Guanjie focuses on resveratrol 98 for 20 years that shows we have enough capability to produce it We research a method with a fully enzymatic method, which is the most advanced grinding technique in our country.
What Is Process Flow Chart Of Resveratrol 98 ?

2、What Is Production process and process conditions Of Resveratrol 98 ?
2.1 Extraction
2.1.1 Extraction equipment: 1000L extraction tanks
2.1.2 Relevant parameters
|
Items |
Process parameters |
|
|
Extraction |
100Kg/batch |
100Kg/批 |
|
Solvent ratio (v/v) and density |
Chloroform:95% ethanol = 6:1 Density ρ = 1.375 (30°C) |
|
|
Number of extractions |
Total 3 extractions |
|
|
Extraction temperature |
30℃ |
|
|
First extraction solvent and amount |
800L solvent volume is 8 times of the feeding volume respectively. |
|
|
Second extraction solvent and dosage |
600L solvent volume is 6 times of the feeding volume respectively. |
|
|
Third extraction solvent and dosage |
400L solvent volume is 4 times of the feeding volume respectively. |
|
|
Extraction time |
0.5 hours/time |
|
|
Amount of petroleum ether and soaking time of crude washing reagent |
The crude product after the last extraction and filtration was washed with 0.5 BV of petroleum ether of the feeding volume and soaked for 20 min. |
|
|
Tank pressure (MPa) |
Atmospheric |
|
2.1.3 Operating procedures
2.1.4 Operation method
2.1.4.1 If chloroform and ethanol two solvents are new solvents to resveratrol 98. Input the two solvents into the extraction tank separately. Stirring and heating to 30 ℃, take a sample to measure the density. Qualified and put into the raw material. After 0.5h of extraction, filter with a vacuum funnel. Take the material in the funnel to repeat the extraction 2 times. After filtration of the crude product (i.e., after the third extraction and filtration) with petroleum ether immersion 20min wash (at this time to ensure that no vacuum buffer tank to be recovered extract), drained to get the crude product. Filtered out of the mixed solvent into the 1000L vacuum concentrator to be recovered. The filtered petroleum ether can be added to the crude extract together with the recovery.
2.1.4.2 If the extraction solvent is a mixture of recycled solvents. The recovered solvent is fed into the extraction tank. First adjust the density of recovery solvent (recovery solvent density <1.375 then need to add chloroform. If the recovered solvent density is >1.375, ethanol should be added. The amount to be added is proportional according to the results of the small test. (The temperature of density measurement is 30℃). After passing the density test, put into the raw material. The subsequent steps are the same as in 2.1.4.1 to obtain the crude product resveratrol 98.
2.1.4.3 Attention.
The first two extractions and filtrations should not be too dry. When the material in the funnel starts to crack, you can stop the filtration. In order to avoid the next extraction of the material is not dispersed. After filtration, the filter bag should be immediately put into the alcohol bucket to soak.
2.2 Alumina decolorization
2.2.1 Equipment: decolorization crystallization tank
2.2.2 Related parameters
|
Items |
Process parameters |
|
|
Extraction |
Amount of solvent ethanol |
500L 5 times the amount of feed |
|
Decolorization times |
Total decolorization 3 times |
|
|
First decolorizing alumina dosage |
150kg alumina dosage is 1.5 times of the feeding amount. |
|
|
Second decolorizing alumina dosage |
100kg Alumina dosage is 1 times of the feeding amount. |
|
|
Third decolorized alumina dosage |
50kg Alumina dosage is 0.5 times of the feeding amount. |
|
|
Amount and soaking time of 95% ethanol as solvent for alumina washing after filtration |
The dosage of each washing was 0.5 times the weight of alumina, and the soaking time was 20 min. |
|
|
Decolorization temperature |
50℃ |
|
|
Decolorization time |
0.5hours/time |
|
|
Tank pressure(MPa) |
Atmospheric pressure |
|
2.2.3 Operating procedures
2.2.4 Operation method
2.2.4.1 Input solvent 95% ethanol into decolorization tank. Stir and heat to 50°C. Put in the crude product after extraction of 2.1.4. Dissolve for 0.5h and put in aluminum oxide. Decolorize for 0.5h and filter with vacuum funnel. The filtered alumina was soaked in solvent 95% ethanol for 20min and drained. The filtrate from the filtration was re-drawn into the decolorization tank with negative pressure. Input alumina according to the proportion, repeat the decolorization for 2 times, filtration of the filtrate. After draining, the alumina is bagged for washing.
2.2.4.2 Caution:
After the second alumina decolorization filtration. If the alumina color is pinkish purple-red, the third alumina decolorization will not be carried out. Directly into the activated carbon decolorization process.
