Step 1. Remove hematoxylin pigments with hot water
At area temperature, include the smashed hematoxylin core product to 20 times the weight of water, heat to 90 ° C, and extract for 1 hour for a total amount of 3 times.
Action 2: Use a mesh crude filter
Use a 180-mesh steel cable mesh to coarsely filter the hematoxylin fluid and slag mixture while it is hot to divide the hematoxylin liquid and slag, and combine each filtrate to get a red and yellow Hematoxylin remove.
Step 3: Purification with filter paper
Place the fast qualitative filter paper on the Buchner funnel, and use a vacuum pump to vacuum (vacuum cleaner degree is 0.098 MPa) to filter the product liquid.
Step 4: Microfiltration membrane filtering, contamination removal and sterilization
Utilize a circulation pump to pass the material fluid with a temperature below 35 ° C through the filter paper through the microfiltration membrane inlet. The input material is polyvinylidene fluoride (PVDF) and the pore dimension is 0.2 μm. The external stress microfiltration membrane layer is gotten used to 0.04. MPa, the non-permeate fluid still flows back to the initial solution container, and the procedure is duplicated until the permeate fluid basically does not drain, and the clear and transparent permeate liquid and the non-permeate fluid containing pollutants are accumulated respectively.
Step 5: Use ultrafiltration membrane to concentrate the Hematoxylin remedy
A hydrophobic polysulfone (PS) ultrafiltration membrane with a molecular weight cutoff of 3000 is made use of to concentrate the clear and translucent feed liquid that has travelled through the microfiltration membrane layer up until the strong material of the feed liquid is 5%. During the microfiltration membrane layer focus process, the membrane operating pressure was adapted to 0.02 MPa. The retentate that has actually not gone through the ultrafiltration membrane layer is a concentrated solution of hematoxylin. The concentrated service is subjected to the following spray drying out procedure. The content of hematoxylin in the permeate is very low and can be reused to extract Hematoxylin.
Action 6. Spray drying out
Make use of a spray dryer to vaporize the water in the Hematoxylin concentrate to prepare hematoxylin pigment powder with high material of reliable pigment components.
1) Cut the hematoxylin timber right into pieces and accomplish vacuum cleaner freeze-drying at 50 ° C for 10 hours, after that squash the dried out aloe vera leaves and pass them through a 50-mesh filter to acquire aloe vera completely dry powder.
Put dry hematoxylin powder right into the extraction kettle, include supercritical methanol as the extraction representative, include ammonia water as the entrainer, the extraction temperature level is 25 ° C, the removal pressure is 7MPa, the removal time is 10 minutes, the methanol circulation rate is 5L/h, and the entrainment Representative circulation rate 0.1 ml/min;
2) Depressurize the supercritical methanol consisting of the remove to separate the removal product. The separation temperature is 10 ° C and the separation pressure is 1MPa. The resulting essence is accumulated;
4) Concentrate to a paste, use D-101 macroporous resin, clean with water and 10% ethanol in turn up until the water is clear, and ultimately elute with 85% ethanol, and eliminate the ethanol from the eluent to obtain concentrated option A;
5) Filter the concentrated remedy A with ethanol solvent, mix the filtrate with polyamide, and placed it on a polyamide chromatography column. Use a combined option of water and methanol with a quantity ratio of 10:1 to 1:1 for gradient elution, and collect the water: Methanol is 8:1 ~ 5:1 and the eluent is concentrated to get focused liquid B, which is then freeze-dried.
Take some hematoxylin, wash it, completely dry it at 110 ° C for half an hour, and grind it right into a powder of 60 mesh. At area temperature, mix the crushed hematoxylin powder and distilled water at a mass ratio of 1:25, change the pH = 9, and preserve the solution. Essence at the boiling temperature level for 50 mins to get the hematoxylin pigment essence. Area the filter paper on a Buchner channel, utilize an air pump to filter the red and yellow hematoxylin pigment extract, collect the filtrate and focus it, and completely dry it in an oven. Made right into Hematoxylin.
