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Method for preparing trimethylolpropane through hydrogenation with high condensation yield

A technology for preparing trimethylolpropane and hydrogen, applied in the field of hydrogenation synthesis, can solve the problems of increased product cost, many reaction by-products, difficult product separation, etc., so as to avoid device corrosion, reduce device material, and improve economy. Effect

Active Publication Date: 2022-04-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The preparation methods of trimethylolpropane include disproportionation method and hydrogenation method, among which the disproportionation method is a relatively mature production process, and the catalyst mostly uses sodium hydroxide and calcium hydroxide. This method has a high unit consumption of formaldehyde and a large amount of formaldehyde by-product Salt and waste water, the three wastes are difficult to treat; and because the catalyst is highly alkaline, there are many reaction by-products, and it is difficult to separate from the product
[0008] It is proposed in CN 201110186413.X that under the catalysis of triethylamine, a large amount of intermediate by-product 2-ethylacrolein (EA) will be produced in the process of condensation of formaldehyde and butyraldehyde into DMB, which needs to be further separated and further reacted with formaldehyde. Not only the process is complicated, but also requires additional energy consumption for separation, increasing product cost

Method used

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  • Method for preparing trimethylolpropane through hydrogenation with high condensation yield
  • Method for preparing trimethylolpropane through hydrogenation with high condensation yield
  • Method for preparing trimethylolpropane through hydrogenation with high condensation yield

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Experimental program
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Effect test

Embodiment 1

[0059] 37wt% formaldehyde, n-butyraldehyde, 5% catalyst aqueous solution, and water are reacted at 40°C in a molar ratio of formaldehyde, n-butyraldehyde, monosodium ethanolamine phosphate, and water at 40°C, and the reaction pressure The gauge pressure is 0.5MPa, the volume of the reactor is 10L (the effective volume of the liquid is 6L), and the residence time is 2h to obtain the condensation reaction solution 3 (stream 5) containing DMB, in which ethanolamine phosphate monosodium salt and N-ethyl di The molar ratio of ethanolamine is 1:5.

[0060] The condensation reaction solution 3 enters the fixed-bed hydrogenation reactor, and under the catalysis of Johnson Matthey Cu 2912 catalyst, DMB is hydrogenated to generate a hydrogenation reaction solution rich in trimethylolpropane (stream 9). The hydrogenation reaction temperature is 100°C, the reaction pressure is 5MPa gauge pressure, and the space velocity is 0.5mL / cm 2 cat. / h, the hydrogen-to-oil ratio (the molar ratio of ...

Embodiment 2

[0067] 37wt% formaldehyde, n-butyraldehyde, 5% catalyst aqueous solution, and water are reacted at 60°C in a molar ratio of formaldehyde, n-butyraldehyde, monopotassium ethanolamine phosphate, and water at 60°C, and the reaction pressure The gauge pressure is 0.3MPa, the volume of the reactor is 10L (the effective volume of the liquid is 6L), and the residence time is 1h to obtain the condensation reaction solution 4 (stream 5) containing DMB, wherein ethanolamine phosphate monopotassium salt and N-ethyl di The molar ratio of ethanolamine is 1:2.

[0068] The condensation reaction liquid 4 enters the fixed-bed hydrogenation reactor, and under the catalysis of Johnson Matthey Cu 4000T catalyst, DMB is hydrogenated to generate a hydrogenation reaction liquid rich in trimethylolpropane (stream 9). The hydrogenation reaction temperature is 160°C, the reaction pressure is 1MPa gauge pressure, and the space velocity is 5mL / cm 2 cat. / h, hydrogen oil ratio (molar ratio) is 4.

[006...

Embodiment 3

[0076] 50wt% formaldehyde, n-butyraldehyde, 4% catalyst aqueous solution and water are reacted at 50°C in a molar ratio of formaldehyde, n-butyraldehyde, ethanolamine phosphate monosodium salt and water at 2.5:1:0.01:1.781, and the reaction pressure The gauge pressure is 0.1MPa, the volume of the reactor is 10L (the liquid effective volume is 6L), the residence time is 3h, and the condensation reaction solution 5 (stream 5) containing DMB is obtained, wherein ethanolamine phosphate monosodium salt and N-ethyl di The molar ratio of ethanolamine is 1:10.

[0077] The condensation reaction liquid 5 enters the fixed-bed hydrogenation reactor, and under the catalysis of the Cu60 / 35T catalyst, DMB is hydrogenated to generate a hydrogenation reaction liquid rich in trimethylolpropane (stream 9). The hydrogenation reaction temperature is 130°C, the reaction pressure is 2MPa gauge pressure, and the space velocity is 3mL / cm 2 cat. / h, hydrogen oil ratio (molar ratio) is 3.

[0078]The ...

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Abstract

The invention provides a method for preparing trimethylolpropane (TMP) through hydrogenation with high condensation yield. The method comprises the following steps: reacting a high-concentration formaldehyde aqueous solution with n-butyraldehyde under the action of an organic amine catalyst to obtain a condensation reaction solution of 2, 2-dihydroxybutyraldehyde (DMB), and concentrating and directly hydrogenating the condensation reaction solution containing DMB to obtain TMP. By adopting the formaldehyde aqueous solution and controlling the structure and content of the organic amine catalyst, on one hand, disproportionation reaction of formaldehyde can be effectively controlled, equipment materials are reduced, and the formaldehyde utilization rate is increased; on the other hand, generation of intermediate products of 2-hydroxymethyl butyraldehyde (MMB) and 2-ethyl acrolein (EA) can be effectively controlled, and the yield of TMP is increased.

Description

technical field [0001] The invention belongs to the field of hydrogenation synthesis, in particular to a method for preparing trimethylolpropane (TMP) by hydrogenation with high condensation yield. Background technique [0002] Trimethylolpropane (TMP) is an important organic chemical intermediate and fine chemical product. Due to its special molecular structure, it can not only replace glycerin to synthesize alkyd resin, but also synthesize polyols such as neopentyl glycol and pentaerythritol. Commonly used in the production of alkyd resins, it can also be used in the production of surfactants, wetting agents, explosives, plasticizers, glass fiber reinforced plastics, rosin esters, advanced aviation lubricants, fiber processing agents, printing inks and polyurethane foams, and can also be used as Resin chain extender, textile auxiliaries and polyvinyl chloride resin heat stabilizer. With the development of domestic trimethylolpropane enterprises, trimethylolpropane will gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/75C07C47/19C07C45/82C07C29/141C07C31/22B01J31/02
CPCC07C45/75C07C29/141B01J31/0258B01J31/0271B01J31/0237C07C45/82B01J2231/342C07C47/19C07C31/22Y02P20/584
Inventor 吕艳红于海彬马岩龙陈雁玲孙文龙王鹏张昊王加琦管兴龙陈来中
Owner WANHUA CHEM GRP CO LTD
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