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A deep drying and water removal method for dipentene

A drying method and technology for dipentene, applied in chemical instruments and methods, purification/separation of hydrocarbons, organic chemistry, etc., can solve the problems such as no reports on the deep drying and water removal method of dipentene, and achieve continuous and stable drying effect. Simple equipment and good application prospects

Active Publication Date: 2020-07-14
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are basically no reports on deep drying and water removal methods for dipentene at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The present embodiment is a deep drying method of dipentene, comprising the following steps:

[0044] 1) Add 1000 g of dipentene (purity: 95.4%) and 500 mL of cyclohexane with a water content of 1275 ppm into the distillation column kettle, and stir under nitrogen protection; heat up to a reflux temperature of 100° C. to 105° C. At the same time, start the cooling device and set the cooling temperature to 0°C; the total reflux is stable for 30 minutes to fully wet the packing in the rectification tower. Phase azeotrope; until the temperature of the gas phase at the top of the tower rises to the boiling point of cyclohexane, 80-82°C, the recovery of cyclohexane in the tower kettle begins. When there is no obvious fraction falling in the collection bottle, and the temperature of the gas phase begins to drop; reduce the temperature in the tower kettle, remove the anti-suckback oil bubbler, connect the vacuum device, control the vacuum degree at 0.095MPa, and the reflux rat...

Embodiment 2

[0050] The present embodiment is a deep drying method of dipentene, the specific implementation method is the same as that of Example 1, the difference is only that the molecular sieve used in step 2) is 5A molecular sieve;

[0051] 825g of the product was obtained; after testing, the water content of the product was 74ppm, and the water removal efficiency was 95.2%.

Embodiment 3

[0053] The present embodiment is a deep drying method of dipentene, and the specific implementation method is the same as in Example 1, except that the entrainer used in step 1) is benzene;

[0054] 854g of the product was obtained; after testing, the water content of the product was 92ppm, and the water removal efficiency was 93.8%.

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Abstract

The invention relates to a deep drying water removing method used for bipentene. The method includes adding to-be-dried bipentene and an entrainer into a batch distillation device, performing azeotrope water carrying, and collecting dipentene fraction through vacuum distillation; and adding the dipentene fraction into an adsorption column carrying activated molecular sieves to perform adsorption so that dried bipentene can be obtained. The method is mainly to meet the using requirements for the water content of a polymerization inhibitor during a production process of tetrafluoroethene; and the drying method is simple in technology and equipment, high in drying efficiency and fast in effect, so that the method is an ideal choice for industrialization, and has good application prospects.

Description

technical field [0001] The invention relates to the field of chemical material drying, in particular to a deep drying method of dipentene. Background technique [0002] Pure tetrafluoroethylene is very easy to self-polymerize, and the self-polymerization is accompanied by a large amount of heat release, and local overheating is prone to disproportionation reaction, which may cause an explosion. Therefore, in order to prevent the self-polymerization or explosion of tetrafluoroethylene, one of the measures usually taken in industrial production is to add an oxygen scavenger to the pure tetrafluoroethylene gas to remove or reduce the trace oxygen present in tetrafluoroethylene to achieve polymerization inhibition. . Commonly used oxygen scavengers are terpenes, such as dipentene, terpinolene, and terpene. Among them, the most important dipentene is a by-product obtained when turpentine is used as a raw material to synthesize camphor or terpineol. It is a liquid mixture compos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C7/00C07C7/06C07C7/13C07C13/21
CPCC07C7/005C07C7/06C07C7/13C07C13/21
Inventor 罗源军刘波吕太勇李斌陈立义
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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