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Preparation method of prenyl acetate

A kind of ritol ester and alcohol ester technology, applied in the field of ritol ester preparation, can solve the problems of increasing solvent recovery, high price, reducing production capacity, etc., and achieves simple preparation reaction conditions, improved equipment utilization, and high product yield. Effect

Inactive Publication Date: 2013-04-03
HUAIAN WAN BANG SPICE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since sodium acetate is a solid, the reaction needs to introduce toluene as a solvent, which not only reduces the production capacity, but also increases the problem of solvent recovery in the subsequent process.
At the same time, chlorinated isopentene is harmful to the environment, and the human body has obvious damage to lung tissue after inhalation, and the price is relatively high
A large amount of salty waste water is produced in the reaction, which brings a burden to the environment

Method used

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  • Preparation method of prenyl acetate
  • Preparation method of prenyl acetate
  • Preparation method of prenyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Reaction molar ratio Acetic anhydride: Pentadienol: Sodium acetate=1:1.8.:0.05.

[0019] 1) Make sure the reactor is clean and dry. Put 1020 kg of acetic anhydride into the reaction kettle with a pump and add 41 kg of sodium acetate. After heating up to 100°C, add 1548 kg of pentadienol dropwise at 100-110°C. After about 4 hours of dripping, at this temperature Constant temperature reaction for 2 hours; reaction end point: the content of pentadienol in the feed liquid is less than 0.5%.

[0020] Reaction equation:

[0021]

[0022] 2) After the reaction, add 260 kg of water to the crude product, stir and let it stand. The lower layer of water is divided to obtain 2420 kilograms of crude pitol ester liquid. Add anhydrous sodium carbonate to the crude pitol ester liquid to adjust Ph to 7.

[0023] 3) Adjust the Ph to 7 in step (2) and carry out rectification of the crude pitol ester liquid, collect the fraction at 70-80°C / 50mmHg to be the finished pitol ester, and ...

Embodiment 2

[0025] Reaction molar ratio Acetic anhydride: Pentadienol: Sodium acetate=1:1.9.:0.05.

[0026] 1) Make sure the reactor is clean and dry. Put 1020 kg of acetic anhydride into the reaction kettle with a pump and add 41 kg of sodium acetate. After heating up to 100°C, add 1634 kg of pentadienol dropwise at 100-110°C. After about 4 hours of dripping, at this temperature Constant temperature reaction for 2 hours; reaction end point: the content of pentadienol in the feed liquid is less than 0.5%.

[0027] Reaction equation:

[0028]

[0029] 2) After the reaction, add 280 kg of water to the crude product, stir and let stand. The lower layer of water is divided to obtain 2430 kilograms of crude pitol ester liquid. Add anhydrous sodium carbonate to the crude pitol ester liquid to adjust Ph to 7.

[0030] 3) After adjusting the Ph to 7 in step 2), carry out rectification of the crude pitol ester liquid, collect the distillate at 70-80°C / 50mmHg, which is the finished pear alco...

Embodiment 3

[0032] Reaction molar ratio Acetic anhydride: Pentadienol: Sodium acetate=1:1.7:0.05.

[0033] 1) Make sure the reactor is clean and dry. Put 1020 kg of acetic anhydride into the reaction kettle with a pump and add 41 kg of sodium acetate. After heating up to 100°C, add 1462 kg of pentadienol dropwise at 100-110°C. After about 4 hours of dripping, at this temperature Constant temperature reaction for 2 hours; reaction end point: the content of pentadienol in the feed liquid is less than 0.5%.

[0034] Reaction equation:

[0035]

[0036] 2) After the reaction, add 260 kg of water to the crude product, stir and let it stand. The lower layer of water is divided to obtain 2180 kilograms of crude pitol ester liquid. Add anhydrous sodium carbonate to the crude pitol ester liquid to adjust Ph to 7.

[0037] 3) Adjust the Ph to 7 in step (2) and carry out rectification of the crude pitol ester liquid, collect the fraction at 70-80°C / 50mmHg to be the finished pitol ester, and o...

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Abstract

The invention discloses a preparation method of prenyl acetate, which comprises the following steps: (1) adding acetic anhydride and sodium acetate into a reaction vessel, heating to 100 DEG C, dropwisely adding pentadienol at 100-110 DEG C, then performing constant temperature reaction for 2 hours at the temperature; (2) after the reaction, adding a proper amount of water into the solution of step (1), stirring, standing, separating to remove water at the lower layer so as to obtain crude prenyl acetate liquid; adding anhydrous sodium carbonate into the crude prenyl acetate liquid to adjust the pH to 7; (3) rectifying the crude prenyl acetate liquid, collecting a fraction of 70-80 DEG C / 50 mmHg to obtain the prenyl acetate finished product. The invention is simple in preparation reaction condition, very high in product yield, and especially suitable for industrial production; the prenyl acetate product yield is above 88%, and the content after rectification is up to more than 97%.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of pitol esters. Background technique [0002] Lithitol esters (prenyl acetate; 2-prenyl acetate; 2-prenyl acetate; 3,3- [0003] Dimethyl allyl acetate; 3-methyl-2-butene acetate; 3,3-dimethylallyl acetate; 3-methyl-2-butene acetate; 3-acetate Methyl-2-butenyl ester; 3-methyl-2-buten-1-ol acetate). The existing production method of piritol ester is prepared through the interaction of prenyl chloride and sodium acetate as raw materials. Because sodium acetate is a solid, the reaction needs to introduce toluene as a solvent, which not only reduces the production capacity, but also increases the problem of solvent recovery in the subsequent process. At the same time, chlorinated isopentene is harmful to the environment, and the human body has obvious damage to lung tissue after inhalation, and the price is relatively high. A large amount of salty ...

Claims

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Application Information

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IPC IPC(8): C07C69/145C07C67/08
Inventor 赵舰
Owner HUAIAN WAN BANG SPICE IND CO LTD
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