Method for preparing trimethylolethane through continuous condensation hydrogenation method

A trimethylolethane, condensation hydrogenation technology, applied in the preparation of carbon-based compounds, hydroxyl compounds, organic compounds, etc., can solve the problem that formate cannot be processed, the calcium method consumes more formaldehyde, and the process is complicated, etc. problems, to achieve the effect of high hydrogenation equipment and technical requirements, low production cost, and short process

Inactive Publication Date: 2017-01-04
湖北泰元新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to provide a method for preparing trimethylolethane (TME) by continuous condensation and hydrogenation, w

Method used

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  • Method for preparing trimethylolethane through continuous condensation hydrogenation method
  • Method for preparing trimethylolethane through continuous condensation hydrogenation method
  • Method for preparing trimethylolethane through continuous condensation hydrogenation method

Examples

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Embodiment 1

[0072] A method for preparing trimethylolethane by continuous condensation hydrogenation, comprising the following steps:

[0073] 1) Add 2 / 3 of the total volume of water or recover dilute formaldehyde solution in the impinging flow micro-mixing reactor, according to the following ratio; the molar ratio of formaldehyde, propionaldehyde, triethylamine and soft water is 2.5:1:0.6: The ratio of 20 is added to the condensation tank, and the temperature of the condensation tank is controlled at 30-40 ° C. The pH of the condensation liquid will fluctuate due to side reactions. The pH in the condensation tank is controlled at 8.5 to 8.9. The residence time is 8 to 12 hours. Contains 8%-18% 2,2-dimethylolpropanal, 1.5%-3% unreacted formaldehyde, 0.5%-1.5% alkali, 1%-3% mono-bis acetals and lipids compound, 75%-85% water;

[0074] 2) Remove unreacted excess formaldehyde, organic base and water by distillation under reduced pressure from the condensation liquid prepared in step 1), and...

Embodiment 2

[0084] A method for preparing trimethylolethane by continuous condensation hydrogenation, comprising the following steps:

[0085] 1) Add 2 / 3 of the total volume of water or recover dilute formaldehyde aqueous solution as bottom water in the impinging flow micro-mixing reactor, according to the following ratio; the molar ratio of formaldehyde, propionaldehyde, ammonia water and soft water is 2.5:1:0.6 : 20 ratio into the condensation tank, the temperature of the condensation tank is controlled at 30-40 ° C, the pH of the condensation liquid will fluctuate due to side reactions, the pH in the condensation tank is controlled at 8.5 to 11, and the residence time is 8 to 12 hours. condensation liquid;

[0086] 2) The condensed liquid prepared by step 1) adopts the conditions of Example 1 to carry out underpressure distillation, and the concentrated liquid obtained contains a large amount of white solids, and the gas chromatogram ( image 3 ) analyzed that the white solid was urot...

Embodiment 3

[0088] In the four-necked flask, add 300ml of soft water, add 8g of aluminum magnesium hydrotalcite as a condensation catalyst, and charge 230ml of formaldehyde (37%) and 90ml of propionaldehyde (99.5%) into the pear-shaped separating funnel respectively. Allow stirring to fully disperse the catalyst in soft water, then slowly add formaldehyde and propionaldehyde dropwise, place the flask in a constant temperature water bath, and keep the temperature in the flask at about 35°C. Add propionaldehyde and formaldehyde dropwise in three to six hours, continue stirring after the dropwise addition, and add propionaldehyde and formaldehyde from the beginning to the end of a total of 10 hours. The above-mentioned reaction solution was placed in a rotary evaporator and evaporated under negative pressure to obtain a concentrated solution for chromatographic analysis. The results are shown in Figure 4 . Depend on Figure 4 It can be seen. . . . Hydrotalcite has a good catalytic eff...

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Abstract

The invention relates to a method for preparing trimethylolethane through a continuous condensation hydrogenation method. According to the method, a condensation reaction still for achieving a continuous hydroxy aldehyde addition reaction of an impinging stream reactor, a gas-liquid-solid three-phase drip bed hydrogenation reactor and a bubbling type fluidized bed hydrogenation reactor are involved, and the two hydrogenation reactors are operated in series and contain a novel nickel hydrogenation catalyst and a main ingredient copper-chrome-aluminum-zinc catalyst respectively. It is guaranteed that formaldehyde and propionaldehyde stably generate a 2,2-dihydroxy methyl propyl aldehyde intermediate under organic weak alkali through the continuous impact steam aldol condensation reactor, generated byproducts are reduced, two hydrogenation reactions of different structures have the advantages of being high in conversion rate, simple in process, high in product purity, good in high temperature stability and the like, and the final yield of trimethylolethane can reach 95% or above.

Description

technical field [0001] The invention relates to the technical field of Zhundong coal chemical wastewater treatment, in particular to a method for preparing trimethylolethane by continuous condensation hydrogenation. Background technique [0002] In recent years, there have been some domestic literatures on the preparation of polyols by hydrogenation. At present, the production of various hydrogenation catalysts such as aldehydes and esters in China has matured, but no enterprises have started to install and industrialize hydrogenated polyols. The hydrogenation process requires very high equipment. The structure of the equipment has a great influence on the process safety and the selectivity of raw materials. Most of the current patents describe the hydrogenation preparation of polyols, but none of them can solve some industrial problems. They are all just in the experimental stage. [0003] Patent CN104140358 mainly describes the problem of hydrogenolysis of DMB esters in ...

Claims

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Application Information

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IPC IPC(8): C07C29/38C07C31/22C07C45/75C07C45/78C07C45/82C07C47/19
CPCC07C29/38C07C45/75C07C45/78C07C45/82C07C31/22C07C47/19
Inventor 董进军董睿张浩洋甘聂文
Owner 湖北泰元新材料科技有限公司
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