Synthesis method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride based on solid base catalysis system

A technology of trimethylammonium chloride and catalytic system is applied in chemical instruments and methods, preparation of aminohydroxy compounds, preparation of organic compounds, etc., and can solve the problems of poor thermal stability, high cost, complicated preparation, etc. The effect of easy adjustment of pH value, short reaction time and high selectivity

Inactive Publication Date: 2012-05-16
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 alkali, which mainly includes metal oxides, hydrated talc-type anion

Method used

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  • Synthesis method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride based on solid base catalysis system
  • Synthesis method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride based on solid base catalysis system
  • Synthesis method of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride based on solid base catalysis system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Liquid-phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride synthesis:

[0034] 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. Filter and remove catalyzer to obtain crude product, crude product adds 4 times of volumes of deionized water (adding in 8 times), controls vacuum at 740mmHg, and temperature carries out continuous stripping underpressure distillation at 48 ℃, obtains solid content: 68.9% ( mass percent); active substance content: 97.7%, ECH content: ≤ 13ppm (GC); dichloroisopropanol (DCP) content: ≤ 29ppm (GC) liquid product.

Embodiment 2

[0036] Liquid-phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride synthesis:

[0037] Add 70g of trimethylamine hydrochloride and 60ml of water in turn into the reaction flask, start stirring until the trimethylamine hydrochloride is completely dissolved, then add 7g of ZnO / 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. Filtration removes catalyst to obtain crude product, and crude product adds 6 times of volumes of deionized water (adding in 10 times), controls vacuum at 760mmHg, and carries out continuous stripping and vacuum distillation at 75° C. to obtain solids content: 70.1% ( mass percent); active substance content: 98.0%, ECH content: ≤ 5ppm (GC); dichloroisopropanol (DCP) content: ≤ 20ppm (GC) liquid product.

Embodiment 3

[0039] Liquid-phase 3-chloro-2-hydroxypropyl-trimethylammonium chloride synthesis:

[0040] 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 3Composite catalyst 14g, keep the pH value of the system at 8. Cool down to 0° C. and add 68 g of ECH dropwise. After dropping, keep warm until: 1) the pH value of the system reaches a peak value of 9.5; 2) the system becomes homogeneous and ends. Filter and remove catalyzer to obtain crude product, crude product adds 8 times of volumes of deionized water (adding in 10 times), controls vacuum at 750mmHg, and temperature carries out continuous stripping and vacuum distillation at 80° C. to obtain solids content: 70% ( mass percent); active substance content: 98.8%, ECH content: ≤ 5ppm (GC); dichloroisopropanol (DCP) content: ≤ 22ppm (GC) liquid product.

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Abstract

The invention relates to a synthesis method of 3-cholro-2-hydroxypropyl-trimethyl ammonium chloride based on a solid base catalysis system. In the synthesis method provided by the invention, a catalyst ZnO, or a composite catalyst of ZnO and KF, or a composite catalyst of ZnO and K2CO3 or a ZnO/K2CO3/NaOH composite catalyst is adopted; advantages of a composite solid base and a low-temperature (0-15 DEG C) and room-temperature (18-25 DEG C) two-stage reaction are combined, and trimethylamine hydrochloride, epoxy chloropropane and water are directly taken as raw materials; and the synthesis method provided by the invention has the advantages of mild reaction condition, easiness in control, less side reaction and high product purity. Continuous steam stripping and reduced-pressure distillation are adopted in refining of products, operation is simplified, and energy consumption is reduced. Liquid-phase 3-cholro-2-hydroxypropyl-trimethyl ammonium chloride can be directly taken as a raw material and subjected to one-step spray drying to obtain a solid product with the moisture content of being lower than 5%, ECH (epoxy chloropropane) content being less than or equal to 5ppm detected by gas chromatography (GC), and DCP(1,3-dichloro-2-propanol) content being less than or equal to 10ppm detected by GC; and operation is easy, convenient and efficient, and no organic volatile solvent is used.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a catalyst based on ZnO and a series of composite solid alkali systems, trimethylamine hydrochloride, water and epichlorohydrin as starting materials, adopting 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 oil field 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 one-step method and two-step method according to the difference of reaction raw materials: wherein one-step method us...

Claims

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Application Information

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IPC IPC(8): C07C215/40C07C213/04C07C213/10
CPCY02P20/584
Inventor 刘代城
Owner JIANGXI CHUAN SHENG TECH CO LTD
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