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Process of synthesizing bis (trihydroxy methyl propane)

A technology of ditrimethylolpropane and trimethylolpropane, which is applied in the field of synthesizing ditrimethylolpropane, can solve the problems of low selectivity of reactants, many by-products, difficulties, etc., and achieve easy recovery and recycling, Ease of industrial production and the effect of meeting a large number of needs

Inactive Publication Date: 2007-11-07
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Usually, in the traditional production process of trimethylolpropane, that is, adopting the Connizzaro method, n-butyraldehyde and formaldehyde react in the process of synthesizing TMP under conditions such as basic catalysts, a small amount of by-product Di-TMP is generated, and then Extract the Di-TMP product from the heavy raffinate of TMP by solvent recrystallization again, the ditrimethylolpropane yield that this process obtains is very low (about 2%~6%), and many patents carry out the above-mentioned method According to reports, such as: US3097245, EP1491521A1, etc.; in addition, on the basis of the traditional production process of TMP, by adjusting the process parameters, the output of the by-product Di-TMP can be increased by 2 to 3 times compared with the traditional process, but Di- The yield of TMP is still low (<20%), and the amount of other by-products becomes larger, such as: CN200610086255.X; US3673226 In the presence of an acidic catalyst, TMP is dehydrated to prepare Di-TMP, and this method has the selectivity of synthesizing Di-TMP Lower (<35%) and lower yield (<15%) defects, because the three methylol groups contained in TMP are all easy to dehydrate and condense under acidic conditions, resulting in a lot of by-products generated by the reaction, and the production cost is high
[0004] The above-mentioned process has the disadvantages of low reactant selectivity, low product yield, and high product cost, and the reaction is difficult to control, side reactions are prone to occur, and the by-product components are complex and high in content. High-purity Di -TMP is also more difficult

Method used

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  • Process of synthesizing bis (trihydroxy methyl propane)
  • Process of synthesizing bis (trihydroxy methyl propane)
  • Process of synthesizing bis (trihydroxy methyl propane)

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) In a four-necked flask equipped with stirring, a thermometer, a dropping funnel and a condenser, first add 144g of 50wt% n-butyraldehyde solution accurately measured, start stirring and be warming up to 50°C, and then stir within 1 hour to 121.2g of triethylamine and 110g of 30wt% formaldehyde solution were dropped simultaneously in the container for reaction, and the reaction was continued for 1.5 hours after the addition was completed, and then the reaction solution was cooled to room temperature; then,

[0027] (2) Add 737g of TMP to the reaction solution obtained in (1) under stirring, and stir to raise the temperature to 90°C, and react for 3h, then cool the reaction solution to room temperature; then,

[0028] (3) Heating the reactants to 80° C. under stirring, and then continuously adding 250 g of 30 wt % formaldehyde solution to the reaction solution obtained in (2) within 1 hour for reaction. After the addition, continue to stir and react for 2 hours to obta...

Embodiment 2

[0031] (1) In the four-neck flask equipped with stirring, thermometer, dropping funnel and condenser tube, first add 144g of 50wt% n-butyraldehyde solution accurately measured, start stirring and heat up to 90°C, then stir for 1.5 hours 120g of ethylenediamine and 110g of 30wt% formaldehyde solution were dropped into the container simultaneously for reaction, and then reacted for 1 hour after the addition, and then the reaction solution was cooled to room temperature; then,

[0032] (2) Add 1072 g of TMP to the reaction solution obtained in (1) under stirring, and stir to raise the temperature to 110° C., carry out the reaction for 2 hours, and then cool the reaction solution to room temperature; then,

[0033] (3) Heating the reactant to 90° C. under stirring, then continuously adding 250 g of 30 wt % formaldehyde solution to the reaction solution obtained in (2) within 1.5 hours for reaction, and continuing to stir for 2 hours after the addition to obtain bis Trimethylolprop...

Embodiment 3

[0036] (1) In the four-neck flask equipped with stirring, thermometer, dropping funnel and condenser tube, first add 144g of 50wt% n-butyraldehyde solution accurately measured, start stirring and be warming up to 30 ℃, under stirring again within 0.5 hours to 60g of 30wt% sodium hydroxide solution and 100g of 30wt% formaldehyde solution were added dropwise in the container to react, and then reacted for another 3 hours after feeding, and then the reaction solution was cooled to room temperature; then,

[0037] (2) Add 134 g of TMP to the reaction solution obtained in (1) under stirring, and stir to raise the temperature to 80° C., carry out the reaction for 1 h, and then cool the reaction solution to room temperature; then,

[0038] (3) Heating the reactant to 50° C. under stirring, then continuously adding 200 g of 30 wt % formaldehyde solution to the reaction solution obtained in (2) within 0.5 hours for reaction, and then stirring and reacting for 4 hours after the addition,...

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Abstract

The present invention discloses process of synthesizing bis(trihydroxymetyl propane) by means of reaction of formaldehyde, n-butyl aldehyde and trihydroxymetyl propane. The synthesis of bis(trihydroxymetyl propane) includes the following steps: the aldol condensation reaction and dewatering reaction of n-butyl aldehyde and formaldehyde in the presence of alkaline catalyst to produce 2-ethyl acrylaldehyde, the subsequent addition reaction of 2-ethyl acrylaldehyde with added trihydroxymetyl propane in alkaline condition to produce intermediate product 2-ethyl-3-(beta, beta-demethylol-butoxy)-1-propanal, and adding formaldehyde into the intermediate product to produce aldol condensation reaction and crossed disproportionation reaction to produce bis(trihydroxymetyl propane). The process has high selectivity and high yield of bis(trihydroxymetyl propane) and other features, and is easy application in industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing ditrimethylolpropane by taking formaldehyde, n-butyraldehyde and trimethylolpropane as raw materials and reacting in the presence of a basic catalyst. Background technique [0002] Ditrimethylolpropane (hereinafter referred to as Di-TMP) is a solid polyol containing four primary hydroxyl groups. As a high value-added deep-processing product of trimethylolpropane (hereinafter referred to as TMP), it has more superior properties It is widely used in the preparation of polyacrylates, polyether glycols, polyurethanes, alkyd resins, synthetic lubricants, plasticizers, surfactants, etc. The application of Di-TMP in aviation lubricating oil has more unique properties, which can ensure excellent lubricating performance under low temperature and high temperature conditions. [0003] Usually, in the traditional production process of trimethylolpropane, that is, adopting the Connizzaro method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C41/18C07C41/01
Inventor 刘乃青徐鸿王硕
Owner CNPC JILIN CHEM GROUP CORP
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