61 results about "Chlorodiphenylphosphine" patented technology

The invention relates to a kind of chiral diphosphite ligands, an iridium composite catalyst thereof, a preparation method and application thereof. The ligands are obtained through using chiral (R)-(S)-1-dimethylamino ethyiferroene as raw materials to react with diphenyl phosphonium chloride under the effect of butyl lithium and then to carry out displacement reaction with diaryl phosphine alkane. The chiral diphosphite ligands respectively act with homotropilidene compositions of iridous chloride, tetrabutyl ammonium iodide and glacial acetic acid, and imine asymmetrical hydrogenization catalysts can be obtained. When the iridium-diphosphine catalysts are used for catalyzing 2-methyl-6-ethyl-N-methylene aniline (EMA-imine) hydrogenization reaction, (S)-N-(1-anisyl-2-propyl)-2-methyl-6- ethylaniline ((S)-NNA) can be obtained, and the antimer excessive value (ee) can reach 86.5 percent. The (S)-NNA and chloracetyl chloride carry out acylation reaction to obtain (S)-metolachlor with the ee value of 86 percent. Thereby, the ligands provided by the invneiton can be used for synthesizing chiral herbicidal chemicals of (S)-metolachlor.

The invention discloses a ruthenium complex catalyzer for acetylene hydrochlorinate and a preparation method and application thereof. The catalyzer is characterized in that active carbon serves as catalyst support, and is loaded with ruthenium chloride and an organic ligand; the molar ratio of the ruthenium chloride and organic ligand is 1:1-6, and ruthenium accounts for 0.1-5.0% of the total weight of the catalyzer; the organic ligand is one or more of triphenylphosphine, pyridine, 2,2'-dipyridyl, acetylacetone, chlorodiphenylphosphine, chlorobenzene, cyclopentadiene, 4-methyl isopropyl benzene and 1,5-cyclooctadiene. The ruthenium complex catalyzer for the acetylene hydrochlorinate and the preparation method and application thereof have the advantages that the preparation process is simple, the catalytic activity and stability of the catalyzer are greatly improved, the catalyzer is more environmentally friendly, and the economy is high.

The invention discloses an environment-friendly synthesis method for diphenyl phosphine chloride and aims to solve the problem of environmental pollution in the conventional process. The method comprises the following steps of: adding phosphorus trichloride, benzene and aluminium trichloride into a three-mouth bottle respectively; introducing nitrogen for protection; stirring intensely; heating to 140 to 150 DEG C; maintaining reflux; discharging a large amount of white smoke until the white smoke disappears; cooling to room temperature; and performing aftertreatment operation comprising the steps of adding an organic solvent into reaction liquid in the step A, stirring for 0.5 hour, adding a decomplexing agent beta-chlorophosphate triethyl ester dropwise for 0.5 hour, stirring for 1.0 hour, standing for 1.0 hour, removing the lower layer of the decomlexing agent layer, distilling the organic solvent layer under reduced pressure to obtain a crude product diphenyl phosphine chloride, and distilling the crude product diphenyl phosphine chloride under high vacuum to obtain the pure product diphenyl phosphine chloride. By the method, the aluminium trichloride is recovered through an environment-friendly idea, so environmental pollution is reduced, a byproduct is increased, and yield is increased. The method is high in yield, low in cost and short in reaction time.

The invention provides a preparation method of a photoinitiator TPO, comprises the following formula: 22.5% of diethyl aniline, 7.5% of absolute methanol, 34% of chlorodiphenylphosphine, and 36% of 2,4,6-trimethyl benzoyl chloride. The method comprises the following steps: 1, stirring and uniformly mixing diethyl aniline and absolute methanol; 2, warming to 20 DEG.C, slowly dropping chlorodiphenylphosphine, preserving heat for 2 hours; 3, pumping out the material, and filtering for later use; 4, uniformly mixing the 2,4,6-trimethyl benzoyl chloride; 5, warming to 80 DEG.C, slowly dropping the material for later use in the step 3, and then preserving for 1 hour; 6, carrying out suction filtering by using a suction filtering groove to obtain the photoinitiator TPO. The process is simple, the flammable and combustible solvent such as methylbenzene is unnecessary to use in the reaction process, the preparation method is safe, reliable and in favor of energy-saving and environment-protecting.

