Method for preparing trimethylolpropane by adopting hydrogenation method

Abstract

The invention provides a method for preparing trimethylolpropane by adopting a hydrogenation method. The method comprises the following steps: performing aldol condensation reaction between n-butanal and a formaldehyde aqueous solution to form a solution containing 2,2-dimethylolbutyraldehyde; performing hydrogenation reaction on the solution containing 2,2-dimethylolbutyraldehyde and hydrogen under the action of a hydrogenation catalyst to obtain a solution containing a product namely trimethylolpropane, wherein the solution containing 2,2-dimethylolbutyraldehyde contains 0.5-3wt% of 2-aldehydemethyl-2-hydroxymethyl butyl methyl ether, and is used as a basic reference. According to the method provided by the invention, a byproduct namely trimethylolpropane methyl ether type substance, which is generated in the process of preparing trimethylolpropane by adopting the hydrogenation method in which the components of the hydrogenation catalyst are used for performing hydrogenation decomposition directly, is optimized, so that the yield of trimethylolpropane is improved.

Description

technical field

[0001] The invention relates to a preparation method of trimethylolpropane. Specifically, a method for preparing trimethylolpropane by hydrogenating 2,2-dimethylolbutyraldehyde is provided. Background technique

[0002] Trimethylolpropane (TMP) is an important chemical intermediate, which is a commonly used chain extender in the resin industry. It has a low melting point and has three methylol groups in its molecular structure. It can react with organic acids to form monoesters or polyesters, react with aldehydes and ketones to form acetals and ketals, and react with diisocyanates to form carbamates. It is mainly used in the fields of alkyd resin, polyurethane, unsaturated resin, polyester resin, coating, etc. It can also be used in the synthesis of aviation lubricants, printing ink, etc., and can also be used as a textile auxiliary agent and heat stabilizer for polyvinyl chloride resin. This product has good thermal stability, acid resistance, alkali resis...

Examples

Embodiment 1

[0037] 267.3g aluminum nitrate (Al(NO 3 ) 3 ), 150.4 grams of copper nitrate (Cu(NO 3 ) 2 ), 47.4g magnesium nitrate (Mg(NO 3 ) 2 ), 31.9g lanthanum nitrate (La(NO 3 ) 3 ), 3.8g molybdenum nitrate (Mo(NO 3 ) 3 ), 4.4g zirconium nitrate (Zr(NO 3 ) 4 ) after mixing, add water to make 2000 ml of solution and put it into a reaction kettle with stirring and heating function, slowly add 2L of 30wt% sodium carbonate aqueous solution into the reaction kettle, control the reaction temperature at 80° C. for 1 hour, and the reaction process requires pH=9 , aged at 60°C for 2h to obtain a suspension, centrifuged the suspension, washed the solid phase with deionized water until the sodium content was lower than 0.25wt%, dried at 90°C for 48h, added 12.8g of sodium pyrophosphate, and placed Calcined at 600°C for 2 hours, and pressed into tablets to obtain hydrogenation catalyst 1 with a total catalyst weight of 163.1 grams.

Embodiment 2

[0039] 225.5g aluminum nitrate (Al(NO 3 ) 3 ), 228.6g copper nitrate (Cu(NO 3 ) 2 ), 10.5g calcium nitrate (Ca(NO 3 ) 2 ), 42.9g cerium nitrate (Ce(NO 3 ) 3 ), 2.1g molybdenum nitrate (Mo(NO 3 ) 3 ), 7.4g zirconium nitrate (Zr(NO 3 ) 4 ) after mixing, add water to form 2000 ml of solution and put it into a reactor with stirring and heating function, slowly add 2L of 30wt% potassium carbonate aqueous solution into the reactor, control the reaction temperature at 90° C. for 1 hour, and the reaction process requires pH=10 , aged at 60°C for 2h to obtain a suspension, centrifuged the suspension, washed the solid phase with deionized water until the sodium content was lower than 0.25wt%, dried at 100°C for 36h, added 23.4g of sodium pyrophosphate, and placed Calcined at 650° C. for 1 hour, and pressed into pellets to obtain hydrogenation catalyst 2 with a total catalyst weight of 195.9 grams.

