- Manufacturing method of alkylhypophosphorous-type compound by circulation-method, and manufacturing method of hypophosphorous-type flame retardants by circulation-method
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The present invention relates to a liquid reagent comprising a hypophosphorous acid or an alkali metal salt of hypophosphorous acid, an initiator and water. A gaseous reactant comprising an alkene having 2 and 4 carbon atoms. A method for producing an alkali metal salt of alkyl hypophosphorous acid or alkylhypophosphorous acid. The present invention relates to a method for preparing an alkyl hypophosphorous-based compound, and a method for producing a hypophosphorous-based flame retardant.
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Paragraph 0112-0118; 0123-0129
(2021/01/09)
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- Mixtures of dialkylphosphinic acids and alkylphosphinic acids, a process for preparation thereof and use thereof
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The invention relates to mixtures of at least one dialkylphosphinic acid of the formula (I) in which R1, R2 are the same or different and are each independently C1-C18-alkyl, C2-C18-alkenyl, C6-C18-aryl, C7-C18-alkylaryl, with at least one alkylphosphonic acid of the formula (II) in which R3 is C1-C18-alkyl, C2-C18-alkenyl, C6-C18-aryl or C7-C18-alkylaryl; to a process for preparation thereof and to the use thereof.
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Page/Page column 10
(2018/11/21)
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- Single ethyl phosphinic acid group containing diethyl phosphinic acid and its salt preparation method
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The invention relates to the field of fine organic chemical industry and polymer materials, and particularly relates to a preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof. The preparation method of diethyl phosphinic acid comprises the following steps: uniformly mixing sodium hypophosphite monohydrate, acetic anhydride and organic solvent; adding organic acid and concentrated sulfuric acid or anhydrous sulfuric acid; cooling and standing; filtering and recovering sodium sulfate to obtain an anhydrous phosphinic acid organic acid solution; adding ethylene and dropwise adding a trigger mixture to obtain a first mixture; and distilling and recovering the organic acid and the organic solvent to obtain a product. The preparation method is simple and easy to implement, the monoethyl phosphinic acid is completely converted into diethyl phosphinic acid, and the prepared diethyl phosphinic acid does not contain the monoethyl phosphinic acid group. In the invention, the diethyl phosphinic acid without the monoethyl phosphinic acid group serves as a reactant and reacts with a metal compound, the obtained diethyl phosphinate does not contain impurities such as organic sodium salt, and the generated waste liquid is simple to dispose.
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Paragraph 0072-0079
(2017/05/18)
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- Tertiary phosphine oxides in reaction with benzaldehyde
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Symmetrical and unsymmetrical tertiary phosphine oxides containing benzyl and 5-chloro-2-thienyl radicals stereoselectively react with benzaldehyde in the sodium amide-THF system to form the E isomers of 1-organyl-2-phenylethene and diorganylphosphinic ac
- Ivanova,Gusarova,Reutskaya,Shaikhutdinova,Arbuzova,Trofimov
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p. 877 - 879
(2007/10/03)
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- Phosphorus-containing compounds and uses thereof
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This invention concerns a new family of phosphorus-containing compounds containing a moiety JQA—in which: A is absent or is —O—, —S— or —NR2—; Q is absent or (if A is —O—, —S— or —NR2—) Q may be —V—, —OV—, —SV—, or —NR2V—, where V is an aliphatic, heteroaliphatic, aryl, or heteroaryl moiety, such that J is linked to the cyclohexyl ring directly, through A or through VA, OVA, SVA or NR2VA; K is O or S; each occurrence of Y is independently —O—, —S—, —NR2—, or a chemical bond linking a R5 moiety to P; and the other variables are as defined herein.
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- Process for preparing phosphinic acids
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The present invention relates to a process for the preparation of phosphinic acids from alkali metal phosphinates, which comprises reacting alkali metal phosphinates in a polar solvent with an inorganic mineral acid and then separating off the phosphinic acid formed.
