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Process method for preparing succinic acid glycol ester

A technology of diol succinate and a process method, applied in the field of preparing diol succinate, can solve the problems of infeasible industrial production, violation of chemical thermodynamic principles, impossible to realize and maintain, etc., to reduce energy consumption, The effect of improving the total yield and improving the yield

Inactive Publication Date: 2021-08-03
宁波窦氏化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the "first step of maleic anhydride and methanol pre-esterification in a fixed bed at a temperature of 60-90°C and a pressure of 0.2-0.8Mpa" described in the patent claims is impossible to realize and maintain
(3) According to several brands of acid resins used in the examples of this patent, except for DNW-II in Example 3, none of them can withstand temperatures above 100°C for a long time
[0007] Therefore can determine patent CN102070448B, its patent description uses acidic resin as catalyst fixed bed to carry out pre-esterification by maleic anhydride and methanol, then reaction rectification produces dimethyl maleate, the technology of selective hydrogenation of DMM is to violate basic The principle of chemical thermodynamics is even more unfeasible in actual industrial production.

Method used

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  • Process method for preparing succinic acid glycol ester
  • Process method for preparing succinic acid glycol ester
  • Process method for preparing succinic acid glycol ester

Examples

Experimental program
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Effect test

Embodiment 1

[0048] According to the method provided by the applicant of this patent in the original application "A kind of process for preparing diol maleate" (application number is 202110180196.7), using maleic anhydride and methanol as raw materials, synthesize 1500g of dimethyl maleate Ester DMM is the main component of crude DMM-1, and its composition is shown in Table 1.

[0049] Table 1: Composition (wt%) of crude DMM-1

[0050]

[0051] Selective hydrogenation of crude DMM-1 was carried out on a self-made fixed bed with a catalyst of 0.3% Pd / Al 2 o 3 The supported catalyst, the carrier active Al 2 o 3 Modified with 0.3% alkali metal K; the loading amount is 6.0g, and it is filled in an isothermal reaction tube reactor using Φ12.7X1.6 (SS316). The temperature is measured by a sleeve-type thermocouple inside and a feedback resistor is used outside Furnace heating and temperature control. The liquid crude DMM-1 is fed by the Yilite P230II high-pressure liquid metering pump, an...

Embodiment 2

[0056] Also according to the method of Example 1, maleic anhydride and methanol were used as raw materials to synthesize 4500 g of crude DMM-2 with dimethyl maleate DMM as the main component, and its composition is shown in Table 3.

[0057] Table 3: Composition (wt%) of crude DMM-2

[0058]

[0059] In this example, the reaction device and catalyst loading for selective hydrogenation of crude DMM-2 are the same as in Example 1. In the reaction conditions, the molar ratio of crude DMM-2 to hydrogen is 1:20, the pressure is 3.1MPa, and the crude DMM-2 The mass space velocity of 2 is 2.0h -1 . When the reaction temperature reaches a steady state at 220° C., the conversion rate of DMM in the reaction is 99.75%, and the selectivity of DMS is 99.87%. The composition of the reaction product is shown in Table 4 Composition-2. When the reaction temperature reaches a steady state at 240° C., the conversion rate of DMM in the reaction is 100%, and the selectivity of DMS is 99.80%. ...

Embodiment 3

[0064] The reaction raw material selected in this embodiment is the thick DMM-2 used in embodiment 2, the reaction device of selective hydrogenation and the catalyst loading are the same as in Example 1, and the mol ratio of thick DMM-2 and hydrogen in the reaction conditions is 1:20, the pressure is 3.1MPa. When the mass space velocity of crude DMM-2 is 3.0h -1 When the reaction temperature reaches a steady state at 240° C., the conversion rate of DMM in the reaction is 100%, and the selectivity of DMS is 100.47%. The composition of the reaction product is shown in Table 5 Composition-4. When the mass space velocity of crude DMM-2 is 4.0h -1 When the reaction temperature reaches a steady state at 250° C., the conversion rate of DMM in the reaction is 100%, and the selectivity of DMS is 99.81%. The composition of the reaction product is shown in Table 5 Composition-5. When the mass space velocity of crude DMM-2 is 6.0h -1 When the reaction temperature reaches a steady state...

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Abstract

The invention discloses a process method for preparing succinic acid glycol ester, which is characterized by comprising the following steps of: (1) mixing crude maleic acid glycol ester with a proper amount of circulating hydrogen and supplementary new hydrogen, preheating to a certain temperature, feeding the mixture into a fixed bed filled with a catalyst, and carrying out hydrogenation reaction to generate a mixture mainly comprising corresponding succinic acid glycol ester; (2) preheating the raw materials, namely, crude maleic acid glycol ester and hydrogen, by a reaction product and residual hydrogen, generating steam through a steam pocket to realize waste heat utilization, then cooling to below 35 DEG C, feeding the mixture into a gas-liquid separator, and separating out a liquid mixture mainly comprising succinic acid glycol ester and hydrogen; and (3) carrying out double-tower rectification on the liquid mixture mainly comprising succinic acid glycol ester to realize light component removal and heavy component removal to obtain the succinic acid glycol ester with the purity of more than 99.5%. Compared with the prior art, the process method for preparing succinic acid glycol ester is simple in technological process, low in energy consumption and high in product yield.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a process for preparing diol succinate. Background technique [0002] The most common diol succinates are Dimethyl Succinate (DMS) and Diethyl Succinate (DES). Dimethyl succinate, also known as dimethyl succinate, has a chemical formula of C 6 h 10 o 4 , molecular weight 146.14, colorless to light yellow liquid, slightly soluble in water (1%), soluble in ethanol, melting point 16-19°C, boiling point 196°C. Dimethyl succinate is widely used as an environmentally friendly high-boiling solvent because of its non-toxicity and degradability. Dimethyl succinate is also a high value-added fine chemical product, mainly used in the production of quinacridone pigment intermediate dimethyl succinate (DMSS), synthetic light stabilizer 622; or directly Used as a synthetic surfactant, pharmaceutical intermediate, fungicide, etc. Diethyl succinate is mainly used as a plasticize...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/303C07C67/54C07C69/40
CPCC07C67/303C07C67/54C07C69/40Y02P20/10
Inventor 窦和瑞
Owner 宁波窦氏化学科技有限公司
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