43results about How to "Reduce separation and purification process" patented technology

The invention provides a method for synthesising halogenated aromatic amine through hydrogenation in a solvent-free condition. The method comprises the following step of: carrying out a liquid-phase hydrogenation reaction on the halogenated aromatic nitro compound shown in formula (I) under the action of hydrogen, in the absence of a solvent and a dehalogenation inhibitor under the action of a carbon-supported large-particle-size precious metal catalyst to prepare the halogenated aromatic amine shown in formula (II). The method provided by the invention is capable of achieving the effect of inhibiting a hydrogenation dehalogenation side reaction in the case of not adding a dehalogenation inhibitor, is high in target product selectivity, and is capable of remarkably increasing the reaction speed.

The invention belongs to the field of recycling of solid waste, and provides a method for preparing liquid fuel by using biomass. The method is characterized by comprising the following steps that thereaction phase and the extract phase are mixed to form a two-phase system to serve as a reaction medium; an acid catalyst, a hydrodeoxygenation catalyst, a biomass raw material and the reaction medium are added into a reactor at the specific mass ratio; a hydrogen source is introduced to have the continuous reaction under the specific temperature and stirring conditions, and cellulose and hemicellulose in the biomass are conversed to be 2,5-2-methylfuran and 2-methylfuran respectively; the water phase and the organic phase are separated, the organic phase rich in 2,5-2-methylfuran and 2-methylfuran is obtained to serve as the liquid fuel, and the unreacted rest materials in the water phase are recycled. The method provided by the invention does not need to pre-process the biomass, can lower temperature and hydrogen consumption and loss needed by the reaction, reduces the separation and purification process, and can integrate 2,5-2-methylfuran and methylfuran into the fuel product directly.

The invention discloses a synthesis method of polysubstituted sulfur-containing or selenium-containing benzo[c,d]indole compounds. Firstly, 8-alkynylnaphthylamine compounds, thioether (diselenide), acatalyst and an additive are placed in a reactor, a solvent is added to the reactor until 8-alkynylnaphthylamine compounds and thioether (diselenide) are completely dissolved, then, the mixture is heated to react, after the reaction, aftertreatment is performed, and the polysubstituted sulfur-containing or selenium-containing benzo[c,d]indole compounds are obtained. The polysubstituted sulfur-containing or selenium-containing benzo[c,d]indole compounds are synthesized with a one-pot one-step method, the reaction operation is simple, intermediate separation and purification processes are reduced, the reaction condition is mild, the reaction selectivity is good, the yield is high, the substrate universality is wide, the reaction materials are simple and easy to obtain, the production cost islow, and the method is applicable to large-scale industrial production as well as small-scale laboratory preparation.

The invention provides a mixed rare-earth modified methane steam reformed nickel-based catalyst and a preparation method thereof. According to the mixed rare-earth modified methane steam reformed nickel-based catalyst, nickel nitrate and the like are used as precursors and are directly immersed and loaded on spherical aluminum oxide modified by mixed rare earth. The mixed rare earth is obtained by mixing two selected from lanthanum-cerium, lanthanum-yttrium, lanthanum-praseodymium, lanthanum-samarium and the like, wherein the loading weight of nickel in the catalyst is 5-30% of the weight of the catalyst and the loading weight of the mixed rare earth is 0.5-10% of the weight of the catalyst; the ratio of the mixed rare earth is 7/3-3/7. With the adoption of the mixed rare earth, the separation cost of the rare earth can be greatly reduced; the preparation method of the catalyst is simple; the catalyst has the good catalytic activity and stability on reforming methane steam in a fixed bed.

The invention provides a synthesis method of a copper-promoted 3-cyano-substituted-indole compound. According to the method, a copper reagent which is cheap and easy to obtain is used as a medium, an indole compound, TMEDA (tetramethylethylenediamine) and acetonitrile are used as raw materials, and the 3-cyano-substituted-indole compound is synthesized. The method has the advantages as follows: the raw materials are cheap and easy to obtain, the TMEDA and the acetonitrile are used as sources of cyano-groups, usage of higher-toxicity cyanide is avoided, special reaction conditions such as ligands, acids, bases, superoxides, microwave radiation and the like are not adopted, operation is simple, conditions are moderate, the yield is higher, and the method has the broad industrial application prospect.

A synthetic method of 2-phenyl-3-cyano benzofuran compounds is disclosed. The method includes weighing an aldehyde compound, an aryl acetonitrile compound, a catalyst and an alkali, according to a mole ratio of 1:1-2:0.2:4, adding into a reaction container, adding a solvent into the container until the aldehyde compound and the aryl acetonitrile compound are fully dissolved, putting the reaction container into an oil bath having temperature of 100-120 DEG C, reacting under stirring for 18-24 h, cooling to room temperature, adding water the volume of which is same as the volume of the solvent, extracting with dichloromethane for 2-4 times, separating by a silica column and distilling under vacuum to obtain a product that is one of the 2-phenyl-3-cyano benzofuran compounds. The method adopts a one-pot manner to produce the 2-phenyl-3-cyano benzofuran compounds, reduces processes of separation and purification of intermediates, and is simple in operation method, mild in reaction conditions, simple and easily available in raw materials, low in production cost, suitable for small-scale preparation in a laboratory and suitable for large-scale industrial production.

