Method for preparing ketal glycerine and/or acetal glycerine

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

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.

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  • Method for preparing ketal glycerine and/or acetal glycerine

Examples

Experimental program
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Embodiment approach

[0057] According to the first embodiment, preferably the tin-titanium-silicon molecular sieve is at 460 cm in the FT-IR spectrum -1 、975cm -1 、800cm -1 and 1080cm -1 There is absorption nearby. Preferably, the tin-titanium-silicon molecular sieve has absorption at 200-300 nm in the UV-Vis spectrum, preferably at 200-260 nm.

[0058] According to the first embodiment, preferably the molar ratio of the tin element to the silicon element in the tin-titanium-silicon molecular sieve is 0.05-10:100, more preferably 0.1-5:100, particularly preferably 0.2-2:100. Preferably, the molar ratio of titanium element to silicon element in the tin-titanium-silicon molecular sieve is 0.05-10:100, more preferably 0.1-5:100, particularly preferably 0.5-4:100. Such proportions of tin, titanium and silicon can further optimize the catalytic activity of the tin-titanium-silicon molecular sieve of the present invention.

[0059] According to the first embodiment, it is preferred that the tin-tit...

preparation Embodiment 1

[0104] In this preparation example, a Sn-Ti-MFI-1 molecular sieve is prepared according to the method of Example 1 of the Chinese patent CN 105217645A specification, and the specific preparation method is as follows:

[0105] (1) At 25°C, stirring and contacting tetrapropylammonium hydroxide aqueous solution (concentration: 15% by weight) with tetrabutyl titanate and tin tetrachloride pentahydrate for 30 minutes to obtain a mixture;

[0106] (2) At 60°C, add silicon molecular sieve S-1 to the above mixture and stir for 0.5h to obtain the mixture (during this contact process, add water or not add water as required, if the feeding in step (1) can meet the requirement of water Feeding requirements, there is no need to add water, if it is not met, you can add water when the mixture containing tetrapropylammonium hydroxide, tetrabutyl titanate and tin chloride is stirred and contacted with silicon molecular sieve, or distill off water, and the rest The preparation examples are simi...

preparation Embodiment 2

[0110] This preparation example prepares the Sn-Ti-MFI-2 molecular sieve according to the method of the Chinese patent CN105217645A specification example 2, and the specific preparation method is as follows:

[0111] (1) At 25°C, stirring and contacting tetrapropylammonium hydroxide aqueous solution (concentration: 20% by weight) with tetrabutyl titanate and tin tetrachloride pentahydrate for 30 minutes to obtain a mixture;

[0112] (2) At 25°C, add silicon molecular sieve S-1 to the above mixture and stir for 0.5h to obtain the mixture; wherein, ensure that the molar ratio of each substance is: silicon source (silicon molecular sieve): alkali source template (four Propyl ammonium hydroxide): titanium source (tetrabutyl titanate): tin source (tin tetrachloride): water=100:15:2:0.1:200, wherein the silicon source is SiO 2 In terms of titanium source as TiO 2 Tin source is calculated as tin element;

[0113] (3) Transfer the above mixture into a sealed stainless steel reaction...

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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-titanium-silicon molecular sieve, and the weight ratio of glycerineto the tin-titanium-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 ketal glycerol and / or aldol glycerol. Background technique [0002] Acetone glycerol (solketal), also known as 1,2-O-isopropylidene glycerol or isopropylidene glycerol, is a colorless and transparent liquid with a boiling point of 82°C, a density of 1.064, a refractive index of 1.4383, and a lightning temperature of 90°C. , ester, ether arene miscibility. It is an important intermediate in organic synthesis, used as a universal solvent, plasticizer, and pharmaceutical excipient (cosolvent, suspending agent). It can be used to synthesize DL-glyceraldehyde, drug carrier dialkyl polyoxyethylene glycerol ether, medical adhesive cyanoacrylate 1,2-isopropyl glyceride, and can also be used as a polyhydroxy protecting group to synthesize high-purity monoglycerides, etc. [0003] Glycerol formal is obtained from the reaction of glycerin and formaldehyde and is used as a solvent for pesticides and drug i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/20B01J29/89
CPCC07D317/20B01J29/89Y02P20/55
Inventor 刘聿嘉夏长久王亚敏杨永佳朱斌彭欣欣林民罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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