CN104817468A - Glycine preparation method - Google Patents
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Abstract
The present invention discloses a glycine preparation method, which specifically comprises: carrying out alkaline hydrolysis on hydantoin, ammonia and water for 30-300 min at a temperature of 100-180 DEG C under reaction pressure of 0.1-6.0 MPa to obtain a glycine aqueous solution, crystallizing, carrying out solid-liquid separation, and collecting the solid to obtain the glycine. The method of the present invention has characteristics of simple operation, low cost, no salt-containing wastewater emission, ammonia recycling, no acid and alkali consumption, good economic benefits, and good environmental benefits.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of preparation method of glycine.
Background technology
Glycine is a kind of important medicine chemical material, be used alone and with Sodium Glutamate etc. with the use of making seasonings, also for the synthesis of wine, brewage goods; In medical, can be used as amino acid preparation, the buffer reagent of duomycin and the synthesis material as golden Sen Shi medicine L-3,4 dihydroxyphenylalanine; The additive of cream, oleomargarine and cheese can also be used as, with quality guaranteed period extended period; Biochemical reagents and solvent is used as in organic synthesis and biological chemistry; In agricultural chemicals, it is the raw material of herbicide glyphosate.Nearly 800,000 tons of the glycine output in the whole world, China is global maximum glycine producing country, but main industrial grade glycine of producing for glyphosate, the production main method due to current amino acetic acid in China mainly contains following three kinds:
(1) chloroactic acid method: first all dropped in reactor by urotropine, then add ammoniacal liquor, then drip Mono Chloro Acetic Acid, reacts at 30 DEG C ~ 50 DEG C, is incubated 3 hours, then analyses through alcohol, obtain product at 72 DEG C ~ 78 DEG C.But the method exists the by products such as ammonium chloride is difficult to removing, poor product quality, refining cost is high; Catalyzer urotropine cannot reclaim, and production cost is high, long reaction time.The method is the technique that amino acetic acid in China manufacturing enterprise generally adopts, and its major cause is that Mono Chloro Acetic Acid is cheaply easy to get, but this process environments pollutes comparatively serious; Moreover the organic impuritys such as the method by-product iminodiethanoic acid, nitrilotriacetic acid(NTA), methylene Padil, cause the purifying of glycine comparatively difficult, greatly limit the use in food, pharmaceutical industries of glycine.
(2) Shi Teleikefa is improved: the method is American-European, Japanese widely used technique; the method take hydroxyacetonitrile as raw material; glycine is prepared through operations such as direct ammonification, alkaline hydrolysis, deamination, acidifying, decolouring, concentrated and purifying; the advantage of this technique is that product is easily refined; production cost is lower, is applicable to large-scale production.But it is harsh that the shortcoming of the method is process conditions, reacted de-salting operation is more numerous and diverse, reaction scheme is longer, glycine and inorganic salt, iminodiethanoic acid, nitrilotriacetic acid(NTA) separation difficulty, especially glycine and by product iminodiethanoic acid separation difficulty, impurity maximum in the glycine product obtained is sodium sulfate and iminodiethanoic acid, effectively sodium sulfate can be removed through repeatedly recrystallization, but the content of iminodiethanoic acid but has no obvious reduction, this had a strong impact on glycine at glycine at food, use in pharmaceutical industries, and the high-content of iminodiethanoic acid even can affect the application of glycine in agricultural chemicals glyphosate in glycine.
