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Preparation method of phosphite ester

A technology of phosphite and chlorophosphite, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Major problems, to achieve the effect of simplifying the process, reducing the difficulty and increasing the product yield

Active Publication Date: 2010-03-31
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0037] (3) Maintenance of the required reaction temperature is difficult due to high exothermicity,
[0038] (4) Due to the high viscosity of the product, the crystal form of the product is not good or the viscosity is too high,
[0039] (5) The content of chloride ions in the product is relatively high, and chloride ions will poison the Rh catalyst in the hydroformylation reaction
Therefore, the phosphite prepared by the above method is not suitable for Rh ligand
[0040] (6) The intermediate product chlorophosphite needs to be purified, which reduces the yield
However, this method uses a large amount of basic ion exchange resin, which doubles the weight of the product, greatly increasing the production cost
Secondly, the toluene used in this method cannot completely dissolve the prepared phosphite, and some products will be taken away when the ion exchange resin is separated by filtration
And, the used toluene and hexane of this method can not finish recrystallization process well in preparation, therefore, still have some impurity, especially chloride ion can not be removed completely

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0081] Embodiment 1: use dichloromethane as solvent, reaction synthesis phosphite

Embodiment 11

[0083]

[0084] 14g 2,2'-biphenol and 40ml PCl 3 (2,2'-biphenol: PCl 3 The molar ratio is 1:6.1) reacted at 100°C for 4hr, then distilled off excess PCl 3, to obtain 19 g of residue, namely intermediate (2-9). Add 100ml of dichloromethane solvent to the intermediate (2-9) for dilution (the molar ratio of intermediate:dichloromethane is 1:21). Then 2,2'-dihydroxy-3,3'-di-tert-butyl-5,5'-dimethoxy-1,1'-biphenyl solution (2,2'-dihydroxy-3,3 '-Di-tert-butyl-5,5'-dimethoxy-1,1'-biphenyl 13.4g, triethylamine 50ml, dichloromethane 20ml, 2,2'-dihydroxy-3,3'- Di-tert-butyl-5,5'-dimethoxy-1,1'-biphenyl:triethylamine:dichloromethane molar ratio is 1:16.7:8.3) slowly drop into intermediate (2-9) solution (the molar ratio of intermediate to 2,2'-dihydroxy-3,3'-di-tert-butyl-5,5'-dimethoxy-1,1'-biphenyl is 2:1) , control the temperature at about -35°C, rise to room temperature after the dropwise addition, and stir for 12hr. The reactants still remain in solution state, add deionize...

Embodiment 12

[0086]

[0087] 14g 2,2'-biphenol and 40ml PCl 3 (2,2'-biphenol: PCl 3 The molar ratio is 1:6.1) reacted at 100°C for 4hr, then distilled off excess PCl 3 , to obtain 19 g of residue, namely intermediate (2-9). Add 80 ml of dichloromethane solvent to the intermediate (2-9) for dilution (the molar ratio of intermediate:dichloromethane is 1:17). Then biphenol solution (2,2'-biphenol 7g, triethylamine 20ml, dichloromethane 10ml, 2,2'-biphenol: triethylamine: the molar ratio of dichloromethane is 1: 6.7: 4.1) Slowly drop into the solution of intermediate (2-9) (the molar ratio of intermediate to 2,2'-biphenol is 2:1), control the temperature at about -20°C, rise to room temperature after the addition, and stir for 12hr . The reactants still remain in solution state, add deionized water to stir, let stand to separate layers, and take the lower organic phase. Heat to distill off the dichloromethane in the organic phase, and then recrystallize in hexane to obtain the product....

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Abstract

The invention discloses a preparation method of phosphite ester. The method comprises the following steps: dissolving chlorinated phosphite ester in dichloromethane, dissolving phenol in triethylamine or a mixed solution of triethylamine and dichloromethane, mixing the solutions to react and obtain raw product, and purifying the raw product through post-treatment to obtain the desired product. The preparation method of phosphite ester of the invention uses dichloromethane as reaction solvent to synthesize phosphite ester; the preparation process does not have any link with high viscosity material, the product is easy to clean and filtrate, the chlorine ions in the product can be removed conveniently and effectively and the quality of the product can be increased.

Description

technical field [0001] The present invention relates to the preparation method of phosphite. Background technique [0002] The main industrial uses of phosphite are as antioxidants, heat stabilizers, anti-aging agents, flame retardants in polymer materials such as plastics and rubber, and as intermediates and transition catalyst ligands for the production of organophosphorus pesticides. It is a hydroxyl derivative of phosphorous acid. According to the number of hydroxyl groups in the molecule, it can be divided into phosphorous acid monoester ROP(OH) 2 , Diphosphite (RO) 2 POH and Triphosphite (RO) 3 p. Among them, the monoester and most of the diester exist in the form of relatively stable tetrahedral phosphonate. [0003] The hydroxyl or alkoxy groups in the phosphite are substituted by halogen atoms to form monohalogenated or dihalogenated phosphites. Among the halogenated phosphorous esters, chlorophosphites are the most important, and they are often intermediates o...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
Inventor 蒋文张佶璘陈建伟
Owner SHANGHAI HUAYI ENERGY CHEM
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