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Continuous synthesis method and application of sulfonated keto-aldehyde condensation compound

A technology for sulfonated ketone-aldehyde condensate and sulfonated acetone, which is applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, chemical/physical processes, etc. It is easy to generate by-products and other problems, so as to achieve the effect of simple preparation method, convenient operation and continuous safe production.

Pending Publication Date: 2020-11-27
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] Aiming at the problems of inaccurate temperature control caused by strong exothermic reaction in the reaction process existing in the synthesis of sulfonated acetone-formaldehyde condensation polymers in the prior art, long reaction time, by-products are easily generated from the reaction mixture, and continuous production cannot be performed. The present invention provides a sulfonate A continuous synthesis method and application thereof of ketone-aldehyde condensate (such as sulfonated acetone-formaldehyde condensate), the present invention effectively overcomes the problem of synthesizing sulfonated aldehyde-ketone condensate by using a microstructure reactor for the preparation of sulfonated acetone-formaldehyde condensate In the process, the temperature control caused by the strong exothermic reaction process is not accurate, the reaction time is long, the reaction mixture is easy to generate by-products, and the problems of continuous production cannot be achieved. The continuous synthesis of sulfonated aldehyde and ketone condensation polymers is truly realized, so it has good The value of actual promotion and application

Method used

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  • Continuous synthesis method and application of sulfonated keto-aldehyde condensation compound
  • Continuous synthesis method and application of sulfonated keto-aldehyde condensation compound
  • Continuous synthesis method and application of sulfonated keto-aldehyde condensation compound

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Embodiment 1

[0072] The sulfonation reaction in embodiment 1,2,3,4,5 takes sodium p-toluenesulfonate, amino-substituted naphthalenesulfonate sodium, sodium pyrosulfite solution, sodium sulfite and sodium lignosulfonate as sulfonating agent respectively, with The sulfonated acetone that generates in the first step reaction is that raw material carries out condensation reaction; Embodiment 1,2 is to carry out sulfonated reaction with acetone, acetophenone as raw material in continuous tank reactor; Embodiment 3,4 is to carry out sulfonated reaction in tube Formaldehyde and acetaldehyde are used as raw materials for condensation reaction in the reactor. Example 5 is a condensation reaction of sulfonated acetone in a microstructure reactor using an aqueous solution of sodium hydroxide (the mass ratio of water to sodium hydroxide is 5:1) as a catalyst.

[0073] The present invention is further explained and illustrated by the following examples, but does not constitute a limitation of the prese...

Embodiment 2

[0080] The acetophenone solution and the amino-substituted naphthalenesulfonate sodium solution are introduced into a volume of 10m 3 In the continuous stirred tank reactor, the ratio of acetophenone solution and amino-substituted naphthalene sulfonate is 1:1.5, and the generated sulfonated acetophenone solution and formaldehyde are respectively passed into another continuous stirred tank reactor, and the temperature is controlled At 0°C, the stirring speed is 120r / min, the average residence time is 160min, the reaction product is collected at the outlet, the product solution is neutralized, dried by rotary evaporation, ethanol is precipitated, dried and ground to obtain a substituted naphthalenesulfonated acetophenone formaldehyde polycondensate, Its solids content is 28%.

Embodiment 3

[0082] The sodium sulfite solution and acetone are pumped into a tubular reactor with a temperature of 20°C, a diameter of 100mm, and a length of 5m by a liquid chromatography pump at an equivalent ratio of 1:3. The residence time of the material is 10min, and the resulting The sulfonated acetone solution and the formaldehyde solution were respectively passed into another tubular reactor, the temperature was controlled at 90°C, and the average residence time was 20 minutes. The solids content was 35%.

[0083] From figure 2 It can be seen from the spectrum that 3425.5cm is the stretching vibration absorption peak of the hydroxyl group; 2923.2cm is the stretching vibration peak of the C-H bond on the aliphatic molecular chain, and 2852.5cm is the CH 3 1619.6cm is the stretching vibration absorption peak of the carbonyl group; 1449.4cm is the asymmetric deformation vibration absorption peak of the methyl group; 1180 and 1045cm are -SO 3 The stretching vibration peak of alkyl ...

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Abstract

The invention provides a continuous synthesis method and application of a sulfonated keto-aldehyde condensation compound, and belongs to the technical field of preparation of high-molecular compounds.According to the invention, a microstructure reactor is used for preparing SAF, so that the problems of inaccurate temperature control, long reaction time, easy generation of by-products from the reaction mixture and incapability of continuous production caused by strong heat release in the reaction process in the SAF synthesis process are effectively solved, and continuous synthesis of SAF is truly realized; and method has good practical popularization and application values.

Description

technical field [0001] The invention belongs to the technical field of polymer compound preparation, and relates to a continuous synthesis method and application of sulfonated ketone-aldehyde condensates. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] The aliphatic water reducer uses aldehydes and ketone carbonyl compounds as the main raw materials to condense under alkaline conditions to obtain aliphatic polymer chains, and through the addition of sulfite to introduce hydrophilic Sulfonic acid groups form a polymer water reducer with surface activity. The most representative one is sulfonated acetone-formaldehyde condensate (SAF), which is prepared from formaldehyde an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C08G6/02C04B24/16C04B103/30C04B103/40
CPCB01J19/0046B01J19/0093C08G6/02C04B24/001C04B2103/408C04B2103/302
Inventor 姚型军姜松舒东博
Owner LIAOCHENG UNIV
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