(3) direct glycolylurea method: the method with hydroxyacetonitrile and carbon ammonium for raw material, its hydroxyacetonitrile, ammonia, carbonic acid gas, water are 1:4:2:46 according to molar ratio, through high-temperature high-voltage reaction, ammonia excretion, carbonic acid gas, generate glycine solution, glycine product is obtained through decolouring, concentrated, crystallisation by cooling, this production technique is the most clean production technique at present, only hydroxyacetonitrile and water is consumed in glycine production process, production cost is low, do not produce any inorganic salt, glycine separation and purification is simple.But have problems equally, in glycine production process, produce some organic impuritys as hydantoic acid, hydantoic acid acid amides, glycine dipeptidase, glycine tripeptide, 2,5-diketopiperazines, G-NH2 and unreacted glycolylurea, these compounds as shown in Figure 1.In addition to the impurities discussed above, also can produce iminodiethanoic acid, nitrilotriacetic acid(NTA) impurity, its reason producing these impurity be due to hydroxyacetonitrile first with ammonia react, generate aminoacetonitriles, then under the effect of carbonic acid gas, ring is become, by a small amount of ammonia solution, High Temperature High Pressure, glycolylurea ring is unstable, resolves into glycine and carbonic acid gas, ammonia.But in this process, the incomplete decomposing of glycolylurea ring, cause producing hydantoic acid, hydantoic acid acid amides, glycine dipeptidase, glycine tripeptide, 2, the impurity such as 5-diketopiperazine, G-NH2, and the aminoacetonitriles generated continues to react with hydroxyacetonitrile, generate iminodiacetonitrile, ammonia three acetonitrile, iminodiethanoic acid, nitrilotriacetic acid(NTA) impurity is finally produced through being hydrolyzed, these impurity effects are to the quality of glycine, especially iminodiethanoic acid, nitrilotriacetic acid(NTA) impurity containing trace in glycine, can affect the use in food, pharmaceutical industries of glycine.Moreover because the carbon nitrogen triple bond in cyanogen root is very easily polymerized, particularly has more brown or black pyropolymer and generate in ammonification and alkaline hydrolysis process, the later stage wishes to get the Glycine crystals of white, needs to decolour with gac; In addition, in actual production process, reaction mass can have corrosion to a certain degree to production unit, thus cause in material containing certain metal ion, and iminodiethanoic acid in impurity, nitrilotriacetic acid(NTA) are all good complexing agents, therefore in feed liquid, metal ion all exists with metal complex form and is difficult to be separated, and affects appearance color and the purity of glycine.
Therefore, be badly in need of finding a kind of glycine production technique can avoiding by-product inorganic salt, organic impurity, glycine purity is high, can meet the application in food, pharmaceutical industries.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of preparation method of glycine, by-product inorganic salt, organic impurity can be avoided as hydantoic acid, hydantoic acid acid amides, glycine dipeptidase, glycine tripeptide, 2,5-diketopiperazine, G-NH2, glycolylurea, iminodiethanoic acid, nitrilotriacetic acid(NTA), glycine yield is high, do not need recrystallization, reach food grade, pharmaceutical grade requirement completely.
For achieving the above object, through studying for a long period of time, find that ammonia or ammoniacal liquor can impel glycolylurea depth hydrolysis, but do not consume ammonia or ammoniacal liquor, and can be reclaimed by simple effective method, ammonia can recycled to the hydrolysing step of glycolylurea.Glycolylurea complete hydrolysis can be become glycine by this method, improves crystalline mother solution quality, well solves and reduces costs, reduce material consumption energy consumption, really realize cleaner production, do not consume any soda acid, do not produce any salt and brine waste thereof, improve yield and the quality of product.
The chemical equation that glycolylurea ammonia hydrolysis reaction prepares glycine is as follows:
For this reason, the present invention proposes following technical scheme:
A kind of preparation method of glycine, to comprise the steps: glycolylurea, ammonia and water in temperature to be 100 DEG C ~ 180 DEG C, reaction pressure is alkaline hydrolysis 30min ~ 300min under 0.1MPa ~ 6.0MPa condition, obtains glycine solution, crystallization, collects solid and obtains glycine.Preferably, alkaline hydrolysis temperature is 140 DEG C ~ 165 DEG C; Reaction times is 120min ~ 180min; Reaction pressure is 3.0MPa ~ 5.0MPa.
Preferably, also comprise while collecting solid and reclaim filtrate, and by the filtrate cycle of recovery to alkaline hydrolysis step; Also comprise before crystallization and glycine solution is carried out ammonia excretion and carbonic acid gas, reclaim ammonia, and the ammonia of recovery is circulated to alkaline hydrolysis step.
Preferred, also comprise decolouring and enrichment step before described crystallization.
Preferably, described ammonia is ammonia, liquefied ammonia or ammoniacal liquor, wherein the ammoniacal liquor preferred mass mark ammoniacal liquor that is greater than 15%.
Preferably, the molar ratio of described glycolylurea, ammonia and water is 1:1 ~ 8.0:15 ~ 50; Preferred, the molar ratio of glycolylurea, ammonia and water is 1:2 ~ 5.0:25 ~ 35; The purity of glycolylurea is more than 95%.Excess of ammonia, the decomposition of glycolylurea is conducive under high temperature, high pressure, if ammonia is very few, cause glycolylurea not thorough in hydrolytic process, produce some intermediate products as impurity such as hydantoic acid, hydantoic acid acid amides, G-NH2s, and if ammonia is very few, the pH of reaction system is low, also can produce the impurity such as glycine dipeptidase, glycine tripeptide, 2,5-diketopiperazines, the above-mentioned situation of the low same appearance of temperature.The yield of the reaction system water yield to glycine has the importance to closing, and the water yield should not very little or too much, very little or all can reduce the yield of glycine too much.
