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Preparation method of chloroacetaldehyde dimethyl acetal

A technology of chloroacetaldehyde dimethyl acetal and anhydrous methanol is applied in the preparation of organic compounds, the preparation of carboxylic acid esters, the preparation of carbon-based compounds, etc., and can solve the problems of harsh reaction conditions, cumbersome reaction steps, low yield and the like, To achieve the effect of simplifying the preparation method, reducing side reactions and improving yield

Pending Publication Date: 2018-04-24
临沂优盛新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many synthetic methods, some reaction conditions are harsher, some reaction steps are tedious and the yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of preparation method of chloroacetaldehyde dimethyl acetal, it may further comprise the steps:

[0024] 1) Add the reactants 650g of anhydrous methanol and 350g of vinyl acetate into the reaction flask, and then add 0.2g of an inhibitory initiator composed of anhydrous ferric chloride and biphenol in any ratio, and control it in an ice-water bath. The temperature is -15-5°C, and a total of 288g of chlorine gas is introduced under stirring. After the chlorine is passed, stir until the feed liquid returns to colorless; the vinyl acetate and chlorine gas are added three times according to the mass ratio of 4:2:1, each The ratio of the amount of vinyl hypoacetate and chlorine added is 1:1;

[0025] 2) Warm up the colorless reaction feed liquid prepared in step 1) to 65°C and stir for 1 hour, then pass in brine to cool down to below 10°C, directly add alkali to adjust the pH value to 6-8, and then turn the feed liquid into a rotary The final product is obtained by v...

Embodiment 2

[0027] A kind of preparation method of chloroacetaldehyde dimethyl acetal, it may further comprise the steps:

[0028] 1) Add the reactant 390g of anhydrous methanol and 350g of vinyl acetate into the reaction flask, and then add 0.3g of an inhibitory initiator composed of phenol and trimethyl orthoformate in any ratio, and control the temperature in the ice-water bath at -15 -5°C, feed in a total of 259g of chlorine gas under stirring, and stir until the feed solution turns colorless after the chlorine feeding is completed; vinyl acetate and chlorine gas are added three times according to the mass ratio of 3:3:1, each time vinyl acetate The ratio of the amount of substance added to chlorine gas is 1:0.9;

[0029] 2) Warm up the colorless reaction feed liquid prepared in step 1) to 65°C and stir for 1 hour, then pass in brine to cool down to below 10°C, directly add alkali to adjust the pH value to 6-8, and then turn the feed liquid into a rotary Evaporator atmospheric pressu...

Embodiment 3

[0032] A kind of preparation method of chloroacetaldehyde dimethyl acetal, it may further comprise the steps:

[0033] 1) Add 1042g of anhydrous methanol and 700g of vinyl acetate into the reaction flask, then add 0.7 g of a polymerization inhibitor composed of p-benzoquinone and anhydrous ferric chloride in any ratio, and control the temperature in an ice-water bath At -15-5°C, feed a total of 692g of chlorine gas under stirring, and stir until the feed liquid fades to colorless after the chlorine feeding is completed; the vinyl acetate and chlorine gas are added three times according to the mass ratio of 4:2:1, each time The ratio of the amount of vinyl acetate and chlorine added is 1:1.2;

[0034] 2) Warm up the colorless reaction feed liquid prepared in step 1) to 65°C and stir for 1 hour, then pass in brine to cool down to below 10°C, directly add alkali to adjust the pH value to 6-8, and then turn the feed liquid into a rotary The final product is obtained by vacuum dis...

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PUM

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Abstract

The invention discloses a preparation method of chloroacetaldehyde dimethyl acetal. The method adopts vinyl acetate, anhydrous methanol and chlorine as reaction raw materials, adopts a step-by-step feeding one-pot boiling method and also adds a polymerization inhibition inducing agent, so that the reaction raw materials can maximally participate in the reaction to generate a target product, the generation of side products can be reduced, and the prepared product is high in yield and high in purity. The preparation method of the invention is controllable in conditions, simple and easy in product separation method and convenient in industrialized operation.

Description

technical field [0001] The invention relates to a preparation method of chloroacetaldehyde dimethyl acetal, which belongs to the technical field of new material chemical organic synthesis. Background technique [0002] Chloroacetaldehyde dimethyl acetal, also known as chloroacetaldehyde dimethyl acetal, can be used as a raw material for pesticides, medicines, organic synthesis, and the synthesis of liquid crystals. It can also be used as a strengthening agent and starch modifier for the production of paper and cardboard, and is an important chemical raw material. At present, there are many public preparation methods of chloroacetaldehyde dimethyl acetal, mainly including (1) reacting acetaldehyde and methanol as raw materials, then introducing chlorine gas at 40°C, and finally neutralizing excess chlorine with milk of lime (2) A high-concentration aqueous solution of chloroacetaldehyde and methanol are dehydrated under the action of anhydrous calcium chloride; (3) Vinyl chl...

Claims

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Application Information

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IPC IPC(8): C07C67/287C07C67/28C07C69/14C07C67/03C07C45/51C07C47/14C07C41/56C07C43/313
CPCC07C41/56C07C45/51C07C67/03C07C67/28C07C67/287C07C69/14C07C47/14C07C43/313
Inventor 牛文博孔霞董付蒙
Owner 临沂优盛新材料科技有限公司
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