CN1277816A - Processing art for extracting propolis and removing lead from it - Google Patents
Processing art for extracting propolis and removing lead from it Download PDFInfo
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- CN1277816A CN1277816A CN00105486A CN00105486A CN1277816A CN 1277816 A CN1277816 A CN 1277816A CN 00105486 A CN00105486 A CN 00105486A CN 00105486 A CN00105486 A CN 00105486A CN 1277816 A CN1277816 A CN 1277816A
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Abstract
The present invention relates to a lead removal technology for propolis extraction, it adopts liquid nitrogen low temperature grinding, repearted cold extraction by using different concentration edible alcohol, freeze-settling and centrifuging to remove lead under critical state, low temperature vacuum concentration, and distillating tower to recover alcohol so as to obtain the lead-removed propolis. Adventages include little loss of volatile oil, extraction rate of propolis up to higher than 96%, quick settling of lead, and low lead content below 0.05ppm.
Description
The present invention relates to a kind of processing art for extracting propolis and removing lead from it.
At present, raising day by day along with China's living standards of the people, the apiculture of China is also flourishing day by day, research to bee product is also more and more paid attention to, particularly bee glue product more and more is subjected to people's welcome and favor, 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, tens of kinds of aromatics, more than 20 kind of Flavonoid substances that human body is necessary, also have rich organic acid, the rare class material of terpene, vitamin, enzyme, polysaccharide etc. to have the natural component of BA.Propolis has peculiar therapeutic action to human numerous disease, can be used for treating beriberi, acne, flat wart, onychomycosis, eczema ..., have well promoting blood circulation and removing blood stasis, softening blood vessel, reducing blood lipid, sterilization, pain relieving, hypoglycemic, prophylactic treatment diabetes, anti-oxidant, antitumor, delay senility, improve gastrointestinal function, stop blood platelet to solidify, improve effects such as microcirculation.Yet existing propolis extraction process is still undesirable, and 1. general producer only smashes propolis, pulverizes with common pulverizer at normal temperatures, causes loss of volatile oil more than half, and propolis is met heat and is clamminess, and pulverizes difficulty, and efficient is extremely low, and yield is not high; 2. adopt 95% alcoholic extraction mostly, yield has only 80%, and the amount that most of water-soluble active ingredient mineral matter, amino acid, enzyme extracts in the propolis is extremely low, and especially the flavonoid class material is the highest in the solubility of 70 ° alcohol, has caused great waste.3. the just sedimentation under field conditions (factors) of general producer, the consumption time is long, and approximately 6-10 month, and lead content 〉=2PPM; 4. the way that adopts the directly logical steam of jacketed pan to boil at present, loss of volatile oil is more than half, the gelatinizations more than half of propolis medicinal extract, the most of loss of functional component, collecting 60%500kg medicinal extract concentrated consuming time is more than 4 hours, steam expends too big; 5. saying of recovered alcohol also do not arranged at present, imitate the alcohol that steams from two and have only 80 °, utilizability is low, and the alcohol waste is serious.In a word, existing propolis extraction process haves much room for improvement.
The object of the present invention is to provide a kind of processing art for extracting propolis and removing lead from it, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this: it is pulverized through liquid nitrogen cryogenics; The variable concentrations edible alcohol is cold soaking repeatedly; Face under Jie's state freezing sedimentation and get rid of filtering lead; Economic benefits and social benefits energy-saving vacuum low-temperature reduced-pressure concentrates; A kind of processing art for extracting propolis and removing lead from it that method that alcohol in high concentration utilizes is again finished is reclaimed in alcohol distillation column distillation, it is characterized in that it is undertaken by following technology:
(1) liquid nitrogen cryogenics is pulverized
1. the bulk propolis is placed under the environmental condition below-4 ℃, freezing 12 hours,
2. the piece glue of deep colling is pounded into the fritter of 0.5cm diameter,
3. the fritter propolis is taken advantage of and is cooler than below-10 ℃, pulverize first pass, become meal with the Universalpulverizer of topping up nitrogen,
