A kind of preparation method and use of 2,4-dichlorophenoxyacetic acid chitosan oligosaccharide ester
A technology of dichlorophenoxyacetic acid chitooligosaccharide ester and dichlorophenoxyacetic acid, which is applied in the field of food additives, can solve the problems of high preparation cost, poor antibacterial effect of antibacterial substances, and poor bacterial action, and achieve simple preparation method, Highlight the effect of antibacterial and low cost
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Embodiment 1
[0039] Take 0.02mol COS (molecular weight of 1500 Da, 85% degree of deacetylation), was dissolved under ice-cooling conditions in 30mL of methanesulfonic acid, the reaction 30min, methane sulfonic acid and methane formed Oligochitosan amino acid Salt.
[0040] Take 0.02mol of 2,4-dichlorophenoxyacetic acid in a round bottom flask was added 17mL of SOCl 2 , 60 deg.] C the reaction 6h, the reaction should be noted that strictly controlled drying conditions to prevent water entering the hydrolysis, after cooling to room temperature, rotary evaporated to remove the unreacted SOCl 2 The resulting clear liquid is the 2,4-dichloro-phenoxy acetyl chloride.
[0041] Chitosan oligosaccharide methanesulfonate was added dropwise 2,4-dichlorophenoxyacetic acid chloride, reacted at room temperature overnight at -20 ℃ After 4h, excess acetone was added, a precipitate, 11000r / min 5min solid-liquid separation by centrifugation, The supernatant was washed with acetone to colorless washing, ethano...
Embodiment 2
[0048] 0.04 mol of shell oligosaccharide, under ice bath conditions, dissolved in 60 ml of methanesulfonic acid, 50 min, to give methanesulfonate.
[0049] Take 0.04 mol of 2,4-dichlorophenoxycetic acid in a round bottom flask, add 34 ml of SOCL 2 , 60 ° C reaction for 6 h, the reaction process should pay attention to strict control of dry conditions to prevent moisture from entering hydrolysis, cooled to room temperature, steaming unreacted SOCL 2 The resulting transparent liquid is 2,4-dichlorophenoxyacetyl chloride.
[0050] The chlorose sulfonate was added dropwise to 2,4-dichlorophenoxycerazocetyl chloride, and at room temperature for 4 h, -20 ° C overnight, excess acetone, a precipitate, 11000 r / min centrifuged 5 min to separate solid-liquid separation, The supernatant was washed with acetone colorless, ethanol was washed twice to obtain a product 2,4-dichlorophenyl acetate shell oligosulcate.
[0051] 2,4-dichlorophenoxy acetate shell oligosulfonate was dissolved in a cer...
Embodiment 3
[0053] Thermal Stability was determined by the thermal analysis instrument of METTLER TOLEDO Instrument Co., Ltd. Detection conditions are: N 2 The flow rate was 20 mL / min, the temperature increase rate was 20 ° C / min, and the heating temperature range was 30 to 450 ° C. Distance of 2,4-dichlorobenzoxoacetate shell oligorate and its thermal loss rate curve Figure one Step of the step (DTG) Figure 5 , Image 6 .
[0054] from Figure 5 , 6 It can be seen that shell oligosaccharides and 2,4-dichlorobenzoxocetate oligosaccharides have gradually lost weights with temperature. There are two weight loss stages between the shell oligosaccharides at 30 to 450 ° C. A first-order weight occurred at 70 ~ 150 ° C, and the second order weight loss occurred at 170 ~ 350 ° C. The modified 2,4-dichlorophenoxacetate shell oligodaccharide also exists between 30 to 450 ° C. One of the first order weights is between 60 and 132 ° C, and the second order weight loss is at 134 to 408 ° C. It can be se...
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