510results about How to "Short reaction path" patented technology

The invention discloses a hydrophobicPOSS (Polyhedral Oligomeric Silsesquioxane)-based hybridization fluorinated acrylate resin as well as a preparation method and an application thereof. The formula of the hydrophobic POSS-based hybridization fluorinated acrylate resin comprises the following raw materials in percentage by weight: 2-12% of POSS-based monomer, 2-11% of hard monomer, 3-16% of soft monomer, 1.5-7% of fluoroacrylate monomer, 3-11% of crosslinking monomer, 0.4-1.3% of triggering agent and 50-79% of solvent. The application of the hydrophobic POSS-based hybridization fluorinated acrylate resin is characterized in that a crosslinking-type copolymer is mixed with a curing agent, the hydrophobic POSS-based hybridization fluorinated acrylate resin aggregates and is self-assembled in a film-forming solvent so as to form a micellar solution, then a phase isolation technology is used for ensuring that the solvent volatilizes on filter paper or a metal screen to form a film so as to construct a composite multi-scale structure, so that a super-hydrophobic coating is prepared. The preparation method has the advantages that a free radical solution polymerization method is adopted, synthetic conditions are simple, reaction routes are simple, raw materials are simple and easy to get, and the preparation technological processes of organic / inorganic hybrid materials are greatly simplified; the hydrophobic POSS-based hybridization fluorinated acrylate resin has wide application prospect in the field of waterproof and dampproof coating and the like.

The invention discloses a POSS (Polyhedral Oligomeric Silsesquioxane) based hybridized fluorinated acrylate resin, and a preparation method and an application thereof. The formula of the resin comprises the following components by weight percent: 0.9-14% of POSS based monomer, 1.5-10% of hard monomer, 2.5-14% of soft monomer, 4-10.5% of acrylic higher ester monomer, 1.8-6% of fluoridized acrylate monomer, 1.8-9% of cross-linked monomer, 0.4-1.5% of initiator and 50-80% of solvent. According to the invention, the acrylic higher ester monomer is introduced as an oleophilic monomer into a fluorinated acrylate copolymer and then a hydrophobic and oleophilic compound multi-scale structure is established on filter paper or a metal filter screen by virtue of aggregating self-assembly of the POSS base in the copolymer; therefore, a hydrophobic and oleophilic coating is prepared. The resin coating prepared from the resin provided by the invention is applicable to the oil-water separation field and capable of removing trace moisture in the fuel oil, and has great practical application significance.

The invention discloses (Ti,M)C nano solid solution powder and a preparation method thereof. The (Ti,M)C nano solid solution powder is prepared from the following components in percentage by weight: 35 to 79.9 percent of Ti, 0.1 to 35 percent of M and the balance of C, wherein the M is at least one of W, Mo, Cr, Ta, V and Nb. The preparation method comprises the following steps of mixing Ti powder, carbon black powder and a powdery raw material of the component M, carrying out high-energy ball milling, drying a mixture obtained after the ball milling, then putting the dried mixture into a crucible, adding a halogenating agent, afterwards, in the protection condition of an Ar gas, carrying out heat preservation for 2h to 4h at 900 to 1,000 DEG C, so as to obtain halogenating agent mixed (Ti,M)C nano solid solution powder, finally, dissolving the halogenating agent by using distilled water, centrifuging and drying, so that the (Ti,M)C nano solid solution powder is subsequently obtained.The method provided by the invention can be used for completing the carbonization and solid-solution reactions of (Ti,M)C at 900 to 1,000 DEG C; the prepared (Ti,M)C solid solution powder has the characteristic of a single-phase component and has the average particle size which is less than 100nm; the powder is high in purity and the content of the C is easy to precisely regulate and control.

A synthetic process of a green efficient agricultural fungicide is disclosed. The synthetic process includes: preparing 4-(methoxymethene)-3-isobenzofuranone by adopting 3-isochromanone as an initial raw material; preparing methyl (E)-2-(2-halomethylphenyl)-3-methoxy acrylate from the 4-(methoxymethene)-3-isobenzofuranone in methanol, a third inert solvent and a halogenating agent; and reacting the methyl (E)-2-(2-halomethylphenyl)-3-methoxy acrylate and 2-hydroxy-6-(trifluoromethyl)pyridine or 6-trifluoromethyl-2-pyridinol salt to obtain picoxystrobin. The synthetic process has characteristics of short reaction steps, mild reaction conditions, simple, convenient and feasible post-treatment, little three-waste, low cost, high yield, and suitability for industrial production. A product is good in appearance, and has external standard purity higher than 98%.

