CN1107139A - Amino acetic acid producing method - Google Patents
Amino acetic acid producing method Download PDFInfo
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- CN1107139A CN1107139A CN 94115497 CN94115497A CN1107139A CN 1107139 A CN1107139 A CN 1107139A CN 94115497 CN94115497 CN 94115497 CN 94115497 A CN94115497 A CN 94115497A CN 1107139 A CN1107139 A CN 1107139A
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- padil
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- water
- acetic acid
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Abstract
The invented method uses urotropine, water, hydrocyanic acid bearing inorganics and ammonium bicarbonate as raw material and the amino acetic acid is produced by adopting heating and pressurizing productive process condition. Said method features easy controlling reaction, capable of circulating application of the mother liquid, without pollution, wide range of selecting raw material, high yield and product easy purified.
Description
The present invention relates to a kind of production method of Padil.
But the intermediate of Padil used as pesticides, the additive of food, feed and medicine, of many uses.What the Padil of China's production at present mainly adopted is chloroactic acid method, it is with Mono Chloro Acetic Acid, liquefied ammonia, water is raw material, under the condition of normal temperature, generate Padil through aminating reaction, this method needs to make sinking agent (produce 1 ton of Padil and need 40 tons of methyl alcohol approximately) with a large amount of methyl alcohol, and methyl alcohol can't all reclaim, approximately volatilize 1.1 tons of methyl alcohol of product per ton, polluted air not only, product cost is improved, produce 1 ton of finished product Padil simultaneously, also can give off nearly 300 kilograms of urotropines (hexamethylenetetramine) of making catalyzer, bring severe contamination to environment.A kind of production method of Padil is disclosed among the day disclosure special permission 49-127915, this method is to be raw material with formaldehyde, volatile salt and prussic acid, under 120 ℃～250 ℃ temperature, water vapor pressure condition, raw material is reacted, produce Padil, the side reaction of this method is many, and wayward, thereby reaction yield is low, Padil is difficult for purifying, and has be difficult for sloughing variegated on the product, has reduced the quality grade of product.
The objective of the invention is to provides a kind of production method of Padil at the prior art above shortcomings, and this method is the reaction yield height not only, and side reaction is few, need not any catalyzer, and mother liquor can be recycled, pollution-free, raw material is easy to get, and reaction is control easily, products obtained therefrom quality height.
The object of the present invention is achieved like this: inorganics, urotropine (hexamethylenetetramine), bicarbonate of ammonia and water with hydrogeneous cyanate radical are raw material, 120 ℃～250 ℃ temperature, 10～50 kilograms/cm
2Under the pressure condition, reacted 3～6 hours, again through the technological process of crystallization and purification, get final product Padil, principal reaction is:
The inorganics of the hydrogeneous cyanate radical in the formula, both can be liquid hydrogen cyanic acid, also can be water miscible prussic acid inorganic salt and water-insoluble prussic acid inorganic salt, when using water-fast prussic acid inorganic salt, must add acid earlier, make it produce prussic acid, be raw material again with prussic acid, urotropine in the formula also can change under reaction conditions of the present invention and can react with the prussic acid root, generates any material that contains methylene radical of second cyanogen, as formaldehyde, polyoxymethylene; Bicarbonate of ammonia in the formula also can be replaced by any water soluble salt of ammonia.
Heat in the reaction process, the purpose of pressurization is in order to realize the highly pressured hydrolysis of prussic acid root under the condition of catalyst-free, when temperature is lower than 120 ℃, reaction is carried out slowly, when being higher than 200 ℃, the easy polymerization reaction take place of resultant Padil, institute's plus-pressure is high more in the reaction, required time is short more, and side reaction is few more, and yield is high more, but in selective pressure, also to consider the ability to bear of equipment,, pressure range is chosen in 10～50 kilograms/cm according to the ability to bear of the present generalization construction equipment of China
2Between be advisable.In production method of the present invention, water is the raw material that participates in reaction, is again solvent, therefore, carry out smoothly for making reaction, must use a certain amount of water, cross when low when the consumption of water, react and be difficult for carrying out, when the consumption of water is too high, resultant concentration is on the low side, is unfavorable for that product separation purifies, so the mol ratio that the consumption of water is chosen in water and prussic acid root is between 1: 20～100.
The present invention compared with prior art has the following advantages: 1, because the main by product of the inventive method is iminodiethanoic acid, azulimic acid, aminoacetonitriles, polyglycine, so mother liquor can be recycled, make them be converted into product again, and owing to adopt pressurization to make the method for prussic acid root hydrolysis, need not use catalyzer, therefore both reduced production cost, making does not again have discharge in the production process, free from environmental pollution; 2, the material choice scope is wide, can select proper raw material to reduce product cost according to market conditions; 3, owing to adopt the manufacturing condition of the pressurization of heating, not only must not use catalyzer, and shortened the reaction times, and improved production efficiency, reduced side reaction, make reaction be easy to control, improved reaction yield, the recovery of being convenient to product is purified, the Padil that utilizes the inventive method to produce, purity can reach 98%, and non-variegation.
