35 results about "P-tert-Butyltoluene" patented technology

The invention discloses a preparation technology of p-tert-butyl benzoic acid, comprising the following steps: firstly, adding toluene, isobutene and concentrated sulfuric acid into a reaction kettle, carrying out alkylation reaction to obtain coarse p-tert-butyl toluene, and rectifying to obtain fine p-tert-butyl toluene; secondly, adding a composite catalyst containing the p-tert-butyl toluene,cobalt acetate and bromide into the reaction kettle, heating and introducing oxygen to obtain coarse p-tert-butyl benzoic acid, decoloring by activated carbon and diatomite , crystallizing and dryingto obtain fine p-tert-butyl benzoic acid. The prepared p-tert-butyl benzoic acid is an organic synthesis intermediate, can be used for the fields of additives, antioxidants, alkyd resin modifying agents, soldering fluid, dye, and the like of polypropylene nucleating agents, polyvinyl chloride heat stabilizers, metal machining and lubricating oil and has excellent performance. The p-tert-butyl benzoic acid has low energy consumption, high yield, simple separation, and the like and can satisfy ever-increasing market demands of the p-tert-butyl benzoic acid.

The invention discloses a method for producing p-tert-butyltoluene, which comprises the following steps of: putting toluene and tert-butyl alcohol in a molar ratio of 1:(2-6) and a catalyst in an amount which is 5 to 30 percent based on the total weight of the toluene serving as a reactant into a reaction kettle under the action of the mesoporous/microporous composite molecular sieve catalyst consisting of a beta zeolite (Hbeta) microporous molecular sieve and an MCM-41 mesoporous molecular sieve, and reacting at the temperature of between 160 and 240 DEG C for 2 to 8 hours to obtain the p-tert-butyltoluene. The preparation process is simple, the catalyst is easy to separate and is reusable, production cost is low, the method is environment-friendly, and safe production is realized.

The invention discloses a method for synthesizing p-tert-butylbenzaldehyde. The method comprises the following steps: a normal atmosphere heterogeneous catalytic oxidation method is adopted; p-tert-butyltoluene as a raw material, sufficient oxygen as an oxygen source and n-hydroxyphthalimide as a free radical evocating agent in an acetonitrile solution react for 4 to 7 hours at a temperature between 50 and 70 DEG C under the condition of a catalyst to directly synthesize the p-tert-butylbenzaldehyde; and the catalyst is a cobalt-loaded mesoporous molecular sieve or a cobalt- and manganese-loaded mesoporous molecular sieve. The method use the cobalt-loaded mesoporous molecular sieve or the cobalt- and manganese-loaded mesoporous molecular sieve as the solid-phase catalyst; compared with the prior liquid-phase catalyst, the target product is easier to separate after reaction; a reactant can rapidly contact catalytic activity center; product molecules rapidly escape from a pore canal, thereby avoiding deep oxidation and improving the selectivity of aldehyde; in addition, micro n-hydroxyphthalimide as the free radical evocating agent is added to the system to trigger the chain transmission reaction of free radicals.

The invention provides a process for synthesizing p-methoxy benzaldehyde or p-tertbutyl benzaldehyde. The process comprises the following steps of: adding an acidifying agent glacial acetic acid and catalysts cobalt acetate and sodium bromide into p-methoxy methylbenzene or p-tertbutyl methylbenzene, introducing oxygen to perform oxidation reaction under a heating condition, and after the reaction, washing feed liquid with water for twice to remove the catalysts and the acetic acid; adding an oil phase after washing into a high-boiling-point solvent, and then performing rectification under vacuum step by step; unmixing and steaming out excessive p-methoxy methylbenzene or p-tertbutyl methylbenzene, then increasing the vacuum degree and the temperature, and collecting a gas-phase condensate to obtain the p-methoxy benzaldehyde or p-tertbutyl benzaldehyde; and continuously raising the rectification temperature, and receiving the gas-phase condensate with water, and performing recrystallization for twice to obtain p-methoxy benzoic acid or p-tertbutyl benzoic acid. According to the process, the discharge of waste water is reduced, the generation of the waste water containing sodium sulfate is avoided, and meanwhile, methylbenzene is not used for extracting the p-methoxy benzoic acid or p-tertbutyl benzoic acid, so that the pollution of the methylbenzene to the environment is reduced.

