CN1720817A - Combination use of absorption and ion exchange for removing lead from propolis - Google Patents
Combination use of absorption and ion exchange for removing lead from propolis Download PDFInfo
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- CN1720817A CN1720817A CNA200310122475XA CN200310122475A CN1720817A CN 1720817 A CN1720817 A CN 1720817A CN A200310122475X A CNA200310122475X A CN A200310122475XA CN 200310122475 A CN200310122475 A CN 200310122475A CN 1720817 A CN1720817 A CN 1720817A
- Authority
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- China
- Prior art keywords
- propolis
- post
- ion exchange
- deleading
- exchange resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005342 ion exchange Methods 0.000 title claims abstract description 10
- 241000241413 Propolis Species 0.000 title claims description 34
- 229940069949 propolis Drugs 0.000 title claims description 34
- 238000010521 absorption reaction Methods 0.000 title description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 9
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004575 stone Substances 0.000 claims abstract description 9
- 239000010457 zeolite Substances 0.000 claims abstract description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003292 glue Substances 0.000 claims abstract description 8
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 8
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 8
- 238000004062 sedimentation Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 231100000252 nontoxic Toxicity 0.000 claims description 2
- 230000003000 nontoxic effect Effects 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 6
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000005909 Kieselgur Substances 0.000 abstract 1
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- 241000256844 Apis mellifera Species 0.000 description 6
- 238000010586 diagram Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000009341 apiculture Methods 0.000 description 2
- 235000013871 bee wax Nutrition 0.000 description 2
- 239000012166 beeswax Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000000153 supplemental effect Effects 0.000 description 2
- BVPWJMCABCPUQY-UHFFFAOYSA-N 4-amino-5-chloro-2-methoxy-N-[1-(phenylmethyl)-4-piperidinyl]benzamide Chemical compound COC1=CC(N)=C(Cl)C=C1C(=O)NC1CCN(CC=2C=CC=CC=2)CC1 BVPWJMCABCPUQY-UHFFFAOYSA-N 0.000 description 1
- 208000002874 Acne Vulgaris Diseases 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010027439 Metal poisoning Diseases 0.000 description 1
- 208000010195 Onychomycosis Diseases 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 206010047601 Vitamin B1 deficiency Diseases 0.000 description 1
- 208000000260 Warts Diseases 0.000 description 1
- 206010000496 acne Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 208000002894 beriberi Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007661 gastrointestinal function Effects 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000008127 lead poisoning Diseases 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011321 prophylaxis Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 201000010153 skin papilloma Diseases 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 201000005882 tinea unguium Diseases 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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- Jellies, Jams, And Syrups (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention discloses a process for removing lead from bee glue which comprises, pre-processing medical stone, zeolite and ion exchange resin, loading into ion exchange column respectively to form a series connection, then accelerating the sedimentation of the ethanol-lixiviated bee glue with diatomaceous earth, carrying out centrifugal filtration to obtain bee glue and ethanol solution, charging a small amount of acetic acid to adjust pH to 5.0-6.0, passing through exchange columns in series connection, carrying out cryoconcentration to the bee glue solution, finally reclaiming ethanol to obtain end product containing lead content <=0.02mg/kg.
Description
The present invention relates to a kind of propolis deleading technique.
Propolis is the resin on honeybee herborization young shoot and the trunk, and sneaks into its mandibular gland secretion and a kind of colloidal solid thing with aromatic odor of processing such as beeswax.Propolis is approximately by 50% resin and the fragrant liquid of plant, and 30% beeswax, 10% aromatic oil material, 5% pollen and 5% comprise other material composition of organ clast.Propolis has significantly and unique biological is active, is applied to fields such as medicine, food, chemical industry more and more widely, and development prospect is wide.
At present, along with the raising of China's living standards of the people, the apiculture of China is flourishing day by day, and bee product, particularly bee glue product more and more are subjected to people's welcome and favor, and is also more and more deep to the research of bee product simultaneously.Because contain tens classes in the propolis, more than 300 kind of natural component, comprising more than 30 kinds of trace element, 20 several amino acids that human body is necessary, tens of kinds of aromatics, more than 70 kind of Flavonoid substances also have rich organic acid, terpenoid substance, vitamin, enzyme, polysaccharide etc. to have the natural component of BA.Propolis has prevention and supplemental treatment effect preferably to human numerous disease, can be used for supplemental treatment beriberi, acne, flat wart, onychomycosis, eczema etc., have well activate blood circulation and disperse blood clots, softening blood vessel, reducing blood lipid, sterilization, pain relieving, hypoglycemic, prophylactic treatment diabetes, anti-oxidant, antitumor, delay senility, improve gastrointestinal function, stop platelet aggregation, improve effects such as microcirculation.
