CN102964228A - Natural cinnamaldehyde extraction process - Google Patents
Natural cinnamaldehyde extraction process Download PDFInfo
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- CN102964228A CN102964228A CN2012105188997A CN201210518899A CN102964228A CN 102964228 A CN102964228 A CN 102964228A CN 2012105188997 A CN2012105188997 A CN 2012105188997A CN 201210518899 A CN201210518899 A CN 201210518899A CN 102964228 A CN102964228 A CN 102964228A
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- distillation
- natural meat
- temperature
- cinnamic aldehyde
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- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 title claims abstract description 55
- KJPRLNWUNMBNBZ-UHFFFAOYSA-N cinnamic aldehyde Natural products O=CC=CC1=CC=CC=C1 KJPRLNWUNMBNBZ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229940117916 cinnamic aldehyde Drugs 0.000 title claims abstract description 51
- 238000000605 extraction Methods 0.000 title claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 43
- 238000010992 reflux Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000004364 calculation method Methods 0.000 claims abstract description 7
- 235000013372 meat Nutrition 0.000 claims description 55
- AXMVYSVVTMKQSL-UHFFFAOYSA-N UNPD142122 Natural products OC1=CC=C(C=CC=O)C=C1O AXMVYSVVTMKQSL-UHFFFAOYSA-N 0.000 claims description 45
- 241000282326 Felis catus Species 0.000 claims description 17
- HWJPHQNEWARZLH-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5-decafluoro-6,6-bis(trifluoromethyl)cyclohexane Chemical compound FC(F)(F)C1(C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C1(F)F HWJPHQNEWARZLH-UHFFFAOYSA-N 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 10
- 238000004458 analytical method Methods 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000004927 fusion Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000010630 cinnamon oil Substances 0.000 abstract 4
- 235000019198 oils Nutrition 0.000 description 29
- 241000196324 Embryophyta Species 0.000 description 12
- 239000000463 material Substances 0.000 description 6
- 241000723347 Cinnamomum Species 0.000 description 5
- 235000017803 cinnamon Nutrition 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229930016911 cinnamic acid Natural products 0.000 description 2
- 235000013985 cinnamic acid Nutrition 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 2
- 241000228197 Aspergillus flavus Species 0.000 description 1
- 235000014489 Cinnamomum aromaticum Nutrition 0.000 description 1
- 244000037364 Cinnamomum aromaticum Species 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The invention discloses a natural cinnamaldehyde extraction process, and relates to the technical field of a forest product chemical industry. The process is implemented by taking natural cinnamon oil as a raw material through carrying out extraction in four stages, wherein in the first stage, the temperature of a distillation still is 110 DEG C, the temperature of the top of a distillation tower is 50 DEG C, and the reflux ratio is 0:1; in the second stage, the temperature of the distillation still is 140 DEG C, the temperature of the top of the distillation tower is 110 DEG C, and the reflux ratio is 10:1; and in the third stage, the internal temperature of the distillation still is 160 DEG C, the temperature of the top of the distillation tower is 140 DEG C, the reflux ratio is 0:1, until the collected distillate achieves the analytical calculation quantity of natural cinnamaldehyde. The process disclosed by the invention can solve the problem that in the processes of distilling cinnamon oil and extracting natural cinnamaldehyde, the cinnamon oil is subjected to partial fusion because the cinnamon oil is heated unevenly, so that the purity of natural cinnamaldehyde finished products and the output capacity of natural cinnamaldehyde are affected.
Description
Technical field
The present invention relates to the forest product industry technical field, especially a kind of is the processing method of extracting the natural meat cinnamic aldehyde the raw material from the natural meat oil of bay.
