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Preparation method of trimethylolethane

A technology of trimethylolethane and methylolpropionaldehyde, which is applied in the field of continuous catalytic hydrogenation of 2,2-dimethylolpropionaldehyde to prepare trimethylolethane, and can solve the effective utilization rate of formaldehyde Low, high formate content, to achieve the effect of reduced formaldehyde consumption, high atomic economy and low production cost

Active Publication Date: 2016-06-15
JIANGSU QINGQUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the present invention is to solve the technical problems of low effective utilization rate of formaldehyde and high formate content in the existing trimethylolethane production technology, and provide an environmentally friendly and high-yield trimethylolethane production method

Method used

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  • Preparation method of trimethylolethane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1) take by weighing 187 grams of copper nitrate, 297g of zinc nitrate hexahydrate, 750g of aluminum nitrate nonahydrate, 64.4g of zirconium oxychloride, 148g of magnesium nitrate and mix and add water to make 5000 milliliters of solutions into the reactor with stirring and heating function, Add 500g of 30% mass fraction of H 2 O 2 Solution, slowly add 25wt% sodium carbonate aqueous solution to the reaction kettle, react at 30 ° C, the pH value is required to be between 9-10 during the reaction, and age at 60-80 ° C for 4-12 hours after the reaction is completed to obtain the corresponding solution. suspensions of mixtures;

[0042] 2) The suspension is centrifuged to obtain solid-liquid two-phase, the solid phase is washed with deionized water, dried at 120 ° C, drying time is 24 hours, calcined at 550-650 ° C for 12 hours, and granulated;

[0043] 3) Using the particles obtained in step 2 as a carrier, vacuum equal volume impregnation of RuCl 3 solution, the loading...

Embodiment 2

[0045] 1) take by weighing 187 grams of copper nitrate, 297g of zinc nitrate hexahydrate, 750g of aluminum nitrate nonahydrate, 64.4g of zirconium oxychloride, 148g of magnesium nitrate and mix and add water to make 5000 milliliters of solutions into the reactor with stirring and heating function, Then add 1000g of 30% mass fraction of H 2 O 2 Solution, slowly add 25wt% sodium carbonate aqueous solution to the reaction kettle, react at 30 ° C, the pH value is required to be between 9-10 during the reaction, and age at 60-80 ° C for 4-12 hours after the reaction is completed to obtain the corresponding solution. suspensions of mixtures;

[0046] 2) The suspension is centrifuged to obtain solid-liquid two-phase, the solid phase is washed with deionized water, dried at 100 ° C, drying time is 36 hours, calcined at 550-650 ° C for 12 hours, and granulated;

[0047] 3) Using the particles obtained in step 2 as a carrier, vacuum equal volume impregnation of RuCl 3 solution, the l...

Embodiment 3

[0049] 1) take by weighing 281 grams of copper nitrate, 297g zinc nitrate hexahydrate, 625g aluminum nitrate nonahydrate, 64.4g zirconium oxychloride, 148g magnesium nitrate and mix and add water to make 5000 milliliters of solutions into the reactor with stirring heating function, Then add 1000g of 30% mass fraction of H 2 O 2 solution, slowly add 25wt% sodium hydroxide aqueous solution to the reaction kettle, react at 30 ° C, the pH value is required to be between 9-10 during the reaction process, and age at 60-80 ° C for 4-12 hours after the reaction, to obtain suspensions of the corresponding mixtures;

[0050] 2) The suspension is centrifuged to obtain solid-liquid two-phase, the solid phase is washed with deionized water, dried at 90°C, the drying time is 48 hours, calcined at 550-650°C for 12 hours, and granulated;

[0051] 3) Using the particles obtained in step 2 as a carrier, vacuum equal volume impregnation of RuCl 3 solution, the loading amount is 1.0%, and calc...

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Abstract

The invention discloses a preparation method of trimethylolethane. The method comprises the following steps: carrying out aldol condensation reaction on propanal and formalin to form a 2,2-dihydroxymethylpropanal-containing solution, and carrying out hydrogenation reaction on the 2,2-dihydroxymethylpropanal-containing solution and hydrogen gas under the action of a hydrogenation catalyst to obtain a solution containing the product trimethylolethane, wherein the 2,2-dihydroxymethylpropanal-containing solution contains 0.5-3 wt% of 2-aldomethyl-2-hydroxymethylpropylmethyl ether. Compared with the traditional technique for preparing trimethylolethane by aldol condensation and Cannizzaro disproportionation reaction, the method disclosed by the invention has the advantages of less wastewater, no coproduct formate and the like, has the characteristics of high conversion rate for the coproduct trimethylolethane acetals in the condensation step in the trimethylolethane hydrogenolysis treatment process, simple process and the like, and can obviously enhance the trimethylolethane yield.

Description

technical field [0001] The invention relates to a preparation method of trimethylolethane, that is, a preparation method of continuously catalyzing the hydrogenation of 2,2-dimethylolpropionaldehyde to prepare trimethylolethane. Background technique [0002] Trimethylolethane (TME) is a unique and multifunctional neopentane structure polyol with three highly reactive hydroxyl groups. Applications include the production of powder coating resins, high solids resins, alkyd resins, polyesters and reducible resins. TME can also be used in titanium dioxide pigments, silicone-modified polyester resins, polyurethanes, epoxy resins, synthetic lubricants, plasticizers, inks, photosensitive chemicals, and adhesives. The neopentane structure provides excellent stability, improved resistance to heat, light, hydrolysis and oxidation; and outstanding weatherability, gloss and chemical resistance. [0003] At present, trimethylolethane is mainly prepared by disproportionation method in in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/141C07C31/22C07C45/75C07C47/19B01J23/89
CPCB01J23/002B01J23/8953B01J2523/00C07C29/141C07C45/75B01J2523/17B01J2523/22B01J2523/27B01J2523/31B01J2523/48B01J2523/305C07C31/22C07C47/19
Inventor 陈伟刚潘红李显明徐卫军胡伟军左学顺
Owner JIANGSU QINGQUAN CHEM CO LTD
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