321 results about "Phenylphosphine" patented technology

The present invention relates to catalyst system for propylene hydrogenation and formylation and process of catalytically synthesizing butyl aldehyde. The catalyst system is triaryl phosphine-Rh(I) catalyst system with proper additive, such as bisphosphite ester, in proper amount. Compared with similar available catalyst, the catalyst system has obviously higher catalytic acitivity, higher selectivity, higher stability and raised n-butyl aldehyde/isobutyl aldehyde ratio in the catalytically synthesized product.

The present invention relates to copper complex with imidazole as ligand. Ionic one-valent copper complex is prepared with pyridyl imidazole, pyridyl benzimidazole or quinolyl benzimidazole as the first ligand, triphenyl phosphine or bridged phenyl phosphine as the second ligand and one-valent copper ion. Neutral copper complex may be further obtained under the action of alkali. The ionic copper complex and the neutral copper complex may convert mutually under the action of acid and alkali. This kind of complex possesses strong room temperature phosphorescence emission and may be used as light emitting material.

The invention discloses a preparation method of trans-4-replacing cyclohexyl formaldehyde and trans-4-replacing cyclohexyl olefin, which uses trans-4-replacing cyclohexyl formic acid as raw material, and prepares the trans-4-cyclohexyl olefin by acyl chloride, silicon hydrogen alkane reduction, and reaction with methyl bromide triphenylphosphine quarter phosphonium. The preparation method of the trans-4-replacing cyclohexyl formaldehyde and the trans-4-replacing cyclohexyl olefin is simple in method, clean in using, and has wide application prospect.

A two part curable composition is provided, where the composition comprises: (a) a first part comprising: (i) a (meth)acrylate component; (ii) 1,4-quinones, such as napthoquione or benzoquinone and derivatives thereof in an amount less than or equal to about 0.05 weight percent; (iii) triaryl or alkaryl phenylphosphine in an amount greater than or equal to about 0.5 weight percent; and (iv) an amine; and (b) a second part comprising: (i) benzoyl peroxide in an amount greater than about 1.0 weight percent.

The invention relates to reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and its synthetic method and application and belongs to the field of preparation of a flame retardant. The synthetic method comprises the following steps: using glacial acetic acid as a solvent, adding para amino benzoic acid into glacial acetic acid, slowly dropwise adding dichlorophenylphosphine oxide into an acetic acid solution of para aminobenzoic acid, continuously stirring and reacting at 85-95 DEG C for 4-6 h, and absorbing hydrogen chloride discharged by the reaction by the use of aqueous alkali; and cooling a reaction product after the end of the reaction, carrying out suction filtration, washing and drying to obtain white powdery bis-(p-aminocarboxyphenyl)phenylphosphine oxide. The bis-(p-aminocarboxyphenyl)phenylphosphine oxide flame retardant has advantages of low toxicity, low smoke, innocuousness, high efficiency and the like, is a reactive flame retardant integrating a carbon source, an acid source and a gas source, and is applied in inherent flame retarding of nylon or thermoplastic polyester copolymer.

The invention relates to a preparation method for a POSS/PDMAEMA organic/inorganic hybrid material according to a thiol-ene click chemistry method. The preparation method comprises the following steps: obtaining PDMAEMA through synthesis according to an RAFT polymerization method; taking dimethyl phenylphosphine as a catalyst, taking n-hexylamine as a reducer, and conducting a reduction reaction on a dithioester group at the tail end of PDMAEMA to generate sulfydryl; conducting thiol-Michael addition reactions on the double bonds of PDMAEMA containing sulfydryl and POSS containing ethenyl according to the thiol-ene click chemistry method to generate a POSS/PDMAEMA organic/inorganic hybrid material with a temperature/pH dual response. The preparation method has the advantages that the prepared POSS/PDMAEMA organic/inorganic hybrid material is small in size, stable in chemical bond, and uniform in particle diameter; due to a click reaction to PDMAEMA, the hydrophilic performance of POSS is effectively improved; in a water solution, the POSS/PDMAEMA organic/inorganic hybrid material is excellent in temperature sensibility and pH sensibility; due to a special structure and the stimulus response performance, the POSS/PDMAEMA organic/inorganic hybrid material is a new-generation environment-friendly new material product, and can be applied to drug carrying, targeted release, metal ion recovery, environmental pollutant adsorption and other fields.