The invention aims to provide a method for compounding 2,4,6-trimethylbenzoyl-diphenylphosphine oxide through 'one-pot process'. According to the preparation method, a sodium, ethanol, chlorodiphenylphosphine and 2,4,6-trifluoromethyl benzoyl chloride 'one-pot process' is firstly adopted for replacing the original diphenyl oxethyl phosphine and acyl chloride process for preparing 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, so that the method can greatly reduce the preparation steps and processes, has the characteristics of low cost, simplicity in operation and high yield and can more effectively meet the increasing market requirements at present.

The invention relates to raw material components and a production method of chlorodiphenylphosphine, and belongs to the technical field of chemical product formulas and production methods. Based on mass part, the raw material components are as follows: 0.8-1.5 parts of an active metal, 1-4 parts of benzene halide, 1-3 parts of phosphorus trichloride, 1-8 parts of an organic solvent and 0.03-0.1 part of a catalyst. The production method comprises the following steps: 1. mixing and adding the organic solvent and the active metal to a dispersing kettle based on the mass part, heating and stirring to disperse the active metal, and adding the benzene halide for a first initiation; 2. cooling the materials after dispersion, adding the same amount of the benzene halide for a second initiation, cooling and adding the remaining benzene halide and the phosphorus trichloride; 3. allowing reaction, adding the catalyst, and heating for reaction; 4. filtering through a press filter cone when the materials are hot; and 5. putting the filter pressed materials in a rectifying still and stirring, distilling off the solvent at normal pressure, rectifying a finished chlorodiphenylphosphine product at negative pressure, checking and packaging. The raw material components and the production method have the advantages of 1. shortening the reaction time, reducing the side reaction and improving the yield; and 2. avoiding a hydrolysis procedure, eliminating sewage discharge and reducing the raw material consumption.

The invention discloses a synthesis method of diphenylphosphine chloride, belongs to that technical field of chemical synthesis and solves the problem of low yield of the prior diphenylphosphoric chloride product. The synthesis method of diphenylphosphine chloride is characterized by comprising the following steps: under that protection of dry nitrogen, opening and stirring, adding benzene, phosphorus trichloride and catalyst to a reactor, and raising the temperature to 50 DEG C-80 DEG C and performing reflux reaction at 50 DEG C-80 DEG C for 2-3 h; after the reaction in step S01 is completed, raising the temperature to 85-200 DEG C and performing reflux reaction at 85-200 DEG C; at that end of step S02, after the reactor is cooled down, adding benzene into the reactor, adding a decomplexing agent, stirring until the decomplexing agent is dissolved and distilling to remove benzol, and then performing vacuum distillation to obtain the front fraction and the rear fraction. The inventionhas the advantages of high product yield.

The invention discloses an aryl phosphine chloride production waste residue treatment process, and particularly a diphenyl phosphine chloride production waste residue treatment process. According to the process, aluminium chloride is separated from potassium chloride by utilizing different solubility of the aluminium chloride and the potassium chloride in n-butyl alcohol; the recycled potassium chloride can be re-utilized directly as a complexing agent; aluminum chloride crystals obtained after hydrolysis can also be sold out directly as a product; a small amount of organic distillation residue is outsourced for treating.

The invention relates to a terphenyl biphosphine three-coordination cuprous halide complex as well as a synthesis method and application and belongs to the technical field of light emitting materials.According to the complex, 1,2-dimethyl-4,5-dibromo-benzene is adopted as initial raw materials, a terphenyl bilithium reagent is synthesized through intermolecular coupling reactions, ligand dbdp issynthesized through a nucleophilic substitution reaction with diphenyl chlorphonium, dbdp is adopted as ligand to react with cuprous halide to synthesize a target product provided by the invention, and finally structures and light emission properties of the target product are represented. Results show that at a normal temperature, a solid terphenyl biphosphine three-coordination cuprous iodide complex emits green light, and a terphenyl biphosphine three-coordination cuprous bromide complex and a terphenyl biphosphine three-coordination cuprous chloride complex emit yellow and green light. Thesynthesis method is simple and easy to operate, in addition, the prepared target product has a microsecond-grade service life at the room temperature, and the result shows that the target product hasa light emission mechanism of thermal activity delayed fluorescence and has great potential of being used as an electroluminescent material applied to OLEDs (Organic Light Emitting Diodes).

