138 results about "N-Butyllithium" patented technology

The invention discloses water-based formaldehyde-free woodworking glue and a preparation method thereof, and relates to the technical field of woodworking glue. When the water-based formaldehyde-free woodworking glue is prepared, firstly, n-butyllithium is used as an initiator to initiate cyclosiloxane and an acrylate monomer to be polymerized, then dimethyl chlorosilane is used for blocking to obtain pre-modified polyacrylate, and the pre-modified polyacrylate is used for preparing the water-based formaldehyde-free woodworking glue. Reacting the pre-modified polyacrylate with vinyl diphenylphosphine, and then reacting with 3-(4-bromophenyl)-1-propylene to obtain modified polyacrylate; secondly, reacting the 4-(trimethoxysilyl) butyraldehyde modified silicon dioxide with chitosan, and then reacting with mercaptoacetic acid to obtain modified silicon dioxide; finally, mixing the modified polyacrylate, the modified silicon dioxide, an emulsifier, a defoaming agent, pure water and a photoinitiator to obtain the water-based formaldehyde-free woodworking glue. The water-based formaldehyde-free woodworking glue prepared by the invention has flame retardance and antibacterial property.

The invention discloses tris (dimethylamino) cyclopentadienyl hafnium and a preparation process thereof.The preparation process of the tris (dimethylamino) cyclopentadienyl hafnium comprises the following steps that S1, an n-hexane solution of n-butyllithium and dimethylamine are subjected to a reaction, and a lithium dimethylamino emulsion is obtained; s2, adding hafnium tetrachloride into the lithium dimethylamino emulsion for reaction, and separating to obtain a liquid-phase product; s3, the liquid-phase product is heated, a tetra (dimethylamino) hafnium concentrated solution is obtained, and the volume of the tetra (dimethylamino) hafnium concentrated solution is 20%-30% of the volume of the liquid-phase product; and S4, obtaining cyclopentadiene, adding the cyclopentadiene into the tetra (dimethylamino) hafnium concentrated solution to react, and filtering to obtain tris (dimethylamino) cyclopentadienyl hafnium. According to the preparation process of the tris (dimethylamino) cyclopentadienyl hafnium, complex solvent components are not needed, the preparation efficiency is improved, and the use amount of the solvent and the preparation cost are reduced.

The invention relates to a novel preparation method of tetra (dimethylamino) tin. The method comprises the following steps: in a nitrogen atmosphere, pumping an n-hexane solution of n-butyllithium and an n-hexane solution of dimethylamine into a pipeline through a propeller, mixing through a T-shaped joint, and reacting through a flow reactor 1 and a flow reactor 2 to obtain a lithium dimethylamide mixed solution; the method comprises the following steps: pumping a lithium dimethylamino mixed solution and a n-hexane solution of tin tetrachloride into a pipeline through a propeller, mixing through a T-shaped joint, and reacting through a flow reactor 3 and a flow reactor 4 to obtain a crude tetra (dimethylamino) tin product; and centrifuging and filtering the tetra (dimethylamino) tin crude product, adsorbing impurities by adopting a resin column, and carrying out reduced pressure distillation to remove the solvent, thereby obtaining the tetra (dimethylamino) tin. The adsorption resin column adopts modified macroporous adsorption resin, and is obtained by reacting, filtering and drying D190 macroporous styrene sulfydryl resin, dichloroethane, tetramethylguanidine, 5-allylpyrimidine-4, 6-diol and an ethylene boric anhydride pyridine complex.

The invention provides primary amino modified solution polymerized styrene-butadiene rubber and a preparation method thereof. The preparation method comprises the following steps: in a polymerization system, initiating polymerization of a butadiene monomer and a styrene monomer by taking n-butyllithium as an initiator and tetrahydrofuran as a polymerization activator to obtain a styrene butadiene rubber active chain; adding a diisocyanate compound into the polymerization system to terminate polymerization, and introducing an isocyanate group to the end part of a styrene butadiene rubber active chain to obtain a styrene butadiene rubber solution; and adding a terminator into the styrene-butadiene rubber solution, stirring, separating out precipitate, and drying to obtain the primary amino modified solution polymerized styrene-butadiene rubber. The primary amino modified solution polymerized styrene-butadiene rubber is prepared by the preparation method, has high polarity and strong binding force with silicon dioxide filler, promotes generation of a more stable filler-polymer network with a more perfect structure, and remarkably improves the dynamic performance of a rubber material.