Background technology
The natural meat cinnamic aldehyde, the chemical name cinnamic acid has another name called cinnamic aldehyde, cinnamic aldehyde, cinnamic aldehyde, its equation are C6H5-CH=CH-CHO, it has cis and trans two kinds of isomer, no matter but phenylacrolein natural or that synthesize all is transconfigurations.The natural meat cinnamic aldehyde is colourless to the pale yellow oily liquid body, has strong cassia bark aromatic odour, the hot fragrance of medicine; In air, easily be oxidized to cinnamic acid, fusing point-7.5 ℃, 253 ℃ of boiling points (normal pressure) are insoluble in water and oil alcohol, are soluble in alcohol, ether, chloroform and benzene, are slightly soluble in water.The natural meat cinnamic aldehyde is widely used in the production of the products such as medicine, spices, food, daily cosmetic, plastics and sensitive materials, and it suppresses the effect of carcinogens Aspergillus flavus in addition.
At present, a kind of method of producing the natural meat cinnamic aldehyde is to extract the natural meat cinnamic aldehyde with distillation method from the natural meat oil of bay in the industrial production, natural meat cinnamic aldehyde extraction equipment is mainly by vaporizer, condenser and collector form, prior art is that the raw material tower reactor that will Oleum Cinnamomi be housed places heating oil tank when extracting the natural meat cinnamic aldehyde, by the oil in the calrod heating tank in the heating oil tank, thereby the Oleum Cinnamomi in the raw material tower reactor is heated.In order there to be enough temperature that the phenylacrolein in the Oleum Cinnamomi is evaporated, the temperature of deep fat generally all surpasses 30 ℃~50 ℃ of the temperature of Oleum Cinnamomi in the raw material tower reactor in the heating oil tank, the Oleum Cinnamomi non-uniform temperature of this type of heating in the raw material tower reactor, higher at Oleum Cinnamomi and raw material tower reactor contact surface place temperature, be easy to cause that Oleum Cinnamomi produces local fusion because temperature is too high in the raw material tower reactor, thereby have influence on the purity of natural meat cinnamic aldehyde finished product and the output capacity of natural meat cinnamic aldehyde.
Summary of the invention
The purpose of this invention is to provide a kind of natural meat cinnamic aldehyde process for extracting, this method is extracted the natural meat cinnamic aldehyde, and not only output capacity is high, and can obtain the high natural meat cinnamic aldehyde of purity.
In order to achieve the above object, the technical solution used in the present invention is: adopt natural meat cinnamic aldehyde extraction equipment to extract the natural meat cinnamic aldehyde with method according to the following steps:
Will place the natural meat oil of bay in the distillation plant to carry out sampling analysis, determine aldehyde contenting amount wherein, and calculate respectively the weight that distillation reaches natural meat cinnamic aldehyde, foreshot and the after cut of setting purity, the extraction raw material of natural meat cinnamic aldehyde is placed a minute four-stage adds thermal distillation in the described distillation plant:
Fs, the temperature of natural meat oil of bay is 110 ℃ in the raw material still kettle of control distillation plant, and the temperature of the distillation cat head of control distillation plant is 50 ℃, and reflux ratio is 0:1, keep the vacuum tightness of collector at 2~3Kpa, enter subordinate phase when complete when overhead product distillates;
Subordinate phase, the temperature of controlling the interior natural meat oil of bay of raw material still kettle of described distillation plant is 140 ℃, the temperature of controlling the distillation cat head of described distillation plant is 110 ℃, reflux ratio is 10:1, keep the vacuum tightness of collector at 2~3Kpa, the amount that reaches the analytical calculation foreshot to the fraction of collecting changes the phase III over to;
Phase III, the temperature of controlling the interior natural meat oil of bay of raw material still kettle of described distillation plant is 160 ℃, the temperature of the distillation cat head of control distillation plant is 140 ℃, reflux ratio is 0:1, keep the vacuum tightness of collector at 2~3Kpa, reach the amount of analytical calculation natural meat cinnamic aldehyde to the fraction of collecting.
