159results about "Preparation by OH and halogen introduction" patented technology

A method of fluorination comprising reacting monosaccharides, oligosaccharides, polysaccharides, composite saccharides formed by bonding of these saccharides with proteins and lipids and saccharides having polyalcohols, aldehydes, ketones and acids of the polyalcohols, and derivatives and condensates of these compounds with a fluorinating agent represented by general formula (I) thermally or under irradiation with microwave or an electromagnetic wave having a wavelength around the microwave region. In accordance with the method, the fluorination at a selected position can be conducted safely at a temperature in the range of 150 to 200° C. where the reaction is difficult in accordance with conventional methods. The above method comprising the irradiation with microwave or an electromagnetic wave having a wavelength around the microwave region can be applied to substrates other than saccharides. When a complex compound comprising HF and a base is reacted under irradiation with microwave, fluorination at a specific position which is difficult in accordance with conventional methods proceeds highly selectively, efficiently in a short time and safely.

The invention provides a method for industrial production of a butoconazole nitrate intermediate, that is 1-chloro-4-p-chlorophenyl-2-butanol (a compound in formula II). The method of the invention comprises: 1. a Grignard reaction, that is, adopting p-chlorobenzyl chloride as a raw material, and performing a Grignard reaction with magnesium powder in a mixed solvent of methyl tertiary butyl ether and tetrahydrofuran; 2. a condensation reaction, that is, continuing reaction by adding epichlorohydrin to obtain the compound II which is an important intermediate for preparing butoconazole nitrate. According to the method, the raw materials are cheap and easily available, the reaction solvent is safer, and the method is suitable for industrial production.

This invention is a process for preparing chlorohydrins by reacting a chlorinating species, such as hypochlorous acid, with at least one unsaturated organic compound, such as propylene or butylene, at a pH of greater than 6.0. The chlorinating species is formed in a first step by reacting a source of chlorine, such as Cl2 gas, with an aqueous pH adjusting source, such as aqueous NaOH.

There are provided a novel norbornene derivative which is a material for a chemically amplifying type photoresist for F₂ laser, possesses excellent transparency and improved dry etching resistivity and has a fluorine-containing ketone unit or fluorine-containing tertiary alcohol unit directly bonded to the norbornene backbone; a fluorine-containing polymer obtained by using the norbornene derivative as a copolymerizable monomer; and a chemically amplifying type photoresist composition comprising the fluorine-containing polymer, a photoacid generator and a solvent.

The invention relates to a new trifluoro methylation reagent and preparation and application thereof, and in particular relates to a compound with a structure shown as a formula I, a preparing method thereof and application thereof as a trifluoro methylation reagent. In the formula, the definition of each group is as defined in the specification. The starting materials of the new trifluoro methylation reagent are cheap and easy to obtain, the reaction condition is mild, the post treatment is simple, the product can be used as a variety of potential trifluoro methylation reagents, the yield is high, the equipment requirement is low, and the new trifluoro methylation reagent has wide prospects of industrial application. (FSO2CF2COO) zM I.

Nonmetallic, chiral organic catalysts are used to catalyze enantioselective fluorination of enolizable aldehydes. Reaction systems composed of an enolizable aldehyde, an electrophilic fluorination reagent, and a nonmetallic chiral catalyst in the form of an imidazolidinone salt are also provided.

The invention discloses a synthesis method of 1-bromo-9,9'-spirodifluorene, belonging to the field of organic chemical synthesis. The method comprises the following steps: in an inert gas protective atmosphere, preparing a Grignard reagent in a methyl tetrahydrofuran solvent by using 1,3-dibromobenzene as an initial raw material, continuing reacting with ortho-halogen iodobenzene and magnesium powder under the catalytic action of zinc bromide, carrying out reaction with fluorenone, carrying out hydrolysis, and carrying out intramolecular closed loop synthesis under the catalytic action of boron trifluoride to obtain the 1-bromo-9,9'-spirodifluorene. The synthesis method has the advantages of simple process and cheap and accessible raw material, obviously lowers the production cost of the product, and widens applicability of fluorene derivatives as an intermediate in organic photoelectric material design and synthesis.