Take a sample to check the color of alumina before the third alumina decolorization filtration. If the color is dark (normally the color of the third alumina decolorization is pinkish red), add 25kg of alumina to the decolorization crystallization tank to continue decolorization for 30 minutes. Then filtered. At this time the solvent 95% ethanol soaking alumina should be increased accordingly.
2.3 Activated carbon decolorization
2.3.1 Decolorization equipment: decolorization crystallization tank
2.3.2 Relevant parameters
|
Items |
Process parameters |
|
|
Decolorization |
Number of decolorizations, amount of activated carbon |
Total decolorization 1 time, the amount of activated carbon is 10 % of the amount of feed. |
|
Amount and soaking time of 95% ethanol as washing solvent for activated carbon after filtration |
The dosage of each washing is 2 times the volume of the weight of activated carbon, and the soaking time is 20min. |
|
|
Decolorization temperature |
50℃ |
|
|
Decolorization time |
0.5 hours/time |
|
|
Pressure in the tank (MPa) |
Atmospheric pressure |
|
2.3.3 Operation process
2.3.3.1 The filtrate obtained in 2.2.4 is sucked under negative pressure into the decolorization crystallization tank and heated to 50℃. Put in the activated carbon, decolorization 0.5h and then filtered by vacuum funnel. After filtration of activated carbon with solvent 95% ethanol soaking 20min after draining, get the filtrate. Firstly, the decolorization crystallization tank was cleaned. And rinse with purified water once. Then the filtrate, i.e. the decolorized solution, was filtered through a fine filtration funnel. Before fine filtration, 5kg of new alumina was put into the fine filtration funnel. The decolorant is then added to 2/3 of the volume of the funnel (be careful not to wash up the alumina). After that, the vacuum valve of the buffer tank is opened for filtration. After filtration, the alumina is soaked in 0.5 times of ethanol for 10min and dried. The dried alumina can be used to decolorize the next batch of alumina. The filtrate is sucked into the cleaned decolorized crystallization tank under negative pressure. The volume of filtrate after decolorization of activated carbon should be about 480-500L. If the volume is less than 480L, add the corresponding amount of 95% ethanol to 480L (the added 95% ethanol can be used to soak the activated carbon and then pumped dry). The dried activated carbon is bagged and set aside.
2.3.3.2 Attention:
If the color of the filtrate after decolorization of activated carbon is dark (normally the color of the filtrate after decolorization of activated carbon is light greenish). If the color of the filtrate after decolorization of activated carbon is dark (normally the color of the filtrate after decolorization of activated carbon is light greenish), the filtrate obtained in 2.3.3.1 shall be sucked into the decolorization crystallization tank under negative pressure and heated up to 50℃. Put in 2% of the amount of activated carbon, decolorization 0.5h after filtering with a vacuum funnel. After filtration of activated carbon with solvent 95% ethanol soak 20min and then pumped dry, get the filtrate. The remaining steps are the same as 2.3.3.1.
2.4 Crystallization
2.4.1 Equipment: decolorization and crystallization tanks
2.4.2 Relevant parameters
|
Items |
Process parameters |
|
|
Crystallize |
Amount of purified water |
750L 7.5 times the feed volume |
|
Decolorizing solution temperature |
Heating to 60℃ |
|
|
Temperature of purified water |
Heating to 70℃ |
|
|
Cooling final temperature |
25~30℃(i.e. room temperature) |
|
|
40% ethanol dosage |
60L |
|
|
Tank pressure(MPa) |
Atmospheric pressure |
|
2.4.3 Operation process
2.4.3.1 2.3.3 crystallization tank in the fine filtration of the filtrate, stirring and heating to 60 ℃, and then heated to 70 ℃ purified water at a rate of about 20 ~ 30L per minute into the crystallization tank (pre-500L speed can be faster, the rest of the 250L speed is gradually slowed down, when added to the crystallization tank solution began to become turbid, then stop adding water), and stop stirring, 65 ℃ insulation 2 hours, and then open the interlayer cooling water valve to reduce the temperature to 40 ℃ every 2 hours to reduce the speed of 10 ℃ can continue to open the interlayer cooling water until the temperature drops to 20 ~ 30 ℃. hours, and then open the mezzanine cooling water valve, every 2 hours to drop 10 ℃ rate of cooling, down to 40 ℃ can continue to open the mezzanine cooling water until the temperature drop to 20 ~ 30 ℃, holding 1 hour (Note: open the cooling water cooling process can be turned on every 30 minutes stirring for 5 seconds), and then filtered with a vacuum funnel (must be used with a special bag), after the crystallization of the drying soaked in 40% ethanol 20min and then pumped dry. The crystals will be loaded into the disk and transported to the vacuum drying oven drying. The mother liquor filtered out is put into No. 12 PE tank for recycling.
