CN101817993B - Method for extracting lac red pigment - Google Patents
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- CN101817993B CN101817993B CN 201010165539 CN201010165539A CN101817993B CN 101817993 B CN101817993 B CN 101817993B CN 201010165539 CN201010165539 CN 201010165539 CN 201010165539 A CN201010165539 A CN 201010165539A CN 101817993 B CN101817993 B CN 101817993B
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Abstract
The invention discloses a method for extracting lac red pigment. The method comprises the following steps of: (1) smashing a dry lac material and immersing the smashed material in ethanol; and heating and refluxing the solution for extraction; (2) filtering liquid obtained by the step (1) for chromatography with a macroporous adsorption resin and eluting the liquid; and (3) concentrating eluent obtained by the step (2) and drying the eluent to obtain the lac red pigment. The method has the advantages that: (1) by using the characteristic that the lac red pigment has better solubility in solution of dilute alcohol, extracting solution is filtered and extracted by using the solution of dilute alcohol for many times; the extracting solution is adsorbed by the macroporous adsorption resin and eluted by concentrated ethanol; and the eluent is concentrated, dried and smashed to obtain concentrated and odorless lac red pigment; (2) by adopting the solution of ethanol for extraction, insoluble residue serving as a lac byproduct can be used as an industrial raw material; (3) the extracting solution passes through the macroporous adsorption resin; and the pigments of effluent are adsorbed completely and can be recycled after distillation.
Description
Technical field
The present invention relates to a kind ofly extract the method for the pigment of natural origin, particularly a kind of extracting method of Lac dye by natural matter.
Background technology
Lac dye is a kind of natural pigment by the tachardia lacca secretion.Lac claims again shellac, that a kind of tachardia lacca parasitizes some leguminous plantss, such as kingwood (Dalbergia obtusifolia), Dalbergia balansae Prain (D.balansae), seedling blue or green (Simao yellow wingceltis) (D.Szemaoensis), suck a kind of red material of secreting behind the myron on the branches such as rope of plaited plants tree (Eriolaena malvacea), pigeonpea (Cajanus cajan), silk tree (Albiziajulibrissin).Lac is as a kind of natural resin, because its stable chemical performance, nontoxic, nonirritant, plasticity-and film-forming properties is strong, electrical insulation capability is good, oil resistant, acidproof, waterproof, protection against the tide, antiultraviolet are widely used in the industrial sectors such as national defence, electrical equipment, coating, machinery, rubber, plastics, medicine, process hides, papermaking, printing, printing ink and food.Because chemosynthesis pigment toxicity is larger, the application in foodstuffs industry is restricted day by day, and natural pigment more and more is subject to the welcome of foodstuffs industry.By the lac pigment that lac is extracted, it is pink that color and luster is, lovely luster, and the look valency is very high, is used for food-processing and can significantly improves the food added value.But because Lac dye is by the secretion of lac insect, or is present in this polypide, a kind of very niff is arranged, had a strong impact on its application in food service industry.In addition, the lac pigment on the market is pulverized extraction together by tachardia lacca secretory product and tachardia lacca now, contains a large amount of granular substances, and is water insoluble, occurs with the throw out state in water, is difficult to smoothen or mixing in food, affects attractive in appearance.Therefore, improve the commercial value of Lac dye, must carry out deep processing and process, in order to obtain the high quality Lac dye.
Lac is unique animal resin, and its composition is different from other natural resin, and the lac moiety is complicated, is comprised of soft resin and hardened resin, and average molecular mass is about 1000, has 1 free carboxy, 5 hydroxyls, 3 ester groups and 1 aldehyde radical in the molecule at least.Contain the materials such as wax, pigment (being divided into haematochrome and yellow pigment), aleutric acid, shelloic acid in the lac.
Lac dye belongs to anthraquinone (anthroquinone) the class pigment in quinone (quinone) class, belongs to dyestuff (dye) the type pigment of water, pure dissolubility from solubility property, is divided into to be A, B, C, D, 5 kinds of color acids of E.Lac pigment can be used in the industry such as textile and dyeing industry, food, and GB 4571-1996 has proposed concrete requirement to food grade Lac dye index.
