CN102161835B - Method for preparing pigment by waste pecan epicarp - Google Patents
Method for preparing pigment by waste pecan epicarp Download PDFInfo
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- CN102161835B CN102161835B CN 201110058337 CN201110058337A CN102161835B CN 102161835 B CN102161835 B CN 102161835B CN 201110058337 CN201110058337 CN 201110058337 CN 201110058337 A CN201110058337 A CN 201110058337A CN 102161835 B CN102161835 B CN 102161835B
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- 239000000049 pigment Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002699 waste material Substances 0.000 title abstract description 6
- 235000009025 Carya illinoensis Nutrition 0.000 title abstract 4
- 241001453450 Carya illinoinensis Species 0.000 title abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 124
- 238000000605 extraction Methods 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000010828 elution Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 238000000746 purification Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 235000019441 ethanol Nutrition 0.000 claims description 65
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 42
- 241000899834 Obovaria olivaria Species 0.000 claims description 29
- 235000001018 Hibiscus sabdariffa Nutrition 0.000 claims description 6
- 235000005291 Rumex acetosa Nutrition 0.000 claims description 6
- 240000007001 Rumex acetosella Species 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 6
- 229940079593 drug Drugs 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 235000003513 sheep sorrel Nutrition 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 3
- 230000003292 diminished effect Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 235000019580 granularity Nutrition 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000004043 dyeing Methods 0.000 abstract description 4
- 238000001704 evaporation Methods 0.000 abstract 2
- 230000008020 evaporation Effects 0.000 abstract 2
- 239000000118 hair dye Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 206010019332 Heat exhaustion Diseases 0.000 description 1
- 206010019345 Heat stroke Diseases 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical class OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000001448 anilines Chemical class 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Chemical class CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007665 chronic toxicity Effects 0.000 description 1
- 231100000160 chronic toxicity Toxicity 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 229920002770 condensed tannin Polymers 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000010909 process residue Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for preparing pigment by waste pecan epicarp, belonging to the technical field of a pigment preparation method. The method is characterized by comprising the following steps: 1) drying raw materials; 2) smashing and extracting the raw materials; 3) carrying out vacuum drying on extracting solution, abandoning filter residues, and combining liquid subjected to vacuum drying; 4) carrying out flash evaporation and concentration on the filtered extraction solution; 5) purifying macroporous resin, and respectively collecting each elution part which is 3 times of column volume; 6) combining parts eluted by 30-70% of ethanol, and carrying out vacuum flash evaporation and concentration to obtain concentrated solution; and 7) concentrating and drying the concentrated solution in vacuum to prepare the bronzing pigment product of the pecan epicarp. The extraction and purification technology adopted by the preparation method is advanced, has the advantages of simple preparation technology, abundant raw material sources, high extraction efficiency and stable performance, is convenient to operate, is easy to realize industrial production, can serve as the pigment application for hair dye and oil treatment, drawing, clothes dyeing, can improve the use ratio of the waste pecan epicarp and provides a source for developing the natural pigment.
Description
Technical field
The invention belongs to pigment preparation method technical field, be specially a kind of method of utilizing discarded hickory nut epicarp to prepare pigment.
Background technology
Pigment is divided into synthetic colour and natural pigment two classes according to its source difference, synthetic colour lovely luster, strong coloring force, not less, the stable performance of fugitive color, consumption, but mainly belong to the phenyl amines pigment with carcinogenesis due to synthetic colour, and people find that successively a lot of synthetic colours have serious chronic toxicity and carinogenicity, and the advantages such as the pigment of plant origin is nontoxic with it, safety, color and luster are naturally bright-coloured, good stability are subject to popular favor all the time.The plant resources of China is abundant, replaces with natural pigment the development trend that synthetic colour has become following food, makeup and dyestuffs industries.