The invention belongs to the technical field of organic synthesis and medicinal chemistry, and discloses a total synthesis method of rhododendron heteroterpenin Rhododaurines A-C. The total synthesis method comprises the following steps: carrying out allyl stereoselective addition on a compound 3 and a compound 5 in a toluene solvent under the conditions of catalysis of n-butyllithium and low temperature of-78 DEG C, and constructing a chiral center to obtain a compound 6; removing a methoxy methyl (MOM) protecting group from the compound 6 under an acidic condition, cyclizing, and reacting to generate rhododaurine C (7); the rhododaurine C (7) is subjected to intramolecular [4 + 2] cycloaddition and oxidation reaction in the illumination and oxygen atmosphere of 300-385 nm, and rhododaurine B (8) and an epoxy epimer epinedodaurine B (9) are obtained; and carrying out protonation and rearrangement on the epidodaurine B (9) by virtue of acid catalysis cyclic ether, so as to generate the rhododaurine A (10). The method can overcome the defects that the content of rhododendron miscellaneous terpenoids Rhododaurines A-C in nature is extremely low, and large-scale extraction is difficult.

The invention provides a method for preparing a CGC ligand, which comprises the following steps: mixing tetra-substituted cyclopentadiene and n-butyllithium under a mechanical vibration condition, carrying out lithiation reaction under an ultrasonic condition, and then carrying out silicification reaction with a disubstituted dichlorosilane solution, the preparation method comprises the following steps: preparing a silicification product into a tetrahydrofuran solution of the silicification product by using tetrahydrofuran, mixing primary amine and n-butyllithium under a mechanical vibration condition, carrying out lithiation reaction under an ultrasonic condition, carrying out amination reaction on an obtained lithiation reaction solution and the prepared tetrahydrofuran solution of the silicification product, and carrying out post-treatment on the obtained amination reaction solution to obtain the CGC ligand. According to the method for preparing the CGC ligand, the CGC ligand is continuously prepared by coupling the ultrasonic microreactor with local mechanical vibration, the danger coefficient is low, the reaction efficiency is high, the cost is saved, the period is short, and meanwhile, the problem that an organic lithium intermediate generated by lithiation reaction is deposited in the microreactor is solved.

The invention discloses a synthesis method of a novel benzosuberone compound, and belongs to the field of organic synthesis. The preparation method comprises the following steps: uniformly stirring methyltriphenylphosphonium bromide in a solvent at room temperature, dropwise adding an n-hexane solution of n-butyllithium in an ice-water bath, stirring a reaction system at room temperature for 30-40 minutes after dropwise adding is completed, then adding an initial raw material phenanthrenequinone 1 in the ice-water bath, transferring the reaction system to 40 DEG C for reaction, and after the reaction is monitored to be complete by a TLC (Thin Layer Chromatography) dot plate, filtering, washing and drying to obtain the phenanthrenequinone 1. And pouring the reaction liquid into a silica gel chromatographic column, and simply filtering by using dichloromethane as an eluent to remove salt and phosphine oxide. And performing rotary evaporation to remove the organic solvent to obtain a crude product, and separating and purifying to obtain a target product 2. The method is short in reaction time and low in reaction cost, provides a practical method for obtaining the seven-membered rigid ring skeleton, and has potential value for synthesis of natural products and bioactive molecules.