The invention relates to polycaprolactone polyol as well as a preparation method and application thereof. The method comprises the following steps that S1, under the protection of the water-free and oxygen-free conditions and inert gas, an initiator, a catalyst, an inhibitor and caprolactone are uniformly mixed; and S2, a system obtained in the step S1 is heated to 120-230 DEG C for reaction for 10-180 minutes so as to carry out ring-opening polymerization reaction, vacuum defoamation is carried out, and cooling and discharging are carried out so as to obtain the polycaprolactone polyol, wherein the inhibitor is one or more of organic phosphine, glyphosate-sodium, ethyldiphenylphosphine or tribenzylphosphine. According to the preparation method, the specific side reaction inhibitor is added, so that the polycaprolactone polyol which is controllable in molecular weight, low in acid value, few in metal residues, narrow in polymer molecular weight distribution and capable of keeping the original excellent physicochemical properties is obtained, and the acid value of the polycaprolactone polyol prepared through the preparation method is less than 0.5 mg KOH/g.

A cycloolefin addition polymer is prepared by addition polymerization of a cycloolefin-functionalized siloxane and optionally norbornene in the presence of catalyst A which is a nickel or palladium complex having a cyclopentadienyl ligand and a methyl, triphenylphosphine or allyl ligand and co-catalyst B, typically tris(pentafluorophenyl)boron or trityltetra(pentafluorophenyl)borate. The polymer is easy to manufacture and has high thermal stability and mechanical strength as well as good gas permeability.

Polyimides displaying low color in thin films, atomic oxygen resistance, vacuum ultraviolet radiation resistance, solubility in organic solvents in the imide form, high glass transition (T_g) temperatures, and high thermal stability are provided. The poly(amide acid)s, copoly(amide acid)s, polyimides and copolyimides are prepared by the reaction of stoichiometric ratios of an aromatic dianhydride with diamines which contain phenylphosphine oxide groups in polar aprotic solvents. Controlled molecular weight oligomeric (amide acid)s and imides can be prepared by offsetting the stoichiometry according to the Carothers equation using excess diamine and endcapping with aromatic anhydrides The polyimide materials can be processed into various material forms such as thin films, fibers, foams, threads, adhesive film, coatings, dry powders, and fiber coated prepreg, and uses include thin film membranes on antennas, second-surface mirrors, thermal optical coatings, and multi-layer thermal insulation (MLI) blanket materials.

The invention discloses a method for synthesizing beta-carotene from vitamin A through a one-pot method. The synthesis method comprises the following steps that firstly, a vitamin A triphenyl phosphine salt reaction solution is obtained, wherein triphenyl phosphine is added in an organic solvent, acid is slowly dropwise added, after dropwise adding is completed, heat preservation is conducted, then vitamin A or a derivative of the vitamin A and alkali 1 are added, a heat preservation reaction continues, and the vitamin A triphenyl phosphine salt reaction solution is obtained; secondly, all-trans beta-carotene is obtained, wherein an acidic medium oxidizing agent and alkali 2 are dropwise added under a low-temperature condition, after the heat preservation reaction is completed, the reaction temperature is increased, the reaction continues, a beta-carotene reaction solution is obtained, a beta-carotene crude product is obtained after post-treatment, and the all-trans beta-carotene is obtained after the beta-carotene crude product is subjected to thermal isomerization. The obtained beta-carotene is crystal solid from red to dark red, the content is larger than 95%, and the yield is 55% or above.

The invention relates to a benzocyclobutene polysiloxane polymer monomer or resin and a preparation method thereof. The invention discloses a dimethyl-4-benzocyclobutene silicon-based ethylmethyl cyclotetrasome disclosed as Formula (III) and a preparation method thereof. The preparation method of the polysiloxane polymer monomer comprises the following steps:Sequentially adding a tetramethyl-tetravinyl-cyclosiloxane solution diluted by solvent methylbenzene and 4-(1-H-1,1-methyl)silicon benzocyclobutene into a reactor, adding a platinum catalyst after applying a nitrogen atmosphere, and reacting at 60-90 DEG C for 20-40 hours; and adding triphenylphosphine, heating under reflux for 3 hours, cooling, filtering, concentrating the filtrate by distillation, adding methanol, mixing, precipitating, filtering, repeatedly precipitating the solid with methanol, and drying the solid to obtain the polysiloxane polymer monomer product. The product has excellent thermal properties, mechanical properties, electric properties and film-forming properties, and has wide development and application prospects as a high-performance dielectric film material or packaging material in the fields of micro-electronics, aerospace, national defence and the like. (III).