Embodiment 3

[0041] 334.1g aluminum nitrate (Al(NO 3 ) 3 ), 135.4g copper nitrate (Cu(NO 3 ) 2 ), 15.2g rubidium nitrate (RbNO 3 ), 15.8g praseodymium nitrate (Pr(NO 3 ) 3 ), 7.5g molybdenum nitrate (Mo(NO 3 ) 3 ), 4.4g zirconium nitrate (Zr(NO 3 ) 4 ) after mixing, add water to make 2000 ml of solution and put it into a reaction kettle with stirring and heating function, slowly add 2L of 30wt% potassium carbonate aqueous solution into the reaction kettle, control the reaction temperature at 85° C. for 1 hour, and the reaction process requires pH=9 , aged at 60°C for 2h to obtain a suspension, centrifuged the suspension, washed the solid phase with deionized water until the sodium content was lower than 0.25wt%, dried at 90°C for 48h, added 6.4g of sodium polyphosphate, and placed Calcined at 550°C for 4 hours, and pressed into pellets to obtain hydrogenation catalyst 3 with a total catalyst weight of 167.0 grams.

technical field

[0001] The invention relates to a preparation method of trimethylolpropane. Specifically, a method for preparing trimethylolpropane by hydrogenating 2,2-dimethylolbutyraldehyde is provided. Background technique

[0002] Trimethylolpropane (TMP) is an important chemical intermediate, which is a commonly used chain extender in the resin industry. It has a low melting point and has three methylol groups in its molecular structure. It can react with organic acids to form monoesters or polyesters, react with aldehydes and ketones to form acetals and ketals, and react with diisocyanates to form carbamates. It is mainly used in the fields of alkyd resin, polyurethane, unsaturated resin, polyester resin, coating, etc. It can also be used in the synthesis of aviation lubricants, printing ink, etc., and can also be used as a textile auxiliary agent and heat stabilizer for polyvinyl chloride resin. This product has good thermal stability, acid resistance, alkali resis...

Examples

Embodiment 1

[0037] 267.3g aluminum nitrate (Al(NO 3 ) 3 ), 150.4 grams of copper nitrate (Cu(NO 3 ) 2 ), 47.4g magnesium nitrate (Mg(NO 3 ) 2 ), 31.9g lanthanum nitrate (La(NO 3 ) 3 ), 3.8g molybdenum nitrate (Mo(NO 3 ) 3 ), 4.4g zirconium nitrate (Zr(NO 3 ) 4 ) after mixing, add water to make 2000 ml of solution and put it into a reaction kettle with stirring and heating function, slowly add 2L of 30wt% sodium carbonate aqueous solution into the reaction kettle, control the reaction temperature at 80° C. for 1 hour, and the reaction process requires pH=9 , aged at 60°C for 2h to obtain a suspension, centrifuged the suspension, washed the solid phase with deionized water until the sodium content was lower than 0.25wt%, dried at 90°C for 48h, added 12.8g of sodium pyrophosphate, and placed Calcined at 600°C for 2 hours, and pressed into tablets to obtain hydrogenation catalyst 1 with a total catalyst weight of 163.1 grams.

Embodiment 2

[0039] 225.5g aluminum nitrate (Al(NO 3 ) 3 ), 228.6g copper nitrate (Cu(NO 3 ) 2 ), 10.5g calcium nitrate (Ca(NO 3 ) 2 ), 42.9g cerium nitrate (Ce(NO 3 ) 3 ), 2.1g molybdenum nitrate (Mo(NO 3 ) 3 ), 7.4g zirconium nitrate (Zr(NO 3 ) 4 ) after mixing, add water to form 2000 ml of solution and put it into a reactor with stirring and heating function, slowly add 2L of 30wt% potassium carbonate aqueous solution into the reactor, control the reaction temperature at 90° C. for 1 hour, and the reaction process requires pH=10 , aged at 60°C for 2h to obtain a suspension, centrifuged the suspension, washed the solid phase with deionized water until the sodium content was lower than 0.25wt%, dried at 100°C for 36h, added 23.4g of sodium pyrophosphate, and placed Calcined at 650° C. for 1 hour, and pressed into pellets to obtain hydrogenation catalyst 2 with a total catalyst weight of 195.9 grams.

Embodiment 3

[0041] 334.1g aluminum nitrate (Al(NO 3 ) 3 ), 135.4g copper nitrate (Cu(NO 3 ) 2 ), 15.2g rubidium nitrate (RbNO 3 ), 15.8g praseodymium nitrate (Pr(NO 3 ) 3 ), 7.5g molybdenum nitrate (Mo(NO 3 ) 3 ), 4.4g zirconium nitrate (Zr(NO 3 ) 4 ) after mixing, add water to make 2000 ml of solution and put it into a reaction kettle with stirring and heating function, slowly add 2L of 30wt% potassium carbonate aqueous solution into the reaction kettle, control the reaction temperature at 85° C. for 1 hour, and the reaction process requires pH=9 , aged at 60°C for 2h to obtain a suspension, centrifuged the suspension, washed the solid phase with deionized water until the sodium content was lower than 0.25wt%, dried at 90°C for 48h, added 6.4g of sodium polyphosphate, and placed Calcined at 550°C for 4 hours, and pressed into pellets to obtain hydrogenation catalyst 3 with a total catalyst weight of 167.0 grams.

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