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Preparation method of trimethylolpropane

A technology for trimethylolpropane and trimethylolpropane acetal, which is applied in the field of preparation of trimethylolpropane, can solve the problems of consumption of alcohol raw materials, by-produced sodium formate, low yield and the like, and achieves considerable economic benefits , the effect of high conversion rate and simple process

Active Publication Date: 2013-09-04
WANHUA CHEM GRP CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The preparation method of trimethylolpropane is divided into hydrogenation method and disproportionation method, wherein the disproportionation method is a relatively traditional process, but there are problems such as high formaldehyde consumption, by-product sodium formate, serious pollution, and low yield; currently more advanced production The process is a hydrogenation process. Only BASF in Germany has an industrialized device in the world. The hydrogenation process is
[0010] In summary, the current method for processing the trimethylolpropane formal contained in the intermediate product DMB prepared by the condensation reaction of formaldehyde and n-butyraldehyde is prone to produce a large amount of acid waste water, and consumes alcohol raw materials, and usually belongs to batch process, and There is no continuous production process that can directly remove the by-product trimethylolpropane acetals in the process of preparing TMP

Method used

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  • Preparation method of trimethylolpropane
  • Preparation method of trimethylolpropane
  • Preparation method of trimethylolpropane

Examples

Experimental program
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Effect test

Embodiment 1

[0051] 175.78 grams of copper nitrate (Cu(NO 3 ) 2 ), 285.57 grams of scandium nitrate (Sc(NO3)3), 428.94 grams of aluminum nitrate (Al(NO3) 3 ) 3 ), 56.06 grams of cadmium nitrate (Cd (NO 3 ) 2 ), 9.02 grams of silver nitrate (AgNO 3 ) after mixing, add water to make 5000 ml of solution and put it into a reactor with stirring and heating function, slowly add 25wt% sodium carbonate aqueous solution into the reactor, control the reaction temperature at 80-90°C, and the reaction process requires pH=9- 10. After keeping the reaction for 1 hour, age at 60°C for 2 hours to obtain a suspension, centrifuge the suspension, wash the solid phase with deionized water until the sodium content is less than 0.25wt%, and dry at 90°C for 48 hours After that, it was fired at 500° C. for 2 hours and pressed into tablets to form the first hydrogenation catalyst 1-1. The total weight of the catalyst was 300 grams.

Embodiment 2

[0053] 268.76 grams of copper nitrate, 222.77 grams of scandium nitrate, 377.76 grams of aluminum nitrate, 78.12 grams of molybdenum nitrate (Mo(NO 3 ) 6 ), 5.28 grams of silver nitrate, mixed with water and made into 5000 milliliters of solution, put it into a reaction kettle with stirring and heating function, slowly add 25wt% sodium hydroxide aqueous solution into the reaction kettle, control the reaction temperature at 80-90°C, and react The process requires PH=9-10, the reaction is maintained for 1.5 hours and aged at 80°C for 1 hour to obtain a suspension, the suspension is centrifuged, the solid phase is washed with deionized water until the sodium content is less than 0.25wt%, and Dry at 120° C. for 24 hours, then burn at 600° C. for 1.5 hours, and then press into tablets to obtain the first hydrogenation catalyst 1-2. The total weight of the catalyst is 300 grams.

Embodiment 3

[0055] After mixing 406.50 grams of copper nitrate, 157.46 grams of scandium nitrate, 257.36 grams of aluminum nitrate, 29.99 grams of cadmium nitrate, and 0.66 grams of silver nitrate, add water to make 5000 milliliters of solution into a reaction kettle with a stirring and heating function, and add 25 wt% potassium carbonate Slowly add the aqueous solution into the reaction kettle, control the reaction temperature at 80-90°C, the reaction process requires pH=9-10, keep the reaction for 2 hours, then age at 70°C for 1.5 hours to obtain a suspension, and centrifuge the suspension , the solid phase was washed with deionized water until the potassium content was lower than 0.25wt%, and dried at 100°C for 30 hours, then burned at 650°C for 1 hour, and then pressed into tablets to obtain the first hydrogenation catalyst 1-3. Weighs 300 grams.

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Abstract

The invention relates to a preparation method of trimethylolpropane. The preparation method adopts two sections of hydrogenation reactors connected in series, wherein the catalyst of the first reactor comprises the following components (based on the total weight of the catalyst) in percentage by weight: 23%-60% of CuO, 15%-30% of Sc2O3, 20%-35% of Al2O3, one or two or three of 1%-10% of CdO, MoO3 and WO3, and 0.1%-2% of Ag2O. The catalyst filled in the second reactor comprises the following components in percentage by weight: 15%-60% of CuO, 10%-30% of B2O3, 20%-40% of Fe2O3, one or two or three of 1%-15% of ZrO2, V2O5 and Nb2O5, and.01%-2% of CoO. The preparation method of the trimethylolpropane disclosed by the invention has a high conversion rate for a by-product trihydroxymethyl propane acetal compound in a condensation process of decomposing trihydroxymethyl propane by hydrogenation, is simple in process, free of acid waste water and the like, and capable of obviously improving the yield of the trihydroxymethyl propane.

Description

Technical field: [0001] The invention relates to a preparation method of trimethylolpropane. Specifically, the by-product trimethylolpropane acetal compounds produced in the process of preparing trimethylolpropane by optimizing the components of the hydrogenation catalyst through the direct hydrogenation decomposition hydrogenation process, thereby increasing the yield of trimethylolpropane rate method. Background technique: [0002] Trimethylolpropane (TMP) is an important organic chemical intermediate and fine chemical product. Due to its unique chemical structure, trimethylolpropane can improve the firmness, corrosion resistance and sealing performance of the resin, and has good stability for hydrolysis, pyrolysis and oxidation. It is mainly used as alkyd resin, polyurethane resin and high-grade Raw materials for paints / coatings, also used in plasticizers, surfactants, advanced lubricants, synthetic leather and thermal insulation materials. [0003] The preparation met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/22C07C29/141B01J23/89B01J23/847B01J23/75
Inventor 姜庆梅曹善健杨在刚宋锦宏胡兵波于方骁杨凯李小平胡鑫何光文
Owner WANHUA CHEM GRP CO LTD
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