Be oxidized to very soon tannic red tannin and quinones after containing a large amount of tannic acids, polyatomic phenol and anthraquinone analog compound, particularly condensed tannin and polyphenol components ingress of air in hickory nut epicarp, these compounds often have darker color.The tannic red element is water-fast red-brown or sorrel pigment, and not only self color is unique, but also has converging action, can make the skin hardening, thereby protects mucous membrane, reduces skin pain and prevent that bacterium from infecting.Hickory nut epicarp is the food-processing waste at present, enormous amount.But so far there are no utilizing discarded hickory nut epicarp to prepare the report of pigment.
Summary of the invention
For the above-mentioned problems in the prior art, the object of the invention is to design provides a kind of technical scheme of utilizing discarded hickory nut epicarp to prepare the method for pigment, the extraction purification technique that adopts is advanced, preparation technology is simple, easy to operate, raw material sources are abundant, extraction yield is high, stable performance, environment-friendly high-efficiency, easy suitability for industrialized production, and the pigment that obtains can be used as the pigment applications of Ran Fa treatment oil, drawing, clothes dyeing.
A kind of described method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that comprising the following steps:
1) raw material is processed: naturally dry after hickory nut epicarp is cleaned, put in 35 ℃ of-45 ℃ of baking ovens dry 20-30 hour, and taking-up, standby;
2) the broken extraction: raw material is put in smashing extractor, add the broken extraction of 50～100% aqueous ethanols or 50～100% aqueous acetone 1～2 time at every turn, raw material is broken into 20～60 purpose granularities, if raw material weight be 1kg aqueous ethanol or aqueous acetone consumption be 6～10 liters, each extraction time is 1～3 minute;
3) filtration under diminished pressure: with the extracting solution suction filtration, discard filter residue, merge suction filtration liquid;
4) flash concentration: the extracting solution after filtering is at 40 ℃-55 ℃, and vacuum tightness is to adopt Reduced Pressure Concentration Device to carry out flash concentration under 0.090Mpa～0.095 Mpa condition, regulates the feed liquor speed of solution to be concentrated, with 150～300 mLmin
-1Flow repeatedly concentrated, reclaim ethanol, obtain amounting to the concentrated solution that every milliliter of concentrated solution contains 0.5～1.0 gram crude drug;
5) macroporous resin purification: by the macroporous adsorbent resin separation and concentration, first use H
2The O wash-out, then carry out gradient elution with 10～80% aqueous ethanol successively, use at last 70% acetone wash-out, the flow velocity of elutriant is 5～15 mLmin
-1, each wash-out position of collecting respectively 3 times of column volumes;
6) continue flash concentration: 20～70% alcohol elutions are merged, at 45 ℃-55 ℃, vacuum tightness is to adopt Reduced Pressure Concentration Device to carry out flash concentration under 0.090Mpa～0.095 Mpa condition, regulates the feed liquor speed of solution to be concentrated, with 150～300 mLmin
-1Flow repeatedly concentrated, get concentrated solution;
7) vacuum-drying: concentrated solution is dry at 45 ℃-55 ℃ lower vacuum concentration, make hickory nut epicarp sorrel pigment product.
A kind of described method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that in step 1), oven temperature is 40 ℃-42 ℃, and be 23-25 hour time of drying.
A kind of described method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that step 2) in: aqueous ethanol concentration is 60-90%, preferred 70-80%; Aqueous acetone concentration is 60-90%, preferred 70-80%.
A kind of described method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that in step 4): the flash concentration temperature is 45 ℃-50 ℃, and feed liquor speed is 200～250 mLmin
-1, every milliliter of concentrated solution contains 0.6-0.8 gram crude drug.
A kind of described method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that step 5), 6) in: H adopted successively
2O, 10% ethanol, 20% ethanol, 40% ethanol, 60% ethanol, 80% ethanol, 70% acetone carry out gradient elution; Elution flow rate is 10～12 mLmin
-1, merging 20% ethanol, 40% ethanol and 60% ethanol alcohol elution, the flash concentration temperature is 50 ℃-52 ℃, feed liquor speed is 200～250mLmin
-1
A kind of described method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that in step 7): drying temperature is 50 ℃-54 ℃.
