Preparation method for trimethylamine oxide

A technology for oxidizing trimethylamine and trimethylamine, which is applied in the direction of organic chemistry, can solve the problems of strong corrosivity of auxiliary hydrochloric acid, incomplete reaction of trimethylamine, complicated separation and purification process, etc., so as to reduce the activation energy of reaction, avoid the loss of raw materials, and improve Effects on Product Yield and Quality

Active Publication Date: 2015-02-11
HONGFENG CHEM GUAN COUNTY HEBEI PROV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The disadvantages of this method are: the volume of the reactor required for the reaction is large, the energy consumption of the subsequent process of concentration and crystallization is high, and the separation and purification processes need to consume silver oxide; the auxiliary material hydrochloric acid is highly corrosive, and corrosion-resistant equipment is required; the separation and purification process is complicated. , it needs to consume organic solvents such as ethanol and methanol, causing serious pollution to the environment and high cost
Its disadvantages are: ①The melting point of hydrate (trimethylamine oxide dihydrate) is about 96°C, and the drying temperature of this method is 60°C-105°C exceeding the melting point of hydrate, which will melt the product, destroy the crystal structure, and change the properties of the product; 2. The 30% hydrogen peroxide aqueous solution used in this method, although the concentration is not high, hydrogen peroxide itself is a very volatile raw material, and it is easy to decompose into oxygen and water with the progress of reaction temperature increase. Reaction with equimolar hydrogen peroxide is likely to cause incomplete reaction of trimethylamine

Method used

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  • Preparation method for trimethylamine oxide

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Experimental program
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Effect test

Embodiment 1

[0061] At room temperature, 165.2 g of an aqueous solution of trimethylamine with a mass fraction of 25.06% was added to the reaction flask, and 51.0 g of an aqueous solution of hydrogen peroxide with a mass fraction of 47.27% was slowly added dropwise under stirring. Water bath control, to avoid excessive temperature rise caused by exothermic reaction, resulting in the decomposition of raw material hydrogen peroxide. Until all the hydrogen peroxide solution is dropped (the molar ratio of trimethylamine to hydrogen oxide is 1:1.01), the electric heating system and the cooling water system are comprehensively controlled, and the temperature is adjusted at 70°C to 75°C for 6 hours, and the reaction is terminated to obtain Oxidize the trimethylamine solution, cool down until the product crystallizes out; let it stand at room temperature to make the crystallization complete. Suction filtration, separation of crystals and mother liquor. Dry the crystals in an oven (40°C-45°C), dis...

Embodiment 2

[0063] At room temperature, 131.2 g of an aqueous solution of trimethylamine with a mass fraction of 30.94% was added to the reaction flask, and 45.0 g of an aqueous solution of hydrogen peroxide with a mass fraction of 53.45% was slowly added dropwise under stirring. Water bath control, to avoid excessive temperature rise due to exothermic reaction, resulting in the decomposition of raw material hydrogen peroxide. After all the hydrogen peroxide solution is dripped (the molar ratio of trimethylamine to hydrogen peroxide is 1:1.03), the electric heating system and the cooling water system are comprehensively controlled and the temperature is adjusted to 70°C to 75°C for 6 hours to obtain oxidation Trimethylamine solution, cool down until the product crystallizes out; let stand to make the crystallization complete. Suction filtration, separation of crystals and mother liquor. Dry the crystals in an oven (45°C-50°C), distill and concentrate the mother liquor under reduced press...

Embodiment 3

[0065] At room temperature, 165.3 g of trimethylamine aqueous solution with a mass fraction of 23.46% was added to the reaction flask, and 67.6 g of a hydrogen peroxide solution with a mass fraction of 41.26% was slowly added dropwise under stirring. During the reaction process, the water bath is controlled until all the hydrogen peroxide solution is dropped (the molar ratio of trimethylamine to hydrogen oxide is 1:1.25), the electric heating system and the cooling water system are comprehensively controlled, and the temperature is adjusted within the range of 65°C to 70°C , reacted for 6 hours to obtain a trimethylamine oxide solution, stirred and cooled until the product crystallized, and stood at room temperature to complete the crystallization. The crystals were separated from the mother liquor. Dry the crystals in an oven (45°C-50°C), concentrate the mother liquor under reduced pressure (temperature 50°C-70°C), separate the crystals from the mother liquor, dry the obtaine...

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Abstract

The invention discloses a preparation method for trimethylamine oxide. The technical scheme that hydrogen peroxide which is more than trimethylamine or stabilizing agent and / or initiating agent is added is adopted to enable the trimethylamine and the hydrogen peroxide to be reacted totally so as to avoid the raw material loss and to reduce the cost; the stabilizing agent is adopted in the reaction, so that the reaction system can be effectively stabilized, the excessive loss of reaction raw materials is controlled, and the yield is improved; the initiating agent is adopted in the reaction, so that the reaction activation energy can be reduced, and the reaction can be initiated at a lower temperature and can be implemented smoothly. The method reduces the raw material cost, reduces the equipment investment, largely decreases the acute reaction degree, stabilizes the reaction progress, and enables the reaction process to be easily controlled; and mother liquor can be recycled, so that the product yield and quality can be improved.

Description

technical field [0001] The invention relates to a method for preparing trimethylamine oxide. Background technique [0002] Trimethylamine oxide, also known as trimethylamine oxide, trimethyl-N-oxide, is the N-oxide formed by trimethylamine, chemical formula: (CH 3 ) 3 NO, the English name is Tri metlyl amine oxide, TMAO for short. Trimethylamine oxide is a colorless needle-like crystal, usually in the form of dihydrate. Easy to absorb moisture, soluble in water, insoluble in ether. Trimethylamine oxide exists widely in nature and is an endogenous substance naturally present in aquatic products, and it is also a characteristic substance that distinguishes aquatic products from other animals. [0003] As a new type, natural and safe animal feed additive, trimethylamine oxide dihydrate has obvious functions of attracting food and promoting growth, and has broad application prospects in aquaculture and animal husbandry. [0004] Its main purpose: [0005] 1) Feed additive;...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C291/04
Inventor 胡冬琴潘咏梅
Owner HONGFENG CHEM GUAN COUNTY HEBEI PROV
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