A diene ring-opening process control system and its application method

A process control and metering tank technology, which is applied in the fields of steroids and organic chemistry, can solve the problems of low diene yield and unstable side reaction, and achieve the effect of complete reaction, safe reaction and guaranteed stability

Active Publication Date: 2021-04-16
湖北民生生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The invention provides a diene ring-opening process control system, which solves the problem in the prior art that the side reaction degree of the ring-opening reaction is unstable due to insufficient control of temperature and pressure, which ultimately leads to a low yield of diene

Method used

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  • A diene ring-opening process control system and its application method
  • A diene ring-opening process control system and its application method
  • A diene ring-opening process control system and its application method

Examples

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Embodiment 1

[0056] Such as Figure 1~4 , the present embodiment proposes a diene ring-opening process control system, including a first raw material tank (not shown) and a second raw material tank (not shown), the first raw material tank is stored with acid anhydride, and the second raw material tank stored in glacial acetic acid,

[0057] It also includes two open-loop tanks 1, and each open-loop tank 1 is provided with a first connecting pipe 2, a second connecting pipe 3, a third connecting pipe 4 and a fourth connecting pipe 5, wherein the two first connecting pipes 2 are respectively connected with meters 6, The two second connecting pipes 3 are jointly connected to a buffer tank 7, the two third connecting pipes 4 are connected to a metering tank 8 after converging, and the two fourth connecting pipes are connected to an oxidation tank 9 after converging, and the oxidation tank 9 is used for oxidation and hydrolysis reactions ;

[0058] The metering tank 8 is provided with the fif...

Embodiment 2

[0089] The present embodiment except the following content, all the other parts are identical with embodiment 1; The difference is:

[0090] A method for using a diene ring-opening process control system, comprising the following steps:

[0091] S1 Add diosgenin to the two open-loop tanks 1, adjust the pressure of the metering tank 8 to -0.06Mpa, connect the metering tank 8 and the first raw material tank, and disconnect the metering tank 8 and the first raw material tank when the liquid level of the metering tank 8 shows 80%. Raw material tank;

[0092] S2 adjust the pressure of any open-loop tank 1 to -0.08Mpa, connect the open-loop tank 1 and the metering tank 8, when the liquid level of the metering tank 8 shows 2%, disconnect the open-loop tank 1 and the metering tank 8;

[0093] S3 adjusts the pressure of the metering tank 8 to -0.06Mpa, connects the metering tank 8 and the second raw material tank, and when the liquid level of the metering tank 8 shows 30%, disconnects...

Embodiment 3

[0102] The present embodiment except the following content, all the other parts are identical with embodiment 1; The difference is:

[0103] A method for using a diene ring-opening process control system, comprising the following steps:

[0104] Add diosgenin into two open-loop tanks 1 of S1, adjust the pressure of the metering tank 8 to -0.05Mpa, connect the metering tank 8 and the first raw material tank, and when the liquid level of the metering tank 8 shows 85%, disconnect the metering tank 8 and the first raw material tank. Raw material tank;

[0105] S2 adjusts the pressure of any open-loop tank 1 to -0.07Mpa, connects the open-loop tank 1 and the metering tank 8, and disconnects the open-loop tank 1 and the metering tank 8 when the liquid level of the metering tank 8 shows 5%;

[0106] S3 adjusts the pressure of the metering tank 8 to -0.05Mpa, connects the metering tank 8 and the second raw material tank, and when the liquid level of the metering tank 8 shows 35%, dis...

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Abstract

The invention provides a diene ring-opening process control system and its use method, including a first raw material tank, a second raw material tank, two open-loop tanks, two buffer tanks, a metering tank and an oxidation tank; , two open-loop tanks, two buffer tanks, the on-off valve assembly between the metering tank and the oxidation tank; also includes a heater arranged in each open-loop tank for heating the open-loop tank and a temperature sensor for detecting temperature and a pressure sensor for detecting pressure, wherein both the temperature sensor and the pressure sensor are electrically connected to the meter on the first connecting pipe. Beneficial effects: conveniently control the temperature and pressure of the ring-opening reaction, and set the pressure in the metering tank and the open-loop tank, so that the loading of raw materials can also be carried out conveniently; adding metering tanks can better control the amount of each reaction raw material At the same time, adding a buffer tank can prevent the reactants in the ring-opening tank from pouring back; through the control of the pressure and temperature during the ring-opening reaction, the yield of diene has been effectively improved.

Description

technical field [0001] The invention relates to the field of chemical equipment, in particular to a diene ring-opening process control system and a use method thereof. Background technique [0002] Pregnancy dienolone acetate (diene for short) is an important intermediate in the synthesis of steroid hormone drugs, and about 70% of steroid hormone drugs use dienes as raw materials. At present, the production process of domestic diene uses diosgenin as raw material, and it is prepared through three steps of ring opening, oxidation and hydrolysis. The specific process route is as follows: [0003] [0004] Among them, the first step reaction is a ring-opening reaction. After adding diosgenin, solid mother liquor, acetic anhydride and acetic acid into the ring-opening tank, the temperature starts to rise. When the internal temperature reaches about 60°C, turn on the vacuum and pump for 5 minutes. When the pressure reaches above -0.08MPa, close the vacuum valve. When the int...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J13/00
CPCC07J13/005
Inventor 邓海锋陈孝华
Owner 湖北民生生物医药有限公司
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