The invention provides an in-chain functionalized solution polymerized styrene-butadiene rubber and an in-chain modification method thereof. The method comprises the following steps: in a polymerization system, initiating polymerization of a butadiene monomer and a styrene monomer by taking n-butyllithium as an initiator and tetrahydrofuran as a polymerization activator to obtain a styrene butadiene rubber active chain; adding a terminator into the polymerization system to terminate the polymerization reaction to obtain a styrene butadiene rubber solution; the method comprises the following steps: adding a thiol compound and a free radical initiator into a styrene-butadiene rubber solution, heating and stirring the styrene-butadiene rubber solution, after a modification reaction is finished, adding alcohol to separate out and precipitate the styrene-butadiene rubber, and drying to obtain the chain-functionalized solution polymerized styrene-butadiene rubber. The in-chain functionalized solution polymerized styrene-butadiene rubber is prepared by the preparation method, and the interface bonding force between the white carbon black and the styrene-butadiene rubber can be enhanced, so that the hysteresis loss of a final tire rubber product is reduced, and the tire rubber product is endowed with high wear resistance, fatigue resistance and excellent wet skid-rolling resistance balance.

The invention belongs to the field of polymer electrolyte membranes, and particularly relates to a block type anion exchange membrane with interstitial alkyl chains and a preparation method of the block type anion exchange membrane. The preparation method comprises the following steps: adding a tetrahydrofuran solution of n-butyllithium into dehydrated toluene for reaction, and then adding alpha, omega-dihaloalkane for reaction to obtain alpha, omega-diphenylalkane; the preparation method comprises the following steps: prepolymerizing biphenyl and 4-imidazole formaldehyde to obtain a prepolymer 1, and prepolymerizing alpha, omega-diphenylalkane and 4-imidazole formaldehyde to obtain a prepolymer 2; mixing the two prepolymerization solutions to obtain a fibrous block polymer with an interstitial alkane chain; and finally, carrying out quaternization and ion replacement to obtain the anion exchange membrane. Microphase separation is constructed in the polymer membrane through a block structure, and the conductivity is improved; an interstitial alkyl chain is introduced into an AEMs main chain to reduce the rigidity of polybiphenyl and improve the flexibility of the membrane; the alkali resistance of the polymer electrolyte membrane is enhanced through the main chain design without ether bonds.

The invention provides a preparation method of a chlorantraniliprole key intermediate 2-amino-5-cyano-N, 3-dimethyl benzamide, which comprises the following steps: taking cheap and easily available o-methylaniline as a raw material, acylating an aniline substrate through Boc anhydride, carrying out ortho-lithiation on n-butyllithium, introducing carbon dioxide gas, and carrying out acid hydrolysis to obtain 2-amino-3-methyl benzoic acid, thereby obtaining the chlorantraniliprole key intermediate 2-amino-5-cyano-N, 3-dimethyl benzamide. The preparation method comprises the following steps: firstly, preparing an isatoic anhydride intermediate, then carrying out triphosgene ring closing to obtain an isatoic anhydride intermediate, carrying out bromine para-position halogenation, carrying out cuprous cyanide high-temperature Rosenmn-von Braun reaction, and finally carrying out methylamine ring opening to obtain the target product 2-amino-5-cyano-N, 3-dimethylbenzamide, and although the route is long, the yield is high, the continuity is good, few industrial three wastes are generated, and the cost is lower, so that the preparation method has great industrial production value.

The invention discloses chain end modified liquid rubber, mixed rubber, a preparation process, a tire and a vehicle, and belongs to the technical field of liquid rubber and manufacturing thereof. According to the liquid rubber, butadiene monomers and a chain transfer agent are added in batches in the preparation process, negative ion active centers are frequently transferred to the chain transfer agent from the tail end of a polybutadiene-based lithium active chain to form new initiation growth centers, then newly introduced butadiene monomers are initiated to grow, the dosage of an n-butyllithium initiator is remarkably reduced, and the stability of the liquid rubber is improved. The production cost is greatly reduced, the generation of sewage is greatly avoided, the monomer concentration of the final rubber product can reach about 80 percent by weight, the productivity is improved, and large-scale production is facilitated; the rubber also enables the filler to have good dispersibility, and has good compatibility with base rubber such as styrene butadiene rubber, natural rubber and the like.