Lac pigment is generally produced washing the look water of seed lac process from virgin rubber and is extracted, as publication number be the invention of CN101215422A relate to a kind ofly from the virgin rubber lac encrusted twig, extract, the method for refining Lac dye, comprising is soaked in water virgin rubber to extract washes glue and filters washing glue by micro-filtration, ultrafiltration.Publication number is that the invention of CN101319094A relates to a kind of lac haematochrome extracting method, comprise the steps: that virgin rubber is broken, washing is also collected and is washed Se Shui, the lac particle of fragmentation is put into container add water washing and agitation as appropriate, it is for subsequent use that look water is washed in collection, repeats several times; Coarse filtration is carried out coarse filtration and is got coarse filtration liquid washing Se Shui; Ultrafiltration is sent coarse filtration liquid into hyperfiltration membrane assembly and is removed by filter suspended substance, bacterium class, protein, latex etc., gets ultrafiltrated; Nanofiltration is sent ultrafiltrated into nanofiltration membrane component and is removed by filter inorganic salts, carbohydrate etc., gets nanofiltration liquid; Reverse osmosis is delivered to the reverse osmosis module filtering and concentrating with nanofiltration liquid, and concentrated solution contains highly purified laccaic acid, i.e. Lac dye, and aftertreatment, it is levigate that the Lac dye liquid that obtains is carried out drying, namely gets the Lac dye product.
Water colo(u)r in the virgin rubber mainly is present in the worm corpse, in washing the glue process, only has the worm corpse is fully ground, and just might make more polychrom be dissolved in washing in the look water and be recycled, and the worm corpse does not fully grind namely and floated and will have a strong impact on the pigment recovery rate by water.Process 0.3%～0.4% of virgin rubber amount so the extraction level of domestic lac pigment is generally, reasonable situation reaches 0.56%.
Summary of the invention
The objective of the invention is the problem for the prior art existence, a kind of process for purification of Lac dye is provided, and the method technique is simple, and is easy to operate, improve yield and the purity drop production energy consumption of Lac dye, fundamentally solved the industrial problem of environmental pollution of lac.
Lac haematochrome extracting method wherein, in turn includes the following steps:
(1) in ethanol, soaks heating and refluxing extraction after the lac raw material pulverizing with drying;
(2) use macroporous adsorption resin chromatography, wash-out behind the liquid filtering with (1) step gained;
(3) elutriant of (2) gained is concentrated, the dry Lac dye that obtains.
Lac haematochrome extracting method of the present invention, wherein: in the step (1), the lac raw material pulverizing of drying is crossed 40～60 mesh sieves, ethanol is rare alcohol, the mode of soaking heating and refluxing extraction in ethanol is: soak first before extracting first, be heated to little boiling and begin to clock, extract altogether 3 times, each extraction time is 1.0～3.0 hours, merges No. three times extracting solution.
Lac haematochrome extracting method of the present invention, wherein: rare alcohol is that volume by volume concentration is 30% ethanol, soaked first 30 minutes before extracting first, being heated to little boiling begins to clock, and keep little and boil, extraction time is 1.5～2 hours for the first time, extraction time is 1 hour for the second time, extraction time is 1 hour for the third time, and the mass ratio of used rare pure volume and dry lac raw material is (10～18) ml: 1g when extracting at every turn.
Lac haematochrome extracting method of the present invention, wherein: for the first time extraction time is 1.5, the mass ratio of used rare pure volume and dry lac raw material extracts 12ml: 1g for the first time during extraction, extracts 10ml: 1g for the second time, extracts for the third time 10ml: 1g.
Lac haematochrome extracting method of the present invention, wherein: macroporous adsorbent resin is 1: 0.76 with the lac raw materials quality ratio of drying in the step (2).
Lac haematochrome extracting method of the present invention, wherein: macroporous adsorbent resin is the AB-8 type macroporous adsorbent resin that Chemical Plant of Nankai Univ. produces in the step (2), and the loading flow velocity is 2.45ml/min/cm
2
Lac haematochrome extracting method of the present invention, wherein: using volume by volume concentration in the step (2) is that 50～80% ethanol is as elutriant.
Lac haematochrome extracting method of the present invention, wherein: using volume by volume concentration in the step (2) is that 80% ethanol is as elutriant.