Preferably, the method for described ammonia excretion and carbonic acid gas is that air-extraction or negative pressure steam division, and particularly preferably negative pressure steams division.
Preferred, the temperature that described negative pressure steams division is 10 DEG C ~ 100 DEG C, and preferable temperature is 45 DEG C ~ 75 DEG C, and the ammonia of recovery is circulated to glycolylurea hydrolysing step.When ammonia excretion, the too high glycine moiety that causes of temperature is polymerized, and the hydrochloric acid of glycine solution is deepened, and brings difficulty to decolouring.
Preferably, described decolouring is one or more in activated carbon decolorizing, film decolouring or resin decolorization, and be particularly preferably film decolouring, film uses nanofiltration membrane.
Preferably, it is 25% ~ 36% (w/w) that described simmer down to is evaporated to Glycine Levels under temperature is 30 DEG C ~ 100 DEG C conditions, and concentrated condensate water circulatory is to the hydrolysis water of glycolylurea.Concentrated temperature is not easily too high, and temperature, higher than 75 DEG C, obtains glycine with yellow, its reason be temperature higher than 75 DEG C, glycine can generating portion polymerization, causes the color burn of mother liquor.
Preferably, described crystallization is crystallisation by cooling under temperature is 0 DEG C ~ 25 DEG C conditions, and preferred temperature is 0 DEG C ~ 10 DEG C.
Beneficial effect of the present invention is:
(1) take glycolylurea as raw material, avoid and use highly toxic substance sodium cyanide, prussic acid and hydroxyacetonitrile, reaction system cleans, and does not have the by products such as inorganic acid salt, iminodiethanoic acid, nitrilotriacetic acid(NTA) to produce, glycine purity is high, remains without chlorion, metal ion;
(2) using ammonia or ammoniacal liquor as hydrolytic reagent, with traditional mineral alkali as compared with sodium hydroxide, potassium hydroxide, hydrated barta, calcium hydroxide, carbonate, supercarbonate etc., ammonia or ammoniacal liquor can reclaim and reuse after hydrolysis, hydrolysis reaction does not consume any soda acid in fact, does not produce any brine waste;
(3) the glycine purity obtained is high, without the need to carrying out recrystallization repeatedly, the glycine of food grade, pharmaceutical grade can be obtained, not containing analogue iminodiethanoic acid, nitrilotriacetic acid(NTA), 2 in glycine, the organic impuritys such as 5-diketopiperazine, glycine separation and purification simply, easily operates, yield is high, environmental protection.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearly, the invention provides following accompanying drawing:
Fig. 1 is the impurity that direct glycolylurea method glycine is produced.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.The experimental technique of unreceipted actual conditions in embodiment, the usually conveniently conditioned disjunction condition of advising according to manufacturer.
Embodiment 1
Prepare a method for glycine, comprise the steps:
In autoclave, add glycolylurea and 540 grams of water that 105.3g massfraction is 95%, be warming up to 165 DEG C, the pressure controlling reaction system is 3.2MPa, then stirs 3 hours at this temperature; After reaction terminates, be cooled to room temperature (18 ~ 25 DEG C), pressure release, to normal pressure, obtains glycine solution, and this aqueous solution is yellowish brown; By glycine solution by negative pressure ammonia excretion and carbonic acid gas under 70 DEG C of conditions, the glycine solution after ammonia excretion and carbonic acid gas carries out film decolouring, and the glycine solution after decolouring is colourless transparent liquid, i.e. glycin mother liquid; Then by glycin mother liquid concentrating under reduced pressure at 65 DEG C, being concentrated into glycine concentration is 33% (w/w), is then cooled to 0 DEG C, suction filtration separates out glycine crystallization, crystallization is dried, and obtain glycine, the glycine crystallization mother liquid after suction filtration is circulated to the hydrolysing step of glycolylurea.