2.4.3.2 Caution:
Crystallization and filtration before putting down a small amount of material into the stainless steel bucket, check whether there are impurity particles, if so, the magazine particles will be put clean before the material is put into the funnel filtration, the bucket of impurities in the material can be put into the mother liquor recycling and crystallization of filtration after going.
2.5 Extraction of solvent recovery
2.5.1 Equipment: 1000L concentration tank
2.5.2 Operation:
First open the vacuum pump and vacuum valve, while opening the circulating water valve, each time through the negative pressure conveying 2.1.4 to be recycled mixed solvent 600-700L into the concentration tank, break the vacuum and open the steam valve steam heating slowly, control the temperature at 70 ℃ to open the stirring atmospheric concentration (pay attention to prevent the explosion of the boil) until the tank body is left about 50L thick paste, stop heating, release the thick paste, repeat the previous step until the recovery is complete, the thick paste, the thick paste, the thick paste, the thick paste, the thick paste, the thick paste, the thick paste, the thick paste, the thick paste, the thick paste. Repeat the previous step until the recovery is complete. Recovered mixed solvent pumped into the mixed solvent resveratrol 98 storage tank.
2.6 Recovery of mother liquor
2.6.1 Equipment: decolorization and crystallization tanks
|
Items |
Process parameters |
|
|
Masterbatch Recycling |
Concentration degree |
Concentrate to 1/3 of the volume of mother liquor |
|
Concentration temperature |
≤70℃ |
|
|
Tank pressure(MPa) |
Negative pressure (-0.07 or more) concentration |
|
2.6.2 Operation method: First open the vacuum pump and vacuum valve, at the same time open the circulating water valve, each time through the negative pressure will be 2.4.3 in the mother liquor to be recovered 600-700L transported into the crystallization tank, open the stirring, vacuum conditions through the steam vacuum concentration (control temperature ≤ 70 ℃), can be continuous feeding concentration, to achieve the required degree of concentration (Note: Recovery of dilute ethanol pumped into the 13th PE storage tank, the volume should be 2/3), break the vacuum after holding 1 hour to open the interlayer cooling water valve, (Note: open the cooling water cooling process can be turned on every 10 minutes for 5 seconds) to be crystallized. Volume should be 2/3 of the volume of mother liquor), break the vacuum, keep warm for 1 hour and then open the interlayer cooling water valve, (Note: open the cooling water cooling process can be opened every 10 minutes stirring for 5 seconds) to be crystallization tank in the liquid cooled to 20 ~ 30 ℃, filtration, 90% of the resveratrol, bagging to be recrystallized. Drain the filtrate.
2.7 Washing aluminum oxide
2.7.1 Equipment: decolorization and crystallization tanks
2.7.2 Procedure
Input solvent 95% ethanol (dosage is 0.5 times of the weight of alumina) into the decolorization crystallization tank, heat it up to 50℃, then put in the decolorized alumina in 2.4, stir it for 30min, filter it and get the filtrate. The filtrate is sucked into the decolorization crystallization tank under negative pressure again, heated to 50 ℃ with stirring, and then add the activated carbon in 2.3.3 which has been used once to decolorize for 30 minutes and then filtered by vacuum funnel, and the filtered activated carbon is soaked with 2 times the volume of activated carbon in 95% ethanol for 20min and then drained, and then get the filtrate. The filtrate was sucked into the decolorization and crystallization tank again under negative pressure, the circulating water valve and steam valve were opened, and the vacuum was concentrated to dryness to get about 90% of resveratrol, which was taken out of the hand hole with a small spatula and bagged up, to be recrystallized. The activated carbon after draining is moved to the coal pile in the boiler room.
2.8 90% Res recrystallization
2.8.1 Equipment: extraction tank, crystallization tank
2.8.2 Parameters
|
Items |
Process parameters |
||
|
Crystallize |
Dosage of solvent 95% ethanol |
90% Res dry weight by 10 times volume |
|
|
Activated carbon dosage |
20% of the dry weight of 90% Res |
||
|
Amount of purified water |
95% ethanol 1.5 times volume |
||
|
Temperature of purified water |
Heating to 70°C |
||
|
Cooling final temperature |
25~30°C (i.e. fresh water temperature) |
||
|
Tank pressure(MPa) |
Atmospheric pressure |
||
2.8.3 Operation process
2.8.3.1 Input 95% ethanol into the extraction tank, heat to 50 ℃, put the resveratrol obtained in 2.6 and 2.7 into the crystallization tank, stir to dissolve, and then put in the activated carbon, decolorize for 30 min and then filter, and the activated carbon is washed with 2 times the weight of the activated carbon by volume of 95% ethanol to obtain the filtrate.
