CN101787121A - New method for synthetizing polyaspartic acid by fumaric acid - Google Patents
New method for synthetizing polyaspartic acid by fumaric acid Download PDFInfo
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- CN101787121A CN101787121A CN 201010134371 CN201010134371A CN101787121A CN 101787121 A CN101787121 A CN 101787121A CN 201010134371 CN201010134371 CN 201010134371 CN 201010134371 A CN201010134371 A CN 201010134371A CN 101787121 A CN101787121 A CN 101787121A
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- acid
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- fumaric acid
- polyaspartic acid
- polyaspartic
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Abstract
The invention discloses a method for synthetizing polyaspartic acid by fumaric acid, which comprises the following steps of (1) fermenting and synthetizing L-polyaspartic acid by taking the fumaric acid and ammonia as raw materials and taking escherichia coli as a catalyst, wherein the molar ratio of the fumaric acid to the ammonia is 1:1; the dosage of the escherichia coli is 0.3-0.5 permillage of the total weight of the raw materials, the fermenting temperature is 36-40 DEG C and the fermenting time is 24 h; and (2) continuously carrying out polycondensation for 10-60min at the temperature of 180-250 DEG C by taking the rough L-polyaspartic acid which is not discolored and obtained in the step (1) as raw material to synthetize the polyaspartic acid. The method can realize the large scale and economization of the production of the polyaspartic acid.
Description
Technical field
The present invention relates to a kind of fumaric acid and NH
3Be raw material, fermentation method makes the L-aspartic acid, and with raw product L-aspartic acid, the disc type successive reaction aggregates into the large-scale production technology of poly aspartic acid.
Background technology
Poly aspartic acid is a kind of polymeric amino acid, artificial synthetic polypeptide, a kind of soluble high-molecular, nontoxic pollution-free, biodegradable environmentally friendly product, its purposes is very extensive, widely applies plant nutrition and industrial dispersion agent, water conditioner, agricultural chemicals, green ecological auxiliary agent etc.
As everyone knows, be that the synthetic poly-aspartic acid method of raw material mostly adopts intermittent type polycondensation method with the L-aspartic acid, the polycondensation time is long, and thermo-efficiency is low, the product efflorescence, Working environment is polluted in the product loading and unloading, and industrial scale is little, and the cost height is difficult to maximize and produces.
The present invention is based on above-mentioned technical background, propose a kind of new poly aspartic acid synthetic method, can realize maximization, economization that poly aspartic acid is produced.
Summary of the invention
The objective of the invention is to: provide a kind of novel method of using synthetizing polyaspartic acid by fumaric acid, with maximization, the economization of realizing that poly aspartic acid is produced.
Above-mentioned purpose of the present invention is achieved by following proposal:
A kind of method of utilizing synthetizing polyaspartic acid by fumaric acid is provided, may further comprise the steps:
1) being raw material with fumaric acid and ammonia, is the synthetic L-aspartic acid of catalyzer fermentation with intestinal bacteria, and wherein the mol ratio of fumaric acid and ammonia is 1:1; Colibacillary consumption is 3 of raw material gross weight ~ 5 ‰; Leavening temperature is 36 ~ 40 ℃, and leavening temperature is 24 hours;
2) the rough L-aspartic acid that had not decoloured that makes with step 1) is a raw material, under 180 ~ 250 ℃ through continuous polycondensation 10 ~ 60 minutes, synthesizing polyaspartic acid.
Step 2) described continuous polycondensation temperature is preferred 220 ~ 240 ℃; Preferred 20 ~ 40 minutes of described continuous polycondensation time.
Step 2) temperature of described continuous polycondensation preferably utilizes the deep fat heating to reach; Described deep fat maximum heating temperature is 320 ℃.
In described continuous polycondensation, can also in reactor, feed rare gas element and protect; The preferred N of described rare gas element
2
The specification of the L-aspartic acid of the rough no bleaching that described step 1) makes is as follows:
Content is 98%
Weight loss on drying 0.40%
Pb ≤0.001%
As ≤0.001%
By method synthetic poly aspartic acid of the present invention, product content is 40%, and viscosity-average molecular weight is between 3000 ~ 8000, and beta-protein matter content can synthesize the product of different viscosity-average molecular weights by the conditioned reaction temperature and the residence time about 70%.