The invention relates to a process for synthesizing p-tert-butylbenzoic acid. The process comprises the following steps of: adding p-tert-butyltoluene and cobalt acetate into a reaction kettle, introducing oxygen-containing gas, triggering at the temperature of between 150 and 155 DEG C, performing oxidation reaction for 0.5 to 1 hour, and continuously reacting at the temperature of between 135 and 145 DEG C for more than 5 hours to obtain a p-tert-butylbenzoic acid crude product; cooling the p-tert-butylbenzoic acid crude product to crystallize, performing centrifuge dripping, and striking and washing by using p-tert-butyltoluene to obtain a centrifugation crude product; and adding the centrifugation crude product into a dissolution kettle, adding methylbenzene, raising temperature and dissolving, filtering when a mixture is hot to remove impurities, adding water to wash, transferring materials to a recrystallization kettle, cooling to crystallize, centrifuging, striking and washing by using methylbenzene, and drying to obtain a p-tert-butylbenzoic acid finished product. The prepared p-tert-butylbenzoic acid is white crystals and does not contain mechanical impurities; and the melting point is 164.0 to 167.0 DEG C, the acid value is 312 to 316mgKOH/g, high performance liquid chromatography (HPLC) purity is more than or equal to 99.2 percent, moisture is less than or equal to 0.08 percent, and methylbenzene is less than or equal to 0.05 percent.

The invention relates to a continuous production process of p-tert-butyl toluene, and in particular relates to a method for synthetizing the p-tert-butyl toluene through catalyzing toluene and tert butyl alcohol by using a metallic oxide-supported molecular sieve catalyst. The invention aims to overcome the shortcomings that catalysts corrode equipment, pollute the environment and are difficult to separate and incapable of being recycled and the like in traditional methods for synthetizing the p-tert-butyl toluene through liquid acid catalysis. The continuous production process of the p-tert-butyl toluene comprises the following steps of (1) preparation of the metallic oxide-supported molecular sieve catalyst and (2) synthetic reaction of the p-tert-butyl toluene. The process disclosed by the invention has the advantages of simpleness, environmental friendliness, low labour intensity and low production cost; by adopting the homemade metallic oxide-supported molecular sieve catalyst, the problems that the liquid acid catalysts corrode equipment and pollute the environment in the traditional production methods are solved; and in the meantime, the homemade catalyst is high in activity, good in heat stability, high in mechanical strength and capable of meeting the requirements of long-period operation in the continuous production process of fixed beds.

The invention provides a synthetic method of p-tert-butylbenzaldehyde. A liquid-phase oxidation method is used, p-tert-butyltoluene as a raw material, oxygen as an oxidizing agent, N-hydroxyl phthalimide as an initiator and acetonitrile as a solvent are used under the action of a catalyst for reacting for 7 hours at the temperature of 70 DEG c under the magnetic stirring rotating speed of 200r/minso as to obtain the p-tert-butylbenzaldehyde. The selected catalyst is a Ni-loaded microporous molecular sieve, and preparation raw materials comprise a nickel salt, a molecular sieve and deionized water; the microporous molecular sieve is used as a carrier for loading of an active component by an impregnation method to prepare the catalyst containing the active component nickel, the catalyst hasrelatively high selectivity and activity, the conversion rate of the raw material in the reaction for preparing the p-tert-butylbenzaldehyde by the liquid-phase oxidation reaches 30.6%, the selectivity of the target product reaches 77.2%. Compared with other catalysts in the prior art, the catalyst has the advantages that the selectivity is obviously improved.

The invention discloses a preparation method of high-grade 4-tert-butylbenzaldehyde and a preparation apparatus of high-grade 4-tert-butylbenzaldehyde. The preparation method of high-grade 4-tert-butylbenzaldehyde comprises the following steps: A) 4-tert-butylbenzaldehyde, water and a catalyst without halogen are mixed in a micrometer bubble reactor for carrying out an oxidation reaction, in order to obtain reaction feed liquid; B) oil-water separation is carried out for reaction feed liquid in order to obtain water phase and oil phase, water phase contains the catalyst, and the oil phase contains 4-tert-butylbenzaldehyde and impurities; and C) 4-tert-butylbenzaldehyde and the impurities are separated in order to obtain high-grade 4-tert-butylbenzaldehyde. 4-tert-butylbenzaldehyde prepared by the preparation method of high-grade 4-tert-butylbenzaldehyde according to an embodiment does not contain halogen, and can be applied to the fields of foodstuff, medicine, perfume and the like.