4. above-mentioned fritter glue is placed below-10 ℃, be ground into the above fine powder of 200 orders with the Universalpulverizer of topping up nitrogen, in order to lixiviate,
(2) use variable concentrations edible alcohol cold soaking repeatedly
1. 70 °, 85 °, 95 ° edible alcohol is taken up in order of priority and squeezes in the steeping tank of belt stirrer, slowly add the propolis fine powder that crushes, the limit edged stirs, and soaks 24 hours, stirred 20-30 minute every 1 hour,
2. earlier 70 ° of edible alcohols are squeezed in the steeping tank of belt stirrer in 1: 1 ratio of inventory, slowly added the propolis fine powder that crushes, the limit edged stirs, and soaks 24 hours, stirred 20-30 minute every 1 hour,
3. extract in the steeping tank 4/5 supernatant, in the settling tank with pump suction band cooling coil,
4. with 85 °, 95 ° edible alcohols in successively squeezing in the steeping tank of residual 1/5 soak at twice with 1: 1 ratio of inventory, repeat aforesaid operations, each soaked 24 hours, extracted 4/5 supernatant respectively, incorporate into pump in the settling tank of above-mentioned band cooling coil,
5. the residual liquid of remainder is reinstated the centrifuge that adds three layers of 80-120 order filter cloth together with residue one and dries, get filtrate and incorporate in the above-mentioned settling tank,
(3) get rid of filtering lead facing under Jie's state freezing sedimentation
1. the propolis supernatant mixture with above-mentioned three kinds of gradient alcoholic extractions pumps in the settling tank of band cooling coil,
2. feed liquid ammonia cooling in the coil pipe to-4 ℃, kept 72 hours,
3. take advantage of cold-draw supernatant 4/5, dry, get filtrate, wait to concentrate with the centrifuge that adds three layers of 80-120 order filter cloth,
(4) adopt economic benefits and social benefits energy-saving vacuum low-temperature reduced-pressure to concentrate
1. vacuumize charging,
Close all concentration tank valves, open vavuum pump, make one or two to imitate vacuums and rise to 0.05MPa and begin charging, an advanced effect when above, when feed liquid rises to concentration tank visor 1/3 place, close charging and divide valve, open two effect chargings subsequently and divide valve, when feed liquid rises to nozzle hole, close charging and divide valve
2. open condensation cycle system and alcohol distillation column
Open the condensation cycle system when exhausting material, open the alcohol distillation column steam valve simultaneously, make pressure reach 3MPa,
3. vacuum decompression concentrates
1, an effect concentrates
A, unlatching vacuum decompressioning and concentrating tank steam valve, gauge pressure is controlled at 0.1-0.2MPa
Vapour pressure≤0.2Mpa,
B, open cooling water, open alcohol distillation column and reclaim distillation, about about 85 ° alcohol distillation to 95 of coming out from concentration tank ° utilizes again
C, vacuum degree control are below 0.08MPa, and along with the evaporation of alcohol, the continuous minimizing of feed liquid needs in time to replenish feed liquid, when below feed liquid is lower than during visor 30cm place, in time replenishes feed liquid and arrive visor 1/3 place
2, two effects concentrate
A, close one and imitate vacuum to 0, complete opening two is imitated vacuum, two effect vacuums are risen to below the 0.08MPa, close the charging main valve, open one and imitate baiting valve and two effect inlet valves, utilize action of pressure to imitate the whole suction two of feed liquid to one and imitate in the evaporators, drive steam valve, and open and stir, when being raised to a certain degree, concentration receives cream
B, put jar and to receive a cream while hot
Making two effect vacuums is 0, emits medicinal extract while hot, solidifies retrogradation in case fluid cools off
(5) reclaim alcohol in high concentration so that utilize again with the alcohol distillation column distillation
1. imitate the alcohol that distills out with one or two and directly feed alcohol distillation column,
2. open steam valve, to gauge pressure be 3MPa, vapo(u)rizing temperature is 105 ℃, tower top temperature is 74-76 ℃, cooling water temperature is controlled at below 10 ℃, can adopt alcohol water summer,
When treating that 3. alcohol concentration reaches more than 95 °, open recovery valve and go into finished product alcohol basin, reclaim cycling and reutilization.
The present invention compared with prior art, its loss of volatile oil is few, propolis recovery rate height can reach more than 96%, plumbous sedimentation is quick, saves time, and lead content is low, can reach below the 0.05ppm, surpass the like product of the Japan and the U.S., the active ingredient of extraction is many, and the recovery rate height.
