18 results about "Tetrachloropropylene" patented technology

Provided is a process for the preparation of 2-chloro-3, 3, 3-trifluoropropene (HCFO-1233xf) by contacting 1, 1, 2, 3-tetrachloro-1-propene (HCO-1230xa) and HF in the presence of a zinc doped alumina catalyst at a suitable temperature and in a suitable molar ratio of HCO-1230xa: HF. Also provided herein is a process for the preparation of 3, 3, 3-trifluoropropene (HFO-1243zf) by contacting 1, 1, 1, 3-tetrachloropropane (HCC-250fb) and HF in the presence of a zinc doped alumina catalyst at a suitable temperature and in a suitable molar ratio of HCC-250fb: HF.

The invention discloses a method and system for preparing 1, 1, 3-trichloropropene through gas phase cracking, and belongs to the technical field of organic synthesis.The method comprises the following steps that 1, 1, 1, 3-tetrachloropropane is preheated to be vaporized and then introduced into a tubular fixed bed reactor provided with a catalyst bed layer to be subjected to a dehydrochlorination reaction, and 1, 1, 3-trichloropropene is obtained; the catalyst bed layer is formed by stacking a self-supporting structured metal catalyst, and the self-supporting structured metal catalyst is made of one or a combination of more of iron, zinc, copper, cobalt and nickel; the self-supporting structured metal catalyst has an open-pore annular structure, the open-pore annular structure is selected from one of a Raschig ring, a Pall ring, a theta ring or a cascade ring, and the catalyst with the corresponding structure can realize high gas flux, carbon deposition blockage resistance and low mass transfer resistance, and is good in catalytic effect, less in carbon deposition and low in maintenance cost. The method provided by the invention has the advantages of high reaction conversion rate and good selectivity on 1, 1, 3-trichloropropene.

A method of synthesizing 3,3,3-trifluoropropene including contacting 1,1,1,3-tetrachloropropane, in the vapor phase, at a temperature sufficient to effect dehydrochlorination to form 1,1,3-trichloro-1-propene. The 1,1,3-trichloro-1-propene is isolated and subsequently contacted, in the vapor phase, with hydrogen fluoride in the presence of a fluorination catalyst at a temperature sufficient to effect formation of 3,3,3-trifluoropropene.

The invention relates to a method for resource utilization of 1, 1, 2-trichloropropane, and the method comprises the following steps: (1) carrying out high-temperature cracking on a material flow containing 1, 1, 2-trichloropropane to obtain a material flow containing 3, 3-dichloropropene; and (2) carrying out chlorination on the material flow containing 3, 3-dichloropropene to obtain a material flow containing 1, 1, 2, 3-tetrachloropropane. According to the method disclosed by the invention, the propylene chlorination by-product 1, 1, 2-trichloropropane can be subjected to high-temperature cracking to obtain 3, 3-dichloropropene, and 1, 1, 2, 3-tetrachloropropane is obtained after the 3, 3-dichloropropene is chlorinated. The byproduct 1, 1, 2-trichloropropane is fundamentally solved, the process route is simple, the flow is short, the reaction conversion rate is high, the selectivity is good, and industrial implementation is facilitated.

The present invention discloses a method for co-producing 3,3,3-trifluoropropene and 2,3,3,3-tetrafluoropropene, introducing 1,1,1,3-tetrachloropropane, 1,1,1,2,3-pentachloropropane and hydrogen fluoride into a first reactor to have a reaction in the presence of a first catalyst to obtain a reaction product of the first reactor; distilling the reaction product of the first reactor to obtain a 3,3,3-trifluoropropene product and a column bottom product, mixing the column bottom product with the hydrogen fluoride, and feeding a resulting mixture into a second reactor to have a reaction in the presence of a second catalyst to obtain a reaction product of the second reactor; and separating hydrogen chloride from the reaction product of the second reactor, and then carrying out water washing, alkali washing and drying to obtain a 2,3,3,3-tetrafluoropropene product. The present invention has the advantages of simple process, high efficiency, high operation flexibility, small investment and low energy consumption.