The invention relates to a propylene recovery method in epoxypropane refining process. In the propylene recovery method, non-condensable gas obtained from the tower top of a light-fraction removing tower is washed with water, and is mixed with gas generated in chlorohydrination, and an obtained mixture is subjected to pressure recovery. The propylene recovery method is simple, and is convenient in operation; the tower top gas of the light-fraction removing tower is introduced into chlorohydrination treatment for recovery, propylene raw material unit consumption of epoxypropane equipment is reduced, and production cost of epoxypropane is reduced.

The invention provides a halopropyl alcohol preparation method, which comprises: (1) a catalyst acid treatment: soaking a catalyst in an acid, washing the catalyst, and drying the catalyst; (2) halo alcoholization: adding hydrogen halide, H2O2, propylene and the catalyst treated in the step (1) to a reaction device, and carrying out a halo alcoholization reaction to obtain halopropyl alcohol; optionally, (3) saponification: carrying out a saponification reaction on the halopropyl alcohol obtained in the step (2) and an alkali metal hydroxide, and separating to obtain propylene oxide and a halogenated alkali metal salt; and optionally, (4) electrodialysis: carrying out bipolar membrane electrodialysis on the halogenated alkali metal salt obtained in the step (3) to obtain the hydroxide of the alkali metal and the hydrogen halide. With the method of the present invention, the halopropyl alcohol can be produced in the extremely high selectivity and extremely high yield manner, and the emissions of wastewater and waste residue are substantially reduced.

1-Chloro-2-methyl-4-acyloxy-2-butene derivatives can be synthesized in good yields and high purity starting from isoprene and employing a chlorohydrin formation reaction in a system made of N-chloroisocyanuric acid derivatives and water, followed by esterification and rearrangement of the crude product mixture.

The invention discloses a micro reaction system and a method for chlorohydrination of chloropropene, belonging to the technical field of synthesis of organic compounds. The micro reaction system comprises one or more microreactor units connected in series, wherein water is injected from the first microreactor unit in one time, and then flows through 0-3 subsequent microreactor units in sequence. Chlorine and chloropropene are injected into each microreactor unit according to a certain distribution ratio. Inside each microreactor unit, chlorine injected firstly is dissolved in a liquid phase, contacts with chloropropene injected later to carry out a chlorohydrination reaction, and the reaction solution outflows from the last microreactor unit, and is aged through a pipeline to obtain the product. The system provided by the invention adopts a multistage series system, can prepare high-concentration dichloropropanol solution, and avoids a cyclic process and reduces the process energy consumption at the same time. Meanwhile, due to the enhanced mixing effect of the microreactor, the method disclosed by the invention can improve the selectivity and the yield of the chlorohydrination process of chloropropene.

The invention provides a method for treating epichlorohydrin wastewater. The method comprises the working procedures of steam stripping, reaction extraction, rectification, hydrolysis rectification and the like, and monochloropropanediol in wastewater and can be effectively recovered. According to the invention, energy consumption in the process is reduced by adopting a reaction extraction method,and an extracting agent and a reaction agent in an extraction reaction process can be recycled, so that resource utilization is realized, and economy is enhanced. The whole process flow is simple, iseasy for industrial implementation, and has a wide application prospect.

The invention provides a method for preparing halohydrin. The method comprises the following steps: 1) halogen alcoholization: halogen hydride, H2O2, and a catalyst are added in a reaction apparatus, and ethylene is added for a halogen alcoholization reaction to obtain halohydrin. The invention also provides a method for preparing ethylene oxide by a halogen alcoholization method, which comprises the step 1) in right claim 1, the method also comprises a step of 2) saponification: halohydrin in the step 1) and hydroxide of alkali metal are subjected to a saponification reaction, then separated to obtain ethylene oxide and alkali halide metal salt; and an optional step of 3) electrodialysis: the obtained alkali halide metal salt is subjected to bipolar membrane electrodialysis to obtain the hydroxide of alkali metal and the halogen hydride. The method is used for preparing halohydrin or ethylene oxide with high selectivity and yield, and greatly reduces the discharge of waste water and waste residue.

