3-methyl-3-butene-1-ol dehydration method and device

A technology of alcohol dehydration and butene, applied in chemical instruments and methods, preparation of hydroxy compounds, separation/purification of hydroxy compounds, etc., can solve problems such as inability to efficiently utilize

Active Publication Date: 2020-07-07
JIANGSU SOBUTE NEW MATERIALS +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of the prepared product is 99.75-99.90%, the formaldehyde content is 0.03-0.05%, and the moisture content is 0.03-0.05%. The method of the invention can effectively remove formaldehyde, the reaction conditions are mild, it is easy to produce on a large scale, and the equipment investment is low. But it will produce urea-based waste salt, which cannot be used efficiently
[0008] In short, ther

Method used

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  • 3-methyl-3-butene-1-ol dehydration method and device

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] use figure 1The shown reaction device carries out the following operation process. In the rectification tower 1, feed the material at a rate of 200kg / h with a mass flow rate, open the steam inlet and outlet valves of the reboiler 6, control the temperature of the reboiler 6 at the bottom of the tower to be 95°C, and the vacuum pressure at the bottom of the tower to be -0.085MPa, open The chilled water inlet and outlet valves of the tower top condenser 2 are used to control the tower top temperature to 55°C and the tower top pressure to -0.088MPa. Open the ethylene glycol solution inlet and outlet valves of the freezing pipe at the bottom of the buffer tank 3 to control the temperature of the freezing pipe to 5°C. Keep the total reflux for 0.6h, open the drainage pipe of the freezing pipe, the drainage rate is 18kg / h, wait for the sample analysis of the top reflux pipe, when the water content is less than 1000ppm, stabilize for 10min, open the discharge pump of the recti...

Embodiment 2

[0036] use figure 1 The shown reaction device carries out the following operation process. In the rectification tower 1, feed the material at a rate of 201kg / h with a mass flow rate, open the steam inlet and outlet valve of the reboiler 6, control the temperature of the reboiler 6 at the bottom of the tower to be 98°C, and the vacuum pressure at the bottom of the tower to be -0.088MPa, open The chilled water inlet and outlet valves of the tower top condenser 2 control the tower top temperature to 58°C and the tower top pressure to -0.090MPa, open the ethylene glycol solution inlet and outlet valves of the freezing pipe at the bottom of the buffer tank 3, and control the freezing pipe temperature to 7°C. Keep the total reflux for 0.8h, open the drainage pipe of the freezing pipe, the drainage rate is 16kg / h, wait for the sample analysis of the top reflux pipe, when the water content is less than 1000ppm, stabilize for 10min, open the discharge pump of the rectification tower 1 ...

Embodiment 3

[0038] use figure 1 The shown reaction device carries out the following operation process. In the rectification tower 1, feed the material at a rate of 198kg / h with a mass flow rate, open the steam inlet and outlet valves of the reboiler 6, control the temperature of the reboiler 6 at the bottom of the tower to be 94°C, and the vacuum pressure at the bottom of the tower to be -0.082MPa, open The chilled water inlet and outlet valves of the tower top condenser 2 control the temperature of the tower top to 53°C and the pressure of the tower top to -0.085MPa, open the inlet and outlet valves of the ethylene glycol solution of the freezing pipe at the bottom of the buffer tank 3, and control the temperature of the freezing pipe to 8°C. Keep the total reflux for 0.5h, open the drainage pipe of the freezing pipe, the drainage rate is 15kg / h, wait for the sample analysis of the reflux pipe at the top of the tower, when the water content is less than 1000ppm, stabilize for 10min, open...

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Abstract

The invention discloses a 3-methyl-3-butene-1-ol dehydration method and a device thereof, and the dehydration method utilizes pressure swing distillation and inorganic salt adsorption modes to efficiently remove residual water and prepare a high-quality product with extremely low water content; the variable-pressure rectification refers to controlling the pressure in a rectifying tower to be -0.08MPa to 0.09 MPa during rectification; the inorganic salt adsorption means that anhydrous sodium acetate adsorbs water. According to the method, the moisture content of the product is efficiently reduced, the purity of the downstream polyether product and the efficiency of the polycarboxylic acid product can be improved, the temperature of the rectifying tower kettle is low (90-100 DEG C), the energy-saving benefit is obvious, the process is green, the operation is convenient, and the industrial application prospect is wide.

Description

technical field [0001] The invention relates to a dehydration method and device for 3-methyl-3-buten-1-ol, belonging to the technical field of fine chemicals. Background technique [0002] 3-Methyl-3-buten-1-ol (MBOH) is the initiator of the side chain-TPEG polyether of the third generation polycarboxylate high-performance water reducer for synthetic concrete. The TPEG polyether synthesized from this raw material, It plays a decisive role in the quality and performance of polycarboxylate high-performance superplasticizer products, making it have a strong ability to maintain the dispersion of cement particles, low dosage, high water-reducing rate, good reinforcement effect, durability, and no rust The advantages of steel and environmental friendliness. In addition, 3-methyl-3-buten-1-ol can be isomerized into isopentenol, which is used as the main raw material for the synthesis of biomimetic pesticide quasi-"pyrethrin" precursor - methyl (ethyl) pyrethroid. The main raw mat...

Claims

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Application Information

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IPC IPC(8): C07C29/74C07C29/76C07C29/80C07C33/025
CPCC07C29/74C07C29/76C07C29/80C07C33/025Y02P20/10
Inventor 王涛杨勇范士敏韩正乔敏冉千平
Owner JIANGSU SOBUTE NEW MATERIALS
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