This invention discloses a catalyst for the chlorofluorination of 1,1,1,3-tetrachloropropane to prepare 2-chloro-3,3,3-trifluoropropylene, the catalyst being designated M. x O y / Fe p O q -MgF2, in which Fe p O q -MgF2 as support, Fe p O q It is a mixture of Fe2O3 and Fe3O4, M x O y M is the active component. x O y It consists of one or more of Al2O3, CuO, ZnO, and La2O3. The catalyst preparation method includes: adding a polyamine to an aqueous solution of a soluble magnesium salt at 30℃~60℃ with stirring, then adding hydrofluoric acid dropwise, and continuing stirring for 10min~60min after the addition is complete; adding a soluble iron salt to the above solution, and continuing stirring for 30min~90min; adding ammonia dropwise to adjust the pH to 8~10, and continuing stirring for 60min~180min; filtering, washing the filter cake with deionized water until the pH of the filtrate is ~7, drying at 80℃~120℃, and calcining at 200℃~260℃ to obtain the supported Fe. p O q The precursor salt of the active component is loaded onto a support using an impregnation method, dried at 80℃~120℃, and calcined at 260℃~320℃ to obtain the desired catalyst. The catalyst in this invention does not involve chromium or antimony compounds, and exhibits high selectivity and yield for 2-chloro-3,3,3-trifluoropropylene, making it valuable for industrial applications.

The invention discloses a co-production method for preparing pentachloropropane by chlorination of 1, 1, 1, 3-tetrachloropropane, and relates to the technical field of organic chemical synthesis, in particular to a co-production method for preparing pentachloropropane by chlorination of 1, 1, 1, 3-tetrachloropropane, which takes 1, 1, 1, 3-tetrachloropropane and chlorine as raw materials to react under the action of a solid chloride catalyst to prepare 1, 1, 1, 2, 3-pentachloropropane and co-produce 1, 1, 1, 3, 3-pentachloropropane. And 3, 3, 3-pentachloropropane is added. The molar ratio of the raw materials is 1.3: 1, chlorine is introduced from the bottom of the reactor, the reaction temperature is 50-120 DEG C, the pressure is 0-0.05 MPa, and at least one of aluminum chloride and the like can be selected as a catalyst. A reaction kettle is adopted, the temperature is initially increased to 80 DEG C, and chlorine is introduced; after the reaction, a crude product is separated by a negative pressure rectification system (containing a low-boiling-point rectification tower and a high-boiling-point rectification tower), unreacted raw materials are recycled by the low-boiling-point rectification tower, qualified 1, 1, 1, 2, 3-pentachloropropane is obtained at the top of the high-boiling-point rectification tower, 1, 1, 1, 3, 3-pentachloropropane is co-produced through tower kettle enrichment, and no sewage is generated in the whole process.

In a process for the production of 1,1,1,2,3-pentachloropropane, optionally in the presence of carbon tetrachloride, by introducing 1,1,1,3-tetrachloropropane, chlorine and a Lewis acid catalyst, the improvement comprising: introducing the Lewis acid as a slurry in a chlorinated hydrocarbon.

This invention discloses a method for preparing 2,3,3,3-tetrafluoropropylene. Using ethylene and carbon tetrachloride as raw materials, 1,1,1,3-tetrachloropropane (HCC-250fb) is first prepared. Then, 1,1,1,3-tetrachloropropane is decomposed to obtain 1,1,3-trichloropropene (HCC-1240za). This 1,1,3-trichloropropene is then reacted with chlorine to generate 1,1,1,2,3-pentachloropropane (HCC-240db). The 1,1,1,2,3-pentachloropropane is then decomposed to obtain 1,1,2,3-tetrachloropropene (HCC-1230xa). The 1,1,2,3-tetrachloropropene is reacted with hydrofluoric acid to generate 2-chloro-3,3,3-trifluoropropene (HCFO-1233xf). Finally, 2,3,3,3-tetrafluoropropylene is prepared using two different methods. This invention has low raw material costs and high yield.

This invention discloses a metal-carbon composite catalyst and method for the continuous preparation of 1,1,1,3-tetrachloropropane. The main component of the catalyst is Cu-Ni-Cl-C / Fe, and the catalyst preparation process includes four steps: mixing, carbonization, displacement, and loading. The catalyst of this invention can efficiently catalyze the telomerization reaction of carbon tetrachloride and ethylene, generating the target product 1,1,1,3-tetrachloropropane with high selectivity. The catalyst exhibits stable performance, maintaining good catalytic effect even after five repeated uses. The conversion rate of carbon tetrachloride and ethylene reaches over 95%, and the selectivity of 1,1,1,3-tetrachloropropane is greater than 98.5%.

