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A kind of n,2,3-trimethyl-2-isopropylbutanamide crystal with short rod shape and its crystallization process

A technology of isopropyl butyramide and trimethyl, which is applied in the field of N,2,3-trimethyl-2-isopropylbutyramide crystal and its crystallization process, can solve the problems of easy agglomeration, filtration and storage. And problems such as inconvenience in the transportation process, to achieve the effect of good crystal morphology reproducibility, improved filtration efficiency, and good fluidity

Active Publication Date: 2022-04-19
GUANGDONG PROVINCIAL BIOENGINEERING INST (GUANGZHOU SUGARCANE IND RES INST)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the crystalline products obtained by this method are slender rod-shaped crystals. Due to the large contact area between the crystals, agglomeration is prone to occur, which brings a lot of inconvenience to the filtration, storage and transportation processes.

Method used

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  • A kind of n,2,3-trimethyl-2-isopropylbutanamide crystal with short rod shape and its crystallization process
  • A kind of n,2,3-trimethyl-2-isopropylbutanamide crystal with short rod shape and its crystallization process
  • A kind of n,2,3-trimethyl-2-isopropylbutanamide crystal with short rod shape and its crystallization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A crystallization process of N,2,3-trimethyl-2-isopropylbutanamide, comprising the steps of:

[0052] 1) Add 400g of commercially available WS-23 and 500g of n-hexane into a 2L jacketed crystallization kettle, set the temperature of the water bath at 25°C, and completely dissolve WS-23 under the stirring condition of 300rpm to obtain solution A;

[0053]2) Cool solution A to 21 °C at a cooling rate of 3 °C / h. At this time, the solution is still clear, indicating that WS-23 is still in a complete solution state. Add 4 g of WS-23 seed crystals (WS -23), stir at 21°C at a constant temperature of 300rpm for 0.5h for the first crystallization, maintain the stirring speed and continue to cool down to 0°C at a cooling rate of 3°C / h for the second crystallization, after the crystallization is completed, quickly use Suction filtration and washing with a pre-cooled Buchner funnel, and drying in a vacuum oven at 30°C for 12 hours to obtain N,2,3-trimethyl-2-isopropylbutanamide wit...

Embodiment 2

[0056] A crystallization process of N,2,3-trimethyl-2-isopropylbutanamide, comprising the steps of:

[0057] 1) Add 100g of commercially available WS-23 and 500g of n-hexane into a 2L jacketed crystallization kettle, set the temperature of the water bath at 30°C, and completely dissolve WS-23 under the stirring condition of 400rpm to obtain solution A;

[0058] 2) Cool solution A to 21 °C at a cooling rate of 12 °C / h. At this time, the solution is still clear, indicating that WS-23 is still in a complete solution state. Add 3 g of WS-23 seed crystals (WS -23), stir at 21°C at a constant temperature of 400rpm for 2 hours for the first crystallization, maintain the stirring speed and continue to cool down to -1°C at a cooling rate of 12°C / h, and perform the second crystallization. After the crystallization is completed, quickly use Suction filtration and washing with a pre-cooled Buchner funnel, and drying in a vacuum oven at 40°C for 12 hours to obtain N,2,3-trimethyl-2-isoprop...

Embodiment 3

[0060] A crystallization process of N,2,3-trimethyl-2-isopropylbutanamide, comprising the steps of:

[0061] 1) Add 350g of commercially available WS-23 and 500g of n-hexane into a 2L jacketed crystallization kettle, set the temperature of the water bath at 25°C, and completely dissolve WS-23 under the stirring condition of 400rpm to obtain solution A;

[0062] 2) Cool solution A to 21°C at a cooling rate of 6°C / h. At this time, the solution is still clear, indicating that WS-23 is still in a complete solution state. Add 14g WS-23 seed crystals (WS obtained by rapid cooling and spontaneous crystallization) -23), stir at 21°C at a constant temperature of 400rpm for 1h for the first crystallization, keep the stirring speed and continue to cool down to 0°C at a cooling rate of 6°C / h, and carry out the second crystallization. Suction filter with a cold Buchner funnel, wash, and dry in a vacuum oven at 40°C for 12 hours to obtain N,2,3-trimethyl-2-isopropylbutanamide with the targe...

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Abstract

The invention discloses a N,2,3-trimethyl-2-isopropylbutanamide crystal with a short rod shape and a crystallization process thereof. The process includes the following steps: 1) dissolving N,2,3-trimethyl-2-isopropylbutanamide in a long rod shape in a solvent to obtain solution A; 2) adding seed crystals after cooling solution A , carry out the first crystallization, continue to lower the temperature until the second crystallization is completed, and obtain N,2,3-trimethyl-2-isopropylbutanamide crystals with the target crystal shape. In the present invention, by optimizing the crystallization process of N,2,3-trimethyl-2-isopropylbutanamide crystals, a short rod-shaped crystal morphology with significantly reduced aspect ratio is obtained, which is better than that of existing crystals. The crystals obtained by the process have better fluidity and can effectively reduce the contact area between particles, thereby achieving the purpose of reducing or preventing the crystal agglomeration of N,2,3-trimethyl-2-isopropylbutanamide. The crystallization process of the invention has simple operation, controllable conditions, good reproducibility of obtained crystal shape, and easy realization of industrialized production.

Description

technical field [0001] The invention relates to the technical field of chemical engineering crystallization, in particular to a N,2,3-trimethyl-2-isopropylbutanamide crystal with a short rod shape and a crystallization process thereof. Background technique [0002] N,2,3-trimethyl-2-isopropylbutyramide (2-Isopropyl-N,2,3-trimethylbutyramide, WS-23), the molecular formula is C 10 h 21 NO, its chemical structural formula is shown in Formula I, its molecular weight is 171.28, and its melting point is 62-64°C. [0003] [0004] WS-23 is almost insoluble in water, soluble in alcohol and oil, and is a new type of cooling agent. Because it can give products a cool and fresh feeling, it is widely used in chewing gum, toothpaste, candy, jelly, jam, starch food, dairy products, meat products, cigarettes, medicines and other products. Compared with WS-23, the shortcomings of traditional cooling agents such as menthol are very obvious: when the dosage is low, there is no cooling e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C233/05
Inventor 李亚军梁磊
Owner GUANGDONG PROVINCIAL BIOENGINEERING INST (GUANGZHOU SUGARCANE IND RES INST)
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