Further, adopt natural meat cinnamic aldehyde extraction equipment, described natural meat cinnamic aldehyde extraction equipment includes evaporation equipment, this evaporation equipment includes the raw material still kettle, on the described raw material still kettle feed heater that is made of shell and tube heat exchanger is installed, the opening for feed of described feed heater is connected with a raw material circulation pump outlet, the discharge port of described feed heater is communicated with the top of described raw material still kettle, the import of described raw material recycle pump is communicated with the bottom of described raw material still kettle, the bottom of described feed heater housing is communicated with the circular-pump oil outlet by the thermal oil entrance, and described feed heater is communicated with the oil return opening of described oily process furnace by the hot oil outlet on housing top; Be connected with distillation tower on the described evaporation equipment, the cat head of this distillation tower is connected with condenser, the outlet of described condenser connects reflux splitter, wherein one road output tube of described reflux splitter is connected to a plurality of collection containers in the collector group by valve respectively by the cylinder of looking with form, and another road output tube connects the backflow interface of described cat head; Having a vacuum pump group to be connected with pipeline by valve by surge tank is connected with each collection container in the described collector group; Ripple net filler is housed in the described distillation tower.
Owing to adopted technique scheme, the present invention compared with prior art has following beneficial effect:
Adopt natural meat cinnamic aldehyde extraction equipment of the present invention to extract, can industrialization extract natural meat cinnamic aldehyde and output capacity height, the purity of the natural meat cinnamic aldehyde that extracts can reach more than 98%.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Fig. 2 is the structural representation of natural meat cinnamic aldehyde evaporation equipment among the present invention.
Embodiment
Being extracted in the special distillation plant of natural meat cinnamic aldehyde carried out, this cover distillation plant as depicted in figs. 1 and 2, distillation plant has an evaporation equipment 6, evaporation equipment 6 is made of a raw material still kettle 6-1 and distillation tower, on the raw material still kettle 6-1 feed heater 6-2 is installed, feed heater 6-2 is fixed by bolts on the raw material still kettle 6-1, feed heater 6-2 inner chamber is equipped with the heat exchange core that is made of many heat transfer tubes that are arranged in parallel and the tube sheet that is enclosed in these heat transfer tube two ends, the outside of these heat transfer tubes is separated into material channel around the dividing plate loopback by 4 dividing plates with the heat transfer tube space outerpace of heat exchange core, material inlet 6-2-1 is located at the top of feed heater 6-2, the outlet of material inlet 6-2-1 and a raw material recycle pump 5 is connected, and the import of raw material recycle pump 5 is connected on the bottom of raw material still kettle 6-1; The material outlet of feed heater 6-2 is located at the bottom of feed heater 6-2, and the top of this material outlet and raw material still kettle 6-1 is connected; Feed heater 6-2 is on the top of heat exchange core, and the upper port of each heat transfer tube is communicated with hot oil outlet 6-2-3 by junction station, and hot oil outlet 6-2-3 is connected with the oil return opening of hot oil furnace 3 by a valve; In the bottom of heat exchange core, the lower port of each heat transfer tube is communicated with hot oil inlet 6-2-2 by junction station, and hot oil inlet 6-2-2 is connected with the outlet of oil pump 4 by a valve, and the import of oil pump 4 is connected with the oil outlet of hot oil furnace 3.Be connected with the distillation tower that 4 interconnective tower joints 7 consist of on the evaporation equipment 6, tower joint 7 is fixed by bolts to the top of raw material still kettle 6-1,4 tower joints 7 are equipped with ripple net filler altogether, be installed by welding with cat head 8 on the tower joint 7 of top, the distillation outlet of cat head 8 is connected with the opening for feed of condenser 9, the discharge port of condenser 9 can distribute outflow by preset proportion with overhead product by reflux splitter 10, an output terminal of reflux splitter 10 by be provided with glass port look the cylinder 12 after, be connected to collector group 11 by a valve that is used for gate action respectively, depending on the flow situation that can observe discharging of cylinder 12 and the color situation of discharging; Another output terminal of reflux splitter 10 is communicated with the backflow interface of cat head 8.Collector group 11 is comprised of 4 collectors, and each collector top is equipped with evacuation port, is provided with switching valve between collector and the collector, and the bottom of each collector is equipped with drain hole.4 collectors in the collector group 11 are connected in the outlet in the vacuum system by the valve of a gate action respectively.Vacuum system is connected and composed by vacuum pump 1 and two surge tanks 2 that are connected on vacuum pump 1 output tube, the outlet of last surge tank 2 is the outlet in the vacuum system, and the effect of vacuum pump group 1 and surge tank 2 thereof is to guarantee to provide to each collector to reach the stable suction force that absolute pressure reaches 2Kpa vacuum tightness.