The utility model provides an n-butyllithium taking bottle which comprises a bottle body and a bottle cap and is characterized in that the bottle body is composed of an inner layer structure and an outer layer structure, an air inlet pipe and a liquid outlet pipe are arranged on the bottle cap, an air inlet valve is arranged on the air inlet pipe, a liquid outlet valve and a buckle are arranged on the liquid outlet pipe, and the liquid outlet pipe and a feeding pipe are connected through the buckle. And an air bag and a feeding needle are arranged on the feeding pipe. The n-butyllithium taking device is connected with an air inlet and liquid outlet device, so that the n-butyllithium taking device is safer when n-butyllithium is taken. When the n-butyllithium bottle topples over or falls off accidentally, the two-layer structure can protect the bottle body from being broken, reagents in the bottle are not prone to being leaked, and accidents are reduced.

The invention provides a method for preparing dienogest through a one-pot method, and belongs to the technical field of medicine synthesis. The method comprises the following steps: forming ethyl cyano anions from n-butyllithium and acetonitrile under an ultra-low temperature condition, carrying out addition reaction on a compound in a formula (1), quenching with acid after the reaction is finished, and then directly dropwise adding concentrated hydrochloric acid to carry out deprotection-transposition reaction, so as to prepare a compound in a formula (2); and after the reaction is finished, adding a sodium bicarbonate aqueous solution to carry out elutriation, and carrying out secondary refining on an obtained crude product to obtain a refined dienogest product. The dienogest is prepared through the addition and deprotection-transposition reaction one-pot method, the solvent dosage can be effectively reduced, meanwhile, solid waste is reduced, the process cost is reduced, and green chemical industrial production of the dienogest is achieved.

The invention relates to a method for preparing (cyclopentadienyl) tris (dimethylamino) hafnium by using nuclear magnetic control, which comprises the following steps: S1, carrying out heating reflux reaction on hafnium tetrachloride, cyclopentadiene and dimethylamine in the presence of n-butyllithium and n-hexane, and after reacting for a certain time, taking supernate to detect a nuclear magnetic hydrogen spectrum; s2, calculating the ratio a of the integral area of the characteristic peak A to the integral area of the characteristic peak B according to the nuclear magnetic hydrogen spectrum, judging whether a is in a target range or not, if a is in the target range, terminating the reaction, separating a liquid phase, distilling and collecting a crude product; and if a value is greater than the maximum value of the target range, adding cyclopentadiene into the reaction system to continue the reaction, and if a value is less than the minimum value of the target range, continuing the reaction until the ratio of the integral area of the characteristic peak A to the integral area of the characteristic peak B in the nuclear magnetic hydrogen spectrum of the reaction supernatant is within the target range, terminating the reaction, separating the liquid phase, distilling and collecting a crude product. The method can effectively improve the safety of the production process, the raw material conversion rate and the product purity.

The invention belongs to the technical field of chemical synthesis of semiconductor materials, and particularly relates to a synthesis method of tetra (dimethylamino) titanium, which comprises the following steps: (1) reacting titanium tetrachloride with dimethylamine to generate an intermediate TiClx [N (CH3) 2] 4-x, where x is an integer from 0 to 4; (2) reacting dimethylamine with an organic metal lithium reagent to synthesize lithium dimethylamino (LiN (CH3) 2); and (3) reacting the intermediate obtained in the step (1) with lithium dimethylamino obtained in the step (2) to obtain tetra (dimethylamino) titanium. By adopting a step-by-step reaction strategy, the dependence on expensive n-butyllithium is fundamentally reduced, the raw material cost is remarkably reduced, meanwhile, the reaction process is optimized by generating an intermediate, the product yield is greatly improved, the generation of byproducts is effectively reduced, and the product purity is improved.