The invention discloses preparation of methyl p-tert-butylbenzoate. The preparation of the methyl p-tert-butylbenzoate comprises the steps of oxidizing tert-butyltoluene in air by using a composite catalyst to obtain p-tert-butylbenzoic acid; and then replacing traditional concentrated sulfuric acid by using p-toluenesulfonic acid, and carrying out esterification reaction to obtain the methyl p-tert-butylbenzoate. Meanwhile, a special treatment process is used for preparation of the methyl p-tert-butylbenzoate, the yield and the purity of products are increased by repeated water carrying of methanol, meanwhile, after being treated, evaporated methanol, an extracted water phase and a catalyst are reused, the cost for raw materials is greatly reduced, and moreover, the preparation of the methyl p-tert-butylbenzoate also has important environmental protection significance.

The invention discloses a separation process after synthesis of p-tertbutyl benzaldehyde (co-produced p-tertbutyl benzaldehyde). The separation process comprises the steps: rectifying an oxidization feed liquid to remove acetic acid, and washing with water to remove a catalyst; heating a washed organic phase to 95-100 DEG C, introducing saturated vapor or nitrogen, stripping, carrying out fractionation under reduced pressure, for separating vapor or nitrogen, p-tertbutyl benzaldehyde and p-tert-butyltoluene, cooling stripped residual liquid and then extracting by using methylbenzene, distilling the p-tertbutyl benzaldehyde after the methylbenzene is recovered, and then recrystallizing the methylbenzene. According to the separation process, the process step is reduced, and sodium sulfate-containing wastewater is prevented from producing.

The invention relates to a preparation method for 2,6-dihydroxytoluene. The preparation method adopts p-tert-butyltoluene as a raw material which is subjected to nitration, reduction and hydrolytic tert-butyl elimination reactions to obtain 2,6-dihydroxytoluene. The preparation method has the characteristics of high selectivity and product purity, low cost, environmental friendliness and the like, and is a route with an industrialization prospect.

The invention discloses a method for preparing p-tert-butylbenzaldehyde by carrying out liquid phase oxidation on p-tert-butyltoluene. The method comprises the following steps: (1) preheating p-tert-butyltoluene and a reaction solvent mixture, and then mixing in an impinging stream reactor to form micron-sized emulsion; (2) enabling the micron-sized emulsion to enter a bubbling tower reactor through an ejector and then react with oxygen to obtain a reaction feed liquid; (3) carrying out oil-water separation on the reaction feed liquid to obtain an oil phase and an aqueous phase; (4) separatingthe oil phase to obtain the product of p-tert-butylbenzaldehyde, wherein the reaction solvent mixture contains p-tert-butyl benzoate, p-tert-butyl benzyl alcohol, water, a catalyst, additives and a pro-oxidant. The method has the advantages of being high in selectivity to p-tert-butylbenzaldehyde and mild in reaction conditions, enabling the catalyst, the additives and the solvent to the recycled, and being green and pollution-free.

The invention provides a refining method of p-tert-butylbenzoic acid. The refining method comprises the following steps: 1, obtaining p-tert-butyltoluene; 2, adding the p-tert-butyltoluene obtained in the step 1 and a supported composite catalyst into a reaction kettle, introducing oxygen, and carrying out an oxidation reaction at a certain temperature to obtain a p-tert-butylbenzoic acid crude product; 3, cooling and crystallizing the p-tert-butylbenzoic acid crude product obtained in the step 2, performing centrifugal spin-drying, and washing with p-tert-butyltoluene to obtain a centrifuged crude product; and 4, adding the centrifuged crude product into a dissolving kettle, centrifuging, and drying to obtain a p-tert-butylbenzoic acid finished product. The method has the beneficial effects that the high-quality product can be obtained by simply washing the crude product with water, the post-treatment process is simplified, the quality of the product can be improved, and the production cost can be reduced.

The invention discloses 1-phenyl-1-(p-tert-butyl methylphenyl)ethane and a synthesis method thereof. The synthesis method comprises the following steps: 1) with styrene and p-tert-butyl toluene as raw materials and under the effect of a solid acid catalyst, performing an alkylation reaction, wherein the reaction formula is shown in the specification; and 2) after the reaction, separating the solid acid catalyst; performing further adsorption, neutralization and decoloration filtration using a solid material consisting of activated clay and magnesium oxide in a mass ratio of 10:1; performing reduced-pressure distillation through a water pump to recycle excess p-tert-butyl toluene; and performing reduced-pressure distillation through a vacuum pump to obtain 1-phenyl-1-(p-tert-butyl methylphenyl)ethane. In the invention, the adopted catalyst can be recycled to avoid environmental pollution; and meanwhile, the use of volatile, toxic and hard-to-treat catalysts such as sulfuric acid and aluminum trichloride is avoided. The preparation technology has the characteristics of mildness and controllability, few byproducts and high yield.