A continuous synthesis device and method for 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetralin

A technology of tetralin and hexamethyl, applied in the direction of organic chemistry, addition of unsaturated hydrocarbons and saturated hydrocarbons to produce hydrocarbons, etc., can solve the problems of poor heat and mass transfer effect, low production capacity, etc., to improve production capacity and degree of automation High, improve the effect of utilization efficiency

Active Publication Date: 2019-04-19
TIANMEN DEYUAN CHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] Although the above method is used for batch reaction, the operation is simple and the equipment investment is small, but the disadvantages of poor heat and mass transfer effect and low production capacity are also obvious.

Method used

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  • A continuous synthesis device and method for 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetralin
  • A continuous synthesis device and method for 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetralin

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preparation example Construction

[0027] A method for the continuous synthesis of 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetralin, comprising the following steps:

[0028] (Ⅰ) Raw material liquid mixing stage: Put the reaction raw materials paracymene, 2,3-dimethyl-1-butene and chloro-tert-butane and cyclohexane into the raw material storage tank respectively, and open the valve to enter the mixing The kettle is evenly mixed;

[0029] (II) Mixed liquid reaction stage: pump the mixture into the tubular reactor, contact with the aluminum trichloride catalyst filled in the reactor, and the Friedel-Crafts alkylation reaction occurs under the action of the catalyst, and the reaction liquid flows out of the tubular reactor , Flow into the transfer kettle, the transfer kettle further stirs the reaction liquid evenly by stirring, and collects the reaction liquid into the washing kettle by overflow method;

[0030] (Ⅲ) Post-treatment stage: add water to the water-washing kettle for quenching, then wash with alkali, and carry out rec...

Embodiment 1

[0036] Add 804kg of p-cymene, 252kg of 2,3-dimethyl-1-butene, 416kg of chloro-tert-butane and 1260kg of cyclohexane into the mixing kettle and stir for 0.5-1h. During the stirring process, 80 kg of aluminum trichloride was charged into the tubular reactor. After the filling is completed, adjust the temperature of the tubular reactor to 10-15°C, and start feeding through the centrifugal pump, and the feeding rate is controlled at 0.7-2.5 mL / s. The temperature in the transfer kettle is controlled at 10-30°C, and the stirring is started when the reaction liquid flows into the transfer kettle. After 4-6 hours of reaction, start sampling through the monitoring port every 30 minutes for monitoring, and replace the catalyst after the 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetralin content decreases. The reaction liquid flows out through the overflow port. When the amount of reaction liquid in the washing kettle reaches 1800L, start adding 700L water to quench the reaction, and then wash with...

Embodiment 2

[0038] Add 402kg of p-cymene, 168kg of 2,3-dimethyl-1-butene, 222kg of chloro-tert-butane and 1008kg of cyclohexane into the mixing kettle and stir for 0.5-1h. During the stirring process, 60 kg of aluminum trichloride was charged into the tubular reactor. After the filling is completed, adjust the temperature of the tubular reactor to 15-20°C, and start feeding through the centrifugal pump, and the feeding speed is controlled at 2-4.5 mL s. The temperature in the transfer kettle is controlled at 15-20°C, and the stirring is started when the reaction liquid flows into the transfer kettle. After 3-5 hours of reaction, start sampling through the monitoring port every 30 minutes for monitoring, and replace the catalyst when the content of 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetralin decreases. The reaction liquid flows out through the overflow port. When the amount of reaction liquid in the washing kettle reaches 1800L, start adding 700L water to quench the reaction, and then wash wit...

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Abstract

The present invention provides an HMT continuous synthesis apparatus and method. The method comprises: taking p-cymene, 2,3-dimethyl-1-butylene, tert-butylchloride cyclohexane as raw materials to prepare a liquid mixture; stirring the mixture uniformly and then placing the mixture into a tubular reactor containing aluminium trichloride; obtaining an HMT reaction liquid in the tubular reactor; carrying out heat insulation while stirring in a transfer kettle and then overflowing the liquid into a hydrolysis kettle; after water washing and alkaline washing, obtaining an HMT crude product by rectification; and obtaining HMT with high purity degree by recrystallization. According to the method provided by the present invention, the process safety is good, the reaction conditions are easy to control, and the product quality is stable, so that HMT continuous large-scale production can be achieved.

Description

Technical field [0001] The present invention relates to the technical field of organic chemicals, more specifically to the key precursor 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydro Continuous synthesis device and method of naphthalene. Background technique [0002] 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene (HMT) is an important intermediate for the synthesis of musk tuna. Tona musk is a polycyclic musk with a tetralin structure. It has excellent properties of acid, alkali and light resistance, no irritation or allergies to the skin. It has a strong musky powdery aroma and is widely used in high-end cosmetics and detergents. After nitromusks were exposed to toxicity problems, about 50% of synthetic musks on the market mainly relied on polycyclic musks, the most representative of which was tonal musks. At present, there are only a handful of manufacturers producing musk, most of which rely on imports and are far from self-sufficient. [0003] The main synthesis processes ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/72C07C13/48
CPCC07C2/72C07C13/48
Inventor 黎明刘升杜晓华黎继俭
Owner TIANMEN DEYUAN CHEM TECH CO LTD
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