2.8.3.2 Input the filtrate obtained in 2.8.3.1 into the crystallization tank, heated to 60 ℃, and then will be heated to 70 ℃ purified water at a rate of 20 ~ 30L per minute into the crystallization tank, add the end of stop stirring, 65 ℃ insulation for 2 hours, and then turn on the cooling water to cool down the temperature of 10 ℃ every 3 hours until the temperature is lowered to 20 ~ 30 ℃, insulation for 1 hour (Note: Turn on the cooling water cooling process can be every 3 hours). Cooling water cooling process can be turned on every 30 minutes stirring for 5 seconds), followed by vacuum funnel filtration, dried crystals with 40% ethanol soaked 10min after draining. The crystals are put into plastic bags and transported to the drying workshop.
2.8.3.3 Notes:
There are two ways to deal with the 90% content of resveratrol obtained from the treatment in 2.6 and 2.7, one is that the resveratrol 90 obtained from each batch of treatment is added to the next batch of the first alumina decolorization, but the dosage of ethanol and the dosage of activated charcoal and purified water should be increased correspondingly according to the parameter in 2.8.2 when dissolving. The other is to dry and wait until the 90% content of resveratrol reaches 25kg or more, then recrystallize according to the method in 2.8.
2.9 Drying
2.9.1 Equipment: vacuum drying oven
2.9.2 Parameters
|
Drying temperature |
Thickness of paving material |
Single drying quantity |
Drying standard |
|
45-50℃ |
Not more than 3cm |
≤35 Kg |
Moisture up to 3.5%±0.5 |
2.9.3 Operating procedures: vacuum drying post standard operating procedures ( ).
2.9.4 operating method: Resveratrol 98 to be dried evenly spread in the baking tray, from top to bottom into the grill, sent to the vacuum drying oven for drying, to reach the drying time, notify the inspector to take samples for testing, sampling and then continue to dry, to be qualified to stop drying after the moisture test, will test the report card affixed to the back of the batch of drying records, and will be dried and weighed in bags of products and then immediately transferred to the crushing room for crushing.
2.10 What Is Crushing, packaging and storage Of Resveratrol 98 ?
2.10.1 The dry product crushed, packaged, labeled, with the product inspection report form transferred to the product storage room.
2.10.2 Packed in double plastic bags + aluminum foil bags + cardboard drums.
2.10.3 Sealed and refrigerated away from light.
2.11 Alcohol distillation
2.11.1 Equipment: alcohol distillation tower
2.11.2 Operating procedures (alcohol distillation tower operating procedures)
2.11.3 Operation process
Use the material pump to pump dilute ethanol from PE storage tank No. 13 into the distillation kettle. The liquid level should not exceed 2/3 of the inner volume of the kettle. open the circulating water valve, the heating steam valve and the bypass to remove steam condensate. close the bypass valve after 1 to 2 minutes. Allow steam to drain automatically through the trap. Open the cooling water inlet valves for the cooler, condenser, and tail gas collection. And open the reflux liquid inlet and outlet valves into the top of the tower to start the full reflux operation.
Observe the changes of the temperature of the top of the tower and kettle and the specific gravity of the reflux liquid (measured by sampling with an alcohol meter). When the concentration of ethanol is more than 93%, gradually open the finished alcohol discharge valve into the No. 11 PE storage tank and gradually close the reflux liquid valve. When the temperature at the top of the tower is stable, the liquid concentration is qualified, and the operation can be stabilized. To the bottom of the kettle to sample the residual alcohol 10% (temperature 25 ℃), close the heating steam valve. Discharge the residual liquid from the bottom of the kettle. Add new dilute alcohol liquid and start the next batch of resveratrol 98 material production.
Note: If the alcohol distillation tower has distilled methanol before, clean the alcohol distillation tower first, and the solvent recovered in the first 10 minutes when the distillation is just started is discharged to the PE tank for methanol, and the ethanol recovered after that is put into the PE storage tank No. 11.
Where To Buy resveratrol 98?
If you are looking to buy resveratrol 98, Guanjie is a bulk resveratrol supplier that offers several advantages. Guanjie's two independent factories and three production lines ensure a reliable and continuous supply. And we have a professional research team and has its own laboratories. Guanjie takes quality control seriously by providing third-party testing. For any solicitations concerning our things, contact us at info@gybiotech.com.