Lac haematochrome extracting method of the present invention, wherein: the macroporous adsorbent resin eluent flow rate is 2.45ml/min/cm
2
Lac haematochrome extracting method of the present invention, wherein: step (3) elutriant is concentrated, and in the drying, first with the elutriant concentrating under reduced pressure, it is dry to reclaim the solvent final vacuum, 70～80 ℃ of drying temperatures, 24 hours time of drying.
Advantage of the present invention is:
(1) utilize Lac dye in dilute alcohol solution, to dissolve preferably characteristics, with the lac raw material pulverizing, repeatedly extract with rare alcoholic solvent, the leaching extracting solution, then extracting solution uses the high concentration ethanol wash-out by absorption with macroporous adsorbent resin, concentrate eluant, drying is pulverized, and obtains the Lac dye of high purity odorless.
(2) in the lac pigment extraction process, adopt ethanolic soln to extract, insoluble sludge can be used as industrial raw material as the lac by product, is used for the industrial sectors such as national defence, electrical equipment, coating, machinery, rubber, plastics, process hides, papermaking and printing.
(3) extracting solution is through macroporous adsorptive resins, and the effluent liquid pigment is adsorbed fully, can reuse after distillation.Be used for the column chromatography elutriant after concentrating, reclaim and to reuse.Macroporous adsorbent resin can be reused after manipulation of regeneration for a long time, and treatment solution generates sodium chloride solution through neutralization, realizes nontoxic discharging.
Embodiment
The ratio of the lac raw material of embodiment 1,30% ethanol and drying
Get dry lac, remove the foreign material that are clipped in wherein, be ground into meal, for subsequent use.
Take by weighing 5 parts of lac meal, every part of 100g puts into the 2000ml beaker, adds 30% ethanol of different volumes, soaks first heating and refluxing extraction when extracting first 30 minutes.Being heated to little boiling begins to clock.Extract altogether 3 times, extracted 2.5 hours for the first time, extracted 2.0 hours for the second time, extracted for the third time suction filtration, sample vacuum-drying 1.5 hours.The gained samples weighing is measured the red content of lac with ultraviolet spectrophotometry (UV).
Embodiment 1 the results are shown in Table 1:
The test-results that table 1. lac different amount 30% ethanol (ml) extracts
By embodiment 1 result as can be known, lac is (10～18) ml: 1g with the ratio of extracting with rare alcohol, can be successful to extract total lac red, its extraction yield is 7.6～6.9%, it is many that 2,3,4, No. 5 samples must be measured, the red content no significant difference of lac.No. 3 sample is compared with No. 2 samples, rare pure consumption has increased by 12.5%, sample must be measured with content without obvious increase, in order to save, select the extracting method of No. 2 samples, that is: lac is to extract 1g: 12ml for the first time with the ratio of extracting with rare alcohol, extracts 1g: 10ml for the second time, extract for the third time 1g: 10ml, can obtain preferably effect in industrial application.
The selection of embodiment 2, lac extraction time and extraction time
Take by weighing 5 parts of lac meal, every part of 100g puts into the 2000ml beaker, and each quantitatively adds rare pure 1200ml, soaks first when extracting first 30 minutes, and heating is extracted.Be heated to little boiling and begin to clock, extraction time is respectively 1.0,1.5,2.0,2.5,3.0hr, suction filtration, sample vacuum-drying.The gained samples weighing is measured the red content of lac with ultraviolet spectrophotometry (UV).
The results are shown in Table 2:
Red must the measuring of the different total lacs of extraction time of table 2.
Embodiment 2 experimental results show that extraction time 1.0～3.0hr must measure difference to lac is red, increase but there is no significance behind the 2hr, consider the production practical situation, extract for the first time and select extraction time 2.0hr to get final product.
Lac meal after the filtration adds respectively the rare alcohol of 1000ml and carries out the second time and for the third time heating extraction, is heated to little boiling and begins to clock, and extraction time is respectively 0.5,1.0,1.5,2.0,2.5hr.
The results are shown in Table 3: red must the measuring of different total lacs of extraction time
From the result who extracts and separate, No. 2～No. 5 the sample extraction yield is higher; No. 1 sample extraction time is short, extracts not exclusively; No. 4, the time of No. 5 sample extraction is long, but red must the measuring of lac there is no increase.Because extracting for the third time to such an extent that amount is less, extract so no longer carry out the 4th time.
