Copolymerization derivative of poly-asparagic acid and synthetic method

[0007] Embodiment 1: The structural formula of the polyaspartic acid copolymer derivative of the present embodiment is:

[0008] In the formula, R is H, (CH 3 ) 2 CH, (CH 3 ) 2 CHCH 2 、CH 3 CH 2 CH(CH 3 ), HOCH 2 、CH 3 CH(OH), HSCH 2 or HOOCCH 2 CH 2 , the range of y/(y+x) is 0.1-0.9, and the range of x+y is 7-70. The optimum range of y/(y+x) in this embodiment is 0.1-0.5, and the optimum range of x+y is 9-30.

[0009] Specific embodiment two: this embodiment synthesizes polyaspartic acid copolymer derivatives according to the following steps: with aspartic acid and For raw materials, where R is H, (CH 3 ) 2 CH, (CH 3 ) 2 CHCH 2 、CH 3 CH 2 CH(CH 3 ), HOCH 2 、CH 3 CH(OH), HSCH 2 or HOOCCH 2 CH 2 , aspartic acid and The stoichiometric number is 1.0-99.9, using microwave technology, under the conditions of microwave frequency 915±50MHz or 2450±50MHz, microwave power 100-30000W, add catalyst and solvent to the reactant, and radiate reaction for 1-40min. The precursor of the polyaspartic acid copolymer derivative can be obtained, and the polyaspartic acid copolymer derivative can be obtained by hydrolyzing the precursor, wherein the stoichiometric number of the catalyst and the reactant is 0.01 to 1.00, and the chemical ratio of the solvent and the reactant The metering number is 0.10~9.99, and the reaction equation is as follows:

[0010]

[0011] Aspartic acid Other amino acids Intermediates

[0012] Intermediate Polyaspartic acid copolymer derivative

[0013] R in the formula is mainly H, (CH 3 ) 2 CH, (CH 3 ) 2 CHCH 2 、CH 3 CH 2 CH(CH 3 ), HOCH 2 、CH 3 CH(OH), HSCH 2 or HOOCCH 2 CH 2; The range of y/(y+x) is 0.1-0.9, the optimal range is 0.1-0.5, and the range of x+y is 7-70, the optimal range is 9-30. In addition to the groups listed above, other groups of R also belong to the protection scope of the present invention, and these products can be prepared by the method of the present invention.

[0014] In the synthesis process, the reaction time will be shortened with the increase of power. Too short reaction time is not conducive to uniform reaction, so a stirring device is added, and the reaction time is not less than 3min. Too high power will lead to dark color of the reaction product, and also It may lead to carbonization of raw materials in a short time, so the most suitable power is 360~5000W. Under different conditions, light yellow, yellow, light brown, brown and dark brown products can be obtained, with a molecular weight of 600-20000. Raw material aspartic acid and The optimal stoichiometric number of the catalyst and the reactant is 1.0-9.9; the optimal stoichiometric number of the catalyst and the reactant is 0.01-0.5; the optimal stoichiometric number of the solvent and the reactant is 0.10-3.0; the optimal radiation reaction time is 3-3. 20min; the catalyst is phosphoric acid, sodium dihydrogen phosphate, sodium phosphate, sulfuric acid, sodium bisulfate, sodium sulfate, ammonium bisulfate, ammonium chloride, ammonium bicarbonate or ammonium carbonate; the boiling point of the organic solvent used is 150-300°C, Including dimethylformamide, dimethyl sulfoxide, propylene carbonate, sulfolane, dimethyl sulfone, methyl ethyl sulfone or diphenyl carbonate, etc.

[0015] Specific embodiment three: according to the stoichiometric number of aspartic acid and glutamic acid in table 1, add raw material to total 25g in the single-necked round bottom flask, take phosphoric acid as catalyst, the stoichiometric number of catalyst and raw material is 0.03, add 25ml of dimethylformamide, the reaction time is 5min under microwave radiation, the microwave power is 900W, and the light brown and fluffy product is obtained, and 40ml of 3mol/L NaOH is added to dissolve the product, and the pH of the solution is adjusted to be neutral, and the product is filtered. The filtrate was added to 250ml of absolute ethanol, the precipitate was collected, and vacuum-dried at 70°C to obtain a polyaspartic acid copolymer derivative.

[0016] Aspartate/Glutamate

[0017] Specific embodiment four: Add aspartic acid and serine to a total of 0.18mol in a single-mouthed round bottom flask, aspartic acid and serine stoichiometric number is 7: 3, with NaH 2 PO 4 As a catalyst, the stoichiometric number of the catalyst and the raw material is 0.05, add 16ml of dimethylformamide, the microwave power is 720W, and when the microwave radiation time (Table 2) is different, fluffy products of different colors are obtained, and 32ml of 3mol/L NaOH is added Dissolve the product, adjust the pH of the solution to be neutral, filter, add the filtrate of the product to 250 ml of absolute ethanol, collect the precipitate, and dry it in vacuum at 70° C. to obtain a polyaspartic acid copolymer derivative.

[0018] radiation time