Below in conjunction with specific embodiment in detail, production method of the present invention is described in detail.
Embodiment 1: with 360 ml waters, 6.48 gram prussic acid, 5.6 gram urotropines, bicarbonate of ammonia is airtight in 500 milliliters of autoclaves is heated to 150 ℃ for 79 grams, is forced into 40 kilograms/cm
2, keep this temperature, pressure after 5 hours, the cooling decompression, sampling analysis, the transformation efficiency of Padil reaches 75%, adopts crystallization process to isolate Padil, and mother liquor then can continue to recycle.
Embodiment 2: in 500 milliliters of autoclaves, add 6.75 gram prussic acid, 5.6 gram urotropines, 59.25 gram bicarbonate of ammonia, 180 milliliters watertight post-heating to 170 ℃, be forced into 30 kilograms/cm
2, keep 5 hours with this understanding after, cooling decompression, the transformation efficiency of sampling analysis Padil reaches 73%, adopts perfectly crystallization process to isolate Padil, mother liquor then can continue to recycle.
Embodiment 3: add 6.75 gram prussic acid, 7.5 gram formaldehyde, 39.5 gram bicarbonate of ammonia, 8.5 gram ammoniacal liquor, 150 ml waters in 500 milliliters of autoclaves after, airtightly be heated to 190 ℃, 20 kilograms/cm of pressure
2, kept this condition 4 hours, cooling decompression back sampling analysis, the transformation efficiency of Padil reaches 78%, and after the employing crystallization process was isolated the Padil method, mother liquor then can continue to recycle.
Embodiment 4: airtight heating to 200 ℃ behind adding 12.74 gram sodium cyanides, 7.5 gram polyoxymethylene, 13.38 gram ammonium chlorides, 270 ml waters in 500 milliliters of autoclaves is forced into 15 kilograms/cm
2, kept with this understanding 3 hours, cooling decompression back sampling analysis, the transformation efficiency of Padil reaches 78%, adds acid again Padil is separated, and after the employing crystallization process is isolated Padil, then can continue after the mother liquor desalination to recycle.
To adopt aforementioned production method production and isolated Padil, and after the employing recrystallization method is purified, the purity of Padil will be reached more than 98%.
Claims (2)
1, a kind of production method of Padil is characterized in that this method raw materials used inorganics and bicarbonate of ammonia for urotropine, water, hydrogeneous cyanate radical, and reaction conditions is 120 ℃～200 ℃ of temperature, 10～50 kilograms/cm of pressure
2, the reaction times is 3～6 hours.
2, the production method of Padil according to claim 1 is characterized in that reaction conditions is that temperature is 180 ℃～190 ℃, and pressure is 30～40 kilograms/cm
2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94115497 CN1107139A (en) | 1994-09-06 | 1994-09-06 | Amino acetic acid producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94115497 CN1107139A (en) | 1994-09-06 | 1994-09-06 | Amino acetic acid producing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1107139A true CN1107139A (en) | 1995-08-23 |
Family
ID=5037533
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94115497 Pending CN1107139A (en) | 1994-09-06 | 1994-09-06 | Amino acetic acid producing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1107139A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305836C (en) * | 2003-10-14 | 2007-03-21 | 重庆三峡英力化工有限公司 | Method for preparing glycine |
| CN1858036B (en) * | 2005-05-08 | 2010-04-28 | 邱高琼 | Environment friendly clean producing method for high purity amino acetic acid |
| CN1958559B (en) * | 2005-10-31 | 2010-12-08 | 安徽省安庆曙光化工(集团)有限公司 | Environmental protection clean technical method for synthesizing aminoacetic acid through fluid bed |
-
1994
- 1994-09-06 CN CN 94115497 patent/CN1107139A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305836C (en) * | 2003-10-14 | 2007-03-21 | 重庆三峡英力化工有限公司 | Method for preparing glycine |
| CN1858036B (en) * | 2005-05-08 | 2010-04-28 | 邱高琼 | Environment friendly clean producing method for high purity amino acetic acid |
| CN1958559B (en) * | 2005-10-31 | 2010-12-08 | 安徽省安庆曙光化工(集团)有限公司 | Environmental protection clean technical method for synthesizing aminoacetic acid through fluid bed |
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| C01 | Deemed withdrawal of patent application (patent law 1993) |