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Production device and preparation method of organic sodium alcoholate

A production device and technology for organic alcohols, applied in the field of preparation of organic alcohol alkali metal salts, can solve problems such as safety accidents, prolongation of process time, fire or explosion, etc.

Active Publication Date: 2020-10-23
江苏金木土新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the boiling point of unsaturated alcohol is generally above 100°C, reaching or exceeding the melting point of metal sodium, during the reaction process of unsaturated alcohol and metal sodium, it is easy to cause metal sodium to heat up and melt into a spherical shape, further aggravating the reaction rate and causing safety accidents. The reaction process is accompanied by the generation of hydrogen gas, and if the hydrogen gas is not removed in time, it will easily cause fire or explosion; the specific surface area of ​​sodium hydride is much larger than that of metal sodium. During the reaction with unsaturated alcohol, hydrogen gas is also generated and the reaction is very violent. Only a small amount Adding sodium hydride to unsaturated alcohol many times not only significantly prolongs the process time, but also the solvent kerosene of sodium hydride is insoluble in water, which has an adverse effect on the polymerization effect when preparing carboxylic acid water reducer

Method used

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  • Production device and preparation method of organic sodium alcoholate

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preparation example Construction

[0031] see figure 1 Shown, a kind of production device and preparation method of organic sodium alkoxide, comprise still anti-rectification device, described still anti-rectification device comprises tower still 1, and described tower still 1 is fixed with the outside of tower still that can be heated and cooled. Jacket 9, the inner cover of the tower kettle 1 is provided with an agitator 2, the top of the tower kettle 1 is connected to the lower end inlet of the rectification column 3, and the outer surface of the rectification column 3 is provided with a steam heating insulator 10, so The bottom of the tower kettle 1 is connected with a finished product tank 8, the top outlet of the rectifying column 3 is connected to the inlet of the total reflux condenser 4, and the bottom outlet of the total reflux condenser 4 is connected to the top inlet of the receiving tank 5, so The outlet at the bottom of the receiving tank 5 is respectively connected with a material reflux pump 6 a...

Embodiment 1

[0044] Weigh 1 part of metal sodium, add it to the tower kettle 1 and replace it with nitrogen for 3 times, open the vacuum device 7 to pump the pressure in the reactor to -0.1MPa, add 0.01% hydroquinone to the allyl alcohol, and Inhale 30 parts of allyl alcohol into the tower kettle 1. Turn on the stirrer 2 and keep the vacuum line of the vacuum pump 7 in an open state. Turn on the jacketed steam heating of the tower kettle 1, raise the temperature to 50°C, stop the steam heating, and control the temperature of the tower kettle 1 at 50±5°C. The allyl alcohol vapor enters the total reflux condenser 4 through the rectification tower 3, and enters the receiving tank 5 after being condensed into a liquid. When the liquid level gauge liquid level of the receiving tank 5 reaches 25%, the material reflux pump 6 is opened to keep the receiving tank The liquid level of the liquid level gauge in 5 remains unchanged, and the remaining materials are pumped back to the rectification towe...

Embodiment 2

[0055] Weigh 52.8 parts of allyl alcohol and 3.3 parts of catalyst C-153 into the polyether reactor, replace with nitrogen for 3 times, and pump the polyether reactor down to -0.1MPa again. Turn on the heating device to raise the temperature of the polyether reactor to 100°C, open the ethylene oxide feed valve, and first feed 1 part of ethylene oxide until the polymerization of ethylene oxide in the polyether reactor begins (temperature rises, pressure drop), continue to feed 4032 parts of ethylene oxide, control the reaction temperature at 120±5°C, and the reaction pressure ≤0.4MPa, after the ethylene oxide feeding is completed, continue the heat preservation reaction for 30min, cool down the polyether reactor to 50°C, and then Vacuum degassing to -0.1MPa, and finally pressurize nitrogen to normal pressure and discharge. Obtained 4100 parts of light brown viscous liquid, named as PEG-1. Tested by hydroxyl value method, the weight average molecular weight is 2390; tested by G...

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Abstract

The invention discloses a production device and a preparation method of organic sodium alcoholate. The production device comprises a kettle reverse rectification device. The method comprises the following steps: adding metallic sodium into the kettle reverse rectification device, then carrying out nitrogen replacement, starting a vacuum device, pumping a reactor to-0.1 MPa, adding organic alcoholinto the reactor, and carrying out a reaction at a certain temperature under a negative pressure condition to obtain an organic sodium alkoxide solution with a certain solid content. According to thepreparation method of organic sodium alcoholate, the boiling point of the organic alcohol is reduced through vacuum rectification, and the distilled organic alcohol flows back to the reaction system again so that direct heat exchange between the material and the backflow material can be promoted, the temperature of the reaction system is reduced, and the problems that the boiling point of the organic alcohol is too high, metal sodium is heated and melted into a spherical shape, the reaction intensity is increased, and the reaction is out of control are well solved.

Description

technical field [0001] The invention relates to a preparation method of an organic alcohol alkali metal salt, in particular to a production device and a preparation method of an organic sodium alkoxide, belonging to the application field of fine chemical technology. Background technique [0002] Polycarboxylate superplasticizer is a third-generation high-performance superplasticizer recently developed after the first-generation lignosulfonate, the second-generation naphthalene-based sulfonate, and aliphatic sulfonate. Water-reducing agent has the characteristics of high water-reducing rate and good slump-retaining property. It has been widely promoted and applied in the fields of infrastructure engineering, civil construction, nuclear power, and hydropower. About 80% of the liquid agent market share. [0003] Polyether macromonomer is the main raw material for the synthesis of polycarboxylate superplasticizers, accounting for 80% to 90% of the mass of polycarboxylate superp...

Claims

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Application Information

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IPC IPC(8): C07C29/70C07C29/94C07C29/80C07C33/03C07C33/025C07C31/30C07C35/46C07C41/26C07C41/42C07C41/46C07C43/178C08G65/28
CPCC07C29/70C07C29/94C07C29/80C07C41/26C07C41/42C07C41/46C08G65/2648C08G65/2609C07C33/03C07C33/025C07C31/30C07C35/46C07C43/178
Inventor 牟中江范士敏迟国福张磊
Owner 江苏金木土新材料有限公司
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