This invention relates to a simple method for modifying β-ketoimine ligand precursors, wherein L... Ph The reaction involves a lithium compound with H2 solution; then a haloalkane is added for C-C coupling; followed by the addition of an acid solution to complete the modification of the β-ketoimine ligand precursor, yielding a terminally alkylated ketoimine. This invention relates to a simple method for modifying β-ketoimine ligand precursors, specifically involving the removal of the proton at the α-position of the β-ketoimine ligand precursor from commercially available n-butyllithium to form a deprotonated β-ketoimine lithium compound, followed by C-C coupling to achieve alkylation at the α-position of the ketocarbonyl group, thus providing a convenient modification of the β-ketoimine ligand precursor.

The application discloses a preparation method of triethyl indium, and relates to the technical field of metal organic source synthesis, wherein a commonly used indium source is mainly trimethyl indium; the trimethyl indium is in a solid state at normal temperature, and is easy to cause the solid indium source to be easy to be hardened and to have excessive residues; when the solid indium source is used in a machine, the concentration output stability is worse than that of a liquid source; the liquid indium source will become an important indium source in the future; the operation method of the triethyl indium in preparation is more complicated; and the purity of the triethyl indium prepared by purification cannot reach a better ideal state. In the application, n-butyllithium and ethyl iodide are reacted under the protection of inert gas, then the reaction product is reacted with indium chloride to generate triethyl indium; the whole operation is simple, raw materials are easy to obtain, and the product has high purity; under the protection of inert gas, the interference of other solution reagents in the preparation process is reduced; therefore, high-quality triethyl indium raw materials can be purified and processed.

The invention discloses a silylene ligand supported metal cobalt catalyst and a preparation method and application thereof, and belongs to the technical field of metal organic catalyst.The preparation method comprises the steps that indole and n-butyllithium serve as raw materials and are subjected to a deprotonation reaction in a tetrahydrofuran solvent at the room temperature, 2-lithium indole is obtained, a tetrahydrofuran solution of chlorosilylene is added at the low temperature, and the 2-lithium indole is obtained; and carrying out nucleophilic substitution reaction at room temperature, and substituting Li in 2-lithium indole with silicon in chlorosilylene to obtain the silylene ligand. The preparation method comprises the following steps: taking a silylene ligand and a cobalt complex as raw materials, carrying out ligand substitution reaction at room temperature in a tetrahydrofuran solvent, and substituting a ligand in the cobalt complex with the silylene ligand to obtain the metal cobalt catalyst supported by the silylene ligand. The prepared metal cobalt catalyst supported by the silylene ligand is used for catalyzing olefin hydrosilylation reaction, ultrahigh catalytic activity is shown, complete conversion of olefin is achieved, Markov products are obtained with excellent selectivity, and therefore the problems of cost and product selectivity in industrial production are solved.

A method for preparing high-purity lithium sulfide by using industrial-grade butyllithium includes the following steps: step A: under an inert gas condition, thoroughly mixing 1.5-2.5 g of lithium chloride, 0.5 L of an industrial-grade n-butyllithium solution (2.5 mol / L) and 1.5-2.5 L of n-hexane to obtain a mixed solution, and charging the mixed solution into a sealed container; step B: under the sealed condition, firstly introducing H2S gas into a gas-washing bottle through a submerged pipe at a rate of 10.5 L / h, then introducing into the mixed solution through the submerged pipe, controlling the reaction temperature at 25-40° C., and continuously stirring for reaction for 4-6 h to obtain a reaction slurry; and step C: under an inert gas condition, filtering the reaction slurry with a G3 sand core funnel to obtain a crude lithium sulfide solid wet material.