Utilize the composition of ion chromatography glycine solution.Result shows, the transformation efficiency of glycolylurea is 96%, and glycine yield only has 65%, and by product is G-NH2, glycine dipeptidase and polypeptide, hydantoic acid, hydantoic acid acid amides, 2,5-diketopiperazine, accounts for 35% in glycolylurea by product and unreacted glycolylurea.The present embodiment obtains 30.8g glycine, and yield is 39.4%, and purity is 96%, and its impurity is mainly hydantoic acid, hydantoic acid acid amides and glycolylurea, and glycine amount residual in glycine crystallization mother liquid is 19.2 grams.After glycine crystallization mother liquid being circulated to the hydrolysing step of glycolylurea, the average yield of final glycine is 66.5%, and the purity of glycine is 93% ~ 96%.
Embodiment 2
Prepare a method for glycine, comprise the steps:
In autoclave, add 105.3g massfraction is the glycolylurea of 95%, the ammoniacal liquor 272g of 25% and water 336g, is warming up to 165 DEG C, and the pressure controlling reaction system is 4.2MPa, then stirs 2 hours at this temperature; After reaction terminates, be cooled to room temperature (18 ~ 25 DEG C), pressure release, to normal pressure, obtains glycine solution, and this aqueous solution is yellowish brown; By glycine solution by ammonia excretion and carbonic acid gas under negative pressure 70 DEG C of conditions, the glycine solution after ammonia excretion and carbonic acid gas carries out film decolouring, and the glycine solution after decolouring is colourless transparent liquid, i.e. glycin mother liquid; By the glycin mother liquid obtained concentrating under reduced pressure at temperature is 65 DEG C, being concentrated into glycine concentration is 33% (w/w), is then cooled to 0 DEG C, the glycine crystallization that suction filtration is separated out, crystal is dried, and obtain glycine, the glycine crystallization mother liquid after suction filtration is circulated to the hydrolysing step of glycolylurea.
Utilize the composition of ion chromatography glycine solution.Result shows, and the transformation efficiency of glycolylurea is 100%, the yield 98% of glycine, and by product is glycine dipeptidase and polypeptide, 2,5-diketopiperazines, accounts for 2% in glycolylurea by product.The present embodiment obtains 60.6g glycine, and yield is 80.4%, and purity is 99.5%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.Glycine amount residual in glycine crystallization mother liquid is 13.2 grams, after being circulated to the hydrolysing step of the glycolylurea of next time, the average yield of final glycine is 99%, and the purity of glycine is 99% ~ 101%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.
Embodiment 3
Prepare a method for glycine, comprise the steps:
Add in autoclave 102.0g massfraction be 98% glycolylurea, massfraction be 60% ammoniacal liquor 141.7g and water 303g, be warming up to 160 DEG C, the pressure controlling reaction system is 4.7MPa, then stirs 2 hours at this temperature; After reaction terminates, be cooled to room temperature (18 ~ 25 DEG C), pressure release, to normal pressure, obtains glycine solution, and this aqueous solution is yellowish brown; By glycine solution by negative pressure ammonia excretion and carbonic acid gas under 75 DEG C of conditions, the glycine solution after ammonia excretion and carbonic acid gas carries out film decolouring, and the glycine solution after decolouring is colourless transparent liquid, i.e. glycin mother liquid; By the glycin mother liquid concentrating under reduced pressure under 70 DEG C of conditions obtained, being concentrated into glycine concentration is 35% (w/w), is then cooled to 0 DEG C, the glycine crystallization that suction filtration is separated out, dry, obtain glycine, the glycine crystallization mother liquid after suction filtration is circulated to the hydrolysing step of glycolylurea.
Utilize the composition of ion chromatography glycine solution.Result shows, and the transformation efficiency of glycolylurea is 100%, the yield 99% of glycine, and by product is glycine dipeptidase and polypeptide, 2,5-diketopiperazines, accounts for 1% in glycolylurea by product.The present embodiment obtains glycine solid 63.5g, and yield is 85.4%, and purity is 99.9%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.Glycine amount residual in glycine crystallization mother liquid is 10.2 grams, after being circulated to the hydrolysing step of the glycolylurea of next time, the average yield of final glycine is 99%, and the purity of glycine is 99% ~ 101%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.
