- Synthesis and thermal properties of spiro phosphorus compounds
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Intumescent materials, 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro- [5,5]-undecane-3,9-dioxide and 3,9-dichloro-2,4,8,10-tetraoxa-3,9- diphosphaspiro-[5,5]-undecane having the capacity to produce dehydrating agent, blowing agent, and undergo carbonization during burning have been synthesized. The thermal behavior of the synthesized materials was investigated using differential thermal analysis, thermal volatilization analysis, programmed vacuum pyrolysis-mass spectrometry, flash pyrolysis-mass spectrometry and off-line pyrolysis-gas chromatography-mass spectrometry. The materials show exothermic degradation after 250 °C. Monitoring the release of hydrogen chloride and water, the blowing agents for the production of carbon foam, clearly indicated the superior performance of the pentavalent phosphorus compound over the trivalent phosphorus compound. The major gaseous degradation products released during pyrolysis showed the presence of sufficient quantities of several alkyl-substituted benzenes and fused aromatics. Suitable degradation mechanism has been proposed and discussed to explain the formation of various organics during thermal degradation.
- Vijayakumar, Chinnaswamy Thangavel,Mathan, Nagarajan David,Sarasvathy, Vijayakumar,Rajkumar, Thangamani,Thamaraichelvan, Arunachalam,Ponraju, Durairaj
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- Catalyst ligand and preparation method and application thereof
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The invention belongs to the technical field of catalysis, and particularly relates to a catalyst ligand and a preparation method and application thereof. The chemical structure of the catalyst ligand is as shown in the formula (I). In-flight R1 Alkyl, cycloalkyl or aryl. The catalyst ligand molecule provided by the invention has a double PNP structure and specific steric hindrance, and when complexed with a chromium catalyst, a double PNP structure can coordinate with two Cr to form two catalytic activity centers, so that the active center is more concentrated, and therefore high catalytic activity is shown. The steric hindrance of the carbon chain structure between the two PNP can inhibit the growth of molecular chains in the polymerization process, making it more prone to the formation of low-carbon products, thereby avoiding the formation of polyethylene waxes and polymers. The ligand disclosed by the invention can enable the chromium catalyst to exhibit higher catalytic activity and catalytic selectivity in the ethylene selective oligomerization process, and has good industrial application value.
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Paragraph 0074-0076; 0084-0086
(2021/09/29)
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- Preparation method of 3,9 - difluoro -2, 4, 8, 10 - tetraoxygen -3, 9 - diphosphorus spiro [5.5] undecane (by machine translation)
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The invention discloses a preparation method of 3, 9 - difluoro -2, 4, 8, 10 - tetraoxygen -3 and 9 - diphosphorus spiro [5.5] undecane, and belongs to the field of organic synthesis. The intermediate 3, 9 - dihalo -2, 4, 8, 10 - tetraoxygen -3, 9 - diphosphorus spiro [5.5] undecane are distilled to obtain 3, 9 - difluoro -2, 4, 8, 10 - tetraoxygen -3, 9 - diphosphorus spiro [5.5] undecane. The method is low in raw material price, simple and convenient to operate and suitable for industrial production. (by machine translation)
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Paragraph 0021; 0022; 0023
(2020/07/15)
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- Novel high-temperature-resistant phosphite antioxidant ST-636 and preparation method and application thereof
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The invention discloses a novel high-temperature-resistant phosphite antioxidant ST-636 and a preparation method and application thereof. The preparation method comprises the following steps: S1, adding reaction mesitylene, pentaerythritol and phosphorus trichloride into a reaction container, and reacting to generate an intermediate, S2, vacuumizing the reaction container, and carrying out a reflux reaction, S3, adding new mesitylene, BHT, triethylamine and di-n-butylamine for reaction to obtain a reaction solution, S4, adding tri-n-butylamine and triethanolamine to carry out neutralization reaction to obtain a product mixed solution, S5, adding a filter aid type diatomite, and then carrying out hot filtration, S6, washing, filtering and drying the crystals, and S7, adding a sodium hydroxide aqueous solution, and carrying out a replacement reaction to obtain the di-n-butylamine. The novel phosphite antioxidant ST-636 prepared by the method has excellent heat-resistant stability and volatility resistance, is widely applied to special plastics with higher processing temperature, and effectively improves and enhances the high-melting processing heat stability, discoloration resistanceand fluid melting stability of the special plastics.