Further specify the present invention below in conjunction with embodiment
Embodiment 1
(1) liquid nitrogen cryogenics is pulverized
1. 200kg bulk propolis is placed under the environmental condition below-4 ℃, freezing 2 hours,
2. the piece glue of deep colling is pounded into the fritter of 0.5cm diameter,
3. the fritter propolis is taken advantage of the Universalpulverizer that is cooler than below-10 ℃ with topping up nitrogen and is not added screen cloth and pulverize first pass, become meal,
4. above-mentioned fritter glue is placed the Universalpulverizer of topping up nitrogen below-10 ℃ to be ground into fine powder more than 200 orders, in order to lixiviate,
(2) use variable concentrations edible alcohol cold soaking repeatedly
1. each 200kg of edible alcohol of 70 ° 85 ° 95 ° is taken up in order of priority and squeezes in the steeping tank of belt stirrer, slowly add the propolis fine powder that crushes, the limit edged stirs, and soaks 24 hours, every stirring in 1 hour 25 minutes
2. earlier 70 ° of 200kg edible alcohols are squeezed in the steeping tank of belt stirrer, slowly added the propolis fine powder that crushes, the limit edged stirs, and soaks 24 hours, stirs 25 minutes every 1 hour
3. extract in the steeping tank 4/5 supernatant, in the settling tank with pump suction band cooling coil,
4. 85 °, 95 ° 200kg edible alcohols are successively squeezed in residual 1/5 steeping tank at twice, repeated aforesaid operations, each soaked 24 hours, extracted 4/5 supernatant respectively, incorporate into pump in the settling tank of above-mentioned band cooling coil,
5. the residual liquid of remainder is reinstated the centrifuge that adds three layer of 100 order filter cloth together with residue one and dries, get filtrate and incorporate in the above-mentioned settling tank,
(3) get rid of filtering lead facing under Jie's state freezing sedimentation
1. the propolis supernatant mixture with above-mentioned three kinds of gradient alcoholic extractions pumps in the settling tank of band cooling coil,
2. feed liquid ammonia cooling in the coil pipe to-4 ℃, kept 72 hours
3. take advantage of cold (4 ℃) and draw up clear liquid 4/5, dry, get filtrate, wait to concentrate with the centrifuge that adds three layer of 100 order filter cloth
(4) adopt economic benefits and social benefits energy-saving vacuum low-temperature reduced-pressure to concentrate
1. vacuumize charging,
Close all concentration tank valves, open vavuum pump, make one or two to imitate vacuums and rise to 0.05MPa and begin charging, an advanced effect when above, when feed liquid rises to concentration tank visor 1/3 place, close charging and divide valve, open two effect chargings subsequently and divide valve, when feed liquid rises to nozzle hole, close charging and divide valve
2. open condensation cycle system and alcohol distillation column
Open the condensation cycle system when exhausting material, open the alcohol distillation column steam valve simultaneously, make pressure reach 3MPa,
3. vacuum decompression concentrates
1, an effect concentrates
A, unlatching vacuum decompressioning and concentrating tank steam valve, gauge pressure is controlled at 0.2MPa,
B, open cooling water, open alcohol distillation column and reclaim distillation, about about 85 ° alcohol distillation to 95 of coming out from concentration tank ° utilizes again
C, vacuum degree control are below 0.08MPa, and along with the evaporation of alcohol, the continuous minimizing of feed liquid needs in time to replenish feed liquid, when below feed liquid is lower than during visor 30cm place, in time replenishes feed liquid and arrive visor 1/3 place
2, two effects concentrate
A, close one and imitate vacuum to 0, complete opening two is imitated vacuum, two effect vacuums are risen to below the 0.08MPa, close the charging main valve, open one and imitate baiting valve and two effect inlet valves, utilize action of pressure to imitate the whole suction two of feed liquid to one and imitate in the evaporators, drive steam valve, and open and stir, when being raised to a certain degree, concentration receives cream
B, put jar and to receive a cream while hot
Making two effect vacuums is 0, emits medicinal extract while hot, solidifies retrogradation in case fluid cools off
(5) reclaim alcohol in high concentration so that utilize again with the alcohol distillation column distillation
1. imitate the alcohol that distills out with one or two and directly feed alcohol distillation column,
2. open steam valve, to gauge pressure be 3MPa, vapo(u)rizing temperature is 105 ℃, tower top temperature is 74-76 ℃, cooling water temperature is controlled at below 10 ℃, can adopt alcohol water summer,
When treating that 3. alcohol concentration reaches more than 95 °, open recovery valve and go into finished product alcohol basin, reclaim cycling and reutilization.
