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Method for preparing dihydrodicyclopentadiene through continuous reaction

A technology of hydroxydihydrodicyclopentadiene and dicyclopentadiene, which is applied in the preparation of hydroxyl addition, organic chemistry, etc., can solve the problems of serious carbonization of raw materials, non-continuous production, long reaction time, etc., and achieve high production efficiency, Easy to operate and good product quality

Inactive Publication Date: 2013-07-03
LIAOCHENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to propose a continuous reaction method for preparing hydroxydihydrodicyclopentadiene in view of the problems of long reaction time, inaccurate temperature control, serious carbonization of raw materials, and non-continuous production in the hydration process of synthesizing dicyclopentadiene

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  • Method for preparing dihydrodicyclopentadiene through continuous reaction

Examples

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Embodiment 1

[0019] Embodiment 1,2,6,7 is to use sulfuric acid, phosphoric acid, p-toluenesulfonic acid, hydrochloric acid as catalyzer respectively in continuous stirred tank reactor, take dicyclopentadiene as raw material to carry out hydration reaction; Embodiment 3,4, 8 is to carry out hydration reaction with p-toluenesulfonic acid, phosphotungstic heteropolyacid and acidic ionic liquid as catalyst respectively in tubular reactor; embodiment 5 is to carry out dicyclopentadiene with sulfuric acid as catalyst in microstructure reactor Hydration reaction.

[0020] Example 1

[0021] Add polycyclopentadiene solution and 5% sulfuric acid solution according to the molar equivalent ratio of 1:5, while adding the temperature at 60°C, the volume is 20m 3 In the continuous stirred tank reactor (belonging to the technical scheme of the present invention), the stirring speed is 200r / min, and the average residence time is 300min. After washing, centrifugal separation and drying, hydroxydihydrodic...

Embodiment 2

[0023] The liquid polycyclopentadiene solution and 85% phosphoric acid solution are in a molar equivalent ratio of 2:1, while the temperature is controlled at 120°C, and the volume is 20m 3 In two identical series continuous stirred tank reactors, the stirring speed is 300r / min, the average residence time is 10min, the outlet pipe is immersed in a flowing room temperature water bath to cool down to terminate the reaction, the reaction product is collected, and the product solution is washed, After centrifugal separation and drying, hydroxydihydrodicyclopentadiene was obtained with a yield of 69%.

Embodiment 3

[0025] The liquid polycyclopentadiene solution and 20% p-toluenesulfonic acid solution are in a molar equivalent ratio of 1:4, and at the same time, the liquid chromatographic pump is pumped into a tube with a temperature of 40 °C, a diameter of 100 mm, and a length of 5 m. In the reactor, the residence time of the material is 5min. The outlet pipe is soaked in a flowing room temperature water bath to cool down to terminate the reaction, and the reaction product is collected. The product solution is washed, centrifuged, and dried to obtain hydroxydihydrodicyclopentadiene. The rate is 59%.

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Abstract

The invention relates to a method for preparing dihydrodicyclopentadiene through continuous reaction. The method comprises the following steps of: simultaneously pumping an acid solution and liquid dicyclopentadiene in a molar equivalence ratio of (0.5-5):1 into a series connection mixed flow reactor, a tube type reactor or a microstructural reactor into and out of which reaction liquid can flow,adjusting reaction temperature to be 20 to 120 DEG C, controlling flow speed to ensure that the total retention time of reaction liquid in the reactor is 0.5s to 3 min, and reacting reaction liquid in the reactor to obtain dihydrodicyclopentadiene. The method is short in reaction time, and high in efficiency; temperature is easy to control; and the prepared product is high in yield and has high quality.

Description

technical field [0001] The invention relates to a process for preparing hydroxydihydrodicyclopentadiene, in particular to a process for preparing hydroxydihydrodicyclopentadiene by continuous reaction, and belongs to the technical field of fine chemicals. Background technique [0002] Hydroxydihydrodicyclopentene synthesized from carbon five components in petrochemical resources can be used as raw materials for polyester resins, urea-formaldehyde resins, melamine resins and alkyd resins; used as tackifiers, plasticizers, coatings, rust removers It can be used as the raw material of agent and printing ink, etc.; it can be used as the third monomer of ethylene-propylene rubber as the raw material of rubber; it is also a good rubber after ring-opening polymerization; it can also be used as the raw material of pesticides and as a good high-energy fuel. Japan and the United States are the countries with the best comprehensive utilization of C5 resources. At present, the separatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C35/37C07C29/06C07C29/08C07C29/04C07C29/05
Inventor 姚型军张艳杜凌云刘军海窦建民
Owner LIAOCHENG UNIV
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