Described smashing extractor can directly be buied from the market, and Reduced Pressure Concentration Device (flash concentration device) also can directly be buied from the market for the designed, designed assembling.
A kind of above-mentioned method of utilizing discarded hickory nut epicarp to prepare pigment has following beneficial effect:
1, utilize discarded plant material to extract pigment, turn waste into wealth, reduced the waste of resource, improved using value and the utilization ratio of hickory nut epicarp, also the exploitation for natural pigment provides new source.
2, hickory nut epicarp is adopted the broken extraction of water-containing solvent, keying action by high-speed stirring, vibration, mixing, infiltration, dipping, make composition in raw material be transferred to solvent within the extremely short time in and reach the stripping balance, complete when having realized pulverizing and leaching process, room temperature is extracted and is avoided the thermo-sensitivity composition to destroy simultaneously, have quick, complete, energy-efficient, easy and simple to handle, the more high advantage of working efficiency of extraction, improved pigment composition extraction yield.Extracting solution adopts vacuum flashing concentrated, has that the concentrated solution heating temperature is low, heated time is short, effectively protect the thermo-sensitivity composition not to be destroyed, and concentrated speed is fast, efficient is high, the advantages such as simple to operate, easy to use, energy-conserving and environment-protective.
3, the extraction purification technique that adopts is advanced, and preparation technology is simple, easy to operate, non-toxic and safe, pollution-free, and production cost is low, and raw material sources are abundant, extraction yield is high, and product performance are stable, easy suitability for industrialized production.By comprehensive development and utilization hickory nut epicarp waste, can increase the added value of agricultural byproducts, therefore have certain economic worth and realistic meaning.
4, this pigment is a kind of natural environmental-friendly pigment, can be applicable to dye send out in treatment oil, drawing, clothes dyeing, has well upper chromatic effect, and the pigment color and luster is unique, stable, does not fade for a long time.After measured, utilize pigment dry powder that the present invention obtains through the colorimetric method for determining absorbancy, the look valency is more than 80.
The percentage composition that relates in present specification unless otherwise indicated all refers to weight percentage.
Embodiment
Now in conjunction with embodiments of the invention and correlation test, the invention will be further described.
1) raw material is processed: naturally dry after hickory nut epicarp is cleaned, put in 40 ℃ of baking ovens dry 24 hours, and taking-up, standby;
2) the broken extraction: raw material is put in smashing extractor, is added at every turn that 70% aqueous ethanol or 70% aqueous acetone are broken to be extracted 2 times, if raw material weight be 1kg aqueous ethanol or aqueous acetone consumption be 8 liters, each extraction time is 2 minutes;
3) filtration under diminished pressure: with the extracting solution suction filtration, discard filter residue, merge suction filtration liquid;
4) flash concentration: the extracting solution after filtering is at 50 ℃, and vacuum tightness is to adopt Reduced Pressure Concentration Device to carry out flash concentration under 0.095 Mpa condition, regulates the feed liquor speed of solution to be concentrated, with 230 mLmin
-1Flow repeatedly concentrated, reclaim ethanol, obtain amounting to the concentrated solution that every milliliter of concentrated solution contains 0.6 gram crude drug;
5) macroporous resin purification: concentrated solution by Diaion HP-20 macroporous adsorbent resin separation and concentration, is adopted H
2O, 10% ethanol, 20% ethanol, 40% ethanol, 60% ethanol, 80% ethanol, 70% acetone carry out gradient elution, and the flow velocity of elutriant is 10 mL min
-1, each wash-out position of collecting respectively 3 times of column volumes;
6) continue flash concentration: 20% ethanol, 40% ethanol and 60% alcohol elution are merged, and at 50 ℃, vacuum tightness is to adopt Reduced Pressure Concentration Device to carry out flash concentration under 0.095 Mpa condition, regulates the feed liquor speed of solution to be concentrated, with 250 mLmin
-1Flow repeatedly concentrated, reclaim ethanol, get concentrated solution;
7) vacuum-drying: concentrated solution is dry at 50 ℃ of lower vacuum concentration, make hickory nut epicarp sorrel pigment product.