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Paragraph 0047-0050
(2020/10/20)
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- A double (2, 4 - dicumylphenyl) quarter [...] phosphite ester preparation method (by machine translation)
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The embodiment of the invention discloses a double (2, 4 - dicumylphenyl) quarter [...] phosphite ester preparation method. The reaction temperature - 5 - 10 °C, micro reduced pressure conditions, to pentaerythritol, amine hydrochloride salt catalyst, aromatic hydrocarbon solvent in dropwise phosphorus trichloride, phases up to 85 - 90 °C, pressure reducing reaction 1 hours, stop after the pressure of the nitrogen protection, to obtain [...][...] phosphite ester reaction solution; the above reaction liquid to heating up to 90 - 100 °C of 2, 4 - dicumyl phenol in the aromatic hydrocarbon solvent, pressure reducing reflux reaction for 4 hours, inject the nitrogen, adding and mixing the [...] reaction system becomes alkaline, cooling to room temperature, filter, to get double (2, 4 - dicumylphenyl) quarter [...] phosphite. The invention through the reaction condition, such as temperature, pressure, time, catalyst, the charging sequence and after treatment of the strict control, eventually get the yield high, narrow melting range, low acid value, excellent hydrolysis resistance performance of high performance products. (by machine translation)
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Paragraph 0027-0028; 0031-0032; 0034-0035; 0037-0038; 0040
(2019/02/06)
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- Synthetic process of antioxidant 626
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The invention discloses a synthetic method of an antioxidant 626, namely bis(2,4-di-tert-butylphenyl)pentaerythritol diphosphite. The method disclosed by the invention comprises the following steps: firstly adding a catalyst to a selected solvent, performing stirring, then adding phosphorus trichloride, introducing nitrogen gas, continuously performing stirring, then dropwise adding pentaerythritol, and absorbing the generated hydrogen chloride gas with a sodium hydroxide solution; purifying the reaction product to obtain a dichloropentaerythritol diphosphite solution; and then, dropwise adding the dichloropentaerythritol diphosphite solution to a 2,4-di-tert-butylphenol aqueous solution, introducing nitrogen gas, performing stirring, absorbing the hydrogen chloride gas generated by reaction with the sodium hydroxide solution, and purifying the reaction product to obtain the product. The method disclosed by the invention has the advantages that the adopted raw materials are low in price, the reaction is easy to perform, side reactions are few, the purity of the product is high, the reaction time is short, the storage time of the product is long, the product has good hydrolysis resistance and stability, and furthermore, the yield of the product is also very high.
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Paragraph 0034; 0035; 0036; 0040; 0042; 0044; 0046; 0048
(2018/07/30)
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- Preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant
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The invention relates to a preparation method of a bis(2,4-dicumylphenyl)pentaerythritol diphosphite antioxidant. The preparation method comprises the steps of dropwise adding phosphorus trichloride at a nitrogen environment in an existing system of pentaerythritol, a catalyst and a solvent so as to obtain dichlone pentaerythritol diphosphite reaction liquid, adding 2,4-dicumylphenol, heating to 130-140 DEG C in the presence of nitrogen to react, carrying out reduced pressure backflow reaction to obtain a reactant, adding organic amine to neutralize and regulate the reactant to be alkaline, continuing to carry out esterification reaction until reaction mediums are still alkaline, cooling, and filtering, so as to obtain bis(2,4-dicumylphenyl)pentaerythritol diphosphite. By controlling the reaction process, high-selectivity and high-yield bis(2,4-dicumylphenyl)pentaerythritol diphosphite with a spiral structure is obtained, the yield of the product is higher than 92%, the recovery rates of generated side effects and an unreacted raw material, namely 2,4-dicumylphenol are higher than 90%, the consumption of the raw materials is reduced, and the simple and feasible operability is realized.
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Paragraph 0021; 0022; 0025; 0026; 0028; 0029; 0031; 0032
(2017/07/04)
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- Amphipathic compound containing hindered phenol and pentaerythritol phosphite, synthetic method and application thereof
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An amphipathic compound containing both anti-static and anti-oxidizing functional groups is composed of a hindered phenol unit, a pentaerythritol phosphite unit, a crown ether unit and a straight-chain segment unit. The synergistic effect is controlled by controlling the length of the straight-chain segment unit to regulate the distance from the hindered phenol to the pentaerythritol phosphite units, and meanwhile, the content of effective functional groups in unit mass of the compound and the compatibility between the compound and resin are also controlled. Through migration of the crown ether group, the hindered phenol unit and the phosphite unit are migrated to the surface of the resin, so that oxidization in air can be eliminated more effectively. Because the hindered phenol unit and the pentaerythritol phosphite unit have large space structures, so that the crown ether structure is prevented from falling off from the surface of the resin, thereby increasing anti-static time of the compound. The compound can be used as an anti-static and anti-oxidizing agent for polypropylene or polyethylene.