Consider from the industrialization aspect, determine that technique extracts 3 times, select the extraction time of No. 2 samples namely: be extracted in for the first time and add rare alcohol and soak after 30 minutes, little boiling extracted 1.5hr, for the second time extract 1.0hr, extract for the third time 1.0hr, merge No. 3 extracting solutions and carry out column chromatography for separation.
The selection of embodiment 3, different macroporous adsorbent resins
Take by weighing 5 parts of lac meal, every part of 100g puts into the 2000ml beaker, quantitatively adds 30% ethanol, and minute 3 extractions add respectively 1200ml, 1000ml, the rare alcohol of 1000ml; Soaked first when extracting first 30 minutes, heating is extracted.Being heated to little boiling begins to clock.Extract altogether 3 times, extracted 1.5 hours for the first time, extracted 1.0 hours for the second time, extracted for the third time 1.0 hours.Merge No. 3 times extracting solution, through 10 kinds of different size macroporous adsorptive resins absorption Lac dye constituents, water flush away relative substance uses 80% ethanol elution lac red again, the elutriant concentrating under reduced pressure, it is dry to reclaim the solvent final vacuum, and the UV method is measured content, look valency, examine or check the performance of various resins, the optimal macroporous adsorbent resin of optimization, the selected resin that descends among the present invention is all produced by Chemical Plant of Nankai Univ., the results are shown in Table 4.
The characterization of adsorption that ten kinds of polymeric adsorbents of table 4. are red to lac
| The resin model | Adsorptive capacity (mg/g) | Resolution factor (80%EtOH) | Adsorption rate (mg/t) |
| AB-8 | 126.7 | 97.9 | 0.48 |
| S-8 | 102.8 | 52.9 | 0.51 |
| K-A | 96.1 | 94.8 | 0.46 |
| SIP-1400 | 82.3 | 88.4 | 0.40 |
| SIP-1300 | 75.9 | 89.5 | 0.32 |
| X-5 | 59.4 | 99.9 | 0.40 |
| NKA-9 | 49.1 | 98.3 | 0.62 |
| D3520 | 47.7 | 92.8 | 0.80 |
| H107 | 36.6 | 78.8 | 0.29 |
| D4006 | 19.0 | 93.1 | 0.72 |
It is red multiple macroporous resin to may be used to extract lac from embodiment 4, has obtained good effect, further these results relatively: low-pole AB-8 type resin has larger adsorptive capacity, and easily absorption is easily resolved, and is more excellent.
The selection of embodiment 5, AB-8 type macroporous adsorption resin chromatography condition
The pre-treatment of AB-8 type macroporous adsorbent resin
Take by weighing AB-8 type macroporous adsorbent resin 5kg, with 95% ethanol repetitive scrubbing, do not produce till the white opacity elimination ethanol, water flush away ethanol until add the water of 2 times of amounts in the ethanol that filters out;
With 5% hydrochloric acid soln washing resin, soak 4hr, filter, then wash with water to pH5～6;
With 2% sodium hydroxide solution washing resin, soak 4hr, filter, then wash with water to approaching neutrality, both can use.
The ratio screening of resin demand and extracting solution carrying capacity
Take by weighing lac meal 1kg, put into Stainless Steel Kettle, press 12L, 10L, 10L add rare ethanol-extracted 3 times, are heated to boiling, and extraction time is respectively 1.5hr, 1.0hr, and 1.0hr merges No. 3 extracting solutions and amounts to 24.3kg, and this liquid is called extracting solution No. 2.
Cut-off footpath 2.5cm, 3 of the chromatography columns of long 50cm take by weighing 3 parts of AB-8 resins, every part of 75g, water wet method dress post.No. 2 extracting solutions are added in the chromatography column, and control loading speed is at 2.5ml/min.
The result: the macroporous resin adsorption amount of liquid, 3 pillars are respectively 1395g, 1410g, 1390g, mean value 1398g.Be equivalent to lac amount 1000g * 1.398/24.3=57.5g.The adsorbable extracting solution that is equivalent to the 57.5g lac of 75g resin, the feed ratio of resin and Lac dye is 1: 0.76.
