Alkyl ketene, preparation method and application thereof

A technology of alkyl ketene and continuous reaction, applied in the direction of water repellent addition, organic chemistry, etc., can solve problems such as complex process, and achieve the effect of simple process, good water resistance and high dimer content

Active Publication Date: 2009-11-11
SHANGHAI DONGSHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product prepared by this method needs to be obtained by cleaning and extracting with dilute acid solution or centrifuging, and the content of alkyl ketene dimer can reach up to 93.5% by weight, but the preparation method is complicated

Method used

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  • Alkyl ketene, preparation method and application thereof
  • Alkyl ketene, preparation method and application thereof
  • Alkyl ketene, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of alkyl ketene dimers:

[0027] Add 120 grams of triethanolamine to a 1000ml reactor, heat up to 55°C, and add 400 grams of C 16 Saturated fatty acid chloride, the dropwise addition time is 2 hours. After the dropwise addition was completed, the mixture was kept at 55° C. for 3 hours. Add 400 grams of 70 DEG C deionized water under stirring then, and continue to stir for 10 minutes, stop stirring, remove the bottom triethanolamine hydrochloride aqueous solution (this process temperature remains on 70 DEG C) after 30 minutes. Add 400 grams of 70° C. deionized water under stirring, and continue to stir for 10 minutes, stop stirring, and remove the bottom water after 30 minutes (the process temperature remains at 70° C.). The prepared sample was transferred to a 1000ml round-bottomed flask while hot, and the remaining moisture was evaporated with a rotary evaporator RV 10 digital display type V (IKA company), and the obtained sample passed through a 200-mesh...

Embodiment 2

[0029] Preparation of alkyl ketene dimers:

[0030] Add 140 grams of triethanolamine and 70 grams of diethanolamine to a 2000ml reactor, heat up to 85°C, and add 300 grams of C 22 Saturated fatty acid chloride, the dropwise addition time is 0.5 hours. After completion of the dropwise addition, the mixture was kept at 85° C. for 0.5 hours. Add 600 grams of 80 DEG C of deionized water under stirring then, and continue to stir for 15 minutes, stop stirring, remove bottom triethanolamine hydrochloride and diethanolamine hydrochloride aqueous solution (this process temperature remains on 80 DEG C) after 20 minutes. Add 600 grams of 70° C. deionized water under stirring, and continue to stir for 15 minutes, stop stirring, and remove the bottom water after 20 minutes (the process temperature remains at 80° C.). The prepared sample was transferred to a 1000ml round-bottomed flask while hot, and the remaining moisture was evaporated with a rotary evaporator RV 10 digital display type...

Embodiment 3

[0032] Add 75 grams of triethanolamine and 75 grams of diethanolamine to a 2000ml reactor, heat up to 80°C, and add 150 grams of C 20 Saturated fatty acid chloride and 150 g C 18 Saturated fatty acid chloride, the dropwise addition time is 1.5 hours. After completion of the dropwise addition, the mixture was kept at 80° C. for 2.0 hours. Then add 450 grams of 75 DEG C deionized water under stirring, and continue to stir for 12 minutes, stop stirring, and remove bottom triethanolamine hydrochloride and diethanolamine hydrochloride aqueous solution (this process temperature remains on 75 DEG C) after 25 minutes. Add 400 grams of 75° C. deionized water under stirring, and continue to stir for 12 minutes, stop stirring, and remove the bottom water after 25 minutes (the process temperature remains at 75° C.). The prepared sample was transferred to a 1000ml round-bottomed flask while hot, and the remaining moisture was evaporated with a rotary evaporator RV 10 digital display type...

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Abstract

The invention discloses alkyl ketene, a preparation method and application thereof. The preparation method comprises the following steps: heating up 30 to 70 portions of amine by weight to a temperature of between 55 and 85 DEG C, adding 100 portions of acyl chloride by weight within 0.5 to 2 hours, and reacting continuously after adding the acyl chloride for 0.5 to 3 hours; adding 100 to 200 portions of water of which the temperature is between 70 and 80 DEG C by weight, mixing and then standing the mixture, and removing a salt solution at the bottom layer; adding 100 to 200 portions of water of which the temperature is between 70 and 80 DEG C by weight again, mixing and standing the mixture, and removing the water at the bottom layer; and dehydrating the mixture, filtering the mixture while the mixture is hot, and cooling the filtered mixture to obtain an alkyl ketene dimer. The method uses no solvent, is more environment-friendly and has simple process; and the product has high content of the alkyl ketene dimer, and has good water resisting effect when the product is used as a sizing agent. The obtained alkyl ketene dimer can be used for sizing paper sheets and can greatly improve the Cobb value of the paper sheets and enhance the ring crushing strength of the paper sheets.

Description

technical field [0001] The invention relates to an alkyl ketene dimer, its preparation method and its application in paper sizing. Background technique [0002] Alkyl ketene dimer is a kind of wax, and its molecular structure can be represented by the following formula: [0003] [0004] R 1 for C 4 ~C 30 Alkyl or C 4 ~C 30 Alkenyl, R 2 for hydrogen or C 1 ~C 8 alkyl. [0005] The melting point of alkyl ketene dimer is 40-52°C. It is used as a sizing agent for papermaking pulp to make the paper impervious to water. It is used for food packaging paper or other corresponding purposes. [0006] At present, in the domestic production of synthetic alkyl ketene dimers, the synthesis reaction temperature is lower than the melting point of alkyl ketene dimers, generally around 25°C. At this temperature, the reaction speed is slow, and a long holding time is required. Moreover, the viscosity of the material is high at this temperature. A large amount of toluene solvent n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/12D21H21/16
Inventor 施晓旦尹东华王养臣
Owner SHANGHAI DONGSHENG NEW MATERIALS
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