Claims (1)
1, a kind of processing art for extracting propolis and removing lead from it, it is pulverized through liquid nitrogen cryogenics; The variable concentrations edible alcohol is cold soaking repeatedly; Face under Jie's state freezing sedimentation and get rid of filtering lead; Economic benefits and social benefits energy-saving vacuum low-temperature reduced-pressure concentrates; A kind of processing art for extracting propolis and removing lead from it that method that alcohol in high concentration utilizes is again finished is reclaimed in alcohol distillation column distillation, it is characterized in that it is undertaken by following technology:
(1) liquid nitrogen cryogenics is pulverized
1. the bulk propolis is placed under the environmental condition below-4 ℃ freezing 12 hours
2. the piece glue of deep colling is pounded into the fritter of 0.5cm diameter
3. the fritter propolis is taken advantage of and is cooler than below-10 ℃, pulverize first pass, become meal with the Universalpulverizer of topping up nitrogen,
4. above-mentioned fritter glue is placed below-10 ℃, the Universalpulverizer of topping up nitrogen is ground into the above fine powder of 200 orders, in order to lixiviate
(2) use variable concentrations edible alcohol cold soaking repeatedly
1. 70 °, 85 °, 95 ° edible alcohol is taken up in order of priority and squeezes in the steeping tank of belt stirrer, slowly add the propolis fine powder that crushes, the limit edged stirs, and soaks 24 hours, stirred 20-30 minute every 1 hour,
2. earlier 70 ° of edible alcohols are squeezed in the steeping tank of belt stirrer in 1: 1 ratio of inventory, slowly added the propolis fine powder that crushes, the limit edged stirs, and soaks 24 hours, stirred 20-30 minute every 1 hour,
3. extract in the steeping tank 4/5 supernatant, in the settling tank with pump suction band cooling coil
4. with 85 °, 95 ° edible alcohols in successively squeezing in the steeping tank of residual 1/5 soak at twice with 1: 1 ratio of inventory, repeat aforesaid operations, each soaked 24 hours, extracted 4/5 supernatant respectively, incorporate into pump in the settling tank of above-mentioned band cooling coil,
5. the residual liquid of remainder is reinstated the centrifuge that adds three layers of 80-120 order filter cloth together with residue one and dries, get filtrate and incorporate in the above-mentioned settling tank,
(3) facing freezing sedimentation filtering lead under Jie's state
1. the propolis supernatant mixture with above-mentioned three kinds of gradient alcoholic extractions pumps in the settling tank of band cooling coil,
2. feed liquid ammonia cooling in the coil pipe to-4 ℃, kept 72 hours,
3. take advantage of cold-draw supernatant 4/5, dry, get filtrate, wait to concentrate with the centrifuge that adds three layers of 80-120 order filter cloth,
(4) adopt economic benefits and social benefits energy-saving vacuum low-temperature reduced-pressure to concentrate
1. vacuumize charging,
Close all concentration tank valves, open vavuum pump, make one or two to imitate vacuums and rise to 0.05MPa and begin charging, an advanced effect when above, when feed liquid rises to concentration tank visor 1/3 place, close charging and divide valve, open two effect chargings subsequently and divide valve, when feed liquid rises to nozzle hole, close charging and divide valve
2. open condensation cycle system and alcohol distillation column
Open the condensation cycle system when exhausting material, open the alcohol distillation column steam valve simultaneously, make pressure reach 3MPa,
3. vacuum decompression concentrates
1, an effect concentrates
A, unlatching vacuum decompressioning and concentrating tank steam valve, gauge pressure is controlled at 0.1-0.2MPa
Vapour pressure≤0.2mpa
B, open cooling water, open alcohol distillation column and reclaim distillation, about about 85 ° alcohol distillation to 95 of coming out from concentration tank ° utilizes again
C, vacuum degree control are below 0.08MPa, and along with the evaporation of alcohol, the continuous minimizing of feed liquid needs in time to replenish feed liquid, when below feed liquid is lower than during visor 30cm place, in time replenishes feed liquid and arrive visor 1/3 place
2, two effects concentrate
A, close one and imitate vacuum to 0, complete opening two is imitated vacuum, two effect vacuums are risen to below the 0.08MPa, close the charging main valve, open one and imitate baiting valve and two effect inlet valves, utilize action of pressure to imitate the whole suction two of feed liquid to one and imitate in the evaporators, drive steam valve, and open and stir, when being raised to a certain degree, concentration receives cream