Macroporous adsorbent resin loading flow rate control
Cut-off footpath 2.5cm, 3 of the chromatography columns of long 50cm take by weighing 3 parts of AB-8 resins, every part of 75g, water wet method dress post.No. 2 extracting solutions are added in the chromatography column, and control loading speed is respectively 5ml/min, 8ml/min, 12ml/min.Do not detected the red composition of obvious lac in the elutriant and namely be judged to be the absorption terminal point, consumption is respectively 1375g, 1350g, 1320g.
Interpretation of result: resin demand is 2.5ml/min with the ratio test coutroi velocity that extracts liquid measure, extracting solution consumption average out to 1398g, and from flow velocity 2.5ml/min to 12ml/min, flow velocity has increased by 3.8 times, and volume containing the sample has only reduced 4.9%, affects without significance.Consider the production practical situation, the loading flow velocity can be controlled at about 12ml/min.
Used chromatography column incipient fusion filter plate area: S=3.14 * (2.5/2)
2=4.9 (cm
2);
Amount to into cm
2Flow velocity: 12ml/min ÷ 4.9cm
2=2.45g/min/cm
2
The investigation of embodiment 6, eluent alcohol concn, consumption, flow velocity
Shellac solution with rare ethanol-extracted contains the red constituents of abundant lac, and this constituents can be adsorbed when flowing through macroporous adsorbent resin.Desorb can be used water miscible organic solvent, such as methyl alcohol, and ethanol, the different concns aqueous solution such as propyl alcohol, propyl carbinol.But from the industrial production cost, the aspects such as labour protection and environment protection are considered, are selected the ethanol effect best.
Cut-off footpath 2.5cm, 5 of the chromatography columns of long 50cm take by weighing 5 parts of AB-8 resins, every part of 75g, water wet method dress post.Each adds extracting solution 1300g No. 2, and flow rate control is at about 12ml/min, add extracting solution after, water washes to effluent liquid substantially colourless, then uses 90%, 80%, 70%, 60%, 50% different concentration ethanol wash-out.
The wash-out terminal point determining: color and luster is thin out.The results are shown in Table 4:
Table 5. different concentration ethanol column chromatography elute effect
According to the eluant strength the selection result, select 80% ethanol better as the eluent effect.
The examination of eluent 80% ethanol consumption
Cut-off footpath 2.5cm, 2 of the chromatography columns of long 50cm take by weighing 2 parts of AB-8 resins, every part of 75g, water wet method dress post.Each adds extracting solution 1300g No. 2, and flow rate control is at about 12ml/min, add extracting solution after, water washes to effluent liquid substantially colourless, then uses 80% concentration ethanol wash-out.When getting off, keeps by colour band volume in mind.Wash-out terminal point inspection method is the same.
The result: 2 chromatography column eluent consumptions are 420g.
The examination of eluent flow velocity
Cut-off footpath 2.5cm, 5 of the chromatography columns of long 50cm take by weighing 5 parts of AB-8 resins, every part of 75g, water wet method dress post.Each adds extracting solution 1300g No. 2, and flow rate control is at 12ml/min, add extracting solution after, water washes to effluent liquid substantially colourless, then uses 80% concentration ethanol wash-out, flow rate control 4,6,8,10,12ml/min, the wash-out terminal point checks with embodiment 5.
The result: the wash-out cumulative volume is respectively 285g, 320g, 358g, 370g, 420g.
Conclusion: 1) along with the increase of flow velocity, consume the volume of elutriant also along with increase;
2) 12ml/min is near the Peak Flow Rate of chromatography column, industrial production chromatography column material, and sieve plate and glass chromatography column below namely are close; Therefore can coutroi velocity 12/3.14 (2.5/2)
2=2.45ml/min/cm
2
Macroporous adsorptive resins is reused test
Get " examination of eluent flow velocity " No. 1 post (4ml/min), wash with water to proportion near 1.0 o'clock, add No. 2 the lac extracting solution, flow velocity 10g/min.Thin out as checking terminal point with color and luster.
The result: the composition ability is 1300g in the 2nd time adsorptive liquid;
The composition ability is 1150g in the 3rd time adsorptive liquid;
The composition ability is 1000g in the 4th time adsorptive liquid.
Macroporous adsorbent resin can be regenerated after using 3 times.
