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A kind of method utilizing cyclohexene and acetic acid to prepare cyclohexanol and cyclohexyl acetate

A technology of cyclohexyl acetate and cyclohexene, which is applied to the preparation of carboxylic acid esters, chemical instruments and methods, hydrolysis preparation, etc., can solve the problems of high price, low selectivity, and large hydrogen consumption, and achieve low production costs , high selectivity, flexible control effect

Active Publication Date: 2020-07-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The oxidation process of cyclohexane is not safe because cyclohexane can form explosive mixtures when mixed with air
In addition, this process also has the disadvantages of low selectivity, low conversion rate and high energy consumption.
The phenol hydrogenation process mainly considers that the price of phenol is much higher than that of benzene, and the hydrogen consumption is large, so the process is subject to some limitations in application
The cyclohexene direct hydration method also has the disadvantage of low conversion rate

Method used

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  • A kind of method utilizing cyclohexene and acetic acid to prepare cyclohexanol and cyclohexyl acetate
  • A kind of method utilizing cyclohexene and acetic acid to prepare cyclohexanol and cyclohexyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Reaction raw materials: cyclohexene is an industrial product with a purity of more than 99.5%, acetic acid is glacial acetic acid with a purity of more than 99.5%, and water is deionized water. Both the first catalyst and the second catalyst are H-type macroporous strong acid styrene series cations Resin, brand NKC-9, 50 g of the first catalyst was charged into the first reactor A, and 50 g of the second catalyst was charged into the second reactor B.

[0047] Step i: The cyclohexene 1 and the acetic acid 2 are respectively charged from the top of the first reactor A by a metering pump and then reacted under the action of the first catalyst to obtain a mixture 3. The reaction conditions were as follows: the catalyst bed temperature was 90 °C; the catalyst bed height-diameter ratio was 10; the reaction pressure was 1.5 MPa; the molar ratio of cyclohexene to acetic acid was 0.8; the weight space velocity of cyclohexene was 2 h -1 .

[0048] The mixture 3 flows into the f...

Embodiment 2

[0055] Reaction raw materials: the same as Example 1, the difference is: the first catalyst and the second catalyst both adopt modified H-type macroporous strong acid styrene series cationic resin NKC-9, and 50g of the first catalyst is loaded into the first reaction In vessel A, 50 g of the second catalyst was charged into second reactor B.

[0056] The preparation method of modified H-type macroporous strong acid styrene series cationic resin NKC-9:

[0057] 2.0 g of sulfamic acid and 200 mL of methanol were respectively added to a 500 mL round-bottomed flask, and stirred to dissolve the sulfamic acid. 180g of NKC-9 resin and the methanol solution dissolved with sulfamic acid were added to the autoclave respectively, the autoclave was installed, heated to 80°C under stirring, cooled after 2 hours, stopped stirring, and the temperature of the autoclave decreased to 80°C. After room temperature, the reaction kettle was disassembled, the catalyst was poured out, dried in the a...

Embodiment 3

[0063] Reaction raw materials: the same as in Example 1.

[0064] Step i: The operation is the same as that in Example 1, except that: the catalyst bed temperature is 95° C.; the reaction pressure is 1.0 MPa; and the molar ratio of cyclohexene to acetic acid is 0.70.

[0065] Step ii: the operation is the same as that in Example 1, except that the catalyst bed temperature is 80°C; the reaction pressure is 2.5MPa; the molar ratio of water and the cyclohexyl acetate in the crude cyclohexyl acetate product containing acetic acid is 1.1; The weight space velocity of the cyclohexyl acetate crude product containing acetic acid is 3h -1 .

[0066] The operations of step iii and step iv are the same as in Example 1.

[0067] The reaction conditions and reaction results of step i are shown in Table 1; the reaction conditions and reaction results of step ii are shown in Table 2.

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Abstract

The present invention relates to a method for preparing cyclohexanol and cyclohexyl acetate by using cyclohexene and acetic acid. The method comprises: 1, carrying out a reaction on cyclohexene and acetic acid under the action of a catalyst to obtain an acetic acid-containing cyclohexyl acetate crude product; 2, carrying out a hydrolysis reaction on water and the acetic acid-containing cyclohexyl acetate crude product, and separating the mixture of cyclohexyl acetate and cyclohexanol from the mixture obtained through the reaction; and 3, rectifying the mixture of cyclohexyl acetate and cyclohexanol so as to respectively obtain cyclohexanol and cyclohexyl acetate. With the method of the present invention, the high-purity cyclohexanol product and the high-purity cyclohexyl acetate product can be obtained, the cyclohexanol selectivity is high, the process is simple, and the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical products, in particular to a method for preparing cyclohexanol and cyclohexyl acetate by using cyclohexene and acetic acid. Background technique [0002] Cyclohexyl acetate is a colorless or slightly yellowish transparent oily liquid with banana and apple aromas. It is mainly used to prepare flavors for food and cosmetics, and is also commonly used as paint and paint solvents. In industry, cyclohexanol and acetic acid are commonly used as raw materials, and concentrated sulfuric acid is used as a catalyst to synthesize cyclohexyl acetate. Due to the strong acidity and strong oxidizing properties of concentrated sulfuric acid, side reactions such as oxidation and dehydration are prone to occur, and at the same time, it is severely corrosive to equipment, the post-treatment process of acid waste liquid is complicated, and catalyst regeneration is difficult, so it belongs to the non-g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/04C07C35/08C07C29/09
CPCC07C29/095C07C67/04C07C69/14C07C35/08
Inventor 王定博张明森郭敬杭
Owner CHINA PETROLEUM & CHEM CORP
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