The invention discloses a preparation method for a photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide. The preparation method comprises the synthesis steps: under the protection of inert gas, carrying out a reaction of aluminium trichloride or tin tetrachloride and trimethylsilane in the temperature range of 0-100 DEG C to obtain aluminium dichloride ions, and rapidly acting with dichlorophenyl phosphine in the reaction system, to obtain a bis(aluminium trichloride or tin tetrachloride)phosphine salt intermediate; then carrying out a reaction of the intermediate and 2,4,6-trimethyl benzoyl chloride, to obtain bis(2,4,6-trimethylbenzoyl)phenyl phosphine; and under the condition of the temperature of 20-50 DEG C, oxidizing by nitrogen dioxide, to obtain the target product. The method avoids use of a dangerous active metal potassium or sodium, and adopts aluminium trichloride or tin tetrachloride with relatively low price and trimethylsilane for on-site generation of the active intermediate to achieve the reaction. The method has the characteristics of low preparation cost, simple and safe operation process, easy control of the reaction process, high product yield, good purity, easy realization of mass production and the like.

The invention relates to a method of preparing alpha-aryl carbonyl compound. With the catalyst of four triphenylphosphine nickel or acetylacetone nickel ligand, the aryl boric acid, the alpha-halogenated carbonyl compound, the ligand and the additive are dissolved in toluene, and after reaction for 10 to 24 hours in 50 to 100 DEG C, the alpha-aryl carbonyl compound is obtained, wherein, the ligand is single-tooth phosphine ligand or double-tooth phosphine ligand; and the additive is absolute potassium phosphate or tri-potassium phosphate. The invention, which utilizes the catalyst with low cost, stable substrate, easy obtaining and gentle reaction conditions, can not only catalyze arylation of ester, amide and ketone, but also can be compatible with beta hydrogen, thereby greatly expanding the range of the substrate. Moreover, the invention possesses great application potential and can directly constitute the main framework of the steride.

The invention provides a synthesis method for ultraviolet photoinitiator XBPO, which comprises the following steps of: putting sodium hydride and solvent benzene into a stirring reaction kettle, dropwise adding dichlorophenyl phosphine, putting catalyst organic base, dropwise adding 2, 4, 6-trimethyl benzoyl chloride, slowly dropwise adding pure water, slowly dropwise adding oxidant, dropwise adding 2% sodium hydroxide, washing with water, concentrating, crystallizing, filtering, and drying to obtain the ultraviolet photoinitiator. The synthesis method has the advantages that the photolytic product of the ultraviolet photoinitiator XBPO has two trimethyl benzoyl chloride and one phenyl phosphine acyl free radical, which are higher in initiation activity, compared with the photo initiation activity of TPO. The wide wave band has light sensitivity, so that the GR-XBPO not only can be independently used, but also can be used in cooperation with the other ultraviolet absorbers.

Compounds having the formulas below. Each R¹ is an aromatic-containing group. Each R² is methyl, phenyl, alkyl, perfluoroalkyl, and trifluoromethyl. M is an alkali metal, and n is a positive integer. A thermoset made by curing a mixture comprising a curing agent and the below phthalonitrile monomer. A method of: reacting a bis(fluorophenyl)phenylphosphine oxide with an excess of an aromatic diol in the presence of an alkali metal carbonate to form the oligomer below.

