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A method for preparing acetal with acrolein

A technology for acrolein and acetal, applied in the field of preparing acetal, can solve the problems of many side reactions, low acetal selectivity, difficult purification and the like

Inactive Publication Date: 2011-12-14
荆州市新景化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The general method of preparing acrolein dimethyl acetal and acrolein diethyl acetal is to dehydrate and condense acrolein with methanol or ethanol under the action of an acidic catalyst, but because of its active nature, acrolein is unstable in acidic medium , and because the structural steric hindrance effect is not obvious, the selectivity of reacting with methanol and ethanol to form acetal is low, there are many side reactions, and purification is difficult, which is not conducive to industrialized large-scale production

Method used

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  • A method for preparing acetal with acrolein
  • A method for preparing acetal with acrolein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put a 500ml three-neck flask equipped with a stirring device, a dropping funnel and a thermometer in a water bath, add 310g (2.09mol) of triethyl orthoformate, start stirring, slowly add 2.2g (0.0139mol) of benzenesulfonic acid, and pass through the water bath device Control the temperature at 30-40°C, add 112g (2.0mol) of acrolein dropwise at a constant speed, finish dropping within 1 hour, continue stirring for 2 hours, then add sodium carbonate, neutralize to PH7-7.5, stir for another 2 hours, and let stand for 4 hours , filter, remove insoluble solids, carry out normal pressure rectification operation, intercept 124-125 ℃ fraction 207g (GC detection, content 98.2%), namely acrolein diethyl acetal, yield 81.2%

[0025] Acrolein diethyl acetal GC detection method:

[0026] GC model: FULI 9790Ⅱ

[0027] Detection conditions: Nitrogen: 0.04MPa Hydrogen: 0.15MPa Air: 0.03MPa

[0028] Column temperature: 100-200°C Injection 200°C Detection 220°C

Embodiment 2

[0029] Embodiment 2: add and do not add the comparative test of solvent in the reaction:

[0030] Test A is with embodiment 1;

[0031] First add 100ml ethanol before test B reaction, other is with embodiment 1;

[0032] At first add 100ml ethyl acetate before test C reaction, other is with embodiment 1;

[0033] The yield and quality of acrolein diethyl acetal obtained after the reaction are shown in the table below:

[0034] Test No.

[0035] Conclusion: As can be seen from the above table, the reaction of the present invention without adding a solvent is better, and the yield and quality of acrolein diethyl acetal obtained after the reaction are better than those obtained with a solvent.

Embodiment 3

[0037] Put a 500ml three-neck flask equipped with a stirring device, a dropping funnel and a thermometer in a water bath, add 280g of trimethyl orthoformate (2.64mol), start stirring, slowly add 1.8g of sulfamic acid (0.019mol), and pass through the water bath device Control the temperature at 30-40°C, add 140g (2.54mol) of acrolein dropwise at a constant speed, finish dropping within 1 hour, continue stirring for 2 hours, then add sodium carbonate, neutralize to PH7-7.5, stir for another 2 hours, and let stand for 4 hours , filtered to remove the insoluble solids, then carry out normal pressure rectification operation, cut 201g of fraction at 89-91°C (GC detection, content 98.8%), which is acrolein dimethyl acetal, yield 81.8%.

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Abstract

The invention discloses a method for preparing an acetal from acrolein. The method comprises that acrolein and trimethyl orthoformate or triethyl orthoformate undergo a reaction under the acidic conditions to produce corresponding acrolein dimethyl acetal or acrolein diethyl acetal, and prepared acrolein dimethyl acetal or acrolein diethyl acetal is neutralized by alkalis and then is rectified toform a refined acetal. The method of the invention does not need a solvent. The method has the advantages of high reaction selectivity, good product quality, simple and convenient operation and the like.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing acetal with acrolein. Background technique [0002] Acetal prepared from acrolein has a wide range of uses. As a reaction intermediate, acetal is increasingly used in the synthesis of pharmaceuticals, pesticides, spices, and resins. [0003] Acetal prepared from acrolein, two important compounds are acrolein dimethyl acetal and acrolein diethyl acetal. [0004] The general method of preparing acrolein dimethyl acetal and acrolein diethyl acetal is to dehydrate and condense acrolein with methanol or ethanol under the action of an acidic catalyst, but because of its active nature, acrolein is unstable in acidic medium , and because the structural steric hindrance effect is not obvious, the selectivity of reacting with methanol and ethanol to form acetal is low, there are many side reactions, and the purification is difficult, which is not conduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/48C07C43/303
Inventor 阎璟琪易光政张仕军
Owner 荆州市新景化工有限责任公司
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