Compared with prior art, the preparation method's of poly aspartic acid of the present invention beneficial effect is: the present invention is a raw material with the L-aspartic acid of rough no bleaching, directly apply to the continuous polycondensation synthesizing polyaspartic acid, not only saved production sequence, workable, and can realize maximizing and produce; In addition, the product colour that makes is shallow, and polycondensation process is not used other raw materials, and by product is carried low amounts of dust secretly except that water vapour, captures with fly-ash separator, and whole process of production is pollution-free.
Synthetic poly aspartic acid of the present invention, molecular structure has peptide bond, and end group has-NH
2(amino) and-the COOH(carboxyl) a large amount of existence, the visual different objects that use of the potential of hydrogen of product are regulated, product application is in extensive range, the cost performance height is particularly suitable for being applied to plant-growth regulator and fertilizer synergist, the green auxiliary agent of agricultural chemicals.Product biological degradation rate 28 days 〉=65%, LD50 〉=6000mg/Kgbw has reached European Union's standard, belongs to the top grade index.
Embodiment
Embodiment 1
Make and prepare poly aspartic acid with the following method:
1) being raw material with fumaric acid and ammonia, is the synthetic L-aspartic acid of catalyzer fermentation with intestinal bacteria, and wherein the mol ratio of fumaric acid and ammonia is 1:1; Colibacillary consumption is 3 ‰ of a raw material gross weight; Leavening temperature is 36 ℃, and leavening temperature is 24 hours;
2) the rough L-aspartic acid that had not decoloured that makes with step 1) is a raw material, the L-aspartic acid that in the continuous condensating reactor, adds 15 kilograms of described rough no bleachings with screw feeder, per minute, under 230 ℃ ± 2 ℃ through continuous polycondensation 30 minutes, during reactor fill N
2Protection per hour obtains 625 kilograms of anhydrous poly aspartic acids, and by-product water vapour is got rid of, and the product viscosity-average molecular weight is 7000, in prior art, uses through commodity L-aspartic acid refining and decolouring and compares as raw material, and cost reduces by 20%.
Embodiment 2
Make and prepare poly aspartic acid with the following method:
1) being raw material with fumaric acid and ammonia, is the synthetic L-aspartic acid of catalyzer fermentation with intestinal bacteria, and wherein the mol ratio of fumaric acid and ammonia is 1:1; Colibacillary consumption is 3 ‰ of a raw material gross weight; Leavening temperature is 38 ℃, and leavening temperature is 24 hours;
2) the rough L-aspartic acid that had not decoloured that makes with step 1) is a raw material, the L-aspartic acid that in the continuous condensating reactor, adds 15 kilograms of described rough no bleachings with screw feeder, per minute, under 240 ℃ ± 2 ℃ through continuous polycondensation 40 minutes, during reactor fill N
2Protection per hour obtains 610 kilograms of anhydrous poly aspartic acids, and by-product water vapour is got rid of, and the product viscosity-average molecular weight is 8500.
Embodiment 3
Make and prepare poly aspartic acid with the following method:
1) being raw material with fumaric acid and ammonia, is the synthetic L-aspartic acid of catalyzer fermentation with intestinal bacteria, and wherein the mol ratio of fumaric acid and ammonia is 1:1; Colibacillary consumption is 5 ‰ of a raw material gross weight; Leavening temperature is 40 ℃, and leavening temperature is 24 hours;
2) the rough L-aspartic acid that had not decoloured that makes with step 1) is a raw material, the L-aspartic acid that in the continuous condensating reactor, adds 15 kilograms of described rough no bleachings with screw feeder, per minute, under 190 ℃ ± 2 ℃ through continuous polycondensation 20 minutes, during reactor fill N
2Protection per hour obtains 650 kilograms of anhydrous poly aspartic acids, and by-product water vapour is got rid of, and the product viscosity-average molecular weight is 6000.