Before the extraction of natural meat cinnamic aldehyde, to 300 kilograms of natural meat oil of bay sampling analysis, acquisition natural meat oil of bay contains natural meat cinnamic aldehyde amount and reaches 76.3%, foreshot content 3.72%, after cut content 19,98%, the result calculates collecting amount according to stratographic analysis: the phenylacrolein amount of collecting=cinnamic aldehyde content-foreshot content * 2, phenylacrolein is collected 206.5 kilograms, the foreshot amount of collecting=foreshot content * 2, and foreshot is collected 22.32 kilograms.,
The natural meat oil of bay is placed a minute four-stage adds thermal distillation in the raw material still kettle 6-1 of distillation plant:
In the fs, the temperature of natural cinnamon fluid is 110 ℃ in the control raw material still kettle 6-1, and the temperature of control cat head 8 is 50 ℃, and the reflux ratio of regulating reflux splitter 10 is 0:1, enters subordinate phase when complete when the oil-water mixture thing that distillates distillates;
In subordinate phase, the temperature of natural cinnamon fluid is 140 ℃ in the control raw material still kettle 6-1, the temperature of control cat head 8 is 110 ℃, the reflux ratio of regulating reflux splitter 10 is 10:1, by adjusting the on off state of the valve in the collector group 11, only allow No. 1 collector gating look the pipeline in cylinder 12 downstreams, be used for collecting foreshot, the outlet vacuum tightness of control surge tank 2 is at 2~3Kpa, changes the phase III over to reach the amount of foreshot of analytical calculation to the overhead product of collecting after;
In the phase III, the temperature of natural cinnamon fluid is 160 ℃ in the control raw material still kettle 6-1, the temperature of control cat head 8 is 140 ℃, the reflux ratio of regulating reflux splitter 10 is 0:1, by adjusting the on off state of the valve in the collector group 11, only allow No. 3, No. 4 collector gatings look the pipeline in cylinder 12 downstreams, be used for collecting natural meat cinnamic aldehyde finished product, the outlet vacuum tightness of control surge tank 2 is at 2~3Kpa, and the amount that reaches analytical calculation natural meat cinnamic aldehyde to the natural meat cinnamic aldehyde finished product of collecting namely changes the quadravalence section over to;
In the quadravalence section, the temperature of natural cinnamon fluid is 170 ℃ in the control raw material still kettle 6-1, the temperature of control cat head 8 is 160 ℃, the reflux ratio of regulating reflux splitter 10 is 0:1, by adjusting the on off state of the valve in the collector group 11, only allow No. 2 collector gating look the pipeline in cylinder 12 downstreams, be used for collecting after cut, the outlet vacuum tightness of control surge tank 2 is at 2~3Kpa, and the natural cinnamon fluid distillation to the raw material still kettle is complete.
The natural meat cinnamic aldehyde purity that present embodiment obtains reaches 98.3%, is 68.8% to the natural meat cinnamic aldehyde extraction yield in the raw material natural meat oil of bay.
