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Solid base catalyst and method for synthesizing 3-chloro-2-hydroxypropyl-trimethyl-ammonium chloride based on solid base catalyst

A technology of trimethylammonium chloride and solid base catalyst, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., and can solve the problems of complex preparation, poor thermal stability, and high cost. Achieve the effects of high selectivity, easy pH adjustment and short reaction time

Inactive Publication Date: 2012-11-21
JIANGXI CHUAN SHENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage is that the alkali strength is uniform, but its thermal stability is not good, it can only be applied to low-temperature reactions, and the preparation is complicated and the cost is high; 2) Inorganic solid bases, which mainly include metal oxides, hydrated talc-like anionic clays and loaded Solid base, etc., which have the characteristics of simple preparation, wide range of base strength distribution, and good thermal stability; 3) Loaded solid base, which is a type of solid base obtained by loading inorganic or organic bases on alumina or molecular sieves

Method used

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  • Solid base catalyst and method for synthesizing 3-chloro-2-hydroxypropyl-trimethyl-ammonium chloride based on solid base catalyst
  • Solid base catalyst and method for synthesizing 3-chloro-2-hydroxypropyl-trimethyl-ammonium chloride based on solid base catalyst
  • Solid base catalyst and method for synthesizing 3-chloro-2-hydroxypropyl-trimethyl-ammonium chloride based on solid base catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Liquid-phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride synthesis:

[0033]Add 70 g of trimethylamine hydrochloride and 64 ml of water in turn into the reaction flask, start stirring until the trimethylamine hydrochloride is completely dissolved, then add 10 g of catalyst ZnO to keep the pH of the system at 7.8. Cool down to 5°C and start adding 66g of ECH dropwise. After dropping, keep warm until: 1) the pH value of the system reaches a peak value of 9.7; 2) the system becomes homogeneous and ends. The catalyst was removed by filtration to obtain the crude product, which was added with 4 times the volume of deionized water (into 8 times), the vacuum degree was controlled at 740mmHg, and the temperature was continuously stripped and vacuum distilled at 48°C to obtain a solid content: 68.9% ( mass percent); active substance content: 97.7%, ECH content: ≤13ppm (GC); dichloroisopropanol (DCP) content: ≤29ppm (GC) liquid product.

Embodiment 2

[0035] Liquid-phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride synthesis:

[0036] Add 70g of trimethylamine hydrochloride and 60ml of water in sequence in the reaction flask, start stirring until the trimethylamine hydrochloride is completely dissolved, then add 7g of ZnO and KF composite catalyst to keep the pH of the system at 8. Cool down to 2°C and add 67 g of ECH dropwise. After dropping, keep warm until: 1) the pH value of the system reaches a peak value of 11; 2) the system becomes homogeneous and ends. The catalyst was removed by filtration to obtain the crude product, and the crude product was added with 6 times the volume of deionized water (adding in 10 times), the vacuum degree was controlled at 760mmHg, and the temperature was 75°C for continuous stripping and vacuum distillation to obtain a solid content: 70.1% ( mass percent); active substance content: 98.0%, ECH content: ≤5ppm (GC); dichloroisopropanol (DCP) content: ≤20ppm (GC) liquid product.

Embodiment 3

[0038] Liquid-phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride synthesis:

[0039] Add 70g of trimethylamine hydrochloride and 70ml of water in sequence in the reaction bottle, start stirring until the trimethylamine hydrochloride is completely dissolved, then add ZnO and K 2 CO 3 Composite catalyst 14g, keep the pH value of the system at 8. Cool down to 0°C and add 68 g of ECH dropwise, and keep the reaction until: 1) the pH value of the system reaches a peak value of 9.5; 2) the system becomes homogeneous and ends. Remove the catalyst by filtration to obtain the crude product, add 8 times the volume of deionized water to the crude product (adding in 10 times), control the vacuum at 750mmHg, and carry out continuous stripping and vacuum distillation at 80°C to obtain a solid content of 70% ( mass percent); active substance content: 98.8%, ECH content: ≤5ppm (GC); dichloroisopropanol (DCP) content: ≤22 ppm (GC) liquid product.

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Abstract

The invention relates to a solid base catalyst and a method for synthesizing 3-chloro-2-hydroxypropyl-trimethyl-ammonium chloride based on the solid base catalyst. In the invention, ZnO (zinc oxide) or the composite catalyst of ZnO and KF (potassium fluoride) or the composite catalyst of ZnO and K2CO3 or the composite catalyst of ZnO / K2CO3 / NaOH is adopted as the solid base catalyst; the advantages of the two stages of reaction at the low temperature (0-15 DEG C) and the room temperature (18-25 DEG C) under the catalysis of the solid base catalyst are effectively combined, and trimethylamine hydrochloride, epichlorohydrin (ECH) and water are directly used as raw materials; and the invention has the advantages of mild reaction condition, less side reaction and high product purity and is easy to control. Continuous steam stripping reduced pressure distillation is adopted to refine the products, thereby not only simplifying the operation but also greatly reducing the energy consumption. Liquid-phase 3-chloro-2-hydroxypropyl-trimethyl-ammonium chloride can be directly used as the raw material to obtain the solid product the water content of which is less than 5 percent (weight percent), the ECH of which is not more than 5ppm (GC) and the DCP (dicumyl peroxide) content of which is not more than 10ppm (GC) through one-step spray drying. The method is simple, rapid and convenient to operate at high efficiency, and avoids using an organic volatile solvent.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a series of composite solid alkali systems based on ZnO as catalysts, trimethylamine hydrochloride, water, and epichlorohydrin as starting materials, and adopts low temperature and room temperature two-stage reaction, continuous stripping A synthetic method for the preparation of liquid and solid phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride by pressure distillation and spray drying. Background technique [0002] 3-Chloro-2-hydroxypropyl-trimethylammonium chloride (CTA), as an important cationic etherification agent, can be used in oilfield chemicals, water treatment agents, non-treatment agents, fabric antistatic agents, electroplating solutions Dispersants, printing and dyeing auxiliaries, etc. [0003] The synthesis method of CTA can be divided into two categories: one-step method and two-step method according to the different reaction raw materials: the one-step m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/06B01J27/138B01J27/232C07C215/40C07C213/04
Inventor 刘代城
Owner JIANGXI CHUAN SHENG TECH CO LTD
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