Claims (7)
1. method of utilizing synthetizing polyaspartic acid by fumaric acid may further comprise the steps:
1) being raw material with fumaric acid and ammonia, is the synthetic L-aspartic acid of catalyzer fermentation with intestinal bacteria, and wherein the mol ratio of fumaric acid and ammonia is 1:1; Colibacillary consumption is 3 of raw material gross weight ~ 5 ‰; Leavening temperature is 36 ~ 40 ℃, and fermentation time is 24 hours;
2) the rough L-aspartic acid that had not decoloured that makes with step 1) is a raw material, under 180 ~ 250 ℃ through continuous polycondensation 10 ~ 60 minutes, synthesizing polyaspartic acid.
2. the described method of utilizing synthetizing polyaspartic acid by fumaric acid of claim 1 is characterized in that: step 2) described continuous polycondensation temperature is 220 ~ 240 ℃.
3. the described method of utilizing synthetizing polyaspartic acid by fumaric acid of claim 1 is characterized in that: step 2) the described continuous polycondensation time is 20 ~ 40 minutes.
4. the described method of utilizing synthetizing polyaspartic acid by fumaric acid of claim 1 is characterized in that: step 2) temperature of described continuous polycondensation utilizes the deep fat heating to reach.
5. the described method of utilizing synthetizing polyaspartic acid by fumaric acid of claim 4, it is characterized in that: described deep fat maximum heating temperature is 320 ℃.
6. the described method of utilizing synthetizing polyaspartic acid by fumaric acid of claim 1 is characterized in that: in described continuous polycondensation, feed rare gas element and protect in reactor.
7. the described method of utilizing synthetizing polyaspartic acid by fumaric acid of claim 6, it is characterized in that: described rare gas element is N
2
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| CN 201010134371 CN101787121A (en) | 2010-03-29 | 2010-03-29 | New method for synthetizing polyaspartic acid by fumaric acid |
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| CN 201010134371 CN101787121A (en) | 2010-03-29 | 2010-03-29 | New method for synthetizing polyaspartic acid by fumaric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196410A (en) * | 2021-12-30 | 2022-03-18 | 河北萌帮水溶肥料股份有限公司 | Saline-alkali soil conditioner and preparation method and use method thereof |
| CN114957650A (en) * | 2022-06-11 | 2022-08-30 | 田钟 | Preparation method of polyaspartic acid potassium and application of polyaspartic acid potassium in plant growth promoter |
| CN114957650B (en) * | 2022-06-11 | 2024-05-10 | 新疆腾域鸿源农业科技有限公司 | Preparation method of potassium polyaspartate and application of potassium polyaspartate in plant growth promoter |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1611526A (en) * | 2003-10-28 | 2005-05-04 | 哈尔滨工业大学 | Wet synthesis of poly aminosuccinic acid by microwave chemical technique |
| CN101130798A (en) * | 2007-08-24 | 2008-02-27 | 安徽华恒生物工程有限公司 | Method for preparing sodium L-aspartate by bio-enzyme |
-
2010
- 2010-03-29 CN CN 201010134371 patent/CN101787121A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1611526A (en) * | 2003-10-28 | 2005-05-04 | 哈尔滨工业大学 | Wet synthesis of poly aminosuccinic acid by microwave chemical technique |
| CN101130798A (en) * | 2007-08-24 | 2008-02-27 | 安徽华恒生物工程有限公司 | Method for preparing sodium L-aspartate by bio-enzyme |
Non-Patent Citations (1)
| Title |
|---|
| 《化工进展》 20010330 方莉等 聚天门冬氨酸的合成及其应用 24-28页 权利要求1-7 , 第3期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196410A (en) * | 2021-12-30 | 2022-03-18 | 河北萌帮水溶肥料股份有限公司 | Saline-alkali soil conditioner and preparation method and use method thereof |
| CN114196410B (en) * | 2021-12-30 | 2023-12-26 | 河北萌帮水溶肥料股份有限公司 | Saline-alkali soil conditioner and preparation method and use method thereof |
| CN114957650A (en) * | 2022-06-11 | 2022-08-30 | 田钟 | Preparation method of polyaspartic acid potassium and application of polyaspartic acid potassium in plant growth promoter |
| CN114957650B (en) * | 2022-06-11 | 2024-05-10 | 新疆腾域鸿源农业科技有限公司 | Preparation method of potassium polyaspartate and application of potassium polyaspartate in plant growth promoter |
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Open date: 20100728 |