The invention discloses a preparation method of O-diphenylphosphine benzoic acid. The preparation method comprises the following steps of: (1) carrying out cracking reaction on alkali metal and triphenylphosphine in an organic solvent to generate diphenylphosphine alkali metal salt and phenyl alkali metal salt; (2) slowly adding diisopropylamine, and enabling diisopropylamine to react with the phenyl alkali metal salt completely; (3) slowly adding O-chlorobenzol formate or O-bromobenzol formate, and enabling the diphenylphosphine alkali metal salt and the O-chlorobenzol formate or the O-bromobenzol formate to carry out coupling reaction and generate O-diphenylphosphino benzoate; (4) firstly hydrolyzing under the alkaline condition, obtaining O-diphenylphosphino sodium benzoate, acidizing and neutralizing under the acid condition, and obtaining the O-diphenylphosphine benzoic acid. The preparation method disclosed by the invention has the advantages that phenyllithium produced by cracking is completely reacted by adding the diisopropylamine, so that the generation of side reaction is effectively suppressed, and the reaction yield is greatly increased; since the triphenylphosphine is adopted as a reaction material, compared with the chlorodiphenylphosphine, the production cost is greatly reduced.

The present invention relates to 1, 2- substitute cyclopentadienyl ruthenium surface chiral ligand in the chemical field and the correspondence synthetic method. The present invention comprises six reaction steps: the cyclopentadienyl ruthenium, after the Fuke acyl reaction, is hydrolyzed into 1-carboxyl cyclopentadienyl ruthenium; then 1-carboxyl cyclopentadienyl ruthenium reacts with oxalyl chloride to generate 1-carboxyl carbonyl cyclopentadienyl ruthenium; 1-oxazoline carboxyl carbonyl cyclopentadienyl ruthenium reacts with beta-amino alcohol to generate lactam compound, and then reacts with methane-sulfonyl chloride to generate 1-oxazoline cyclopentadienyl ruthenium; 1-oxazoline cyclopentadienyl ruthenium reacts with sec-butyllithium first, and then reacts with diphenyl chloride phosphate to generate (S, Sp)-1,2-substitute cyclopentadienyl ruthenium P, N- ligand; 1-oxazoline cyclopentadienyl ruthenium reacts with sec-butyllithium first, and then reacts with trimethylchlorosilane to generate (S,Sp)-1- oxazoline-2-trimethyl cyclopentadienyl ruthenium. Then the trimethyl is shucked off to generate (S,Rp)-1,2-substitute cyclopentadienyl ruthenium P,N- ligand. The structure is as follows: in the formula: R: a represents isopropyl, b represents tert-butyl.

The invention relates to a preparation method of diphenyl phosphine chloride, which belongs to the technical field of chemical synthesis, and comprises the following steps: adding benzene and aluminumtrichloride into a reaction kettle, adding phosphorus trichloride into the kettle while stirring, slowly heating the mixture to 120 DEG C, and carrying out a reaction for 12 hours; stopping heating,cooling the reaction product to 60 DEG C, adding a decomplexing agent in batches, heating the reaction product to 80 DEG C, and stirring the reaction product for 2 hours; desolventizing the reaction product, and rectifying the reaction product to separate out phenyl phosphine dichloride and diphenyl phosphine chloride; after the rectification, the product is properly cooled, then slowly adding residual liquid into a 20% hydrochloric acid solution, stirring the mixture for 2 hours, centrifuging the mixture to obtain a wet decomplexing agent product and an aluminum chloride solution, drying thewet decomplexing agent product, and recycling the dried wet decomplexing agent product, and using the aluminum chloride solution for preparing a flocculating agent. According to the method, a new decomplexing agent is used, so that the solid waste problem of diphenyl phosphine chloride production is solved, the production cost is reduced, and the product has market competitiveness.

The invention relates to an organic phosphonate nitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound, and a preparation method thereof. The structure of the organic phosphonatenitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound is disclosed in the invention. The preparation method comprises following steps: a cage phosphate amine and triethylamineare added into an organic solvent, the air in a reactor is replaced by nitrogen gas, at 20 DEG C, dibenzyl phosphonium chloride is added drop by drop in 1h, wherein the dibenzyl phosphonium chloride:cage phosphate amine :triethylamine molar ratio is controlled to be 1:1:1 to 1:1.2:1, and the dropwise adding temperature is controlled to be 50 DEG C or lower; after dropwise adding, the temperatureis increased to 80 to 110 DEG C for 4 to 6h of backflow reaction, then an obtained product is subjected to cooling, filtering, water washing, and vacuum drying so as to obtain the slightly yellow solid dibenzyl phosphinous-N-cage phosphate amine. The dibenzyl phosphinous-N-cage phosphate amine is an excellent phosphonate nitrogen cooperative fire retardant, and is suitable to be taken as fire retardants of polyamide, polyester, polyurethane, glass fiber reinforced plastic, and polyolefin materials; the preparation method is simple; equipment investment is low; and industrialized production isconvenient to realize.

