Anti-inflammatory rapid hemostatic medical adhesive material and preparation method thereof
A fast, carboxymethyl chitosan technology, applied in pharmaceutical formulation, application, pharmaceutical science and other directions, can solve problems such as poor hemostasis performance, and achieve the effects of improving hemostasis performance, hemostasis performance, and good bacteriostatic performance.
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preparation example 1
[0023] The preparation of preparation example 1α-n-butyl cyanoacrylate
[0024] This preparation example is used for preparing required n-butyl cyanoacrylate, specifically comprises the following steps:
[0025] (1) Butyl ester transesterification reaction
[0026] CNCH 2 COOC 2 h 5 +C 4 h 9 OH—C 2 h 5 ONa→CNCH 2 COOC 4 h 9 +C 2 h 5 Oh
[0027] In a 5L three-necked beaker equipped with a stirrer and a thermometer, put 1400ml of ethyl cyanoacetate and 1200ml of n-butanol, turn on the stirring, condense water, and add 25g of sodium ethylate to 40°C and above; heat up to 100°C and the top temperature reaches 78 Start distilling ethanol at -82°C. When the internal temperature reaches 110°C and the top temperature reaches 98-100°C, stop heating and collect about 680ml of ethanol;
[0028] Cool down to an internal temperature of about 50°C, turn on the heating, change the bottle with the vacuum pump to receive n-butanol, the vacuum degree is -0.1MPa, and change the bot...
preparation example 2
[0038] Preparation Example 2 The preparation of n-octyl cyanoacrylate
[0039] This preparation example is used for preparing required n-octyl cyanoacrylate, specifically comprises the following steps:
[0040] (1) with step (1) in the preparation example 1;
[0041] (2) with step (2) in the preparation example 1;
[0042] (3) Synthesis of n-octyl α-cyanoacrylate
[0043]
[0044]Add 380ml of methanol-formaldehyde solution and 0.95ml of piperidine into a 5L three-neck flask equipped with a stirrer, dropping funnel, condenser, and water separator. When the temperature in the bottle reaches 40°C or above, start adding cyanoacetic acid After adding 750ml of octyl esters dropwise, collect methanol until the internal temperature reaches 120°C; then add 300ml of petroleum ether dropwise, start dehydration, and speed up stirring. After the water is finished, collect about 300ml of petroleum ether; when the internal temperature reaches 130°C, add 20g of phosphorus pentoxide and ...
Embodiment 1
[0049] The preparation method of the medical adhesive material for rapid hemostasis described in the present embodiment comprises the following steps:
[0050] (1) According to the mass ratio of 55wt%: 45wt%, take the above-mentioned n-butyl cyanoacrylate and n-octyl α-cyanoacrylate and fully mix them to obtain a medical glue matrix, which is set aside;
[0051] (2) get carboxymethyl chitosan and be placed in the ionic liquid (accounting for the 8wt% of described carboxymethyl chitosan quality) of 1-methylimidazolium trifluoroacetate salt (accounting for the 8wt% of described carboxymethyl chitosan quality) and vasonia sap (with vasone directly Squeeze to obtain juice, account for 5wt% of described carboxymethyl chitosan quality) in the airtight container, get rid of air and charge CO2 in the container 2 , control the temperature in the airtight container to 80°C and the pressure to 8MPa, so that the charged CO 2 The gas is in a supercritical state, and under the condition th...
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