4. In the known method output carboxylate was 74%.

Example 10

In a flask with a capacity of 250 ml, equipped with a magnetic stirrer, under nitrogen atmosphere download 46,4 mmole of butadiene-1,3, dissolved in 75 ml of a mixture of cyclohexane with neprasam, 7 the l 1.1 mol/l solution of triisobutylaluminum (CHIBA) and 4,069 g of the solution of neodecanoate neodymium, obtained in example 5. Add 3 ml of 1.0 mol/l solution of diisobutylaluminium (DIBAH), stirred for 30 minutes and add 10 ml of 0.07 mol/l solution of ethylaminoethanol (EACH) 2,31 mmole (chlorine). The obtained catalytic complex used for the polymerization of butadiene-1,3.

Charged to the reactor 1100 g of butadiene-1,3, dissolved 8.4 l of a mixture of cyclohexane with neprasam, heated to a temperature of 40°add 1.65 mmole catalytic complex, 6.8 ml of 1.0 mol/l solution DEBUG and conducting the polymerization of butadiene-1,3 in 3 hours at a temperature of 55-60°With up to a conversion of 93%. Define the structure of the polybutadiene. The content of CIS-1,4 units is 98.5%, a polydispersity of 3.14.

Example 11

In the flask, as in example 10, the load of 7.6 mmol of butadiene-1,3, dissolved in 50 ml of a mixture of cyclohexane with neprasam, 6.9 ml of 1.1 mol/l solution CHIBA and 2.9 g of the solution of neodecanoate neodymium (1.5 mmole)obtained in example 7. Reaction to withstand the weight 19 hours at 20°and add it to 2.9 ml of 1.0 mol/l solution DIBAG. Stirred for 5 minutes and use a catalytic system for polymerization.

Charged to the reactor 1045 g of butadiene-1,3, dissolved in 8.2 l of a mixture of cyclohexane with neprasam, heated to a temperature of 40°With add of 1.57 mmole obtained by catalytic complex, 7 ml of 1.0 mol/l solution DEBUG and 22.5 ml,1 mol/l of diisobutylaluminium (DIBAH). Conduct polymerization for 3 hours at 55-60°With up to a conversion of 97%. Get polybutadiene content of CIS-1,4-units 98,8%, a polydispersity 2,84.

As can be seen from the examples, the proposed method of obtaining netinteractive component of catalyst for the polymerization of diene hydrocarbons reach almost full interaction with neodymium neodecanoate acid and thereby gain polymers with a high content of CIS-1,4-units.

1. The method of obtaining netinteractive component of catalyst for the polymerization of diene hydrocarbons by reacting the neodymium oxide or its salt with a carboxylic acid with 8 to 20 carbon atoms in the environment of the solvent is carried out in the presence of halogenated acids and/or Lewis acid under continuous stirring, wherein interact oxide of neodymium or salts thereof, carboxylic acids, halogenated acids and/or Lewis acid in a solvent environment directly in the processes of dispersion and the continuous renewal of the reaction surface, held by surface milling 0,055-5.0 m21 l volume of the reaction mass, and the interaction of neodymium oxide or its salt is carried out at a molar ratio of carboxylic acid: neodymium from 3,3:1,0 to 5,0:1,0.

2. The method according to claim 1, characterized in that the processes of disperse the Finance of neodymium oxide or its salt, carboxylic acids, halogenated acids and/or Lewis acid and the continuous renewal of the reaction surface carried out in sequence or simultaneously during 1,0-3,0 h, and if necessary, the reaction mass to circulate.

3. The method according to claim 1, characterized in that the sequential processes of dispersion of the reaction mass and the continuous renewal of the reaction surface dispersion is carried out to achieve the conversion of 75-85%, then complete the interaction unreacted oxide of neodymium or its salt with the continuous renewal of the reaction surface for 0.5-1.0 hours

4. The method according to claims 1 to 3, characterized in that the solvent used is preferably an aliphatic, cycloaliphatic, aromatic hydrocarbons, mixtures thereof, organohalogen compounds.

5. The method according to claim 1, characterized in that the synthesis component of the catalyst for polymerization of diene hydrocarbons in the process of dispersion is conducted preferably at a frequency of rotation of the agitator 500-2000 min-1.

6. The method according to claim 1, characterized in that the Lewis acid is introduced into the process dispersion is preferably in the esters, acetylacetone, acetonitrile, chloroparaffin, chlorobenzene.

7. The method according to claims 1 to 3, characterized in that the resumption of the reaction surface is oxide of neodymium or its salt is carried out with the help of beaded, ball, disc mills, rotary-pulsation dispersant or other devices with a surface milling 0,055-5.0 m21 l volume of the reaction mass.

8. The method according to claim 1, characterized in that the interaction of neodymium oxide or its salt with a carboxylic acid optionally initiate the substances formed with them a stable complexes, for example, ethers, water, hydrogen chloride, acetylchloride, alkylphosphate, amines, acetylacetone.



 

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