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Synthetic method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and aqueous solution product obtained during preparation process thereof

A technology of trimethylammonium chloride and a synthesis method, applied in the field of aqueous solution products, can solve the problems such as the catalyst cannot be recycled, the pH value is difficult to control, the efficiency is low, etc., and the yield is high, the pH value is easy to control, and the energy consumption is low. Effect

Inactive Publication Date: 2011-04-06
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] One of the technical problems to be solved in the present invention is to provide a synthetic method of 3-chloro-2-hydroxypropyl-trimethylammonium chloride, to overcome the difficulty in adjusting and controlling the pH value in the prior art, low efficiency, and the catalyst Disadvantages such as inability to recycle

Method used

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  • Synthetic method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and aqueous solution product obtained during preparation process thereof
  • Synthetic method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and aqueous solution product obtained during preparation process thereof
  • Synthetic method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and aqueous solution product obtained during preparation process thereof

Examples

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Effect test

Embodiment 1

[0035] 1, Synthesis of 3-chloro-2-hydroxypropyl-trimethylammonium chloride aqueous solution:

[0036] Add 70g of trimethylamine hydrochloride and 64ml of water into the reaction flask, start stirring until the trimethylamine hydrochloride is completely dissolved, then add alkaline Al 2 o 3 Catalyst 10g, keep the pH value of the system at 7.8, after cooling down to 5°C, add 66g of epichlorohydrin (ECH) dropwise, and keep it warm until the pH value of the system reaches the peak value of 9.7. At this time, the system is a homogeneous system. It lasted 3 hours; then, it was transferred to room temperature and reacted for 2 hours at 18°C. When the pH value of the reaction system dropped to 8.8, the reaction was completed; the catalyst was filtered to remove the crude product, and 2 times the volume of deionized water was continuously added to the crude product. Control the vacuum degree at 740mmHg, and carry out continuous vacuum azeotropic distillation at 48°C to obtain solid co...

Embodiment 2

[0040] 1, Synthesis of 3-chloro-2-hydroxypropyl-trimethylammonium chloride aqueous solution:

[0041] Add 70g of trimethylamine hydrochloride and 60mL of water in sequence in the reaction bottle, start stirring until the trimethylamine hydrochloride is completely dissolved, then add KF / basic Al 2 o 3 Composite catalyst 7g, keep the pH value of the system at 8. Cool down to 2°C and add 67g of ECH dropwise. After dropping, keep warm until the pH value of the system reaches the peak value of 10. At this time, the system is a homogeneous system, which lasts for 5 hours. Then, turn to room temperature 25 ℃ and react for 2 hours, when the pH value of the reaction system drops to 7.8, the reaction ends; the catalyst is removed by filtration to obtain the crude product, and 4 times the volume of deionized water is continuously added to the crude product, and the vacuum degree is controlled at 760mmHg, continuous vacuum azeotropic distillation at 58°C to obtain solid content: 70.1% (...

Embodiment 3

[0045] 1, Synthesis of 3-chloro-2-hydroxypropyl-trimethylammonium chloride aqueous solution:

[0046] 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 K 2 CO 3 / Neutral Al 2 o 3 Composite catalyst 14g, keep the pH value of the system at 8. Cool down to 0°C and add 68g of ECH dropwise. After dropping, keep warm until the pH value of the system reaches the peak value of 9.5. At this time, the system is a homogeneous system, which lasts for 4 hours. Then, turn to room temperature and react at 25°C for 2.5 hours. When the pH value of the reaction system drops to 7.8, the reaction ends; the catalyst is removed by filtration to obtain the crude product, and the crude product is continuously added with 1 times the volume of deionized water, and the vacuum degree is controlled at 750mmHg. Vacuum azeotropic distillation at 60°C to obtain solid content...

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Abstract

The invention provides a synthetic method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, which effectively combines advantages of compound solid base and two-stage reaction at low temperature and room temperature, directly takes trimethylamine hydrochloride, epichlorohydrin and water as raw materials, has the advantages of moderate reaction conditions, less side reaction and high product purity and is easy to control. Product refining adopts continuous vacuum constant boiling distillation, thus simplifying operation and greatly reducing energy consumption. In the invention, liquid-phase 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is directly taken as a raw material to obtain a solid product by one-step spray drying, wherein, the water content of the product is less than 5% (mass percent), ECH is not more than 5ppm (GC) and the DCP (dichloro-isopropanol) content is not more than 10ppm (GC).The synthetic method has the advantages of simple, direct, convenient and efficient operation and being free from an organic volatile solvent.

Description

【Technical field】 [0001] The present invention relates to a kind of synthetic method of 3-chloro-2-hydroxypropyl-trimethylammonium chloride, particularly a kind of synthetic method of 3-chloro-2-hydroxypropyl-trimethylammonium chloride and its preparation The aqueous solution product obtained in the process. 【Background technique】 [0002] 3-Chloro-2-hydroxypropyl-trimethylammonium chloride (CTA), as an important cationic etherification agent, can be used in the dispersion of oilfield chemicals, emulsifiers, hard water softeners, fabric antistatic agents, and electroplating solutions Agents, printing and dyeing auxiliaries, etc. At present, its most important application is to react with starch to prepare cationic starch used in the paper industry. [0003] The synthesis method of CTA can be divided into one-step method and two-step method according to the difference of reaction raw materials: wherein one-step method uses trimethylamine hydrochloride (TMAC) and epichlorohy...

Claims

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Application Information

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IPC IPC(8): C07C215/40C07C213/04B01J21/04B01J27/12B01J27/232
CPCY02P20/584
Inventor 林棋李心忠
Owner MINJIANG UNIV
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