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- Process for preparing salts of dialkylphosphinic acids
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The invention relates to a process for preparing salts of dialkylphosphinic acids, which comprisesa) reacting alkylphosphonous and/or hypophosphorous acid and/or alkali metal salts thereof with olefins in the presence of a free-radical initiator to give dialkylphosphinic acids and/or alkali metal salts thereof andb) reacting the dialkylphosphinic acids and/or alkali metal salts thereof obtained according to a) with metal compounds of Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr, Ce, Bi, Sr, Mn, Li, Na and/or K to give the metal dialkylphosphinate salts.The invention likewise relates to the use of the metal dialkylphosphinate salts prepared by the process according to the invention for preparing flame retardants.
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- Synthesis of asymmetric P,P-dialkyl-P',P'-diphenylethylenediphosphine dioxides
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Asymmetric P,P-dialkyl-P',P'-diphenylethylenediphosphine dioxides were synthesized by the addition of dialyklphosphinous acids to diphenylvinylphosphine oxide in toluene without a catalyst and in DMSO in the presence of concentrated aqueous alkali.The method for isolating dipropyl- and dibutylphosphinous acids obtained by reactions of diethylphosphite with the corresponding alkylmagnesium bromides was improved. - Key words: ethylenediphosphine dioxides; diphenylvinylphosphine oxide; dialkylphosphinous acids; PH-acids; PH-addition.
- Bondarenko, N. A.,Bozhko, O. K.,Tsvetkov, E. N.
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p. 134 - 136
(2007/10/02)
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- Synthesis of alkyl phosphinic acids from silyl phosphonites and alkyl halides
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Mono- and di-substituted phosphinic acids have been synthesised in a one-pot reaction, by the addition of alkyl halides to silyl phosphonites, under mild and flexible conditions.
- Boyd, E. Andrew,Regan, Andrew C.,James, Keith
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p. 4223 - 4226
(2007/10/02)
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- INVESTIGATION OF THE REACTION BETWEEN DIALKYLPHOSPHINE OXIDES AND CARBONTETRACHLORIDE
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The time dependent formation of intermediates and end products in the reaction between Et2P(O)H and CCl4 is analysed using (31)P-NMR technique.The various reaction steps are studied separately in order to elucidate the overall mechanism.A key step is the disproportionation of Et2P(O)H catalysed by Et2PCl and Et2P(O)Cl, in a cyclic process, the latter being produced initially by the reaction between Et2P(O)H and CCl4.The diethylphosphine formed during disproportionation reacts immediately with CCl4, driving the reaction through the intermediates, Et2PCl and Et2PCCl3which react with Et2P(O)OH producing Et2P(O)Cl, (Et2PO)2O, and Et2P(O)CHCl2, as end products.The influence of the substituents on rate and product yields was studied with n-propyl, n-butyl, n-octyl, and allyl as substituents in the dialkylphosphine oxide.
- Aksnes, Gunnar,Majewski, Piotr
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p. 261 - 274
(2007/10/02)
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- Photochemical Rearrangement of Dialkylphosphinic Azides in Methanol and Other Protic Solvents
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On photolysis in methanol di-t-butylphosphinic azide (4; R=But) rearranges with loss of nitrogen to give methyl NP-di-t-butylphosphonamidate (6; R=But, X=OMe) (71percent), presumably by way of a monomeric metaphosphonimidate (5; R=But) which is trapped by the solvent.Analogous rearrangements occur in other alkohols and in t-butylamine, althogh di-t-butylphosphinic amide is also a substantial product in ethanol and the major product in isopropyl alcohol.Di-isopropylphosphinic azide (4; R=Pri) behaves in a similar way, but in methanol the less hindered diethylphosphinic azide (4; R=Et) suffers extensive solvolysis to methyl diethylphosphinate.
- Harger, Martin J. P.,Stephen, Michael A.
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p. 736 - 740
(2007/10/02)
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