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Method for preparing AKD by serialization

A formula and acyl chloride technology, applied in the field of continuous preparation of AKD, can solve the problems of complicated equipment structure, inability to obtain high-quality products, etc., and achieve the effect of reducing viscosity

Active Publication Date: 2010-09-29
SUZHOU TIANMA SPECIALTY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The method described in the above patent has complicated equipment structure, and the acid chloride and tertiary amine are added in proportion at one time, so high-quality products cannot be obtained, and improvements in process and equipment are needed.

Method used

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  • Method for preparing AKD by serialization
  • Method for preparing AKD by serialization
  • Method for preparing AKD by serialization

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Experimental program
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Effect test

Embodiment 1

[0044] The mixing reactor has a diameter of 100 mm, an effective length of 840 mm, and a rotation speed of 50 to 70 rpm. The feeding amount is: 10.8~27.0 kg / hour of stearyl chloride (octadecyl carbon contains 35%, 16 carbon contains 65%), 4.2~12.6 kg / hour of triethylamine. The feeding method is to add all the triethylamine and 1 / 3 to 2 / 3 of the acid chloride at the first feeding position at the two feeding ports, and the second feeding position is about 80-120 mm away from the first feeding position. , add the remaining amount of acid chloride. When the material is added to the first feeding position, the reaction will release heat immediately, and the temperature will rise sharply. The heat of reaction must be removed quickly by means of a cooling system. The temperature of the reactant is controlled at 65-110°C. After about 7-15 minutes, the reactor is discharged. The mouth begins to discharge the reaction product in the form of paste, which enters the continuous extractor,...

Embodiment 2

[0046]The mixing reactor has a diameter of 219 mm, an effective length of 1400 mm, and a rotation speed of 50 to 70 rpm. Feeding amount is: stearyl chloride (octadecane contains 35%, sixteen carbon contains 65%) 132 kilograms~108 / hour, triethylamine 51.8~42.4+ kilograms / hour. The feeding method is to add all the triethylamine and 20-80% of the acid chloride in the two feeding ports respectively at the first feeding position, and the second feeding position is about 1-3 minutes away from the first feeding position, and add remaining amount of acid chloride. When the material is added to the first feeding position, the reaction exotherms and the temperature rises sharply. The heat of reaction must be removed quickly with the help of the cooling system (hollow shaft and external jacket), and the temperature of the reactant should be controlled below 115°C, about 9-15°C. Minutes later, the reactor discharge port began to discharge a paste-like reaction product, which entered the ...

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Abstract

The invention provides a method for preparing AKD by serialization. The method includes the following steps: reaction of acyl chloride and tertiary amine is carried out, acyl chloride in formula ratio is divided into two or three parts, each part is 10-90% of the formula ratio, the rest part of acyl chloride is added in times after 30-300 seconds, triethylamine in formula ratio and first part of acyl chloride are simultaneously, respectively and continuously added at the front end of a reactor; material is continuously fed into a hybrid reactor from different feeding holes by virtue of a plurality of metering pumps, the material is subject to hybrid reaction in the hybrid reactor by stirring, cutting and malposition moving, and the temperature of material is controlled; the material is remained in the reactor, discharged from the outlet of the reactor and enters into a continuous extractor, and meanwhile diluted hydrochloric acid is continuously added into the extractor, is dispersed with reaction product to form uniform mixed solution and then enters into a slope precipitator, separation of oil phase and water phase is carried out, the oil phase is discharged from the upper outlet, and the water phase is discharged from the lower outlet; and the oil phase is namely the AKD, and the water phase is triethylamine hydrochloride solution.

Description

technical field [0001] The invention relates to a method for continuously preparing AKD (alkyl or alkenyl ketene dimer). Background technique [0002] At present, AKD products on an industrial scale are all produced in batches. With the growth of AKD demand and the expansion of production scale, the production mode of continuous preparation is the development direction of AKD production technology. [0003] Regarding the continuous preparation of AKD, the patent EP550107 discloses a method for preparing by reacting acid chlorides and tertiary amines in the absence of a solvent, which uses two step-connected reactors. Add tertiary amine to the first reactor, then add acid chloride continuously, transfer the material to the second reactor with a gear pump, and then add the two materials continuously under equilibrium conditions. The reactants were held for 60 minutes in the first reactor and 15 minutes in the second reactor. [0004] Patents WO03 / 045936, US7078569, and CN159...

Claims

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Application Information

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IPC IPC(8): C07D305/12
Inventor 谭安琪任海峰
Owner SUZHOU TIANMA SPECIALTY CHEM
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