Because higher lead content is arranged in the propolis, and (lead 〉=5mg/kg) takes for a long time not that the deleading propolis certainly will cause chronic lead poisoning, so deleading is a CCP in the propolis production and processing.There are not deleading technique, lead content severe overweight in some producer's bee glue purifying technology at present; Some producer adopts the natural sedimentation deleading, and elapsed time is long, and lead content 〉=2mg/kg, surpasses the relevant requirement of limiting the quantity of of country; Some enterprises adopts adsorbents adsorb deleadings such as active carbon, and its effect can not guarantee and active ingredients such as a large amount of flavonoids of adsorbents adsorb such as active carbon, thereby causes a large amount of losses of functional component; Also have indivedual producers to adopt technology deleadings such as the lixiviate of gradient alcohol, freezing sedimentation, means of supercritical extraction propolis etc., its deleading is respond well, but equipment requires height, and complicated operation is not suitable for popular the popularization.
The invention provides a kind of deleading technique easily, deleading is respond well, and equipment is simple, easy to operate, is applicable to each producer with alcohol equal solvent bee glue purifying.
The present invention is achieved in that and will be respectively charged in the ion exchange column after the preliminary treatment such as medical stone, zeolite, ion exchange resin, formation is connected in series, after the propolis after the edible alcohol lixiviate is with acceleration sedimentation, centrifugal filtrations such as diatomite, becoming the propolis wine seminal fluid, add little acetic acid and make its pH between 5.0-6.0.Exchange column by being connected in series then, cross behind the post propolis liquid through low temperature concentrate, recovered alcohol, just become the finished product of effective deleading, its lead content≤0.02mg/kg, deleading process loss of effective components≤1%.
Concrete technology is as follows:
1. medical stone, zeolite, ion exchange resin preliminary treatment
40-100 order medical stone, zeolite are cleaned the back soaked 10-24 hour with weak acid, and then extremely neutral with rinsed with deionized water, adorn post then.
Ion exchange resin is selected the weak-type cationic ion-exchange resin for use, requires itself and organic adsorption capacity little, with being rinsed into neutral back dress post with ionized water after acid, the alkali treatment.
2. the selection of pillar
Ion exchange column requires to make with pmma material or other non-toxic materials, and its post directly is 25-200 centimetre, and the post height is 1.0 meters-2.5 meters, and wall thickness is 3 millimeters-45 millimeters, the two ends end socket.
3. mode is connected in series
Medical stone post, zeolite column, ion exchange resin column connected mode are seen accompanying drawing (Fig. 1, Fig. 2, Fig. 3).
Fig. 1 is connection diagram simply connected figure; Fig. 2 is connection diagram duplex figure; Fig. 3 is connection diagram three figure.
4. propolis liquid is accelerated sedimentation
Propolis liquid is added the 0.1%-1% diatomite (100-200 order) of propolis amount after initial filter, stir 0.5 About-2 hours, leave standstill after 12-48 hour and will precipitate centrifugal removal, propolis liquid is for subsequent use.
5. cross post
Propolis liquid is flow through the exchange column that connects, and flow velocity is looked post footpath and post Gao Erding, and flow is the 0.1-1 ton / hour.
6. concentrate, finished product
The propolis liquid of crossing the post deleading through low temperature concentrate, alcohol reclaims, the packing of product, get final product plumbously≤ 0.02mg/kg the propolis finished product.
Deleading technique is extracted in technological process 1 propolis virgin rubber for example:
Virgin rubber pulverizing → 4-6 doubly 2-3 days → centrifugal impurity elimination of 95% alcohol lixiviate → freezing paraffin removal → diatomite quickens precipitation → accent PH → mistake ion-exchange columns in series → concentrated finished product
Technological process is the processing art for extracting propolis and removing lead from it in 2 beehive drop cloth, beehive cover net, the beekeeping equipment for example:
Beehive drop cloth, beehive cover net → 2-6 be 95% alcohol-pickled → centrifugation or isolated by filtration → freezing paraffin removal → diatomite acceleration sedimentation → mistake ion-exchange columns in series doubly
Claims (6)
- A kind of propolis deleading technique, it is used diatomite and quickens sedimentation, medical stone, zeolite, cationic ion-exchange resin connect into the series connection ion exchange column adsorb, ion exchange lead removal, its deleading effect can reach lead content≤0.02mg/kg, deleading process effective bee glue components loss≤1%, this technology lead tolerance is lower than the content behind the propolis deleading of the same trade, also is lower than the requirement of external bee product lead≤0.15mg/kg.Its equipment is simple, and is easy to operate, is fit to each the tame enterprise that extracts, processes propolis with the edible alcohol equal solvent.Its technology is performed as follows: its technology is specific as follows:1. medical stone, zeolite, ion exchange resin preliminary treatment40-120 order medical stone, zeolite are cleaned the back soaked 10-24 hour with weak acid, extremely neutral with rinsed with deionized water again, adorn post then.Ion exchange resin is selected the weak-type cationic ion-exchange resin for use, requires itself and organic adsorption capacity little, with being rinsed into neutral back dress post with ionized water after acid, the alkali treatment.