The invention provides a novel method for preparing an intermediate compound of aromatic sesquiterpenes Commiphoranes C-D. The method comprises the following steps: substituting the ortho-position of a compound 1 with iodine through n-butyllithium and diiodoethane to obtain a compound 2; removing methoxyl by using boron tribromide to obtain a compound 3; performing nucleophilic substitution on 3-allyl bromide and potassium carbonate to synthesize a compound 4; carrying out Grignard reaction to obtain a compound 5; oxidizing into a compound 6 through a Dess-Martin oxidizing agent; finally, (CH3Si) 3SiH and triethyl boron are subjected to intramolecular free radical series cyclization, so that synthesis of an aromatic sesquiterpene Commiphoranes C-D intermediate compound is successfully completed, sufficient preparation is made for follow-up total synthesis of the natural product, key intramolecular free radical series cyclization has the capacity of efficiently constructing a polycyclic system, and the synthesis process is simple and convenient. According to the preparation method, the defects of expensive reagents, long 14-step linear synthesis route, low yield and the like in the existing synthesis route are overcome; the popularization potential is high.

The invention provides a kilogram-level preparation method of an organic photoelectric conjugated tin reagent, and belongs to the field of organic synthesis and organic photoelectric materials. The method comprises the following steps: in a dry 20L reaction device, dissolving a conjugated thiophene compound in tetrahydrofuran, keeping nitrogen positive pressure protection, dropwise adding a tetrahydrofuran solution of n-butyllithium and a tetrahydrofuran solution of trimethyltin chloride in a low-temperature reaction system, stirring for reaction, after the reaction is completed, standing for phase splitting, collecting an organic phase, drying, and concentrating filtrate to obtain the conjugated thiophene compound. And recrystallizing to obtain the organic photoelectric conjugated tin reagent. According to the method, efficient macro preparation of various conjugated tin reagents can be achieved, 1-1.2 kg of target products can be prepared through single-batch reaction, and the method has the advantages of being high in yield, easy and convenient to operate, low in cost, good in environmental friendliness and the like.

The invention discloses a kilogram-level preparation method of an organic photoelectric conjugated boron reagent, and belongs to the technical field of organic synthesis and organic photoelectric materials. A kilogram-level preparation method of an organic photoelectric conjugated boron reagent comprises the following steps: uniformly mixing aryl halide and tetrahydrofuran in an inert gas atmosphere to obtain a mixed system 1; placing the mixed system 1 in a liquid nitrogen environment, then dropwise adding a THF solution of n-butyllithium, and stirring to obtain a mixed system 2; and adding a boric acid ester compound into the mixed system 2 for reaction, and finally performing purification treatment to obtain a target product, namely the organic photoelectric conjugated boron reagent. The preparation method of the conjugated boron reagent is efficient, safe and capable of achieving large-scale production, has the advantages of being easy and convenient to operate, low in cost, high in yield, good in purity and the like, is suitable for various benzene series, thiophene, fluorene and other substrates, achieves kilogram-level stable preparation, solves the amplification problem, improves supply chain autonomy, and is suitable for industrial production. The application requirements in the fields of high-end medicines and materials are met.

The invention provides a synthesis method of a high-purity hafnium-zirconium metal complex precursor, and belongs to the technical field of high-dielectric-constant materials for super-large-scale integrated circuits. According to the method, hafnium tetrachloride or zirconium tetrachloride is used as a metal source and sequentially reacts with dialkylamine, n-butyllithium and an alkyl magnesium halide Grignard reagent through a one-pot method in a high-purity inert atmosphere, an intermediate does not need to be separated, and a target precursor is obtained after filtration, washing and rectification. The method is simple and convenient in process operation, mild in reaction condition and low in energy consumption; the raw materials are wide in source and low in price, the product yield reaches 82%-88%, and the metal purity is stabilized to be 6N; when the precursor is used for preparing a hafnium oxide / zirconium thin film through atomic layer deposition (ALD), the thickness of the thin film reaches 14.3 nm under 100 cycles, the non-uniformity is smaller than or equal to 0.90%, the requirement of a gate dielectric layer of a super-large-scale integrated circuit for a high-purity and high-efficiency precursor can be met, and the precursor is suitable for industrial amplification production.