The invention discloses a method for preparing bis(diphenylphosphino), and belongs to the technical field of diphosphine ligands. According to the technical scheme, the method for preparing bis(diphenylphosphino) comprises the following steps: adding tetrahydrofuran and a lithium metal into a reaction kettle, dropwise adding chlorodiphenylphosphine at 20-60 DEG C, dropwise adding dichloralkane at 20-60 DEG C after the chlorodiphenylphosphine is completely reacted, adding an amino antioxidant or a phenol antioxidant after the reaction is completed, depressurizing, removing tetrahydrofuran, adding diluted hydrochloric acid, filtering, and recrystallizing the filter cakes, thereby obtaining bis(diphenylphosphino). The method disclosed by the invention is typical one-pot reaction, is small in equipment investment, simple in equipment and convenient to operate, and due to addition of the antioxidant, the operation steps are greatly simplified, and the yield of the product is increased.

The invention provides a method for preparing triphenylphosphine in a reducing manner. Phenylphosphonicdichloride or chlorodiphenylphosphine is used as a reducing agent, and raw materials are low in price and easily obtained; under the effect of a catalyst, the phenylphosphonicdichloride or chlorodiphenylphosphine and triphenylphosphine oxide are subjected to reducing reaction, stabilities of phosphine oxygen double bonds in the triphenylphosphine oxide and oxidation products (phenylphosphonic dichloride or diphenylphosphinyl chloride) of a reducing agent are different, the stabilities of thedouble bonds of the phenylphosphonic dichloride and the diphenylphosphinyl chloride are good, the double bonds of the triphenylphosphine oxide are broken under the effect of the catalyst, the double bonds of the formed phenylphosphonic dichloride and the formed diphenylphosphinyl chloride are not easily damaged by the catalyst, and therefore, triphenylphosphine can be obtained under gentle conditions; the oxidation products (the phenylphosphonic dichloride or the diphenylphosphinyl chloride) of the reducing agent are important organic synthesis intermediate (such as synthesis of organic phosphate); and moreover, the amount of the catalyst required in the method is small, and the catalysis efficiency is high.

The invention discloses a selenium atom-containing fluorescence probe, and a preparation method and an application thereof, and belongs to the field of functional materials. The structural general formula of above material is represented by formula (I) shown in the description; and in the formula (I), Ar is a carbazolyl or diphenylamino group, and Ph is a phenyl group. The preparation method of the material concretely comprises the following steps: reacting carbazole/diphenylamine with dichlorophenylphosphine/diphenylchlorophosphine to form a derivative containing an N-P structure, and carrying out chemical modification to introduce selenium atoms in order to form the selenium atom-containing fluorescence probe. The method has the advantages of simple synthesis steps, mild conditions, low production cost and high thermal stability. Se=O double bonds are formed through the reaction of the selenium atoms and hypochlorite radicals in order to generate fluorescence change. The selenium atom-containing fluorescence probe has the advantages of high sensitivity and high selectivity.

The invention provides a nine-site functional fluorenyl aromatic single-phosphine oxide electroluminescent material and a preparation method thereof, and relates to a luminescent material and a preparation method thereof, aiming at solving the technical problem that a blue light phosphorescent device is low in external quantum efficiency due to the existing electroluminescent material. The preparation method provided by the invention comprises the following steps of: 1, preparing a bromo-intermediate; and 2, dropwise adding n-butyllithium into the bromo-intermediate, cooling, dropwise adding chlorodiphenylphosphine for reaction, reacting under room temperature, extracting, drying, dissolving with methylene dichloride, oxidizing by adding hydrogen peroxide, extracting, drying, and carrying out column chromatography to obtain the electroluminescent material. The electroluminescent material prepared by the invention is taken as a phosphor material, so that the high-efficiency deep blue light emission can be successfully realized; and the electroluminescent material is taken as a blue light phosphorescent body material, so that the high triplet-state energy level (3.01eV) and the stable power efficiency (35.61m/W) can be realized.