The invention discloses an electrolyte for improving high temperature and high voltage performance of a lithium ion battery and application thereof in the lithium ion battery. The electrolyte comprises lithium salt, organic solvent and additive, wherein the additive is composed of methoxyl diphenylphosphine and cathode surface film-forming additive, content of the methoxyl diphenylphosphine in the electrolyte is 0.01-10.0wt.%, and content of the cathode surface film-forming additive in the electrolyte is 0.02-5wt.%; the organic solvent is composed of 10-50wt.% of cyclic carbonate and 30-70wt.% of linear carbonate; and concentration of the lithium salt in the electrolyte is 0.5-2.5mol/L. According to the electrolyte provided by the invention, MDP and cathode surface film-forming additive are used simultaneously as combined additive, stability of a positive electrode material of the lithium ion battery under high voltage can be improved, decomposition of the electrolyte on surface of the positive electrode is inhibited, and cycle performance of the high-voltage lithium ion battery under normal temperature and high temperature is improved.

A polysulfone-polyimide copolymer is prepared from polysulfone, polyimide, Ni as catalyst, triphenyl phosphine as coordinate agent, Zn powder as reducer and non-protonic solvent as reaction medium through reacting at 60-120 deg.C, adding non-protonic solvent, dichlorodiphthaleine imide prepared from chlorophenyl anhydride and diamine, and the dichloroaryl compound and its derivative, and continuously reacting for 2-8 hr. Its advantages are high output rate (91-100%), high performance, and low cost.

(1E, 2E)-1,2-bi(5-methoxyl-2-diphenylphosphine benzylidene) hydrazine is a dual-phosphine ligand containing an imine group. An aromatic ring has methoxyl which supplies electrons so that double metal has the stronger coordination capability. According to the synthetic method, intermediate 5-methoxyl-2-(diphenylphosphino)benzaldehyde and hydrazine hydrate serve as raw materials, formic acid serves as a catalyst, and the raw materials and the formic acid flow back in methyl alcohol to obtain bis-imine bis-phosphine four-tooth ligand L. Bis-imine bis-phosphine four-tooth ligand L and Cu(CH3CN)4CIO4 in-situ catalytic Sonogashira cross coupling reaction is carried out, the catalytic system is very high (the yield reaches to 99%) in reactivity to aryl iodide and is active to aryl bromide to some degree, alkyne self-coupling products can be well avoided, the reactive system is simple, and post-processing is convenient. Adopted Cu is low in cost, easy to obtain, economical and clean, and takes part in the Sonogashira coupled reaction instead of expensive and toxicant Pd. No rganic amine used as a solvent or alkali is used. The (1E, 2E)-1,2-bi(5-methoxyl-2- diphenylphosphine benzylidene) hydrazine has very good application prospects in industrial production in the future.

The invention discloses a graphene reinforced and toughened biodegradable polyester compound and a foaming material thereof. The preparation method comprises the following steps: A, preparing GO/DMF dispersion liquid; B, dissolving a polyfunctional epoxy chain extender in DMF, adding a triphenylphosphine catalyst, and inducing a chemical reaction to obtain GO-epoxy powder; and C, carrying out meltblending on the dried PBAT, PLA and GO-epoxy powder through a circulating twin-screw internal mixer, and carrying out mold pressing to obtain the graphene reinforced and toughened biodegradable polyester composite sheet. According to the invention, epoxy resin grafted graphene oxide is used as a compatilizer and a reinforcing agent; the compatibility of the PBAT/PLA compound is improved, the tensile strength and elongation at break of the PBAT/PLA compound are improved, the tensile strength of the obtained graphene reinforced and toughened biodegradable polyester compound is 25-55 MPa, and the elongation at break of the obtained graphene reinforced and toughened biodegradable polyester compound is 100-600%. And high-pressure CO2 foaming is carried out to prepare the low-density, high-hardness, high-strength and high-toughness graphene reinforced and toughened biodegradable polyester composite foaming material.

The invention relates to a preparation method of a polyfluorene blue high-molecular luminescent material modified by zinc oxide quantum dots. The method comprises the synthesis of 1,4-di-n-butoxybenzene, the synthesis of 1,4-dibutoxy-2, 5-bis(bromomethyl)benzene, the synthesis of 1,4-dibutoxy phenyl-2,5-tri phenylphosphine bromine, the synthesis of 1,4- dibutoxy-2,5-divinyl benzene, the synthesisof 2,7-dibromofluorene, the synthesis of 2,7-dibromo-9,9-dioctyl benzene and the synthesis of a polymer-based nanocomposite. Compared with the prior art, the present invention has the following advantages that the preparation technology is simple and the cost is low; the heat stability of the polymer is excellent; the unique quantum confinement effect and the fluorescent characteristic of the added ZnO quantum dots enable the polymer fluorescent emission spectrum to make an obvious blue shift, and the fluorescent strength is obviously enhanced; in addition, ZnO is a good electron transport material, ZnO introduced into a luminescent layer polymer is capable of effectively balancing the ratio of electron and hole for forming exciton and increasing the luminescent efficiency of the devices.