The invention discloses a preparation method of clethodim and an intermediate thereof. The preparation method of the intermediate comprises the step of acidifying a compound A to obtain a compound B.According to the invention, the compound B is obtained by acidifying the compound A, and reacts to obtain a compound D, and the compound D reacts to obtain clethodim, so that the reaction condition are mild, the operation is simple, the preparation process of the compounds A-D does not require separation, water washing, layering, rearrangement and other operations, the clethodim preparation process flow is simplified, the reaction time is shortened, the production efficiency is improved, the post-treatment is simple, water washing, layering and other processes are not needed, separation and purification are facilitated, the wastewater treatment burden is not increased, three wastes are reduced, the production cost is reduced, the environmental protection requirement is met, and the methodis suitable for industrial production.

The invention discloses a 3-cyanoindole compound synthesis method which includes: firstly, taking indole compound, benzyl cyanide and CuI according to the molar ratio of 1:1-2:1-2, placing the indole compound, the benzyl cyanide and the CuI in a reaction vessel, and adding solvent into the reaction vessel until the indole compound and the benzyl cyanide are completely dissolved; then, placing the reaction vessel in oil bath at the temperature of 100-130 DEG C with stirring for reaction for 30-34h, cooling to the room temperature, adding water as same as the solvent in volume, and extracting for 2-4 times by the aid of dichloromethane; and finally, separating by means of silica gel column chromatography prior to reduced pressure distillation so that the product, namely, the 3-cyanoindole compound is obtained. The 3-cyanoindole compound is synthesized by the aid of 'one-pot' reaction, and accordingly the intermediate separation and purification process is omitted, and the method is simple to operate, mild in reaction conditions, available in reaction raw materials, low in production cost and applicable to small-scale laboratorial preparation and large-scale industrial production.

The present invention discloses new 1,3-dihydroxy-3,7-dimethyl-6-octen-2-one synthesis method, which comprises racemic synthesis and enantioselective synthesis. According to the present invention, commercially available 6-methyl-5-hepten-2-one (CAS:110-93-0) is adopted as a starting material, two one-pot series connection reaction systems are adopted, simple operations are performed, the separation purification of the intermediate is effectively avoided, the high-yield racemic synthesis of the 1,3-dihydroxy-3,7-dimethyl-6-octen-2-one is achieved, and the asymmetric synthesis method for enantioselective synthesis of (R)-1,3-dihydroxy-3,7-dimethyl-6-octen-2-one and (S)-1,3-dihydroxy-3,7-dimethyl-6-octen-2-one is developed. The present invention further discloses an intermediate compound.

The invention discloses a transforming adsorbing method to separate and recycle C3+ hydrocarbon from composite gas, which is characterized by the following: the composite gas is filled in the adsorbing tower with adsorbant, which is separated through transforming adsorbing course; the adsorbing tower possesses alumina, activated charcoal and silica gel with middle and micro-hole structure and specific area at 300-1500m2/g, whose bulk rate is 5-50% alumina, 5-90% activated charcoal, 0-90% silica gel; the content of activated charcoal is more than alumina, which can separate and recycle C3+ hydrocarbon through extracting step.

The invention discloses a synthesis method of 7-chloroquinaldine. 2-nitrotoluene, SiO2-HEPIMBr, m-chloroaniline, crotonaldehyde, TEOS, 2-bromoethanol, imidazole and 3-chloropropyltriethoxysilane are taken as main raw materials. According to the synthesis process, m-chloroaniline and crotonaldehyde are subjected to Skraup reaction under action of an immobilized ion catalyst SiO2-HEPIMBr, and 7-chloroquinaldine is obtained. SiO2 immobilized hydroxyl ionic liquid HEPIMBr is prepared with a grafting method, in the reaction, few by-products are produced and no 5-isomer is produced, so that the separation and purification process is reduced, purity of a product is improved, yield of the product is increased, and higher market competitiveness is achieved.

The invention discloses a preparation method of an isoquinolinone derivative, which comprises the following steps: weighing an 8-alkynyl-1-aryl naphthylamine compound and a catalyst according to a molar ratio of 1:(0.1-1.5), putting the 8-alkynyl-1-aryl naphthylamine compound and the catalyst into a reaction vessel, and adding a solvent into the reaction vessel until the 8-alkynyl-1-aryl naphthylamine compound is completely dissolved; and placing the reaction container at 80-150 DEG C, carrying out a stirring reaction for 0-36 h, and carrying out post-treatment to obtain the product polysubstituted isoquinolinone compound. The method is simple in operation method, mild in reaction condition, good in reaction selectivity, high in yield, convenient to separate and purify, wide in substrate universality, simple and easily available in reaction raw materials, low in production cost and good in application prospect.

The invention discloses a genetically engineered bacterium community based on artificial design and a construction method and application thereof. The genetically engineered bacterium community based on artificial design comprises a recombinant engineering bacterium 1 containing a GtF3 'H gene and a CPR gene and a recombinant engineering bacterium 2 containing an MpOMT gene. The construction method comprises the following steps: constructing a recombinant engineering bacterium 1 and a recombinant engineering bacterium 2; culturing into a culture solution; and mixing to obtain the genetically engineered bacterium community. In the genetically engineered bacterium community, GtF3 'H catalyzes a hydroxylation reaction of a substrate naringenin to synthesize an intermediate product eriodictyol, CPR is a cofactor for the GtF3' H to perform a catalytic function and transfers electrons of NADPH to GtF3 'H to perform a hydroxylation reaction, and MpOMT catalyzes an oxygen methylation reaction of the intermediate product eriodictyol to synthesize hesperetin.