9 results about "Benzotrichloride" patented technology

The application discloses a continuous production process and equipment for a trifluoromethylbenzene tower, and belongs to the field of organic fluorine chemistry. The production process comprises the following steps: S1: continuously feeding trichloromethylbenzene and hydrogen fluoride into a tower reactor connected with a heat exchanger circulating cooling system in a reverse direction, so that a three-stage continuous fluorination reaction occurs in the tower reactor to obtain crude trifluoromethylbenzene, and unreacted hydrogen fluoride is separated into liquid at the top of the tower and then flows back into the tower reactor; S2: the crude trifluoromethylbenzene obtained in the reaction is subjected to nitrogen bubbling in a bubble tower, and then is continuously distilled in a rectifying tower to obtain finished trifluoromethylbenzene; and S3: byproduct hydrogen chloride generated in the fluorination reaction is introduced into a hydrochloric acid tank to obtain hydrochloric acid, and the content of hydrofluoric acid in the hydrochloric acid is less than 1000 ppm. The method can greatly improve the utilization rate of raw material hydrogen fluoride, improve the purity of byproduct hydrochloric acid, reduce the generation amount of waste acid, avoid the sharp change of pressure in the reaction process, and realize large-scale, continuous, stable and safe production of trifluoromethylbenzene.

The present application relates to the technical field of fine chemicals synthesis, and discloses a method for high-selectivity co-production of phthaloyl chloride and benzoyl chloride. The method uses dimethylbenzene and trichlorobenzene as raw materials, and feeds them into a photochlorination reaction tower to heat the materials. Then, the reaction tower is kept in a micro-negative pressure condition to perform photochlorination reaction. After the reaction is completed, the liquid is directly fed into a reaction kettle, and phthalic acid and a catalyst are added. Finally, the reaction liquid is separated by rectification to obtain the products phthaloyl chloride and benzoyl chloride. The present application greatly improves the selectivity of dimethylbenzene photochlorination reaction, and inhibits the ring chlorination side reaction. The present application can realize flexible co-production of m-phthaloyl chloride and p-phthaloyl chloride and benzoyl chloride, and can flexibly adjust the generation ratio of phthaloyl chloride and benzoyl chloride according to the raw material supply and product demand, thereby greatly improving the production flexibility of the reaction device.

The application belongs to the technical field of organic synthesis and particularly relates to a synthesis method of electronic-grade 2,3,4-trihydroxybenzophenone. The application comprises the following steps: catalytic reaction: taking water as a solvent, mixing water and a catalyst uniformly, adding pyrogallic acid, heating the system to 40-50 DEG C, continuously adding trichloromethylbenzene, performing insulation reaction, cooling the system to 10-15 DEG C after the reaction is completed, crystallizing and precipitating, and then filtering to obtain a crude wet product; purification treatment: removing impurities from the crude wet product to obtain the high-purity 2,3,4-trihydroxybenzophenone. The application does not need to react in an organic solvent system, is green and environmentally friendly, does not need nitrogen protection, has low production cost, and is suitable for industrialized processing and production, and the prepared 2,3,4-trihydroxybenzophenone has high purity and high yield.

The invention belongs to the technical field of organic synthesis, and particularly relates to a green synthesis method of electronic-grade 2, 3, 4-trihydroxy benzophenone. The method comprises the following steps: catalytic reaction: taking water as a solvent, uniformly mixing water and a catalyst, adding pyrogallic acid, heating the system to 40-50 DEG C, continuously adding trichlorotoluene, carrying out heat preservation reaction, cooling to 10-15 DEG C after the reaction is completed, crystallizing, separating out and filtering to obtain a crude wet product; and purification treatment: removing impurities from the crude wet product to obtain the high-purity 2, 3, 4-trihydroxy benzophenone. The method does not need reaction in an organic solvent system, is green and environment-friendly, does not need nitrogen protection and is low in production cost, and the prepared 2, 3, 4-trihydroxy benzophenone is high in purity and yield and suitable for industrial processing production.

The present invention provides an improved process for the preparation of benzonitrile compounds More particularly, the present invention relates to an improved process for the preparation of benzonitrile compounds of Formula (I) by nitrilation of the corresponding benzotrichloride compounds of Formula (II).

The utility model discloses a tail gas absorption device in trichlorotoluene production, which belongs to the technical field of trichlorotoluene production, and comprises an absorption tank, the left side surface of the absorption tank is fixedly connected with a fixed plate, the left side surface of the fixed plate is fixedly connected with a filter cartridge, the right side surface of the absorption tank is fixedly connected with a support plate, and the support plate is fixedly connected with the filter cartridge. A liquid storage box is fixedly installed on the upper surface of the supporting plate, a liquid pump is fixedly installed on the upper surface of the liquid storage box, the output end of the liquid pump fixedly communicates with a liquid discharging pipe, and the end, away from the liquid pump, of the liquid discharging pipe penetrates through the absorption tank and extends into the absorption tank; and the end, away from the infusion pump, of the liquid drainage pipe fixedly communicates with a liquid drainage spraying disc, and the upper surface of the absorption tank fixedly communicates with a communicating pipe. According to the tail gas absorption device in trichlorotoluene production, organic matters and the like in tail gas can be physically adsorbed, the purpose of removing pollutants is achieved, the tail gas can be efficiently absorbed and treated, and the subsequent treatment requirement of the tail gas can be met.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and determining ibrutinib SM3 and impurities thereof based on gas chromatography. The impurities comprise any one or more of acrylic anhydride, trichlorotoluene, propionyl chloride, 3-chloropropionyl chloride, benzoyl chloride, acrylic acid and benzoic acid; the ibrutinib SM3 and impurities jointly form a composition to be detected. According to the method, (5% phenyl)-diphenylmethylsiloxane is adopted as a chromatographic column of a stationary liquid, or other stationary liquids with the same polarity are adopted; the ibrutinib SM3 and impurities of the ibrutinib SM3 are separated by adopting temperature programming; the temperature programming setting is as follows: the initial temperature is 35 + / -5 DEG C and is maintained for 5 + / -1 minutes, and the temperature is raised to 210 + / -10 DEG C at the rate of 30 + / -5 DEG C / min and is maintained for 8 + / -2 minutes. The method provided by the invention can effectively separate, identify and quantify various related substances in ibrutinib SM3, and has the advantages of short separation time, strong specificity, high sensitivity and good durability.

The present invention discloses an improved process for preparing a benzonitrile compound of formula (I) from the corresponding trichlorotoluene compound of formula (II).

The invention relates to a method and a device for industrially producing dichlorotoluene and application of a catalyst. The invention provides a method for industrially producing dichlorotoluene, which comprises the step of reacting m-chlorotoluene with chlorine in the presence of a catalyst, and the catalyst is a compound catalyst of a metal compound and a sulfur-containing compound. The main product of the reaction is 2, 5-dichlorotoluene, a small amount of byproducts are 3, 4-dichlorotoluene and 2, 3-dichlorotoluene, the primary reaction conversion rate of the raw materials is high, the main product 2, 5-dichlorotoluene is high in selectivity, and the byproduct trichlorotoluene is low. Wherein the catalyst is a compound catalyst of metal compounds such as aluminum, iron, nickel, titanium, copper, zirconium, antimony and the like and a sulfur-containing compound. According to the invention, a process for preparing 2, 5-dichlorotoluene, which is easy to industrialize, few in reaction steps, good in product directionality, high in yield and purity and low in production cost, can be provided.