Embodiment 4
Prepare a method for glycine, comprise the steps:
The massfraction adding 102.0g in autoclave is 98% glycolylurea and water 360g, and enclosed high pressure reactor, then passes into the ammonia of 68g in reactor, after logical ammonia terminates, be rapidly heated to 160 DEG C, controlling reaction system pressure is 4.5MPa, stirs 2 hours at this temperature; After reaction terminates, be cooled to room temperature (18 ~ 25 DEG C), pressure release, to normal pressure, obtains glycine solution, and this aqueous solution is yellowish brown; Glycine solution is heated to ammonia excretion and carbonic acid gas under 75 DEG C of conditions by negative pressure, and the glycine solution after ammonia excretion and carbonic acid gas carries out film decolouring, and the glycine solution after decolouring is colourless transparent liquid, i.e. glycin mother liquid; Then the glycin mother liquid obtained is carried out concentrating under reduced pressure under 70 DEG C of conditions, being concentrated into glycine concentration is 35% (w/w), then 0 DEG C is cooled to, the glycine crystallization that suction filtration is separated out, dry, obtain glycine, the glycine crystallization mother liquid after suction filtration is circulated to the hydrolysing step of glycolylurea.
Utilize the composition of ion chromatography glycine solution.Result shows, and the transformation efficiency of glycolylurea is 100%, the yield 99% of glycine, and by product is glycine dipeptidase and polypeptide, 2,5-diketopiperazines, is about 1% in glycolylurea by product.The present embodiment obtains glycine solid 63.5g, and yield is 85.4%, and purity is 99.9%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.Glycine amount residual in glycine crystallization mother liquid is 10.2 grams, after being circulated to the hydrolysing step of the glycolylurea of next time, the average yield of final glycine is 99%, and the purity of glycine is 99% ~ 101%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.
Embodiment 5
Prepare a method for glycine, comprise the steps:
In autoclave, add glycolylurea and water 630g that 102.0g massfraction is 98%, enclosed high pressure reactor, then passes into the ammonia of 85g in reactor, after logical ammonia terminates, be rapidly heated to 155 DEG C, the pressure controlling reaction system is 4.1MPa, stirs 3 hours at this temperature; After reaction terminates, be cooled to room temperature (18 ~ 25 DEG C), pressure release, to normal pressure, obtains glycine solution, and this aqueous solution is yellowish brown; Glycine solution is heated to 75 DEG C of ammonia excretions and carbonic acid gas by negative pressure, and the glycine solution after ammonia excretion and carbonic acid gas carries out film decolouring, and the glycine solution after decolouring is colourless transparent liquid, i.e. glycin mother liquid; By the glycin mother liquid concentrating under reduced pressure at 70 DEG C obtained, being concentrated into glycine concentration is 35% (w/w), then 0 DEG C is cooled to, the glycine crystallization that suction filtration is separated out, and collect glycine crystallization mother liquid, crystallization is dried, and obtain glycine, the glycine crystallization mother liquid after suction filtration is circulated to the hydrolysing step of glycolylurea.
Utilize the composition of ion chromatography glycine solution.Result shows, and the transformation efficiency of glycolylurea is 100%, the yield 99% of glycine, and by product is glycine dipeptidase and polypeptide, 2,5-diketopiperazines, accounts for 1% in glycolylurea by product.The present embodiment obtains 63.5g glycine solid, and yield is 85.4%, and purity is 99.9%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.Glycine amount residual in glycine crystallization mother liquid is 10.2 grams, after being circulated to the hydrolysing step of the glycolylurea of next time, the average yield of final glycine is 99%, and the purity of glycine is 99% ~ 101%, reaches the quality standard of food grade, pharmaceutical grade glycine by analysis completely.
In above-described embodiment, the molar ratio of glycolylurea, ammonia and water is 1:0 ~ 8.0:15 ~ 50, and hydrolysising reacting temperature is 100 DEG C ~ 180 DEG C, and reaction pressure is 0.1MPa ~ 6.0MPa, and the reaction times is that 30min ~ 300min all can realize goal of the invention; Preferably, the molar ratio of glycolylurea, ammonia and water is 1:2 ~ 5.0:25 ~ 35, and hydrolysising reacting temperature is 140 DEG C ~ 165 DEG C, and the reaction times is 120min ~ 180min, and reaction pressure is 3.0MPa ~ 5.0MPa.In ammonia excretion and carbonic acid gas, Heating temperature is 10 DEG C ~ 100 DEG C and can realizes, and preferable temperature is 45 DEG C ~ 75 DEG C; In concentrated, thickening temperature is 30 DEG C ~ 100 DEG C, and temperature is that 45 DEG C ~ 65 DEG C effects are better, and in crystallization, Tc is 0 DEG C ~ 25 DEG C, and Tc is that 0 DEG C ~ 10 DEG C effects are better.
