290.91 g of ammonium carbonate with a purity of 99.0% and also 750 g of deionized water were contributed to a 1000 ml pressure-resistant zirconium-lined activator with a feeding and also stirring gadget, as well as the temperature level was raised to 65 ° C. to acquire an aqueous ammonium carbonate solution. From the feed port of the activator, 142.5 g of a preheated 40wt% hydroxyacetonitrile liquid service (50 ° C, pH=3.0) was injected with a pressure pump, and also the molar ratio of hydroxyacetonitrile, ammonium carbonate and also water was 1:3:46.4, Throughout the procedure of adding the hydroxyacetonitrile aqueous remedy, the activator was warmed to 100 ° C. for response, as well as the stirring rate was 120 r/min, the speed of including the hydroxyacetonitrile liquid solution was 8.0 g/min, and the liquid level of the reaction product was 96%. After the addition of the aqueous hydroxyacetonitrile remedy, the reactor was sealed, and also the temperature was promptly elevated to 150 ° C. The stress in the reactor was 4.2 MPa, and also the response was proceeded by mixing as well as keeping for 3 hrs.
After the response was finished, the temperature level was decreased to about 100 ° C., and then the stress was launched to regular pressure. The acquired reaction feed liquid was poured into a beaker and cooled down to space temperature to acquire 1152 g of an aqueous solution including Glycin and ammonium bicarbonate. The response feed liquid was brown yellow. The web content of glycine in the reaction option by ion chromatography was 6.484 wt%, and also no glycine dipeptide, hydantoin, diketopiperazine, glycine tripeptide, glycinamide, iminodiacetic acid (iminodiacetonitrile), The yield of glycine was 99.6% (determined as hydroxyacetonitrile) from pollutants such as nitrilotriacetic acid (aminotriacetonitrile), hydantoin and hydantoin amide.
The response feed fluid obtained above is warmed to 100 ° C on an electrical furnace, and also the metal zirconium powder audit for about 305ppm of the total mass of the response feed fluid is included, and after that gets in the stripping tower to focus and get rid of ammonia and also carbon dioxide by stripping till say goodbye to. Free ammonia was spotted, and afterwards deionized water was contributed to obtain a glycine liquid service. The content of Glycin in the glycine aqueous service by ion chromatography was 15.5 wt%, as well as glycine dipeptide, hydantoin, diketopiperazine, glycine tripeptide, glycine were not detected. Contaminations such as aminoamide, iminodiacetic acid (iminodiacetonitrile), nitrilotriacetic acid (aminotriacetonitrile), hydantoic acid, hydantoic acid amide, etc. Those Glycin aqueous option goes through membrane layer decolorization therapy to obtain a pale yellow service after decolorization, and afterwards focused under minimized pressure in a vacuum concentration pot lined with zirconium material to a glycine content of 40% by weight, entering into an unrefined product condensation kettle lined with zirconium material Cool to room temperature to accomplish formation, obtain unrefined product condensation mommy liquor and also solid product by suction filtering, as well as dry the gotten strong item to get 57.58 grams of light yellow crystals (glycin crude product) whose primary material of Glycin is 97.5%. The condensation price was 75%.
The unrefined item formation mommy alcohol obtained by suction filtration is 124.75 grams in total, wherein the material of glycine is 15wt%, and the content of ammonium sulfate is 5.2 wt%. Phase-membrane electrodialysis has 3 chambers, particularly, the fluid chamber, the liquid chamber (light chamber) as well as the receiving chamber (concentration chamber). Throughout the desalination process, ammonium sulfate moves to the focus chamber. When the ammonium sulfate material in the feed chamber is minimized to less than 0.5 wt%, the Glycin is 15.72 wt%, and also the overall mass of the fluid in the feed chamber is 118.89 grams. After desalination by electrodialysis, the retention rate of glycine reaches 99.5%, the salt elimination rate reached 90.4%. The desalted Glycin option is reused to those minimized stress concentration action to get unrefined glycine.
The Glycin unrefined product obtained over was dissolved in water, then 1wt% of turned on carbon was included for decolorization treatment, as well as the activated carbon was divided by suction purification. The crystals are suction filteringed system and also dried to acquire a recrystallized glycine item, the main material of glycine is ≥ 99.9%, and also the item high quality gets to the nationwide requirement for food grade Glycin (GB25542-2010). The Glycin recrystallization mommy liquor acquired by suction filtration is recycled to the following set of glycine unrefined item recrystallization step. After the mom alcohol was reused, the complete return of Glycin was 99.5% (computed in hydroxyacetonitrile).
