Process for preparing trimethylolpropane by adopting centrifugal filtering calcium method

A technology of trimethylolpropane and preparation process is applied in the new process field of plate filter press method, which can solve the problems of environmental hazards of sewage, waste of manpower and material resources, etc., and achieve the effects of reducing extraction, reducing floor space and reducing sedimentation process.

Active Publication Date: 2013-07-10
江西高信前沿科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the traditional filtration process not only wastes a lot of manpower and material resources, but also produces a large amount of sewage, which also causes certain harm to the environment.

Method used

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  • Process for preparing trimethylolpropane by adopting centrifugal filtering calcium method
  • Process for preparing trimethylolpropane by adopting centrifugal filtering calcium method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Feed according to 10mol n-butyraldehyde, feed formaldehyde, n-butyraldehyde, and calcium hydroxide according to 3.2:1:0.8, the mass content of calcium hydroxide is 90%, obtain the reaction liquid for separation, start the screw centrifuge to The speed is 3000 rev / min. Centrifuged out is a clear mother liquor, the removal rate of impurities is 98%, the specific operation is as follows: figure 1 The reaction solution in the reaction solution tank 1 containing suspended solids in the reaction solution is taken out by the pump 2 to the horizontal screw centrifuge 3, and enters the drum 11 through the feed pipe 7, and the strong centrifugal force generated by the high-speed rotating drum 11 makes the The solid phase settles to the inner wall net 12 of the drum, and the relative motion of the conveying screw 10 and the drum 11 is caused by the different rotation speed, so that the solid phase flows out of the slag car 4 from the sink 15, and the liquid phase flows from th...

Embodiment 2

[0032] (1) Feed according to 10mol n-butyraldehyde, formaldehyde, n-butyraldehyde, and calcium hydroxide are fed according to 3.2:1:0.8, (calcium hydroxide content is 90%) to obtain the reaction liquid for separation, start the screw centrifuge to rotate at 3500 turn / min. The centrifugation is clear mother liquor, and the impurity removal rate is 99%, and the specific operations are the same as in Example 1;

[0033] (2) The centrifuged mother liquor enters the concentration tower for evaporation, and calcium formate is separated during the concentration process, and the trihydric solution is subjected to rectification in the light component separation tower, and finally trihydric is distilled in the trihydric separation tower to obtain trihydric. 2.101 kg of trimethylolpropane with a mass content of 99.5% was obtained, and the yield in terms of n-butyraldehyde was 84.2%.

Embodiment 3

[0035] (1) Feed according to 10mol n-butyraldehyde, formaldehyde, n-butyraldehyde, and calcium hydroxide are fed according to 3.2:1:0.8, (calcium hydroxide content is 90%) to obtain the reaction liquid for separation, start the screw centrifuge to rotate at 4000 turn / min. The centrifugation is clear mother liquor, and the impurity removal rate is 99%, and the specific operations are the same as in Example 1;

[0036] (2) The centrifuged mother liquor enters the concentration tower for evaporation, and calcium formate is separated during the concentration process, and the trihydric solution is subjected to rectification in the light component separation tower, and finally trimethylolpropane is obtained by distillation in the trihydric separation tower. 2.053 kg of trimethylolpropane with a mass content of 99.5% was obtained, and the yield in terms of n-butyraldehyde was 82.2%.

[0037] Compared with the plate filter press separation method in Examples 1-3, the settling process...

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Abstract

The invention discloses a process for preparing trimethylolpropane by adopting a centrifugal filtering calcium method. The preparation process is characterized by comprising the following steps of: condensing and performing a formic acid neutralization reaction by taking n-butyl aldehyde and formaldehyde as raw materials and taking technical grade calcium hydroxide as a basic catalyst to obtain acrude trimethylolpropane reaction liquid which contains di-trimethylolpropane and calcium formate serving as side products; and separating solid phase residues from the reaction liquid in a horizontal spiral centrifugal filtering way, concentrating, recovering, refining trimethylolpropane and tableting. Compared with a plate type filter press separating method, the process has the advantage: a settling process before separating and an extracting process after separating are reduced. The arrangement of a settling tank is saved, the floor area of the entire process is reduced, and over two hours of settling time is saved; the generation of a large amount of washing sewage in a production process is avoided; and due to the reduction in extraction, the consumption of an extracting agent is saved, and the production efficiency is increased.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a process for preparing trimethylolpropane using a centrifugal filter type calcium method, in particular to a centrifugal filter using a horizontal spiral unloading method in the filtration process of a calcium method trimethylolpropane reaction liquid. A new process that replaces the original plate filter press with the filtration method. Background technique [0002] In industry, TMP mainly uses n-butyraldehyde and formaldehyde as the main raw materials, and undergoes condensation reaction under the action of a basic catalyst to produce the intermediate dimethylol butyraldehyde, which is further reacted with formaldehyde to generate trimethylolpropane. [0003] At present, the production process of trimethylolpropane in China is divided into sodium method and calcium method, that is, sodium hydroxide or calcium hydroxide are used as raw materials. The calcium process h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/22C07C29/76C07C31/04C07C51/42C07C53/06
Inventor 董进军郭勇潘孝明刘仰明余璐宋生权吕海平
Owner 江西高信前沿科技有限公司
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