Method: with the 3rd used macroporous resin water flush away ethanol, with 5% hydrochloric acid displaces water, soak 4hr, wash disacidify water with water, again with the flushing of 1% aqueous sodium hydroxide solution, immersion 4hr washes with water to the pH value and is about 7, reuses.
Embodiment 7
Take by weighing 3 parts of lac meal, every part of 100g puts into the 2000ml beaker, quantitatively adds 30% ethanol, minute 3 extractions, the 1st group: be followed successively by adding 1000ml, 1000ml, the rare alcohol of 1000ml; Soaked first when extracting first 30 minutes, heating is extracted.Being heated to little boiling begins to clock.Extract altogether 3 times, extracted 1.0 hours for the first time, extracted 1.0 hours for the second time, extracted for the third time 1.0 hours.Merge No. 3 times extracting solution, through K-A specification macroporous adsorptive resins absorption Lac dye constituents, water flush away relative substance uses 80% ethanol elution lac red again, the elutriant concentrating under reduced pressure, and it is dry to reclaim the solvent final vacuum, and the UV method is measured content, look valency; Second group: be followed successively by adding 1800ml, 1800ml, the rare alcohol of 1800ml; Soaked first when extracting first 30 minutes, heating is extracted.Being heated to little boiling begins to clock.Extract altogether 3 times, extracted 3.0 hours for the first time, extracted 3.0 hours for the second time, extracted for the third time 3.0 hours.Merge No. 3 times extracting solution, through SIP-1400 specification macroporous adsorptive resins absorption Lac dye constituents, water flush away relative substance uses 50% ethanol elution lac red again, the elutriant concentrating under reduced pressure, and it is dry to reclaim the solvent final vacuum, and the UV method is measured content, look valency; The results are shown in Table 6.
The comparison of the product amount of gained under the different rare pure amounts of table 6., extraction time, macroporous resin type and the ethanol concn condition
The comparison of the quality product of gained under the different rare pure amounts of table 7., extraction time, macroporous resin type and the ethanol concn condition
Although from embodiment 7 as can be known first group different with ethanol concn with second group of rare pure amount, extraction time, macroporous resin type, the yield of the Lac dye that extracts is all higher, steady quality.
The pilot scale scale-up of embodiment 8, preparation Lac dye
Get dry lac raw material, remove the foreign material that are clipped in wherein, be ground into meal, cross 60 mesh sieves, take by weighing 13kg, put into the multi-function extractor of 200L, soaked 30 minutes before extracting first, press 156L, 130L, 130L volume by volume concentration are 30% rare ethanol-extracted 3 times, and steam heating to little boiling begins to clock, extraction time is respectively 1.5hr, 1hr, 1hr gets the 1st 98.0kg of extracting solution, the 2nd 117.7kg, the 3rd 121.8kg, the liquid of three extractions amounts to 337.5kg, and No. 3 extracting solutions are equally divided into 4 parts, mix, for subsequent use.
Dress post: 4 of mounting glass chromatography columns, long 95cm, internal diameter 9.5cm, add 4.3kg AB-8 type macroporous adsorbent resin in every chromatography column, then wet method dress post uses respectively 95% ethanol, 5% hydrochloric acid, 1% sodium hydroxide is clean with plastic resin treatment, washes with water to the pH value to be about 7.
Column chromatography: loading flow velocity 190g/min, 80% ethanol elution flow velocity 190g/min.
Concentrated and dry: the elutriant concentrating under reduced pressure, it is dry to reclaim the solvent final vacuum.70～80 ℃ of drying temperatures, time of drying 24hr.The UV method is measured content, the look valency, and test-results sees Table 7:
Table 8. pilot scale scale-up result
The yield of prepared Lac dye product is 6.8%, and every quality index detects according to foodstuff additive Lac dye State Standard of the People's Republic of China GB4571-1996, all meets the requirements, and detected result sees Table 8.
