Method for synthesizing 4-hydroxy-4'-isopropoxy-diphenyl sulfone compound by micro-channel reactor

A technology of microchannel reactor and isopropoxy, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of long reaction time, high reaction temperature, and low conversion rate, and achieve the goal of reaction time Short, high yield, high conversion effect

Active Publication Date: 2020-06-19
沈阳感光化工研究院有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] Synthesis of 4-hydroxy-4'-isopropoxy-diphenyl sulfone by traditional kettle reaction, mainly using bisphenol S and 2-bromopropane, using toluene or chlorobenzene as solvent, adding sodium hydroxide or hydroge...

Method used

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  • Method for synthesizing 4-hydroxy-4'-isopropoxy-diphenyl sulfone compound by micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Reaction equation:

[0021]

[0022] Dissolve 20 grams of bisphenol S in 3.2 grams of sodium hydroxide and 50 milliliters of aqueous solution in a three-necked flask, add 9.8 grams of 2-bromopropane in another one-necked flask, and pass it into the microchannel reactor with a metering pump respectively, the reaction temperature 60 degrees, the reaction time is 5 minutes. The obtained reaction liquid was added into a three-necked flask, and the precipitation was carried out at room temperature for 5-10 hours. Filter, wash with water until neutral, and dry to obtain 21.5 g of white powder. Content 99.4%, yield 92.0%.

Embodiment 2

[0023] Embodiment 2: the difference between this example and embodiment 1 is:

[0024] In this example, 20 grams of bisphenol S are dissolved in 3.2 grams of sodium hydroxide and 50 milliliters of aqueous solution in a three-necked flask, and 9.8 grams of 2-bromopropane are added in another one-necked flask, which are passed into the microchannel reactor with metering pumps respectively. The reaction temperature is 60 degrees, and the reaction time is 4 minutes. The obtained reaction liquid was added into a three-necked flask, and the precipitation was carried out at room temperature for 5-10 hours. Filter, wash with water until neutral, and dry to obtain 21.1 g of white powder. Content 99.2%, yield 90.5%.

Embodiment 3

[0025] Embodiment 3: the difference between this example and embodiment 1 is:

[0026] In this example, 20 grams of bisphenol S are dissolved in 3.2 grams of sodium hydroxide and 50 milliliters of aqueous solution in a three-necked flask, and 9.8 grams of 2-bromopropane are added in another one-necked flask, which are passed into the microchannel reactor with metering pumps respectively. The reaction temperature is 60 degrees, and the reaction time is 3 minutes. The obtained reaction liquid was added into a three-necked flask, and the precipitation was carried out at room temperature for 5-10 hours. Filter, wash with water until neutral, and dry to obtain 20.6 g of white powder. Content 99.1%, yield 88.3%.

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Abstract

The invention discloses a method for synthesizing a 4-hydroxy-4'-isopropoxy-diphenyl sulfone compound by a micro-channel reactor, and belongs to the technical field of chemical products. The preparation method comprises the following steps: (1) adding 4,4-dihydroxy diphenyl sulfone (bisphenol S), sodium hydroxide and water into a three-neck bottle, and stirring until the materials are completely dissolved, wherein the molar ratio of bisphenol S to sodium hydroxide is 1:1, and the weight of the added water is 2.5-10 times that of bisphenol S; (2) adding 2-bromopropane into another single-mouthbottle, wherein the molar ratio of 2-bromopropane to bisphenol S is 1:1; (3) respectively introducing into a micro-channel reactor by using a metering pump; (4) carrying out a reaction at a reaction temperature of 50-80 DEG C for 3-5 minutes; (5) adding the obtained reaction solution into another clean medium-three-neck bottle, cooling to room temperature, and separating out for 5-10 hours; and (6) filtering, washing with water, and drying to obtain the product. The method has the advantages of short reaction time, low alkali consumption, high conversion rate and high yield.

Description

technical field [0001] The invention belongs to the technical field of chemical products, in particular to a method for synthesizing 4-hydroxyl-4'-isopropoxyl-diphenylsulfone compound in a microchannel reactor. Background technique [0002] 4-Hydroxy-4'-isopropoxy-diphenylsulfone (trade name D-8, company product code F-108), is a very good color developer in thermosensitive recording materials. It has a wide range of uses and has the advantages of excellent preservation performance of recorded images. [0003] Synthesis of 4-hydroxy-4'-isopropoxy-diphenyl sulfone by traditional kettle reaction, mainly using bisphenol S and 2-bromopropane, using toluene or chlorobenzene as solvent, adding sodium hydroxide or hydrogen Potassium oxide aqueous solution needs to add a phase transfer catalyst due to two-phase reaction, the reaction temperature is high, the reaction time is long, the conversion rate is low, and the yield is low. Contents of the invention [0004] In view of the...

Claims

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Application Information

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IPC IPC(8): C07C315/04C07C317/22
CPCC07C315/04C07C317/22
Inventor 李昌德祁咏梅马思聪李善柱沈困知王越许锦凤刘勇
Owner 沈阳感光化工研究院有限公司
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