The invention discloses an environment-friendly preparation method of a phosphorus flame retardant, namely 2-(diphenylphosphinoyl)-1, 4-benzenediol. Chlorodiphenylphosphine is taken as a reaction raw material, a one-pot method is adopted for skipping the purification process of the chlorodiphenylphosphine and further directly synthesizing the 2-(diphenylphosphinoyl)-1, 4-benzenediol, and a solvent and a purification solvent, which are used by the environment-friendly preparation method are alcohols, so that the environment-friendly preparation method has the advantages of low toxicity, high yield of above 90%, capability of greatly reducing production cost and effect of meeting environment-friendly and high-efficient requirements.

The invention discloses 1,2-bis(diphenylphosphino) benzene prepared by using a compound (chlorodiphenylphosphine) shown in the formula (2) as one of raw materials. The preparation method sequentially comprises the steps of (a) adding metallic sodium into a reaction container containing toluene, heating, reflowing and stirring; (b) adding mixed liquor of the compound shown in the formula (2) and toluene when metallic sodium is melted into sodium beads, and controlling the temperature to be 100-130 DEG C during the adding process; (c) continuously performing reaction for 11-12 hours at 100-130 DEG C; (d) slowly cooling a reaction system to the room temperature, then adding tetrahydrofuran, and stirring for 0.5-1.5 hours; (e) cooling to 18-20 DEG C, adding 2-bromochlorobenzene, and then stirring for 11-12 hours; and (f) performing pressure reduction and concentration on a reacted mixture, adding methanol, stirring and crystallizing to obtain 1,2-bis(diphenylphosphino) benzene. The preparation method is simple, efficient, and high in yield, and 1,2-bis(diphenylphosphino) benzene is high in purity.

The invention discloses a polycarboxylic acid water reducer and a preparation method thereof. The polycarboxylic acid water reducer comprises the following raw materials in percentages by mass: 100-120 parts of polyoxyethylene-based allyl ester macromonomers, 1-5 parts of sodium methallyl sulfonate, 50-80 parts of acrylic acid, 5-10 parts of potassium hydroxide, 70-90 parts of tap water, 2-5 partsof chlorodiphenylphosphine and 0.5-1 part of copper chloride. Reaction conditions are simple, reaction steps are also simple, and the tap water can be directly used for carrying out charging reaction. The disclosed polycarboxylic acid water reducer has high water reducing ability and low slump, and can meet the requirement of processing of concrete well.

The invention relates to a novel method for synthesizing chlorodiphenylphosphine by a one-step process. The method comprises the following steps: respectively adding phosphorus trichloride, benzene and aluminum trichloride into a three-necked bottle, performing programmed heating to 140-150 DEG C while stirring under the protection of nitrogen, carrying out a heat insulation reaction at the temperature of 140-150 DEG C until no reflux state, and cooling the obtained reaction solution to room temperature; adding an organic solvent to the reaction solution, performing stirring for several hours,dropwise adding a decomplexing agent, stirring the obtained solution for several hours after the drop-by-drop addition of the decomplexing agent is finished, standing the solution to layer the solution, separating out the obtained decomplexing agent layer, carrying out reduced pressure distillation on the obtained organic solvent layer to obtain crude chlorodiphenylphosphine, and distilling the crude chlorodiphenylphosphine under a high vacuum to obtain pure chlorodiphenylphosphine. The method reduces the environmental pollution by recovering the aluminum trichloride, increases the yield of abyproduct, increases the income, and also has the advantages of high yield, low cost and short reaction time.

The invention discloses a method for preparing N,N-dimethyl-(R)-1-[(S)-2-(diphenylphosphine)ferrocenyl]ethylamine by a continuous flow microchannel reactor. The method comprises the following steps that an organic solvent solution of N,N-dimethyl-(R)-1-[(S)-2-ferrocenyl]ethylamine and an n-hexane solution of n-butyllithium are respectively introduced into a microchannel reactor constant temperature module by a metering pump for constant temperature treatment; then, the solutions enter a first mixing module for reaction; after the reaction is completed, the mixed solution enters a second mixingmodule to react with chlorodiphenylphosphine; acidification, extraction, drying and distillation are performed to obtain a crude product of the product of N,N-dimethyl-(R)-1-[(S)-2-(diphenylphosphine)ferrocenyl]ethylamine; the crude product is subjected to alcohol recrystallization to obtain the product of N,N-dimethyl-(R)-1-[(S)-2-(diphenylphosphine)ferrocenyl]ethylamine. The method has the advantages that the operation is simple, convenient and safe; the yield is high.