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

The invention discloses a method for continuous extraction and distillation and separation of acetonitrile- toluene azeotrope. The method is described as the following: using propyl benzene, butylbenzene, isobutylbenzene, sec- butylbenzene, tertiarybutyl phenol, mesitylene, p- diethyl benzene or tertiary-butyl toluene as the extractant, operating in a extracting- fractionating tower at a normal pressure or reduced pressure with a mass ratio of extractant in extracting- fractionating tower to overhead being 2: 1- 10: 1 and a feeding temperature of extractant of 25- 80 Deg. C, the acetonitrile- toluene azeotrope entering from the middle of extracting- fractionating tower, picking the qualified content of acetonitrile from the head of tower with a reflux ratio of 1: 1- 5: 1, toluene and solvent from the bottom of the tower flowing into the middle of the extractant recovery tower, the toluene being picked from the head of extractant recovery tower with a reflux ratio of 2: 1- 10: 1, and the high-purity extractant which can be circularly used being picked from the bottom of the extractant recovery tower. The merit of the invention is that using extractant to destroy acetonitrile- toluene azeotrope,the high purity acetonitrile and toluene are prepared.

The invention discloses a method for producing p-tert-Butyltoluene by using mordenite for catalyzing toluene and tertiary butanol, which uses a mordenite catalyst, n(SiO2) / n(Al2O3)=30, the catalyst is conducted activating treatment for 3 hours at 550 DEG C, or the catalyst is conducted treatment for 4 hours at 100 DEG C in 0.2mol / L NaOH solution, then the p-tert-Butyltoluene is obtained after roasting at 550 DEG C. At the reaction temperature of 150-190 DEG C, liquid space velocity is 1-8ml / gcatXh, and mole ratio of the toluene / the tertiary butanol is 1:1-1:6. In a fixed bed reactor, toluene percent conversion is 10-33%, and selectivity of the p-tert-Butyltoluene achieves 35-75%. The method can continuously produce the p-tert-Butyltoluene under soft reaction conditions, and overcomes the shortcoming that in the traditional production method, liquid acid catalysts corrode equipment, environmental contamination is caused, interval liquid phase reaction is big in production strength, and production rate is low.

The invention discloses a method of synthesizing p-tert-butyl toluene with a caprolactam ionic liquid as a catalyst. The method comprises the following steps: (1) adding methylbenzene into a reaction kettle, and adding the caprolactam ionic liquid, and adding isobutylene or tert-butyl alcohol; (2) regulating and controlling reaction temperature and time; (3) allowing the mixture to stand for layering, separating a supernatant, and rectifying the supernatant to prepare a product p-tert-butyl toluene; and (4) washing a subnatant in methylbenzene and performing vacuum-drying to remove the methylbenzene to obtain recyclable caprolactam ionic liquid. In the method, the caprolactam ionic liquid is low in cost, is mild in synthetic conditions and can be used for large-scale industrial production. Separation and after-treatment on the product are very simple so that an alkali-washing process in the prior art can be omitted, thereby simplifying the process and increasing production efficiency without generation of waste water. The caprolactam ionic liquid can be recycled for the next reaction just through simple treatment, thereby effectively reducing production cost.

The invention discloses a preparation and after-treatment method of p-tert-butylbenzoic acid. The preparation method of the p-tert-butylbenzoic acid includes the steps: firstly, performing tert-butylation on toluene to obtain p-tert-butyl toluene; secondly, oxidizing the p-tert-butyl toluene; finally, performing crystallization to obtain the p-tert-butylbenzoic acid. Crystallization mother liquidis retreated after crystallization, p-tert-butylbenzoic acid remained in the mother liquid is further acquired, the yield of the p-tert-butylbenzoic acid is improved, waste sodium sulfate in the mother liquid is after-treated to obtain industrial-grade sodium sulfate, waste emission in the preparation process is reduced, the waste sodium sulfate is converted into recyclable industrial-grade sodiumsulfate, a certain economic benefit is achieved, and environment-friendly significance is remarkable.

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 intermittent extraction and distillation and separation of acetonitrile- toluene azeotrope, belonging to the separation technique of acetonitrile- toluene. The method is described as the following: using propyl benzene, butylbenzene, isobutylbenzene, sec- butylbenzene, tertiarybutyl phenol, p- diethyl benzene or tertiary-butyl toluene as the extractant, operating in a extracting- fractionating tower at a normal pressure or reduced pressure with a mass ratio of extractant to overhead of 2: 1- 10: 1 and a feeding temperature of extractant of 25- 80 Deg. C, picking separately acetonitrile, the transition section I of a low rate of acetonitrile, and transition section II of toluene and toluene- extractant from the extracting- fractionating tower by controlling the temperature and reflux ratio of the head of extracting- fractionating tower; when the constitute of extractant in heating kettle approaches to the requirement, pumping the extractant into elevated container and feeding material to prepare for the intermittent extraction and distillation and separation of next batch. The merit of the invention is that using extractant to destroy acetonitrile- toluene azeotrope,the high purity acetonitrile and toluene are prepared, and the operation is flexible with a single towel.

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 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 discloses a preparation and post-treatment method of p-tert-butylbenzoic acid. During the preparation, p-tert-butyltoluene is obtained by tert-butylation of toluene, and then p-tert-butyltoluene is oxidized, and then analyzed crystallization treatment to obtain p-tert-butylbenzoic acid; wherein, after the crystallization treatment, the crystallization mother liquor is reprocessed to further obtain the residual p-tert-butylbenzoic acid in the mother liquor, which improves its productivity, and, in the mother liquor The waste product sodium sulfate is post-treated to obtain industrial grade sodium sulfate. In this way, the discharge of waste materials in the preparation process is reduced, and the waste product sodium sulfate is converted into reusable industrial grade sodium sulfate. In this way, it not only brings certain economic benefits , and the significance of environmental protection is more prominent.