B, put jar and to receive a cream while hot
Making two effect vacuums is 0, emits medicinal extract while hot, solidifies retrogradation in case fluid cools off,
(5) reclaim alcohol in high concentration so that utilize again with the alcohol distillation column distillation
1. imitate the alcohol that distills out with one or two and directly feed alcohol distillation column,
2. open steam valve, to gauge pressure be 3MPa, vapo(u)rizing temperature is 105 ℃, tower top temperature is 74-76 ℃, cooling water temperature is controlled at below 10 ℃, can adopt alcohol water summer,
When treating that 3. alcohol concentration reaches more than 95 °, open recovery valve and go into finished product alcohol basin, reclaim cycling and reutilization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001054864A CN1140184C (en) | 2000-06-14 | 2000-06-14 | Processing art for extracting propolis and removing lead from it |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001054864A CN1140184C (en) | 2000-06-14 | 2000-06-14 | Processing art for extracting propolis and removing lead from it |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1277816A true CN1277816A (en) | 2000-12-27 |
| CN1140184C CN1140184C (en) | 2004-03-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB001054864A Expired - Fee Related CN1140184C (en) | 2000-06-14 | 2000-06-14 | Processing art for extracting propolis and removing lead from it |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313020C (en) * | 2003-12-25 | 2007-05-02 | 南昌大学 | Combination use of absorption and ion exchange for removing lead from propolis |
| CN102018728A (en) * | 2009-09-17 | 2011-04-20 | 北京久和开源营养科技有限公司 | Propolis extraction process |
| CN102224892A (en) * | 2011-05-09 | 2011-10-26 | 大连海尔思科技有限公司 | Propolis extraction process |
| CN102441010A (en) * | 2011-12-12 | 2012-05-09 | 南京中科集团股份有限公司 | Preparation method of deleaded refined propolis |
| CN101669594B (en) * | 2009-09-29 | 2012-07-04 | 皖南大鹏天然产物有限公司 | Method for removing lead in ginkgo biloba extract (GBE) |
| CN102764274A (en) * | 2012-07-03 | 2012-11-07 | 江苏江大源生态生物科技有限公司 | Method for extracting propolis |
| CN104721235A (en) * | 2015-04-07 | 2015-06-24 | 北京农科亿健蜂产品研究院 | Producing method of high-quality propolis |
| CN105104506A (en) * | 2015-09-11 | 2015-12-02 | 江苏红豆杉药业有限公司 | Preservation method for taxus chinensis fruits |
| CN106367593A (en) * | 2016-08-25 | 2017-02-01 | 安徽华铂再生资源科技有限公司 | Process of producing lead-tin alloy from high-tin regenerated lead |
| CN106435194A (en) * | 2016-09-30 | 2017-02-22 | 刘振 | Efficient desulfurization technology for waste lead-acid cell lead plaster |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100556413C (en) * | 2007-12-24 | 2009-11-04 | 中国农业科学院蜜蜂研究所 | Oil-soluble propolis soft capsule and preparation method thereof |
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2000
- 2000-06-14 CN CNB001054864A patent/CN1140184C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313020C (en) * | 2003-12-25 | 2007-05-02 | 南昌大学 | Combination use of absorption and ion exchange for removing lead from propolis |
| CN102018728A (en) * | 2009-09-17 | 2011-04-20 | 北京久和开源营养科技有限公司 | Propolis extraction process |
| CN101669594B (en) * | 2009-09-29 | 2012-07-04 | 皖南大鹏天然产物有限公司 | Method for removing lead in ginkgo biloba extract (GBE) |
| CN102224892A (en) * | 2011-05-09 | 2011-10-26 | 大连海尔思科技有限公司 | Propolis extraction process |
| CN102441010A (en) * | 2011-12-12 | 2012-05-09 | 南京中科集团股份有限公司 | Preparation method of deleaded refined propolis |
| CN102764274B (en) * | 2012-07-03 | 2013-08-28 | 江苏江大源生态生物科技有限公司 | Method for extracting propolis |
| CN102764274A (en) * | 2012-07-03 | 2012-11-07 | 江苏江大源生态生物科技有限公司 | Method for extracting propolis |
| CN104721235A (en) * | 2015-04-07 | 2015-06-24 | 北京农科亿健蜂产品研究院 | Producing method of high-quality propolis |
| CN105104506A (en) * | 2015-09-11 | 2015-12-02 | 江苏红豆杉药业有限公司 | Preservation method for taxus chinensis fruits |
| CN105104506B (en) * | 2015-09-11 | 2018-10-26 | 江苏红豆杉药业有限公司 | A kind of store method of taxus fruit |
| CN106367593A (en) * | 2016-08-25 | 2017-02-01 | 安徽华铂再生资源科技有限公司 | Process of producing lead-tin alloy from high-tin regenerated lead |
| CN106367593B (en) * | 2016-08-25 | 2018-05-01 | 安徽华铂再生资源科技有限公司 | A kind of technique using high tin Production of Secondary Lead terne metal |
| CN106435194A (en) * | 2016-09-30 | 2017-02-22 | 刘振 | Efficient desulfurization technology for waste lead-acid cell lead plaster |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1140184C (en) | 2004-03-03 |
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