Claims (2)
1. natural meat cinnamic aldehyde process for extracting is characterized in that extracting according to the following steps the natural meat cinnamic aldehyde:
Will place the natural meat oil of bay in the distillation plant to carry out sampling analysis, determine water content wherein, and calculate respectively the weight that distillation reaches natural meat cinnamic aldehyde, foreshot and the after cut of setting purity, the extraction raw material of natural meat cinnamic aldehyde is placed a minute four-stage adds thermal distillation in the described distillation plant:
Fs, the temperature of natural meat oil of bay is 110 ℃ in the raw material still kettle of control distillation plant, and the temperature of the distillation cat head of control distillation plant is 50 ℃, and reflux ratio is 0:1, keep the vacuum tightness of collector at 2~3Kpa, enter subordinate phase when complete when overhead product distillates;
Subordinate phase, the temperature of controlling the interior natural meat oil of bay of raw material still kettle of described distillation plant is 140 ℃, the temperature of controlling the distillation cat head of described distillation plant is 110 ℃, reflux ratio is 10:1, keep the vacuum tightness of collector at 2~3Kpa, when the fraction of collecting reaches the amount of analytical calculation foreshot, change the phase III over to;
Phase III, the temperature of controlling the interior natural meat oil of bay of raw material still kettle of described distillation plant is 160 ℃, the temperature of the distillation cat head of control distillation plant is 140 ℃, reflux ratio is 0:1, keep the vacuum tightness of collector at 2~3Kpa, reach the amount of analytical calculation natural meat cinnamic aldehyde to the fraction of collecting.
2. natural meat cinnamic aldehyde process for extracting according to claim 1, it is characterized in that: adopt natural meat cinnamic aldehyde extraction equipment, described natural meat cinnamic aldehyde extraction equipment includes evaporation equipment (6), described evaporation equipment (6) includes raw material still kettle (6-1), the feed heater (6-2) that is made of shell and tube heat exchanger is installed on the described raw material still kettle (6-1), the opening for feed of described feed heater (6-2) is connected with the outlet of a raw material recycle pump (5), the discharge port of described feed heater (6-2) is communicated with the top of described raw material still kettle (6-1), the import of described raw material recycle pump (5) is communicated with the bottom of described raw material still kettle (6-1), the bottom of described feed heater (6-2) housing is communicated with circular-pump (4) oil outlet by thermal oil entrance (6-2-2), and described feed heater (6-2) is communicated with the oil return opening of described oily process furnace (3) by the hot oil outlet (2-3) on housing top; Be connected with distillation tower (7,8) on the described evaporation equipment (6), the cat head (8) of this distillation tower (7,8) is connected with condenser (9), the outlet of described condenser (9) connects reflux splitter (10), wherein one road output tube of described reflux splitter (10) is connected to a plurality of collection containers in the collector group (11) by valve respectively by the cylinder (12) of looking with form, and another road output tube connects the backflow interface of described cat head (8); There is a vacuum pump group (1) to be connected by each collection container with in the described collector group (11) that surge tank (2) and pipeline pass through respectively valve; Described distillation tower is equipped with ripple net filler in (7,8).
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103272024A (en) * | 2013-04-16 | 2013-09-04 | 阚兆云 | Traditional chinese medicine extract |
CN103342632A (en) * | 2013-06-24 | 2013-10-09 | 广西壮族自治区林业科学研究院 | Method for separating high-purity cinnamyl aldehyde and cinnamyl acetate from cinnamon oil |
CN108392846A (en) * | 2018-04-28 | 2018-08-14 | 江苏宝盛龙城药业有限公司 | Vacuum distillation apparatus and technique |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103272024A (en) * | 2013-04-16 | 2013-09-04 | 阚兆云 | Traditional chinese medicine extract |
CN103342632A (en) * | 2013-06-24 | 2013-10-09 | 广西壮族自治区林业科学研究院 | Method for separating high-purity cinnamyl aldehyde and cinnamyl acetate from cinnamon oil |
CN108392846A (en) * | 2018-04-28 | 2018-08-14 | 江苏宝盛龙城药业有限公司 | Vacuum distillation apparatus and technique |
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Application publication date: 20130313 Assignee: Guangxi Tengxian Fuhua Chemical Co.,Ltd. Assignor: Guangxi Jingguo Perfume Co.,Ltd. Contract record no.: X2024980000323 Denomination of invention: Extraction process of natural cinnamaldehyde Granted publication date: 20141224 License type: Common License Record date: 20240108 |
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