The invention discloses a supported catalyst and method for preparing 1, 1, 1, 3-tetrachloropropane, and belongs to the technical field of industrial catalysis and organic chemistry, the supported catalyst comprises an alumina carrier and a ferrous chloride-phosphate ester complex active component supported by the alumina carrier; active components of the ferrous chloride-phosphate complex are loaded on the alumina carrier through an impregnation method, and an impregnation solution is prepared from anhydrous ferrous chloride, anhydrous phosphate and an anhydrous organic solvent in an anhydrous environment. The supported catalyst is simple and convenient in preparation process, low in cost, high in catalytic activity, high in carbon tetrachloride conversion rate, good in 1, 1, 1, 3-tetrachloropropane selectivity, easy to recycle, good in reusability and easy to popularize and use, and the problem that an existing catalyst is difficult to recycle or prone to inactivation can be solved.

The invention provides a method for continuously preparing 1, 1, 2, 3-tetrachloropropene through ultrasonic catalysis, and relates to the technical field of preparation of 1, 1, 2, 3-tetrachloropropene. The method comprises the following steps: 1, 1, 1, 1, 3-tetrachloropropane continuously enters a first ultrasonic reaction kettle, a catalyst is added for reaction, and 1, 1, 1, 3-tetrachloropropane is partially converted into 1, 1, 3-trichloropropene; the liquid mixture reacted in the first ultrasonic reaction kettle and chlorine gas continuously enter a second ultrasonic reaction kettle, a catalyst is added for continuous reaction, and 1, 1, 3-trichloropropene is chlorinated and converted into 1, 1, 1, 2, 3-pentachloropropane; a liquid mixture reacted in the second ultrasonic reaction kettle continuously enters a third ultrasonic reaction kettle, a catalyst is added for continuous reaction, and 1, 1, 1, 2, 3-pentachloropropane is converted into 1, 1, 2, 3-tetrachloropropene. The catalyst is subjected to ultrasonic treatment in an ultrasonic kettle to form a uniform system, and the concentration of the catalyst is 0.001%-0.9%. The catalyst is good in dispersity, simple in process and easy for continuous production.

This invention discloses a method for synthesizing 1,1,1,3-tetrachloropropane, belonging to the field of fine chemical intermediate synthesis technology. The method uses chloroform, chlorine, and ethylene as raw materials. Chloroform is mixed with a specific solid chloride catalyst as a mother liquor and added to a reactor. Chlorine and ethylene are continuously introduced from the bottom of the reactor. An addition reaction occurs under reaction conditions of 80-120℃ and 0.5-1.5 MPa, wherein the molar ratio of chloroform, chlorine, and ethylene is controlled at 1.6:0.8:1. The crude product generated is separated by distillation in a recovery tower, and unreacted chloroform and ethylene are returned to the reactor for recycling. No wastewater is generated throughout the reaction process. This invention features a simple process, high reaction selectivity, high catalyst activity and reusability, significantly improved raw material utilization, low equipment material requirements, low investment, and easy implementation for continuous industrial production. It overcomes the technical shortcomings of existing technologies, such as numerous by-products, complex control, large catalyst consumption, and difficult wastewater treatment.

This invention discloses a process for synthesizing tetrachloropropene from carbon tetrachloride, comprising the following steps: S1) Preparation of 1,1,1,3-tetrachloropropane via telomerization reaction. Carbon tetrachloride is used as a raw material, and ethylene is subjected to telomerization reaction under the catalysis of a metal-carbon composite catalyst. The metal-carbon composite catalyst is prepared by a four-step process of mixing, carbonization, displacement, and loading, and directionally catalyzes the generation of crude 1,1,1,3-tetrachloropropane. This application significantly improves the catalytic activity and product selectivity of the telomerization reaction between carbon tetrachloride and ethylene by employing a self-prepared metal-carbon composite catalyst. It can directionally generate the 1,1,1,3-tetrachloropropane intermediate, effectively suppressing side reactions and improving the yield of the target product and the conversion rate of raw materials. This catalyst, prepared by a four-step process of mixing, carbonization, displacement, and loading, has a stable structure, long service life, and can be recycled multiple times, significantly reducing catalyst consumption and production costs, and solving the problems of poor selectivity and insufficient stability of traditional catalysts.