A provided method for low-mercury catalyst with good heat stability comprises preparation of active carbon, preparation of an adsorption solution, and adsorption processing. The adsorption processing steps comprises ultrasonic assisted adsorption, microwave assisted adsorption and vacuum penetration adsorption. The prepared low-mercury catalyst comprises, in percent by weight, 4.3% of mercuric chloride, 8.6% of zinc chloride, 8.6% of palladium chloride, 2.87% of platinum chloride, 2.87% of tetrabutyl ammonium chloride, 2.87% of tripotasium triphenylphosphine-3,3',3''-trisulfonate, and 0.18% of water. The low-mercury catalyst possesses the mechanical strength of 98.6%, the granularity of 3-6 mm (98%), the bulk density of 460 g/L, and the mercuric chloride ignition loss of 0.39%. The prepared low-mercury catalyst is good in heat stability and low in mercuric chloride loss rate. When the low-mercury catalyst is applied to vinyl chloride synthesis reaction, the acetylene conversion rate is 99.93%, the vinyl chloride selectivity is close to 100%, and the vinyl chloride yield is 95.2%.

A novel multi-aryl bridged long-chain diphosphine ligand is disclosed. A semi-calix[4]arene is taken as a structural skeleton and subjected to double-side decoration, so that a novel phosphine-nitrogen ligand is designed and synthesized, and also the novel ligand and a palladium salt are used for in-situ catalysis of a Suzuki coupling reaction. The preparation method of the ligand comprises: synthesizing a semi-calix intermediate bis(5-tert-butyl-3-hydroxymethyl-2-methoxyphenyl)methane, brominating the intermediate and bridging with an intermediate 2-bromo-6-diphenylphosphanylpyridine to obtain the multi-aryl bridged long-chain diphosphine ligand. The advantages comprise that the novel diphosphine ligand employs the calixarene fragment as the main body, pyridine structure is used to stabilize the molecule and to adjust the molecular cavity, and the ligand is used to catalyze the Suzuki coupling reaction in the presence of trace palladium for carbon-carbon bond construction in organic synthesis. The ligand is stable in structure; the synthesis reaction is short in time, mild in condition, high in yield, easy for mass production and commercialization; and the catalyst use amount is small when the ligand is used for Suzuki coupling reactions, and it is expected that functional groups with specific function can be introduced for promoting synthesis of multiple medicaments.

The invention discloses a method for synthesizing bis(diphenylphosphino)-alkane, belonging to the field of organic synthesis. The method comprises the following steps of: enabling triphenylphosphine to react with lithium hydride to generate a lithium diphenylphosphide intermediate under anhydrous and anoxybiotic conditions, and then directly reacting with dibromoalkane to synthesize a bis(diphenylphosphino)-alkane compound. According to the method disclosed by the invention, the intermediate generated during the preparation of lithium diphenylphosphide by using the lithium hydride has no affects on follow-up reaction, the reaction process is optimized, the reaction is easier to control, the separation cost is reduced, and the method is more suitable for industrial production.

The present invention relates to a process for the production of (-)3,4-divanillyl tetrahydrofiran of formula (2) which comprises (a) isolating) (-) secoisolariciresinol of formula (1) from the heartwood and roots of Taxus wallichiana by an improved process which consists of partitioning of the alcoholic extract of the heartwood and roots of T. wallichiana between water and chlorinated solvent, (b) extracting the chlorinated solvent extract with alkali and (c) isolating (-) secoisolariciresinol from the alkali extract upon neutralization with mineral acid and extracting with organic solvent and (d) crystallizing it from suitable organic solvent, (e) dissolving the isolated (-) secoisolariciresinol in suitable organic solvent and (f) reacting with triphenyl phosphine halide at 0-80° C. for 1-10 hours and (g) isolating (-) 3,4-divanillyl tetrahydrofuran by column chromatography.