In above-mentioned steps 1) in oven temperature be 35 ℃, 42 ℃, 45 ℃, be 20 hours, 25 hours, 30 hours time of drying.Step 2) in: aqueous ethanol concentration 50%, 60%, 80%, 90%, 100%; Aqueous acetone concentration is 50%, 60%, 80%, 90%, 100%, the broken extraction 1 time, if raw material weight be 1kg aqueous ethanol or aqueous acetone consumption be 6 liters, 7 liters, 9 liters, 10 liters, each extraction time is 1 minute, 3 minutes.In step 4): the flash concentration temperature is 45 ℃, 48 ℃; Feed liquor speed is 150 mLmin
-1, 200 mLmin
-1, 250 mLmin
-1, 300 mLmin
-1, every milliliter of concentrated solution contains 0.6 or 0.8 gram crude drug.In step 5) and step 6): first use H
2The O wash-out, then carry out gradient elution with 15% ethanol, 25% ethanol, 35% ethanol, 45% ethanol, 55% ethanol, 70% ethanol, 70% acetone; The flow velocity of elutriant is 5 mL min
-1, 8 mL min
-1, 10 mL min
-1, 12 mL min
-1, 15 mL min
-1Merge 25% ethanol, 35% ethanol, 45% ethanol, 55% ethanol and 70% alcohol elution, the flash concentration temperature is 45 ℃ or 48 ℃.Also can first use H
2The O wash-out, then carry out gradient elution with 20% ethanol, 30% ethanol, 50% ethanol, 60% ethanol, 70% ethanol, 70% acetone, merge 30% ethanol, 50% ethanol, 60% alcohol elution.In step 7): drying temperature is 45 ℃ or 55 ℃.Other processing step is the same, also can obtain beneficial effect of the present invention.Adopt the yield of the pigment product that above-mentioned preparation method makes 8.5%～18.8%.This pigment is sorrel or red-brown pulvis, and the product of making can be solid pigment, dissolves with polar organic solvent during use, makes paste after can also adding the blenders such as dispersion agent and wetting agent.
For further illustrating beneficial effect of the present invention, describe below by corresponding correlation data.
1. the impact of broken extraction conditions on extraction efficiency.
The amount and the yield that obtain pigment in this table refer to that raw material through amount of pigment and yield that fragmentation extraction, flash concentration, macroporous resin adsorption enrichment, continuation flash concentration, vacuum-drying obtain after becoming dry powder, has omitted macroporous resin purification and flash concentration drying process in table.By table 1 data as can be known: adopt the extraction conditions of embodiment 1 and embodiment 6, namely adopt 70% acetone and 70% ethanol to extract, the extraction efficiency of pigment is the highest, shows that acetone has stronger penetration power than ethanol to plant tissue.Consider that ethanol compares with acetone, have advantage safer, inexpensive, that be easy to get, therefore 70% ethanol is preferred embodiment.
2. in order to determine the quality of Smashing extraction method, adopt broken extraction conditions and the conventional extracting method of embodiment 6 to compare test, the extraction conditions of conventional extracting method is as far as possible consistent aspect solvent strength, solvent load, the results are shown in Table 2.
As shown in Table 2: thermal backflow is extracted and need to be heated at higher temperature, makes polyphenol components be subject to heat collapse, and bothers during operational cost, and the extraction yield of pigment is minimum.Though supersound extraction, cold soaking extraction are that room temperature is extracted with the diacolation extraction, need not heating, bother when the time length that extraction needs, operational cost, extraction yield is not high.Compare with conventional extracting method, adopt Smashing extraction method to extract rapidly and efficiently, the pigment that obtains is stable, extraction yield is high.
3. the Color of pigment and stability test, test-results such as following table 3.
Test-results shows: the pigment product of the present invention's preparation is red-brown or sorrel, tries out the pigment of Yu dyeing hair, the damp look of clothes, drawing, and color and luster is unique, satisfactory for result, colour-fast for a long time.Observed colour stable, lasting eight months.
