59 results about "O-chlorotoluene" patented technology

The invention relates to a method for preparing 6-chloro-3-aminotoluene-4-sulfoacid (hereinafter referred to as CLT acid) in a direct nitrification way by taking o-chlorotoluene as a raw material. The method comprises the following steps of: obtaining o-chlorotoluene nitrate by taking acidic Beta zeolite as a catalyst and acetyl nitrate as a nitrifying agent; reducing the o-chlorotoluene nitrate by utilizing iron powder; recrystallizing the reduced product and separating out 6-chloro-3-aminotoluene crystal and 6-chloro-4-aminotoluene containing little 6-chloro-3-aminotoluene by adopting an acid extraction method; adding dichlorobenzene and sulfuric acid in the 6-chloro-3-aminotoluene crystal, and carrying out sulfonation at 170-190 DEG C to obtain the CHLOROT acid; and carrying out sulfonation on the 6-chloro-4-aminotoluene containing little 6-chloro-3-aminotoluene to obtain 2B acid containing little CLT acid. The invention has the characteristics of low pollution, high yield, simple process, low device requirements, and the like.

The invention provides a production process for preparing chlorobenzonitrile through ammoxidation. The production process comprises the following steps of: portioning air, ammonia, water vapor and o-chlorotoluene together; gasifying the o-chlorotoluene and then mixing the gasified o-chlorotoluene with air, ammonia and water vapor, and conveying the mixture to a fluidized bed reactor for reaction under the action of a catalyst; and after the reaction, cooling and crystallizing the generated product through a cold trap, thereby obtaining crude chlorobenzonitrile, wherein the catalyst is VaPbCecSbdOx multi-component catalyst, and wherein a=1, b=0.7-2, c=0.3-1, d=0.5-1, and the value of x is determined according to valence state balance when V, P, Ce and Sb are +5 valent, +5 valent, +4 valent, +5 valent and -2 valent, respectively. The production process provided by the invention employs the VaPbCecSbdOx as the active catalyst; and the catalyst is simple to fabricate, mild in reaction temperature, long in catalyst service life, high in activity, high in selectivity and the like; as a result, side reaction in the production process is suppressed, the production process of chlorobenzonitrile is improved and the yield of product is obviously improved.

The invention discloses production equipment and a preparation technology for an o-chlorotoluene Grignard reagent. The equipment comprises a first-stage reaction kettle, a second-stage reaction kettle, a tetrahydrofuran storage tank, an o-chlorotoluene storage tank, a magnesium chip storage tank and a toluene storage tank; the center parts of the first-stage reaction kettle and the second-stage reaction kettle are both provided with a separation net for obstructing magnesium chips; and pipelines are employed for connection of the reaction kettles and the storage tanks. Combination of the continuous production equipment and the corresponding preparation technology for the o-chlorotoluene Grignard reagent solves the problems that initiation is difficult and magnesium chips are difficult to separate in a conventional industrial preparation process of the o-chlorotoluene Grignard reagent, and helps to improve the yield of the o-chlorotoluene Grignard reagent.

The invention provides a method for preparing monochlorotoluene with a toluene chloridizing method. The method comprises the following specific steps of: adding iron powder or iron chloride serving as a catalyst into a toluene liquid, adding an aid, introducing chorine gas under a light-shading situation, controlling the temperature of an entire chloridizing process at 0-30 DEG C, and controlling the chlorine-introducing amount to keep the transformation rate of toluene between 96 percent and 99 percent; and cooling, and filtering an ion liquid out to obtain a toluene mono-chlorinated mixed solution. After the aid and iron or iron chloride serving as a catalyst used in the method are mixed and applied to toluene chloridizing, the selectivity of a product on toluene chloride is effectively increased, the highest selectivity on chlorotoluene / o-chlorotoluene is up to 2.1, the selectivity on m-chlorotoluene is less than 0.15 percent, and the selectivity on total dichlorotoluene is less than 1.0 percent.

The invention provides a method for producing chloroethylene by homogeneous mercury-free catalysis. According to the method, acetylene and hydrogen chloride are taken as raw materials and chloroethylene is generated under the effect of a homogeneous catalyst. One or more of PdCl2, AuCl3, FeCl3, ZnCl2 and CuCl2 are taken as catalysts, one or more of NH4Cl, NaCl, KCl, BaCl2, MgCl2 and CaCl2 are taken as cocatalysts, o-nitrochlorobenzene, o-chlorotoluene or o-dichlorobenzene is taken as a solvent, and a homogeneous catalysis system is formed. Under the reaction conditions of normal pressure and temperature of 130 DEG C, the acetylene conversion rate and the chloroethylene selectivity can reach about 95% and more than 95%, and the catalyst life is more than 3,000 hours. The method adopts the nontoxic and mercury-free homogeneous catalyst for producing the chloroethylene, so that a supported catalyst for producing chloroethylene by hydrochlorination of acetylene in existing production is avoided, the problems of easiness for generating carbon deposit sintering and the like in a conventional process carrier are avoided, and homogeneous production of the chloroethylene is realized.