- 2. the selection of pillarIon exchange column requires to make with pmma material or other non-toxic materials, and its post footpath is by 25-200 centimetre, 1.0 meters-2.5 meters of post high requests, and wall thickness requires 3 millimeters-45 millimeters, the two ends end socket.
- 3. mode is connected in seriesMedical stone post, zeolite column, ion exchange resin column connected mode are seen accompanying drawing 1.
- 4. propolis liquid is quickened sedimentation0.1%-1% diatomite (100-200 order) with propolis liquid adding propolis amount after filter just stirred about 0.5-2 hour, left standstill after 12-48 hour and will precipitate centrifugal removal.Propolis liquid is standby.
- 5. cross postPropolis liquid is flow through the exchange column that connects, and flow velocity is looked post footpath and post Gao Erding, flow from the 0.1-1.0 ton/hour.
- 6. concentrated, finished productThe propolis liquid of crossing the post deleading through low temperature concentrate, alcohol reclaims, the packing of product gets final product plumbously≤the propolis finished product of 0.02mg/kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310122475XA CN1313020C (en) | 2003-12-25 | 2003-12-25 | Combination use of absorption and ion exchange for removing lead from propolis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310122475XA CN1313020C (en) | 2003-12-25 | 2003-12-25 | Combination use of absorption and ion exchange for removing lead from propolis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1720817A true CN1720817A (en) | 2006-01-18 |
| CN1313020C CN1313020C (en) | 2007-05-02 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200310122475XA Expired - Lifetime CN1313020C (en) | 2003-12-25 | 2003-12-25 | Combination use of absorption and ion exchange for removing lead from propolis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1313020C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101176565B (en) * | 2007-12-05 | 2011-04-13 | 青海康普生物科技股份有限公司 | Method for reducing heavy metal plumbi content in sha ji fruit juice raw material by ion exchange process |
| CN101991606B (en) * | 2009-08-12 | 2012-07-04 | 牛建伟 | Preparation method of solid water-soluble lead-removed propolis |
| CN110184135A (en) * | 2019-05-23 | 2019-08-30 | 江苏蜂奥生物科技有限公司 | A kind of antibacterial dish washing liquid of propolis and preparation method thereof |
| CN110403893A (en) * | 2019-08-06 | 2019-11-05 | 江苏蜂奥生物科技有限公司 | A kind of mildy wash containing propolis extract |
| CN110639226A (en) * | 2019-09-24 | 2020-01-03 | 江苏蜂奥生物科技有限公司 | Method for removing impurities in propolis |
| CN110665470A (en) * | 2019-09-24 | 2020-01-10 | 江苏蜂奥生物科技有限公司 | Adsorbent used in propolis extraction process and preparation method thereof |
| CN112826007A (en) * | 2021-01-28 | 2021-05-25 | 北京农科亿健蜂产品研究院 | Device and method for removing heavy metals by propolis mixed liquid |
| CN113750120A (en) * | 2021-10-11 | 2021-12-07 | 北京德蜂堂健康科技有限公司 | Propolis extract and production process and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140184C (en) * | 2000-06-14 | 2004-03-03 | 侯加源 | Processing art for extracting propolis and removing lead from it |
| CN1220497C (en) * | 2001-09-18 | 2005-09-28 | 姜德勇 | Antivirus antioxidizing active extract of proplis and its molecular inclusion compound |
-
2003
- 2003-12-25 CN CNB200310122475XA patent/CN1313020C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101176565B (en) * | 2007-12-05 | 2011-04-13 | 青海康普生物科技股份有限公司 | Method for reducing heavy metal plumbi content in sha ji fruit juice raw material by ion exchange process |
| CN101991606B (en) * | 2009-08-12 | 2012-07-04 | 牛建伟 | Preparation method of solid water-soluble lead-removed propolis |
| CN110184135A (en) * | 2019-05-23 | 2019-08-30 | 江苏蜂奥生物科技有限公司 | A kind of antibacterial dish washing liquid of propolis and preparation method thereof |
| CN110403893A (en) * | 2019-08-06 | 2019-11-05 | 江苏蜂奥生物科技有限公司 | A kind of mildy wash containing propolis extract |
| CN110639226A (en) * | 2019-09-24 | 2020-01-03 | 江苏蜂奥生物科技有限公司 | Method for removing impurities in propolis |
| CN110665470A (en) * | 2019-09-24 | 2020-01-10 | 江苏蜂奥生物科技有限公司 | Adsorbent used in propolis extraction process and preparation method thereof |
| CN112826007A (en) * | 2021-01-28 | 2021-05-25 | 北京农科亿健蜂产品研究院 | Device and method for removing heavy metals by propolis mixed liquid |
| CN113750120A (en) * | 2021-10-11 | 2021-12-07 | 北京德蜂堂健康科技有限公司 | Propolis extract and production process and application thereof |
| CN113750120B (en) * | 2021-10-11 | 2023-10-24 | 北京德蜂堂健康科技有限公司 | Propolis extract and production process and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1313020C (en) | 2007-05-02 |
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