What finally illustrate is, above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by above preferred embodiment to invention has been detailed description, but those skilled in the art are to be understood that, various change can be made to it in the form and details, and not depart from claims of the present invention limited range.
Claims (10)
1. a preparation method for glycine, is characterized in that, to comprise the steps: glycolylurea, ammonia and water in temperature to be 100 DEG C ~ 180 DEG C, reaction pressure is alkaline hydrolysis 30min ~ 300min under 0.1MPa ~ 6.0MPa condition, obtain glycine solution, crystallization, collect solid and obtain glycine.
2. the preparation method of glycine according to claim 1, is characterized in that: also comprise while collecting solid and reclaim filtrate, and by the filtrate cycle that reclaims to alkaline hydrolysis step; Also comprise before crystallization and glycine solution is carried out ammonia excretion and carbonic acid gas, reclaim ammonia, and the ammonia of recovery is circulated to alkaline hydrolysis step.
3. the preparation method of glycine according to claim 1, is characterized in that: also comprise decolouring and enrichment step before described crystallization.
4. the preparation method of glycine according to any one of claims 1 to 3, is characterized in that: described ammonia is ammonia, liquefied ammonia or ammoniacal liquor.
5. the preparation method of glycine according to claim 1, is characterized in that: the molar ratio of described glycolylurea, ammonia and water is 1:1 ~ 8.0:15 ~ 50.
6. the preparation method of glycine according to claim 1, is characterized in that: the method for described ammonia excretion and carbonic acid gas is that air-extraction or negative pressure steam division.
7. the preparation method of glycine according to claim 6, is characterized in that: the temperature that described negative pressure steams division is 10 DEG C ~ 100 DEG C.
8. the preparation method of glycine according to claim 1, is characterized in that: described decolouring is one or more in activated carbon decolorizing, filter membrane decolouring or resin decolorization.
9. the preparation method of glycine according to claim 1, is characterized in that: it is 25% ~ 36% (w/w) that described simmer down to is evaporated to Glycine Levels under temperature is 30 DEG C ~ 100 DEG C conditions.
10. the preparation method of glycine according to claim 1, is characterized in that: described crystallization is crystallisation by cooling under temperature is 0 DEG C ~ 25 DEG C conditions.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108003077A (en) * | 2017-12-21 | 2018-05-08 | 河北威远生物化工有限公司 | A kind of preparation of amino-acid compound and purification process |
| CN109678744A (en) * | 2017-10-18 | 2019-04-26 | 阳泉煤业（集团）有限责任公司 | A kind of method that serialization prepares glycine |
| CN113105352A (en) * | 2021-04-16 | 2021-07-13 | 铂尊投资集团有限公司 | Method for preparing food-grade and feed-grade zinc glycinate and implementation device thereof |
| CN113861056A (en) * | 2021-10-02 | 2021-12-31 | 上海弘渼生物科技有限公司 | Synthetic method of hydrophilic micromolecule amino acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241599A (en) * | 2011-05-07 | 2011-11-16 | 安徽国星生物化学有限公司 | Method for preparing glycine |
| CN103880690A (en) * | 2014-04-03 | 2014-06-25 | 重庆紫光国际化工有限责任公司 | Environment-friendly clean production method of glycine |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241599A (en) * | 2011-05-07 | 2011-11-16 | 安徽国星生物化学有限公司 | Method for preparing glycine |
| CN103880690A (en) * | 2014-04-03 | 2014-06-25 | 重庆紫光国际化工有限责任公司 | Environment-friendly clean production method of glycine |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678744A (en) * | 2017-10-18 | 2019-04-26 | 阳泉煤业（集团）有限责任公司 | A kind of method that serialization prepares glycine |
| CN109678744B (en) * | 2017-10-18 | 2021-11-26 | 阳泉煤业（集团）有限责任公司 | Method for continuously preparing glycine |
| CN108003077A (en) * | 2017-12-21 | 2018-05-08 | 河北威远生物化工有限公司 | A kind of preparation of amino-acid compound and purification process |
| CN113105352A (en) * | 2021-04-16 | 2021-07-13 | 铂尊投资集团有限公司 | Method for preparing food-grade and feed-grade zinc glycinate and implementation device thereof |
| CN113861056A (en) * | 2021-10-02 | 2021-12-31 | 上海弘渼生物科技有限公司 | Synthetic method of hydrophilic micromolecule amino acid |
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