The invention provides a method for preparing dichlorotoluene, and relates to the field of preparation of organic intermediates. The method provided by the invention uses more than one of 2,3-dichlorotoluene, 2,4-dichlorotoluene and 2,5-dichlorotoluene as raw materials, and uses supported palladium as a catalyst to prepare o-chlorotoluene by continuous reaction in a fixed bed. The method providedby the invention uses industrial by-products 2,3-dichlorotoluene, 2,4-dichlorotoluene and 2,5-dichlorotoluene as the raw materials; the supported palladium catalyst has good selectivity and long service time and realizes high yield of o-chlorotoluene.

The invention discloses a method for preparing o-chlorotoluene through methylbenzene loop chlorination. The method particularly includes the steps that iron powder or ferric trichloride is added into methylbenzene to serve as catalysts, [BMTM]Cl-nZnCl2 ionic liquid serves as an assistant (n is equal to 1, 2 or 2.5), and stirring is carried out; dry chlorine is led in, a suitable temperature is controlled under the dark condition to conduct chlorination, the o-chlorotoluene is obtained in a high-selectivity manner, and alkali liquor absorption is carried out after tail gas condensation to remove excessive unreacted chlorine; and after reacting is ended, a reacting product and the ionic liquid assistant are separated, the separated ionic liquid can be repeatedly used. Compared with the prior art, the method can well improve the methylbenzene conversion rate, and the o-chlorotoluene selectivity reaches 88%; in addition, the separated and recycled [BMTM]Cl-nZnCl2 ionic liquid is repeatedly used, the production cost is reduced, and the method is suitable for o-chlorotoluene industrial production.

The invention discloses an o-chlorotoluene catalytic nitration method by using microwaves for assisting zeolite. The method comprises the following steps of adding solvents into a container; sequentially adding o-chlorotoluene, acetic anhydride, nitrosonitric acid, modified zeolite molecular sieve catalysts and silicon dioxide loaded perfluorinated sulfonic acid resin; performing microwave temperature rise for 4 to 12min; performing heat insulation for 8 to 10min; terminating the reaction. The microwave technology is applied to the o-chlorotoluene nitration process; the reaction progress is greatly accelerated; meanwhile, silicon dioxide is used for loading perfluorinated sulfonic acid resin; the perfluorinated sulfonic acid resin is dispersed into SiO2 networks or pore passages; the effective surface area is greatly increased, so that the acid positions of the perfluorinated sulfonic acid resin are sufficiently exposed, so that the potential of the resin catalyst is achieved; the conversion rate and the yield are improved; in addition, the modified zeolite molecular sieve catalyst Bibeta provides acid centers and pore passage structures; the shape selection catalyst effect is provided; the reaction selectivity is improved; the yield is as high as 80.9 percent; the selectivity of the 2-chloro-4-nitrotoluene is as high as 84.1 percent. The method has the advantages that the operation is easy; the energy is saved; the efficiency is high; the control is easy; the method belongs to a green and environmental-friendly o-chlorotoluene nitration method.

The invention discloses a method for preparing o-chlorotoluene. The method comprises the following steps: adding a raw material toluene and a FeCl3-loaded macroporous metal silica gel catalyst into a reaction kettle; introducing chlorine into the reaction kettle for a liquid-phase ring chlorination reaction between the toluene and chlorine; after the reaction is complete, aerating to remove residual chlorine and hydrogen chloride gas in the reaction liquid; rectifying the reaction liquid to separate out unreacted toluene and a little dichlorotoluene to obtain mixed chlorotoluene; and then, separating high-purity p-chlorotoluene from the mixed chlorotoluene by using a melt crystallization process. According to the method disclosed by the invention, the FeCl3-loaded macroporous metal silica gel catalyst is adopted for catalyzing the selective chlorination of toluene, the reaction is fast, the catalytic activity is high, the o-chlorotoluene selectivity is good, the requirements for the technological conditions are low, the catalyst consumption is low, the catalyst has high activity and can be recycled, and the method has a good industrial prospect.

The invention relates to the field of organic silicon chemistry and provides o-benzyldiethoxymethylsilane and a preparation method thereof. The preparation method solves the problem that in the existing sodium condensation method-based synthesis of o-substituted benzyldiethoxymethylsilane, a large amount of a solvent is used so that environmental pollution is caused and solvent recycle is difficult. The o-benzyldiethoxymethylsilane is synthesized from methyltriethoxysilane and o-chlorotoluene as raw materials by a sodium condensation method. The preparation method does not adopt a toluene solvent, allows mild reaction conditions, has simple processes and is suitable for large-scale industrial production.

The invention discloses a synthesis method of o-chlorobenzoic acid. The synthesis method comprises the following steps: adding a mixed o-chlorobenzoic acid solution and o-chlorotoluene and inflating oxygen obtained by vaporizing liquid oxygen into a reactor, detecting the pressure in the reactor by using a gas pressure detecting instrument, reacting at a temperature of 125-180 DEG C after a requirement is met, condensing and stratifying o-chlorotoluene vapor by using a condenser and a water segregator, removing water, reflowing the o-chlorotoluene into the reactor, and when the content of theo-chlorobenzoic acid reaches 98.5%, discharging and passing through subsequent treatment equipment. By the synthesis method, a technological process is short, the yield is high, the cost is low, the environment pollution is low, pure oxygen replaces air, the reaction speed is high, and basically no waste gas is discharged; a solvent is not required during the reaction, a large amount of wastewaterin a diazotization method and a chlorination hydrolysis method is avoided, and an oxidation technology is greatly improved, the reaction conversion rate is high, the selectivity is good, and the crude product content is high.