Method for preparing ketal glycerine and/or acetal glycerine

A technology of glycerol aldo and glycerol ketal, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as long reaction time, cumbersome post-processing, and environmental pollution, and achieve high aldehydes /ketone conversion rate, high aldehyde/ketal glycerol yield, and low energy consumption for separation

Active Publication Date: 2020-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Catalyst can choose H 2 SO 4 , HCl and other liquid strong acid catalysts, but this process has disadvantages such as long reaction time and cumbersome post-treatment. At the same time, they participate in the reaction in a homogeneous manner with the reaction liquid, and also have disadvantages such as corrosion of equipment and pollution of the environment.

Method used

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  • Method for preparing ketal glycerine and/or acetal glycerine

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0045] This preparation example prepares Sn-MFI molecular sieve, the specific preparation method is:

[0046] Add tin tetrachloride pentahydrate (SnCl 4 .5H 2 O) Dissolve in water, add this aqueous solution to ethyl orthosilicate (TEOS) and stir, add tetrapropyl ammonium hydroxide (TPAOH, 20% aqueous solution) and water under stirring, and continue stirring for 30 minutes to obtain a chemical composition of 0.03SnO 2 : SiO 2 :0.45TPA:35H 2 The clear liquid of O was then crystallized at 433K for 2 days, then the obtained solid was filtered, washed with distilled water, dried at 393K for 5 hours, and then calcined at 823K for 10 hours to obtain a molecular sieve sample. Among them, the amount of TEOS is 15.31g, the amount of TPAOH is 33.67g, SnCl 4 .5H 2 The amount of O is 0.38g, and the amount of water is 39.64g.

preparation Embodiment 2

[0048] This preparation example refers to "Nemeth L, Moscoso J, Erdman N, et al. Synthesis and characterization of Sn-Beta as a selective oxidation catalyst[J].Studies in Surface Science&Catalysis, 2004,154(04):2626-2631" Methods The Sn-Beta molecular sieve was prepared. The preparation method of the Sn-Beta molecular sieve was as follows:

[0049] Add tin tetrachloride pentahydrate (SnCl 4 .5H 2 O) Dissolve in water, add this aqueous solution to ethyl orthosilicate (TEOS) and stir, add tetraethyl ammonium hydroxide (TEAOH) under stirring, stir until TEOS evaporates to obtain alcohol, add hydrogen fluoride (HF) to the clear liquid , Form a thin layer of paste. Finally, a suspension of dealumination nano Beta seed crystal (20nm) and water was added to obtain a chemical composition of 0.03SnO 2 : SiO 2 : 6TEA: 15H 2 O: 10HF clear liquid, then crystallize at 413K for 10 days, then filter the obtained solid, wash with distilled water, dry at 393K for 5 hours, and then calcined at 823...

preparation Embodiment 3

[0051] This preparation example refers to the literature "Yang X, Wu L, Wang Z, et al. Conversion of dihydroxyacetone to methyl lactate catalyzed by highly active hierarchicalSn-USY at room temperature[J]. Catalysis Science&Technology,2016,6(6):1757- Sn-USY molecular sieve is prepared by the method of 1763". The preparation method of Sn-USY molecular sieve used is:

[0052] The H-USY molecular sieve was mixed with nitric acid, treated at 85°C for 8 hours, the sample was filtered and washed with deionized water, and dried at 120°C for 12 hours to obtain a solid sample. Mix this solid sample with tin tetrachloride pentahydrate (SnCl 4 .5H 2 O) Mix for 1h to obtain a chemical composition of 0.03SnO 2 :100SiO 2 The mixed liquid was dried at 100°C for 12 hours, and finally calcined at 550°C for 3 hours to obtain a molecular sieve sample. Among them, the amount of H-USY is 2.0g, the amount of nitric acid is 50mL, and SnCl 4 .5H 2 The amount of O is 0.6g.

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Abstract

The invention relates to a method for preparing ketal glycerine and/or acetal glycerine. The method comprises the following steps: contacting glycerine and a reaction raw material with a catalyst in areactor, and reacting to obtain a product containing ketal glycerine and/or acetal glycerine, wherein the reaction raw material contains aldehyde and/or ketone, the molar ratio of glycerine to aldehyde and/or ketone is 1:(1-10), the reaction temperature is 30-180 DEG C, the reaction time is 1-10 hours, the catalyst contains a tin-silicon molecular sieve, and the weight ratio of glycerol to the tin-silicon molecular sieve based on dry basis weight is (1-40):1. The method provided by the invention has high aldehyde/ketone conversion rate and high acetal/ketal glycerine selectivity.

Description

Technical field [0001] The present invention relates to a method for preparing ketone glycidol and / or aldehyde glycidol. Background technique [0002] Solketal, also known as 1,2-O-isopropylidene glycerol or isopropylidene glycerol, colorless and transparent liquid, boiling point 82℃, density 1.064, refractive index 1.4383, lightning 90℃, and water, alcohol , Ester and ether aromatic hydrocarbons are mutually soluble. It is an important organic synthesis intermediate, used as a universal solvent, plasticizer, and pharmaceutical excipients (cosolvent, suspending agent). It can be used to synthesize DL-glyceraldehyde, drug carrier dialkyl polyoxyethylene glyceraldehyde, medical adhesive cyanoacrylate 1,2-isopropyl cross-glyceride, and can also be used as a polyhydroxyl protecting group to synthesize high purity The monoglyceride and so on. [0003] Glycerin formal is obtained by the reaction of glycerin and formaldehyde as a solvent for pesticides and pharmaceutical injections. L...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06C07D317/20C07D317/26C07D317/72C07D319/08B01J29/70
CPCC07D319/06C07D317/20C07D317/26C07D317/72C07D319/08B01J29/7049B01J2229/18Y02P20/55
Inventor 刘聿嘉夏长久彭欣欣朱斌林民罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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