The invention belongs to the technical field of chemical synthesis of fluorine-containing organic matters, and discloses a preparation method of 2, 3, 3, 3-tetrafluoropropene. The method comprises the following steps: (1) by taking 1, 1, 1, 3-tetrachloropropane (TCP) and AHF as raw materials, carrying out continuous gas-phase catalytic fluorination reaction in the presence of a gas-phase fluorination catalyst to obtain a 1, 1, 1-trifluoropropene product; (2) metering 1, 1, 1-trifluoropropene and chlorine, adding the 1, 1, 1-trifluoropropene and chlorine into a photochlorination reactor, reacting to generate 2, 2-chloro-1, 1, 1-trifluoropropene (HCFC-243db), and then carrying out saponification reaction under the action of 30% sodium hydroxide to obtain HCFO-1233xf; (3) adding HCFO-1233xf, HF and a catalyst into a reactor, reacting at 20-80 DEG C for 4-5 hours, and rectifying to remove light components and heavy components to obtain HCFC-244bb; and (4) adding the HCFC-244bb and diluent gas into a reactor to carry out thermal cracking reaction, and carrying out rectification, light component removal, heavy component removal and drying on a product to obtain the HFO-1234yf. The reaction efficiency is improved by optimizing the synthesis route and process conditions, the process is simple, the energy consumption is low, the raw materials are easy to obtain, the cost is low, and the industrial synthesis route has extremely high industrial competitiveness.

This invention provides a method for preparing 1,1,2,3-tetrachloropropene using a microchannel reaction. The method includes the following steps: (1) dichloropropene feedstock undergoes a first chlorination reaction in a microchannel reactor to obtain a first material containing tetrachloropropane; (2) the first material undergoes a first purification to obtain tetrachloropropane, and the tetrachloropropane undergoes a first dehydrochlorination reaction to obtain a second material containing trichloropropene; (3) the second material undergoes a second chlorination reaction in a microchannel reactor to obtain a third material containing pentachloropropane; (4) the third material undergoes a second dehydrochlorination reaction to obtain a fourth material containing tetrachloropropene; (5) the fourth material undergoes a photocatalytic isomerization reaction in a microchannel reactor to obtain 1,1,2,3-tetrachloropropene. The method provided by this invention can shorten the reaction time, significantly improve the reaction yield, and has good economic benefits and industrial application potential.

The present application relates to a method for producing 1,1,2,3-tetrachloropropane from a mixture of 1,3-dichloropropene and 3-chloropropene. The method comprises the following steps: a) subjecting a raw material comprising a mixture of 1,3-dichloropropene and 3-chloropropene, and Cl2 to a first chlorine addition reaction at a temperature T1, so as to obtain a first product; b) subjecting the first product to a first chlorine substitution reaction under UV at a temperature T2, so as to obtain a second product; and c) subjecting the second product to a second chlorine addition reaction at a temperature T3, so as to obtain a third product, which comprises 1,1,2,3-tetrachloropropane. A second aspect of the present application relates to a method for producing 1,1,2,3-tetrachloropropene from a mixture of 1,3-dichloropropene and 3-chloropropene. The present application further relates to a 1,1,2,3-tetrachloropropane product and a 1,1,2,3-tetrachloropropene product produced by using the methods described in the first and second aspects.

The invention relates to a preparation method of 3, 3, 3-trifluoropropene and a composite coordination catalyst of 3, 3, 3-trifluoropropene, and belongs to the technical field of fluorine-containing olefin synthesis. 1, 1, 1, 3-tetrachloropropane and hydrogen fluoride are used as raw materials, zirconium and hafnium ions are used as a composite active center, fluoro-modified 4, 4 '-dipyridyl is used as a bimetallic catalyst of a ligand, and raw material pretreatment, catalyst activation, four-factor coupling catalytic reaction and double-tower separation circulation are performed to prepare the fluorine-containing fluorine-containing compound. The process optimizes catalyst activation, gradient heating and reaction working conditions, provides universal, high-purity, high-productivity, energy-saving and series-connection sectioning working conditions and the like, and the reactor is flexible and selectable; and refining the product through HCl and HF separation towers, and recycling HF. The method is simple in process, efficient, environment-friendly, high in conversion rate and selectivity, stable in catalyst and suitable for industrial production.