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Composite carrier heteropolyacid catalyst and method for synthesizing epoxysuccinic acid by using same

A synthesis method and technology of heteropolyacids, which are applied in catalyst activation/preparation, chemical elements of heterogeneous catalysts, molecular sieve catalysts, etc., can solve the problems of low utilization rate, low catalytic efficiency and high heavy metal content

Active Publication Date: 2021-03-19
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of high heavy metal content, low catalytic efficiency and low utilization rate of the catalyst for synthesizing epoxysuccinic acid existing in the prior art, the present invention provides a hybrid Polyacid catalyst and method for synthesizing epoxysuccinic acid using the catalyst

Method used

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  • Composite carrier heteropolyacid catalyst and method for synthesizing epoxysuccinic acid by using same
  • Composite carrier heteropolyacid catalyst and method for synthesizing epoxysuccinic acid by using same
  • Composite carrier heteropolyacid catalyst and method for synthesizing epoxysuccinic acid by using same

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Synthesis of phosphomolybdenum heteropoly acid: 96.4g sodium molybdate (Na 2 MoO 4 2H 2 O, M=241), 11.94g disodium hydrogen phosphate (Na 2 HPO 4 12H 2O) and 620mL of distilled water were added to a clean three-necked glass reactor, and the stirring was started and the temperature was raised until the system boiled, and kept in a boiling state for 50 minutes, and the pH of the system was adjusted to 1.5-1.8 with hydrochloric acid with a concentration of 30% by mass percentage, and continued heating and reflux for 2.5 hour, cooled to room temperature and quickly poured the reaction solution into ice water, the mixed system was separated by standing, extracted with ether, and the oil layer was recrystallized by distilled water to obtain light yellow crystals to obtain the phosphomolybdenum heteropolyacid catalyst H 3 PMo 12 o 40 41.64g;

[0032] (2) Composite carrier heteropolyacid catalyst TS-41 / H 3 PMo 12 o 40 Preparation: Weigh 4.57g of the phosphomolybde...

Embodiment 2

[0035] (1) Synthesis of phosphotungstate heteropoly salt catalyst: accurately weighed 16.5g of sodium tungstate (Na 2 WO 4 2H 2 O, M=330), 0.40g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 Add 80mL of distilled water into a clean three-necked glass reactor, start stirring and heat up until completely dissolved, adjust the pH of the system to 6~7 with hydrochloric acid with a concentration of 30% by mass, continue to keep warm for 2~3 hours, cool to 0°C and Refrigerate overnight in the refrigerator, and the yellow-white needle-like crystal obtained by cold filtration is the ammonium phosphotungstic heteropolyacid catalyst (NH 4 ) 3 PW 12 o 40 ·3H 2 O 10.68g;

[0036] (2) Composite supported heteropolyacid catalyst (NH 4 ) 3 PW 12 o 40 Preparation: Weigh 1.83g of phosphotungstic heteropolyacid ammonium salt synthesized in step (1) and dissolve it in 3g of deionized water; at the same time, measure 20mL of butyl titanate and mix it with 62mL of isopropanol solutio...

Embodiment 3

[0039] The composite loaded heteropolyacid catalyst that utilizes embodiment 1 dry recovery to carry out the catalytic synthesis of epoxysuccinic acid:

[0040] Accurately weigh 196g of the reaction material maleic anhydride, 100g of sodium hydroxide aqueous solution with a mass percentage concentration of 32%, and 150g of deionized water, and add them to a clean three-port glass reactor in sequence; start stirring and heat up to 55~60°C, When the system is in a homogeneous liquid state, add 9.8g of the composite supported heteropolyacid catalyst TS-41 / H recovered in Example 1 3 PMo 12 o 40 And raise the temperature to 70°C, turn on the dripping device connected to the reaction kettle, and drop 167g of hydrogen peroxide aqueous solution with a mass percentage concentration of 45% within 1.5 hours, and keep it at 70±2°C for 2 hours. Cool down, filter, and discharge to obtain 601 g of a light yellow epoxysuccinic acid aqueous solution, and 9.47 g of the catalyst was recovered...

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Abstract

The invention discloses a composite carrier heteropolyacid catalyst and a method for synthesizing epoxysuccinic acid by using the same. The composite carrier heteropolyacid catalyst is composed of heteropolyacid and a carrier; the structural formula of the heteropolyacid is M3PX12O40.nH2O, wherein M is one of lithium, sodium, potassium ions and ammonium ions, X is tungsten and / or molybdenum, n is0-12; the carrier is one of titanium dioxide, silicon dioxide, a TS type titanium silicalite molecular sieve, aluminum oxide and activated carbon. The method for synthesizing epoxysuccinic acid by using the composite carrier heteropolyacid catalyst comprises the following steps of: mixing maleic anhydride, liquid caustic soda and water, stirring the mixture, heating the mixture to 55-60 DEG C; adding the heteropoly acid catalyst, continuously heating to 70 + / -5 DEG C; and dropwise adding a hydrogen peroxide solution, carrying out heat preservation reaction, cooling, and filtering to obtain theepoxysuccinic acid. The catalyst provided by the invention has high catalytic activity and enhanced surface activity after being immobilized and stronger adsorption capacity, improves the catalytic efficiency of epoxidation and the utilization rate of hydrogen peroxide, and is easy to recover; and the content of W and Mo heavy metal elements in the product is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a composite carrier heteropolyacid catalyst and a method for synthesizing epoxysuccinic acid using the catalyst. Background technique [0002] Epoxysuccinic acid is a good cross-linking agent and can be used as a raw material for plasticizers, surfactants and water treatment agents. The synthesis of epoxysuccinic acid usually adopts the direct catalyzed epoxidation of maleic anhydride. In the late 1950s, George&Paul discovered that in Na 2 WO 4 Under the action of catalysis, maleic acid can be oxidized by hydrogen peroxide to generate epoxysuccinic acid; Hosoi et al. also made a systematic study on the synthesis reaction conditions of epoxysuccinic acid earlier. Domestic patent CN101538362B discloses a maleic anhydride epoxidation synthesis method using sodium tungstate as a catalyst; the patent whose authorization announcement number is CN128679...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J27/188B01J29/89B01J37/10B01J37/03C07D303/48C07D301/12
CPCB01J27/19B01J27/188B01J29/89B01J23/002B01J37/10B01J37/036C07D303/48C07D301/12B01J2523/00B01J2523/47B01J2523/51B01J2523/69Y02P20/584
Inventor 王燕平程终发刘全华申义驰
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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