The invention discloses a method for producing p-tert-Butyltoluene by using mordenite for catalyzing toluene and tertiary butanol, which uses a mordenite catalyst, n(SiO2) / n(Al2O3)=30, the catalyst is conducted activating treatment for 3 hours at 550 DEG C, or the catalyst is conducted treatment for 4 hours at 100 DEG C in 0.2mol / L NaOH solution, then the p-tert-Butyltoluene is obtained after roasting at 550 DEG C. At the reaction temperature of 150-190 DEG C, liquid space velocity is 1-8ml / gcatXh, and mole ratio of the toluene / the tertiary butanol is 1:1-1:6. In a fixed bed reactor, toluene percent conversion is 10-33%, and selectivity of the p-tert-Butyltoluene achieves 35-75%. The method can continuously produce the p-tert-Butyltoluene under soft reaction conditions, and overcomes the shortcoming that in the traditional production method, liquid acid catalysts corrode equipment, environmental contamination is caused, interval liquid phase reaction is big in production strength, and production rate is low.

The invention discloses a kind of 1-phenyl-1-(p-tert-butyltolyl)ethane and a synthesis method thereof, the steps are as follows: 1) using styrene and p-tert-butyltoluene as raw materials, in the presence of a solid acid catalyst Under the action, through the alkylation reaction, the reaction formula is as follows: 2) After the reaction is completed, the solid acid catalyst needs to be separated, and the solid material composed of activated clay and magnesium oxide with a mass ratio of 10:1 is used for further adsorption and neutralization And decolorize and filter, recover excess p-tert-butyltoluene through water pump vacuum distillation, and then vacuum pump vacuum distillation to obtain. The catalyst selected in the invention can be recycled, does not pollute the environment, and simultaneously avoids the use of catalysts such as sulfuric acid, aluminum trichloride and the like which are volatile, poisonous and difficult to handle. The preparation process has the characteristics of mild and controllable, few by-products and high yield.

The invention provides a method for preparing p-tert-butyltoluene, wherein the novel reactor includes a plurality of Venturi mixers connected alternately in sequence and a tubular reactor with internals, and the tubular reaction with internals The outer wall of the device is provided with a jacket. It also relates to a method for combining p-tert-butyltoluene with a novel reactor, using isobutylene and toluene as raw materials, under the catalysis of concentrated sulfuric acid, toluene is fed in a single strand, concentrated sulfuric acid is fed in a single strand, and isobutylene is fed in multiple strands. Synthesis of p-tert-butyltoluene by continuous liquid-liquid two-phase alkylation reaction through a novel reactor group. The invention creates the novel reactor group for synthesizing p-tert-butyltoluene and its use method. The novel reactor group is applied to the continuous liquid-liquid two-phase alkylation reaction process of toluene and isobutylene, which not only has the advantages of uniform material mixing , the reaction temperature is controllable, the target product yield is high, the catalyst consumption is small, etc., and it can realize efficient, low-cost and continuous production of p-tert-butyltoluene.

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 discloses a method for continuous extraction and distillation and separation of acetonitrile- toluene azeotrope. The method is described as the following: using propyl benzene, butylbenzene, isobutylbenzene, sec- butylbenzene, tertiarybutyl phenol, mesitylene, p- diethyl benzene or tertiary-butyl toluene as the extractant, operating in a extracting- fractionating tower at a normal pressure or reduced pressure with a mass ratio of extractant in extracting- fractionating tower to overhead being 2: 1- 10: 1 and a feeding temperature of extractant of 25- 80 Deg. C, the acetonitrile- toluene azeotrope entering from the middle of extracting- fractionating tower, picking the qualified content of acetonitrile from the head of tower with a reflux ratio of 1: 1- 5: 1, toluene and solvent from the bottom of the tower flowing into the middle of the extractant recovery tower, the toluene being picked from the head of extractant recovery tower with a reflux ratio of 2: 1- 10: 1, and the high-purity extractant which can be circularly used being picked from the bottom of the extractant recovery tower. The merit of the invention is that using extractant to destroy acetonitrile- toluene azeotrope,the high purity acetonitrile and toluene are prepared.

The invention discloses a method for synthesizing p-tert-butyltoluene by using caprolactam ionic liquid as a catalyst, comprising the following preparation steps: (1) firstly adding toluene into a reaction kettle, then adding caprolactam ionic liquid, and finally adding isobutylene or t-butyltoluene Butanol; (2) regulate and control temperature of reaction and time; (3) leave standstill stratification, separate supernatant, rectification obtains product p-tert-butyl toluene; (4) lower floor liquid in step (3) is used toluene Washing, drying in vacuo to remove toluene, the recyclable caprolactam ionic liquid can be obtained. The caprolactam-based ionic liquid used in the present invention is cheap and has mild synthesis conditions, and is suitable for large-scale industrial production; the separation and post-treatment process of the product is very simple, and the alkali washing process in the traditional process can be omitted, thereby simplifying the process and improving production. High efficiency, and no waste water is generated; the caprolactam-based ionic liquid can be used for the next reaction after simple treatment, which can effectively reduce the production cost.