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Preparation method of low chloride stabilizer

A technology of stabilizers and chlorides, applied in chemical instruments and methods, phosphorus organic compounds, compositions for inhibiting chemical changes, etc.

Inactive Publication Date: 2004-04-07
CLARIANT FIANCE (BVI) LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for some polyolefin applications where clarity is desired, hazy stabilizers can cause the polyolefin to appear somewhat hazy

Method used

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  • Preparation method of low chloride stabilizer
  • Preparation method of low chloride stabilizer
  • Preparation method of low chloride stabilizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Preparation of crude chlorinated benzene solution (35% w / w) of stabilizer mixture

[0050] In a jacketed glass reactor equipped with mechanical stirring and reflux condenser, under a nitrogen atmosphere, at an internal temperature of 75°C and stirring, reflux 90g (0.584mol) of biphenyl, 204g (1.53mol) of anhydrous chlorinated A mixture of aluminum and 305 g (2.218 mol) of phosphorus trichloride was used for 6 hours, during which time hydrochloric acid gas evolved and was captured with water in a scrubber. The reaction mixture was cooled, and excess phosphorus trichloride was distilled off at an internal temperature of 63-65° C. and a reduced pressure of 400-180 mbar. The crude melt was cooled to 35°C and diluted with 220 g of chlorinated benzene.

[0051] In a 2.5L jacketed glass reactor equipped with mechanical stirring and an external water-cooled reflux condenser, 482 g (2.334 mol) of 2,4-di-tert-butylphenol, 362 g (4.576 mol) of pyridine and 600 g of ch...

Embodiment 2

[0053] Example 2 : comparative example

[0054] 1000 g of the crude chlorinated benzene solution (35% w / w) of the stabilizer mixture obtained according to Example 1 was cooled to -10° C. and stirred for 1 hour. Filter the mixture with precipitated residual AlCl 3 - Separation of pyridine complexes. Gaseous ammonia (4.0 g) was bubbled through the filtrate at 0-5°C and maintained at this temperature for 1 hour. One portion shaken with water showed a pH of 8-9. Under the conditions of 100-110° C. / 350-310 mbar, finally 170° C. / 5,000mg / kg.

Embodiment 3

[0055] Example 3: Preparation of LCT stabilizer mixture with low chloride content.

[0056] 1000 g of the crude chloride benzene solution (35% w / w) of the stabilizer mixture obtained according to Example 1 was cooled to 5-10° C. under stirring. Add 5.0 g (0.01 mol) sodium tetraborate decahydrate (Na 2 B 4 o 7 10H 2 (0), 2.5 g (0.14 mol) of water and 5.0 g (0.04 mol) of sodium sulfate were stirred for 1 hour, during which time the solution glowed. Thereafter, 8.0 g (0.11 mol) of powdered calcium hydroxide, 5.0 g (0.09 mol) of calcium oxide and 5.0 g of diatomaceous earth Clarcel DIFB (RTM) were added and stirred at 25° C. for 3 hours. After filtration, evaporate the filtrate with a vacuum rotary evaporator under the conditions of 100-110°C / 350-310°C and finally 170°C / <10mbar. The residue yielded 350 g of LCT stabilizer mixture as a clear pale yellow solid (Tg = 65°C). The residual chloride content was 1,000 mg / kg.

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Abstract

A process for the preparation of a stabilizer mixture containing a low amount of chloride comprisinga) 50-80% by weight of tetrakis(2,4-di-tert-butylphenyl)biphenylene diphosphonite and its isomers,b) 5-25% by weight of bis(2,4-di-tert-butylphenyl)biphenylene monophosphonite and its isomers, andc) 5-25% by weight of a tris(2,4-di-tert-butylphenyl) phosphite, and where the sum of components (a), (b) and (c) is not greater than 100% by weight, by reacting biphenyl under Friedel-Crafts condition with phosphorus trichloride and aluminium trichloride and by reacting the product mixture with 2,4-di-tert-butyl-phenol in the presence of a tertiary amine or an aromatic amine and a solvent, separating the formed two layers, which process comprises treating the solvent layer with water, a base and a desiccant, separating the precipitate from the solution containing the stabilizer mixture and evaporating the solvent.

Description

technical field [0001] The present invention relates to a new process for the preparation of mixed stabilizers containing small amounts of chlorides, suitable for stabilizing organic materials against oxidation and thermal or photodegradation. Background technique [0002] US-4,075,163 discloses the synthesis of tetrakis(2,4-di-tert-butylphenyl)biphenylene diphosphonites suitable for stabilizing organic materials against oxidation and thermal or photodegradation (column 7, Table 1, compound 12). This compound is commercially available, for example, as Sandostab P-EPQ (RTM) from the Swiss company Clariant. [0003] EP-A-0 633 287 discloses in Example 1 that the commercial product Sandostab P-EPQ (RTM) is a mixture of several compounds comprising a) 65% by weight of tetrakis (2,4-di-tert-butyl Phenyl) biphenylene diphosphonite, b) 15% by weight of bis(2,4-di-tert-butylphenyl) biphenylene monophosphonite, c) 13 parts by weight of Tris(2,4-di-tert-butylphenyl)phosphite, d) 1....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K15/32C07F9/02C07F9/145C07F9/48C08K5/51C08K5/526C08K5/5393
CPCC08K5/51C07F9/02
Inventor V·V·托安R·萨拉特
Owner CLARIANT FIANCE (BVI) LTD