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Method for catalytically synthesizing laminine by using solid and liquid phases

A technology of laminine and ethanol solution, applied in the field of preparation of high-purity laminine, can solve problems such as separation and purification difficulties

Inactive Publication Date: 2014-09-17
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of trimethylation rate, Na-Ni-Y doped molecular sieve has the highest and best selectivity, which also shows that the higher the doping rate, the better the catalytic effect, such as image 3 As shown, it can be seen from the figure that the catalytic efficiency of Na-Ni-Y doped molecular sieve with 6% nickel content is the highest in terms of trimethylation rate, but it can only reach 80%. Byproducts such as methylation are still as high as 20%, making separation and purification still very difficult. Even if an ion exchange column is used, the purity can only reach about 98.5%, and the yield of trimethylated products is only about 40%.

Method used

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  • Method for catalytically synthesizing laminine by using solid and liquid phases
  • Method for catalytically synthesizing laminine by using solid and liquid phases
  • Method for catalytically synthesizing laminine by using solid and liquid phases

Examples

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Embodiment 1

[0037] The present invention, a kind of method of solid-liquid two-phase catalytic synthesis laminin, specifically comprises the following steps:

[0038] (1) Select 100 g of NaY molecular sieves with a high silicon-aluminum ratio of 6.7, soak them in a saturated acidic nickel chloride solution for 24 hours, filter, and dry at 120° C. for 1 hour. The nickel content is 6.04%, and the average particle size is 1.1 μm to obtain Na- Ni-Y molecular sieve Ⅰ;

[0039] (2) Weigh 100g Na-Ni-Y type molecular sieve I, mix it with 100g nickel chloride hexahydrate powder, put it in a muffle furnace, and heat it stepwise. The specific heating procedure is: first, the temperature rises every minute Increase by 2°C, keep the temperature constant for 45 minutes when it rises to 90°C; then turn to increase by 1°C per minute, and keep the temperature constant for 30 minutes when it rises to 140°C; finally turn to increase by 2°C per minute, keep the temperature for 2 hours when it rises to 1200°C; ...

Embodiment 2

[0048] The present invention, a kind of method of solid-liquid two-phase catalytic synthesis laminin, specifically comprises the following steps:

[0049] (1) Select 100 g of NaY molecular sieves with a high silicon-aluminum ratio greater than 7.0, soak them in a saturated acidic nickel chloride solution for 24 hours, filter, and dry at 120°C for 1 hour. The nickel content is 6.11%, and the average particle size is 1.3 μm, to obtain Na- Ni-Y type molecular sieve Ⅰ;

[0050] (2) Weigh 100g Na-Ni-Y type molecular sieve I, mix it with 100g nickel chloride hexahydrate powder, put it in a muffle furnace, and heat it stepwise. The specific heating procedure is: first, the temperature rises every minute Increase by 2°C, keep the temperature constant for 45 minutes when it rises to 90°C; then turn to increase by 1°C per minute, and keep the temperature constant for 30 minutes when it rises to 140°C; finally turn to increase by 2°C per minute, keep the temperature for 2 hours when it r...

Embodiment 3

[0054] (1) Select 100 g of NaY molecular sieves with a high silicon-aluminum ratio greater than 7.0, soak them in a saturated acidic nickel chloride solution for 24 hours, filter, and dry at 120°C for 1 hour. The nickel content is 6.11%, and the average particle size is 1.3 μm, to obtain Na- Ni-Y type molecular sieve Ⅰ;

[0055] (2) Weigh 100g Na-Ni-Y type molecular sieve I, mix it with 100g nickel chloride hexahydrate powder, put it in a muffle furnace, and heat it stepwise. The specific heating procedure is: first, the temperature rises every minute Increase by 2°C, keep the temperature constant for 45 minutes when it rises to 90°C; then turn to increase by 1°C per minute, and keep the temperature constant for 30 minutes when it rises to 140°C; finally turn to increase by 2°C per minute, keep the temperature for 2 hours when it rises to 1200°C; while hot Pour the mixed material into 1L of water under stirring, stir to normal temperature, filter and dry to obtain Na-Ni-Y type...

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Abstract

The invention discloses a method of catalytically synthesizing laminine by using solid and liquid phases and belongs to the technical field of preparation of high-purity laminine. The method comprises the following steps: first, fully mixing a Na-Ni-Y type molecular sieve I and nickel chloride hexahydrate powder according to a certain weight ratio, heating the mixture grade by grade, and then cooling, filtering and drying to obtain a Na-Ni-Y type molecular sieve II with the nickel content of 12-14%; and then, adding the prepared Na-Ni-Y type molecular sieve II into a mixed solution of a zinc lysine complex and dimethyl carbonate, then adding a mixed solution of ammonia water and ammonium chloride and catalytically synthesizing laminine by using solid and liquid phases through controlling the process conditions. As the prepared Na-Ni-Y type molecular sieve II has relatively high catalytic activity, the selectivity and efficiency of solid-and-liquid two-phase catalytic synthesis of laminine are improved. The purity of the laminine prepared by the method is over 99%.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-purity laminacin, and in particular relates to a solid-phase stepwise high-temperature method for preparing ultra-highly doped nickel Y molecular sieves, and then passing the ultra-highly doped nickel Y molecular sieves through a solid-liquid two-phase catalytic synthesis method Preparation of high-purity laminin (salt). Background technique [0002] Kelp is the dry fronds of kelp, kelp, or pterophyte kelp, also known as kelp, lunbu, sea kelp, wakame, etc. It contains alginic acid, amino acids, polysaccharides, mannitol, phytol and a variety of Vitamins and rich iodine, it has various pharmacological effects such as antihypertensive, blood lipid regulation, anticoagulant, antibacterial, hypoglycemic, antiviral, antitumor, immune regulation, antiradiation, antifatigue, antioxidation, and hypoxia resistance . Laminin, also known as N-trimethyllysine, is the main active ingredient in ke...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/26B01J29/14
Inventor 李群王越李晓雯李子超赵昔慧倪偲王剑平张超
Owner QINGDAO UNIV
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