The invention provides a method for preparing halogen ethanol, wherein the method comprises: (1) acid treatment of a catalyst, wherein a catalyst is soaked in an acid, the soaked catalyst is washed, and the washed catalyst is dried; (2) halogen alcoholization, wherein hydrogen halide, H2O2, ethylene and the catalyst treated in the step (1) are added to a reaction device, and a halogen alcoholization reaction is performed to obtain the halogen ethanol; optionally (3) saponification, wherein the halogen ethanol obtained in the step (2) and the hydroxide of an alkali metal are subjected to a saponifying reaction, and separation is performed to obtain ethylene oxide and a halogenated alkali metal salt; and optionally, (4) electrodialysis, wherein the halogenated alkali metal salt obtained in the step (3) is subjected to bipolar membrane electrodialysis to obtain the hydroxide of the alkali metal and the hydrogen halide. According to the present invention, the halogen ethanol is prepared in the forms of the extremely high yield and the extremely high selectivity, and the emission of wastewater and waste residue is substantially reduced.

The invention provides a method for preparing halogen ethyl alcohol. The method comprises the following step: (1) halogen alcoholization: adding halogen hydride, H2O2, ethylene and a Ti heteroatom-containing molecular sieve into a reaction device, and carrying out halogen alcoholization reaction to obtain the halogen ethyl alcohol. The invention also provides a method for preparing ethylene oxide with a halogenohydrin method. The method comprises the following steps: (1) halogen alcoholization: adding halogen hydride, H2O2, ethylene and a Ti heteroatom-containing molecular sieve into the reaction device, and carrying out the halogen alcoholization reaction to obtain the halogen ethyl alcohol; (2) saponification: carrying out saponification reaction on the halogen ethyl alcohol in the step (1) and a hydroxide of alkali metal, and separating to obtain the ethylene oxide and alkali halide metal salt; optionally (3) electroosmosis: carrying out bipolar membrane electroosmosis on alkali halide metal salt obtained in step (2) to obtain the hydroxide of alkali metal and the halogen hydride. According to the methods, the halogen ethyl alcohol or the ethylene oxide can be prepared at extremely high selectivity and yield, and the discharging of waste water and waste residues can be drastically lowered.

The present invention relates to industrial production of epoxy propane. The tubular reactor consists of 5-80 serially connected reaction units, and each unit consists of one piece of chlorine predissolving reaction tube and one piece of propylene chlorohydrinizing reaction tube. The outlet of the last propylene chlorohydrinizing reaction tube is the outlet of the propylene chloride, the chlorine inlet of the first chlorine predissolving reaction tube is the inlet of the technological water, all the inlets of the propylene chlorohydrinizing reaction tubes are connected to the propylene material pipe, all the gas inlets of the chlorine predissolving reaction tubes are connected to the chlorine material pipe, and propylene material and chlorine material are fed into all reaction units simultaneously.

The invention discloses a method for synthesizing chlorohydrin by the reaction of 30 to 36 wt% industrial hydrochloric acid and ethylene oxide. The molecular ratio of the ethylene oxide to the chlorine hydride is kept between 1.01 and 1.05; in the method, a self-prepared supported catalyst is used, so that the side reactions are effectively inhibited and the conversion rate is improved; and a fixed bed reactor is used, the reaction temperature is controlled to between 30 and 60 DEG C, and the 47 to 53 wt% aqueous solution of chlorohydrin can be finally obtained. The method has the advantages of simplifying the production process and lowering production cost.

A method of preparing chlorohydrins and a method of preparing epichlorohydrin by using chlorohydrins prepared using the method are provided. The method of preparing chlorohydrins by reacting polyhydroxy aliphatic hydrocarbon with a chlorination agent in the presence of a catalyst includes at least one combination of a series of unit operations including a first reaction step, a water removal step, and a second reaction step, in that respective order, wherein the method further includes purifying chlorohydrins from a reaction mixture discharged from a final reaction step of the plurality of reaction steps. The method of preparing epichlorohydrin includes reacting chlorohydrins prepared using the method of preparing chlorohydrins, with an alkaline agent.