The invention belongs to the technical field of deuterated organic chemical synthesis, and particularly relates to a synthesis method of deuterated 9-phenyl anthraceneboronic acid-D8, which comprises the following steps of: 1, halogenation reaction: reacting 9-phenyl anthracene-D9, bromo-succinimide (NBS) and triethylamine (TEA) in dichloromethane at low temperature to generate an intermediate 9-phenyl-10-bromoanthracene-D8; step 2, carrying out nucleophilic reaction of forming carbon negative by pulling out bromine with strong in a low-temperature environment of-65 DEG C to-70 DEG C, reacting n-butyllithium with the intermediate 9-phenyl-10-bromoanthracene-D8 in 2-methyltetrahydrofuran to generate 9-phenyl anthracene lithium; then triisopropyl borate is added for a boronation reaction, and the 9-phenyl anthracene boric acid-D8 is obtained after hydrochloric acid hydrolysis and purification. The purity of the deuterated 9-phenyl anthracene boric acid-D8 is greater than or equal to 99.8%, the deuteration rate is greater than or equal to 98%, and the deuterated 9-phenyl anthracene boric acid-D8 is suitable for being used as

The invention relates to the technical field of electronic materials, and provides a high-purity metal complex precursor synthesis device which is characterized in that a reaction kettle is arranged for reaction, and the reaction kettle is communicated with an n-hexane / tetrahydrofuran storage tank, an n-butyllithium storage tank and a DMSO storage tank; a hydrochloric acid aqueous solution dropwise adding tank, a cyclopentadiene / substituted cyclopentadiene dropwise adding tank, a bromopropane / liquefied dimethylamine dropwise adding tank and a solid feeder are used for adding raw materials, a reaction kettle is communicated with a barrel-cone type three-in-one filter for filtering, the barrel-cone type three-in-one filter is communicated with a distillation kettle / liquid separation kettle for distilling or liquid separation, the distillation kettle / liquid separation kettle is communicated with a rectifying tower for rectifying, and the rectifying tower is communicated with a rectifying tower for rectifying. The distillation kettle / liquid separation kettle is communicated with the reaction kettle for material returning; the distillation kettle / liquid separation kettle is communicated with a distillation condenser for distilling, condensing and recycling raw materials; according to the preparation method disclosed by the invention, the n-propyl cyclopentadiene can be firstly prepared, and then the n-propyl cyclopentadienyl zirconium trichloride is prepared; and finally, preparing to obtain the n-propyl cyclopentadienyl tri (dimethylamino) zirconium.

The invention discloses a solid defoamer suitable for ceramic glazing and a preparation method thereof. The solid defoamer comprises the following formula: 10-30 parts of rhamnose, 0.0001-0.05 parts of a DMC bimetallic catalyst, 5-20 parts of polyoxyethylene, 5-40 parts of polyoxypropylene, 0.1-2.5 parts of a hydrogen capping agent, 5-20 parts of polydimethylsiloxane, 5-20 parts of carborane, 1-5 parts of n-butyllithium, 0.0001-0.009 parts of cis-dichlorodiammineplatinum, 3-8 parts of methyldichlorosilane, 0.0001-0.01 parts of ferric chloride, 0.8-4 parts of ammonium chloride, 10-30 parts of bovine bone ash, 6-20 parts of fumed silica, 0.001-3.5 parts of light calcium carbonate, 0.8-3.0 parts of phenoxyethanol, 0.001-0.2 parts of iodopropynyl n-butylcarbamate, and 20-40 parts of water. The present invention utilizes carborane to enhance ceramic properties while avoiding the problem of residue disposal. The dispersion of silicon dioxide and light calcium carbonate ensures uniform dispersion and stable ceramic components. The use of cattle bone ash as a dispersant ensures uniform dispersion and a moist ceramic surface.