The invention discloses a synthesis method and an intermediate compound of morphine-6-Beta-D-glucuronide. The synthesis method comprises the following steps: (1) carrying out a reaction on 3-acetyl morphine and acyl-protected glucuronate in an organic solvent 1 under the catalysis of lewis acid so as to obtain an intermediate shown as a formula (IV); (2) hydrolyzing the intermediate shown as the formula (IV) with lithium hydroxide and neutralizing the intermediate shown as the formula (IV) with hydrobromic acid in a mixture solvent of C1-C4 alkanol and water; and washing the intermediate with the C1-C4 alkanol and drying, thereby obtaining the intermediate compound of the morphine-6-Beta-D-glucuronide, wherein the definitions of substituent groups in the formula (III) and the formula (IV) are shown in the specification. The synthesis method has the advantages of moderate condition and high yield, and is simple to operate and easy to industrialize.

The invention discloses a method for preparing 3-aminopyrrolidine hydrochloride by using a one-pot method. Under an ice-water bathing condition, pyrrole is dissolved in acetonitrile, a catalyst di(triphenyl phosphine) cupric nitrate is added at the same time, nitric acid is added dropwise to conduct a reaction to generate reaction liquid containing 3-nitropyrrole, the reaction liquid is subjectedto extraction by water and ethyl acetate, and an organic phase is obtained after separation is conducted; the obtained organic phase is subjected to reduction by pumping in hydrogen gas under the palladium catalysis condition, and a crude product of 3-aminopyrrolidine is obtained; and a solvent ethyl acetate is added into the crude product of 3-aminopyrrolidine, HCl gas is pumped in to conduct a reaction, and 3-aminopyrrolidine hydrochloride is obtained. The experiment route of the method is simple and short, the raw materials are cheap and easy to get, and the reaction condition is mild.

The invention discloses a preparation method of an agricultural bactericide. The method includes following steps: carrying out a reaction between 3-isochromanone, which is used for a starting raw material, and an acetol of a formamide compound, performing hydrolysis to obtain 4-([alpha]-hydroxyl)-methylene-2-H-benzopyrane-3-(4H)-one, performing methylation to obtain 4-(methoxylmethylene)-3-isobenzopyrone, preparing (E)-2-(2-halomethyl)-3-methoxylmethyl acrylate from the 4-(methoxylmethylene)-3-isobenzopyrone in methanol, a third inert solvent and a halogenation reagent, and performing a reaction between the (E)-2-(2-halomethyl)-3-methoxylmethyl acrylate and 2-hydroxyl-6-trifluoromethylpyridine or 6-trifluoromethyl-2-pyridine alkoxide to obtain picoxystrobin. The method is short in reaction processes, is mild in conditions, is simple and convenient in post treatment, is less in waste gas, waste water and waste solid, is high in yield and is suitable for industrial production. Appearance of the agricultural bactericide is good and an external standard content of the agricultural bactericide is more than 98%.

The present invention provides technological process of preparing PMIDA as the intermediate of glyphosate, and features that imino diacetonitrile is used as material in preparing PMIDA (N-phosphonyl methyl imino diaceteic acid).

The invention relates to a preparation method of an isoxazoline insecticide, which relates to the technical field of chemical industry, and comprises the following steps: 1) coupling reaction: mixingan intermediate 1 with nitromethane in a solvent, adding a palladium catalyst and a ligand to carry out catalytic coupling, reacting, and separating and purifying to obtain an intermediate 2; 2) cyclization reaction: mixing the intermediate 2 and an intermediate 3, adding the mixture into a mixed solution of a dehydrating agent and alkali, carrying out full cyclization reaction, and purifying to obtain an intermediate 4; and 3) condensation reaction: mixing the intermediate 4 and an intermediate 5, adding a condensing agent, carrying out full condensation reaction, and carrying out separationand purification to obtain an isoxazoline compound 6. The method has the advantages of short reaction route, accessible raw materials, fewer three wastes and high purity of the purified product, and is suitable for industrial production.

A method for preparing silodosin intermediate is disclosed. Said intermediate has the structure of (M), wherein R is benzyl or benzoyl. Said preparation method has the characteristics of short reaction route, simple operation, low cost, high yield, stable process, etc. The method is suitable for industrial production, and has extra-high industrial application value. Intermediate compounds for preparing the intermediate represented by M are also disclosed.