The every determination of quality index result of table 9 Lac dye
| Project | GB4571-19 96 indexs | Sample through No. 1 post gained | Sample through No. 2 post gained | Sample through No. 3 post gained | Sample through No. 4 post gained |
| Absorbancy (E0.01% solution 0.05cm colourimetric number 490nm | ≥0.65 | 6.81 | 6.15 | 6.18 | 6.59 |
| Weight loss on drying, % | ≤10 | 2.81 | 2.79 | 2.85 | 2.69 |
| Ignition residue % | ≤0.8 | 0.22 | 0.28 | 0.31 | 0.29 |
| PH value | 3.0-4.0 | 3.19 | 3.35 | 3.22 | 3.22 |
| Plumbous (Pb) mg/kg | ≤5 | 0.52 | 0.49 | 0.56 | 0.29 |
| Arsenic (As) mg/kg | 2 | 0.12 | 0.15 | 0.11 | 0.08 |
Lac dye quality index absorbancy, weight loss on drying, ignition residue, the detection of pH value is undertaken by the GB4571-1996 standard, plumbous (Pb) and arsenic (As) detect by GB/T5009.12-2003 and GB/T5009.11-2003 respectively, use as seen from table its weight loss on drying of Lac dye that the inventive method is produced, ignition residue, plumbous, the indices such as arsenic significantly are lower than national standard, especially plumbous, the limit value that arsenic poisonous metal content is stipulated in the national standard, significantly improved the application security of food dye, absorbancy is much larger than national standard, pH value meets the requirements, the requirement of the red product quality indicator conformance with standard of lac.
The pilot scale scale-up is the result show, extracts the red feasible process of total lac with lac, and technique is more stable.
Above embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (3)
1. lac haematochrome extracting method is characterized in that, in turn includes the following steps:
(1) in ethanol, soaks heating and refluxing extraction after the lac raw material pulverizing with drying;
(2) use macroporous adsorption resin chromatography, wash-out behind the liquid filtering with (1) step gained;
(3) elutriant of (2) gained is concentrated, the dry Lac dye that obtains;
In the described step (1), the lac raw material pulverizing of drying is crossed 40 ~ 60 mesh sieves, described ethanol is rare alcohol, described mode of soaking heating and refluxing extraction in ethanol is: soak first before extracting first, being heated to little boiling begins to clock, extract altogether 3 times, each extraction time is 1.0～3.0 hours, merges No. three times extracting solution;
Described rare alcohol is that volume by volume concentration is 30% ethanol, soaked first 30 minutes before extracting first, being heated to little boiling begins to clock, and keep little and boil, extraction time is 1.5～2 hours for the first time, for the second time extraction time is 1 hour, and extraction time is 1 hour for the third time, and the mass ratio of used rare pure volume and dry lac raw material is 10～18ml:1g when extracting at every turn;
Macroporous adsorbent resin is 1:0.76 with the lac raw materials quality ratio of drying in the described step (2);
Macroporous adsorbent resin is AB-8 described in the described step (2), and the loading flow velocity is 2.45ml/min/cm
2
Using volume by volume concentration in the described step (2) is that 50～80% ethanol is as elutriant;
Described macroporous adsorbent resin eluent flow rate is 2.45ml/min/cm
2
Described step (3) elutriant is concentrated, in the drying, and first with elutriant concentrating under reduced pressure, vacuum-drying, 70 ~ 80 ℃ of drying temperatures, 24 hours time of drying.
2. want 1 described lac haematochrome extracting method according to right, it is characterized in that: extraction time is 1.5 hours for the first time, the mass ratio of used rare pure volume and dry lac raw material during extraction: extract 12ml:1g for the first time, extract 10ml:1g for the second time, extract for the third time 10ml:1g.
3. lac haematochrome extracting method according to claim 1 is characterized in that: using volume by volume concentration in the step (2) is that 80% ethanol is as elutriant.
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| CN102775811A (en) * | 2012-08-01 | 2012-11-14 | 乌鲁木齐三高和药业有限公司 | Process of extracting flavonoids from Coreopsis bicolor |
| CN102816455A (en) * | 2012-08-06 | 2012-12-12 | 集美大学 | Method for extracting pigment and pectin from pineapple peels |
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| CN101319094A (en) * | 2008-06-16 | 2008-12-10 | 深圳职业技术学院 | Lac haematochrome extracting method |
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| CN101215422A (en) * | 2008-01-21 | 2008-07-09 | 中国林业科学研究院资源昆虫研究所 | Method for refining lac red coloring matter |
| CN101319094A (en) * | 2008-06-16 | 2008-12-10 | 深圳职业技术学院 | Lac haematochrome extracting method |
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