The invention belongs to the technical field of ceramic precursors, and particularly relates to a silicon-boron-carbon-nitrogen ceramic precursor with a main chain containing alkynyl and a preparation method of the silicon-boron-carbon-nitrogen ceramic precursor. Comprising the following steps: (1) dropwise adding an n-butyllithium solution into an ether solvent, stirring, continuously dropwise adding trichloroethylene, and reacting to obtain an alkynyl dilithium salt turbid solution; (2) adding boron trichloride into the alkynyl dilithium salt turbid solution to carry out primary dechlorination polycondensation reaction, and dropwise adding dichlorosilane to carry out secondary dechlorination polycondensation reaction after the reaction is completed; (3) adding hexamethyldisilazane into the system in the step (2) to carry out an end-capping reaction, collecting supernate after the reaction is finished, and distilling at normal pressure to remove the solvent, so as to obtain a silicon-boron-carbon-nitrogen ceramic precursor crude product; and (4) dissolving the silicon-boron-carbon-nitrogen ceramic precursor crude product in an organic solvent, carrying out dialysis treatment, and carrying out atmospheric distillation on the solution in a dialysis membrane to remove the solvent so as to obtain the silicon-boron-carbon-nitrogen ceramic precursor with the main chain containing alkynyl, and the ceramic yield of the silicon-boron-carbon-nitrogen ceramic precursor in the high-temperature ceramization process can reach more than 70%.

The application relates to a solution polymerization styrene-butadiene SSBR rubber and a preparation method thereof, and belongs to the technical field of solution polymerization styrene-butadiene rubber. The preparation raw materials of the solution polymerization styrene-butadiene SSBR rubber include 25-35 parts of styrene, 30-40 parts of butadiene, 75-85 parts of a cyclohexane solution, 0.5-1.5 parts of a polarity regulator, 2-5 parts of an atomization terminator and 0.5-2.5 parts of n-butyllithium. The preparation raw materials of the atomization terminator include 75-85 parts of isopropyl alcohol, 15-20 parts of an antioxidant 1520, 0.5-1.5 parts of cyclohexane, 0.3-0.6 parts of citric acid, 2-4 parts of a plant polyphenol extract and 0.2-0.5 parts of a crosslinking agent. By compounding the antioxidant 1520 and the multi-source purified plant polyphenol extract in the atomization terminator and matching the tannin acid-boric acid composite crosslinking system, a multiple synergistic heat-resistant protection and structure reinforcing mechanism is formed, and the defects of easy oxidative degradation, easy molecular chain rupture and serious performance attenuation of the traditional solution polymerization styrene-butadiene SSBR rubber under a high-temperature environment are effectively improved.

The invention provides a preparation method of an IVB group metal organic precursor, which comprises the following steps: treating an amine ligand into corresponding lithium amide by using n-butyllithium before use, reacting IVB group metal chloride with the lithium amide, obtaining an amine group metal organic precursor mixed solution after the reaction is ended, discharging residual gas, filtering, desolventizing, and carrying out reduced pressure distillation to obtain the IVB group metal organic precursor. The amino metal organic precursor is obtained. The invention further discloses a deposition method of the IVB group metal organic precursor. The deposition method comprises the following step of performing thin film deposition on the prepared amino metal organic precursor, the prepared cyclopentadienyl metal organic precursor and an oxygen source to prepare a metal oxide thin film. The reaction is promoted by adjusting the use amount of alkylamine, the use amount of a toluene solvent is reduced, and then the alkylamine is applied to a corresponding oxide thin film deposition process. The process has the advantages of good safety and high economical efficiency.

The invention relates to a preparation method of a carborane derivative, which comprises the following steps: reacting carborane with n-butyllithium in an ether solvent in an inert gas atmosphere, adding an inorganic base and a copper catalyst after the reaction is completed, reacting for a period of time, adding pyridine, stirring for a period of time, filtering, washing, and drying to obtain the carborane derivative. And finally, adding a compound L-R1, and carrying out heating reaction to obtain a derivative in which H on one or two carbons on carborane is substituted by R1. According to the preparation method disclosed by the invention, the complete reaction can be carried out only by one solvent, the operation is obviously simpler, and the cost is lower. More importantly, the method provided by the invention significantly improves the yield of the carborane derivative, and has certain application prospects.