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Paragraph 0108
(2017/01/02)
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- The method for manufacturing the same and diphosphonate threotol Pentaphenol (by machine translation)
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PROBLEM TO BE SOLVED: industrial advantage obtained by the method having excellent productivity, and, for a flame proofing agent when used as a good physical properties and high flame resistance imparting compound and a manufacturing method thereof. SOLUTION: the diphosphonate threotol Pentaphenol represented by eq. (1), (i) a median diameter of at most 30 μm volume, (ii) at least 98% purity, (iii) the specific halide compound content of at most 200 PPM spirocyclic diphosphonate threotol Pentaphenol. (Ar 1 and Ar 2 C6-20 each independently of substd./ non-substituted aryl group; R 3-R 6 are each independently H, C6-20 substituted and non-substituted aryl group, or C1-20 saturated or unsaturated, straight chain or branched alkyl group) selected drawing: no (by machine translation)
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Paragraph 0100
(2017/02/24)
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- Preparation method of phosphite antioxidant 9228
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The invention relates to a preparation method of a phosphite antioxidant 9228. The preparation method comprises the following steps: pentaerythritol and an organic solvent are added to a reactor, a catalyst and phosphorus trichloride are added while the mixture is stirred at the temperature of 50-60 DEG C, the mixture reacts at the temperature and then is heated to 100-120 DEG C slowly and subjected to a reflux reaction, and an intermediate dichloropentaerythritol diphosphite solution is obtained; 2,4-dicumylphenol and an organic solvent are added to the intermediate, the mixture is subjected to a reflux reaction under the action of a catalyst, the organic solvent is removed through distillation under reduced pressure, then a neutralization solvent and a neutralizer are added to the reaction system, a neutralization reflux reaction is performed, a crude product is filtered, re-crystallized, centrifuged, washed and dried, and the target products are obtained. The required raw materials are widely supplied on the market and low in price, and the preparation method has the advantages that reaction conditions are mild, control is simple and convenient, a byproduct HCl is easy to recover and the like and can meet large-scale production conditions of enterprises.
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Paragraph 0030; 0031
(2017/06/02)
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- PHOSPHORUS-CONTAINING COMPOUNDS AND POLYMERIC COMPOSITIONS COMPRISING SAME
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Phosphorus-containing compounds of formula (I): (I) wherein m, n, R, R1 and R2 are as set forth in the claims. The compounds of formula (I) can be used to provide polymers with flame retardant properties.
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Page/Page column 27
(2010/04/06)
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- Cyclic chlorophosphites as scaffolds for the one-pot synthesis of α-aminophosphonates under solvent-free conditions
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New α-aminophosphonates of the type (OCH2CMe 2CH2O)P(O)CH(NHCO2R)(R′) [6a-i, 7a-e, and 8a-c] have been synthesized in high yields by a three-component reaction using (OCH2CMe2CH2O)PCl (3), benzamide (or urethane or benzyl carbamate), and an aldehyde without using any catalyst under solvent-free conditions. This route can be readily adapted for bis-aminophosphonates as well as optically active binaphthoxy α-aminophosphonates; it also tolerates the phenolic -OH group as shown by the synthesis of hydroxy functionalized aminophosphonates. Partial hydrolysis of compounds 7a-d leads to products in which the phosphorinane ring is cleaved first. Compounds (OCH2CMe2CH2O)P(O)CH[NHC(O)Ph] (9-anthryl) (6f) and optically pure (R,S)-(-)-(C20H 12O2)P(O)CH(NHCO2Et)(Ph) (14a) were characterized by X-ray crystallography.
- Swamy, K. C. Kumara,Kumaraswamy, Sudha,Kumar, K. Senthil,Muthiah
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p. 3347 - 3351
(2007/10/03)
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- PROCESS FOR THE PRODUCTION OF PENTAERYTHRITOL DIPHOSPHONATES
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A process for producing a pentaerythritol diphosphonate represented by the formula (5) characterized by (A) reacting phosphorus trichloride with pentaerythritol in the presence of an inert solvent to obtain pentaerythritol dichlorophosphite (reaction (a)), (B) reacting the pentaerythritol dichlorophosphite with an aralkyl alcohol to obtain a pentaerythritol diphosphite (reaction (b)), and (C) heat-treating the pentaerythritol diphosphite in the presence of a halogenated compound on the condition of a temperature of from 80 to 300°C (reaction (c)): wherein Ar1 and Ar2, which may be the same as or different from each other, each represents a substituted or unsubstituted aryl group having from 6 to 20 carbon atoms, and R3, R4, R5 and R 6 which may be the same as or different from each other, each represents a hydrogen atom, a substituted or unsubstituted aryl group having from 6 to 20 carbon atoms, or a saturated or unsaturated hydrocarbon group having from 1 to 20 carbon atoms. According to the production process of the invention, a particular pentaerythritol diphosphonate capable of being utilized as a fire retarding agent and the like can be provided with high purity and high yield by an industrially advantageous process excellent in productivity.
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Page/Page column 16; 21
(2010/02/14)
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- Pentaerythritol diphosphite stabilizers and process
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Pentaerythritol diphosphites corresponding to the formula STR1 being useful for stabilizing organic materials against thermal, oxidative and actinic degradation and a process for the preparation thereof.
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