Claims (7)
1. method of utilizing discarded hickory nut epicarp to prepare pigment is characterized in that comprising the following steps:
1) raw material is processed: naturally dry after hickory nut epicarp is cleaned, put in 35 ℃ of-45 ℃ of baking ovens dry 20-30 hour, and taking-up, standby;
2) the broken extraction: raw material is put in smashing extractor, add the broken extraction of 50～80% aqueous ethanols or 50～80% aqueous acetone 1～2 time at every turn, raw material is broken into 20～60 purpose granularities, if raw material weight be 1kg aqueous ethanol or aqueous acetone consumption be 6～10 liters, each extraction time is 1～3 minute;
3) filtration under diminished pressure: with the extracting solution suction filtration, discard filter residue, merge suction filtration liquid;
4) flash concentration: the extracting solution after filtering is at 40 ℃-55 ℃, and vacuum tightness is to adopt Reduced Pressure Concentration Device to carry out flash concentration under 0.090Mpa～0.095 Mpa condition, regulates the feed liquor speed of solution to be concentrated, with 150～300 mLmin
-1Flow repeatedly concentrated, reclaim ethanol, obtain amounting to the concentrated solution that every milliliter of concentrated solution contains 0.5～1.0 gram crude drug;
5) macroporous resin purification: by the macroporous adsorbent resin separation and concentration, first use H
2The O wash-out, then carry out gradient elution with 10～80% aqueous ethanol successively, use at last 70% acetone wash-out, the flow velocity of elutriant is 5～15 mLmin
-1, each wash-out position of collecting respectively 3 times of column volumes;
6) continue flash concentration: 20～70% alcohol elutions are merged, at 45 ℃-55 ℃, vacuum tightness is to adopt Reduced Pressure Concentration Device to carry out flash concentration under 0.090Mpa～0.095 Mpa condition, regulates the feed liquor speed of solution to be concentrated, with 150～300 mLmin
-1Flow repeatedly concentrated, get concentrated solution;
7) vacuum-drying: concentrated solution is dry at 45 ℃-55 ℃ lower vacuum concentration, make hickory nut epicarp sorrel pigment product.
2. a kind of method of utilizing discarded hickory nut epicarp to prepare pigment as claimed in claim 1, is characterized in that in step 1), oven temperature is 40 ℃-42 ℃, and be 23-25 hour time of drying.
3. a kind of method of utilizing discarded hickory nut epicarp to prepare pigment as claimed in claim 1, is characterized in that step 2) in: aqueous ethanol concentration is 60-80%; Aqueous acetone concentration is 60-80%.
4. a kind of method of utilizing discarded hickory nut epicarp to prepare pigment as claimed in claim 1, is characterized in that step 2) in: aqueous ethanol concentration is 70-80%; Aqueous acetone concentration is 70-80%.
5. a kind of method of utilizing discarded hickory nut epicarp to prepare pigment as claimed in claim 1, it is characterized in that in step 4): the flash concentration temperature is 45 ℃-50 ℃, and feed liquor speed is 200～250 mLmin
-1, every milliliter of concentrated solution contains 0.6-0.8 gram crude drug.
6. a kind of method of utilizing discarded hickory nut epicarp to prepare pigment as claimed in claim 1, is characterized in that step 5), 6) in: H adopted successively
2O, 10% ethanol, 20% ethanol, 40% ethanol, 60% ethanol, 80% ethanol, 70% acetone carry out gradient elution; Elution flow rate is 10～12 mLmin
-1, merging 20% ethanol, 40% ethanol and 60% alcohol elution, the flash concentration temperature is 50 ℃-52 ℃, feed liquor speed is 200～250mLmin
-1
7. a kind of method of utilizing discarded hickory nut epicarp to prepare pigment as claimed in claim 1, it is characterized in that in step 7): drying temperature is 50 ℃-54 ℃.
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| CN107163616A (en) * | 2017-05-22 | 2017-09-15 | 郭良 | A kind of method and its purification process for extracting walnut green husk pigment |
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| CN102161835A (en) | 2011-08-24 |
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