CN1680285A - Industrial production of natural capsaicin crystal by molecular distilling and washing method - Google Patents
Industrial production of natural capsaicin crystal by molecular distilling and washing method Download PDFInfo
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- CN1680285A CN1680285A CN 200510013075 CN200510013075A CN1680285A CN 1680285 A CN1680285 A CN 1680285A CN 200510013075 CN200510013075 CN 200510013075 CN 200510013075 A CN200510013075 A CN 200510013075A CN 1680285 A CN1680285 A CN 1680285A
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- scavenging agent
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Abstract
An industrial method for producing capsaicin crystal by molecular distilling and washing technology is carried out by leaching peel powder of pepper with No.6 solvent oil etc. organic solvent, de-pressuring and deeply compressing the leach liquor, molecular distilling for concentrate, washing and separating mixture of MgCO3, CaCO3, ZnCO3, Na2CO3, NaOH and NaCl and mixture decontaminant of MgCl2, Ca2CO3 and ZnCl2, and obtaining capsanthin coloring matter, oleoresin capsicum, and capsaicin crystal. Its advantages include simple operation, high extracting rate and good separating effect.
Description
Technical field
The present invention relates to the commercial run of production of natural capsaicin crystal by molecular distilling and washing
Background technology
The commercial run of producing natural capsicine adopts solvent extration more at present, as CN1110622A and CN1439630A solvent extration, obtains high-purity capsaicin through four phase-splittings.To natural capsicum alkaline extraction report more still be laboratory work.Remove and use supercritical CO
2Outside the extraction process, also have the macroporous adsorbent resin method, solvent extraction solution after the nonpolar or low polar macroporous adsorption resin of HPD is handled, is handled through the HPD polar macroporous adsorption resin again, can obtain high-purity capsaicin.Also have molecular distillation and the cut-and-try work of macroporous adsorbent resin bonded, as CN1392136A, solvent extraction solution carried out the quadratic component distillation after, handle the acquisition high-purity capsaicin again through the HPD polar macroporous adsorption resin.
Summary of the invention
The commercial run that the purpose of this invention is to provide a kind of production of natural capsaicin crystal by molecular distilling and washing, it is through a molecular distillation with the solvent extraction concentrated solution, just can obtain high-purity capsaicin through the scavenging agent washing again, obtain products such as high-quality capsanthin and oleoresin capsicum simultaneously, whole process does not have waste water, waste residue and exhaust gas emission have realized suitability for industrialized production.
The concrete steps that molecular distillation washing method of the present invention is produced the commercial run of capsaicine crystals are:
1) peel powder of hot pepper adds 3～5 times of volume organic solvents (W/V, Kg/ liter) in the lixiviate jar, and 45～70 ℃, stirring and leaching 1.5～4 hours repeats lixiviate 3～4 times, merges vat liquor, and concentrating under reduced pressure reclaims solvent, gets enriched material; Said solvent is No. 6 solvent oils, ethanol or acetone.
2) enriched material carries out molecular distillation, and control process parameters is as follows: vacuum tightness 10
-2～1Pa, 150～170 ℃ of distillation temperatures, material flow 1～2Kg/min, 20～28 ℃ of condensing surface temperature, knifing rotating speed 250～400rpm;
3) molecular distillation gained heavy phase effluent liquid adds the I scavenging agent, and agitator treating is 30～60 minutes in washing tank, tells water, obtains the capsanthin product.Said I scavenging agent is MgCO
3, CaCO
3, ZnCO
3, Na
2CO
3, NaOH and NaCl mixture aqueous solution; Said heavy phase effluent liquid: I scavenging agent=1: 4～10 (W/V, Kg/ liter).
4) the light phase overhead product of molecular distillation gained adds II scavenging agent and No. 6 solvent oils, in purification pot, heats up 60～80 ℃, and stirring and refluxing 30～50 minutes is divided and removed water; Organic phase stirs with the 30rpm rotating speed in stirred pot, cools to room temperature naturally, tells oleoresin capsicum product (peppery cellulose content 8～40%), obtains the high-purity capsaicin crystal product in crystallizer, and total alkali is more than 99%.Said light phase overhead product: II scavenging agent=1: 100～200 (W/V, Kg/ liter), said light phase overhead product: No. 6 solvent oil=1: 80～100 (W/V, Kg/ liter).Said II scavenging agent is MgCl
2, Ca
2CO
3With ZnCl
2Mixture aqueous solution.
Said I scavenging agent composition proportion is: MgCO
3: CaCO
3: ZnCO
3: Na
2CO
3: NaOH: NaCl=10: 5: 1: 30: 10: 20 (mol ratio), I scavenging agent operating weight concentration (solid content) is 0.5～1%.
Said II scavenging agent composition proportion is MgCl
2: Ca
2CO
3: ZnCl
2=4: 1: 2 (mol ratio), II scavenging agent operating weight concentration (solid content) is 0.5～2%.
The present invention has following major advantage:
1. the present invention adopts molecular distillation and I scavenging agent and II scavenging agent to handle and just can produce capsaicine crystals, oleoresin capsicum and capsanthin, and technology is easy, and is with short production cycle, reaches the purpose of capsicum deep processing and comprehensive utilization.
2. used I scavenging agent and the II scavenging agent of the present invention is with low cost, and whole technological process is only used a kind or 2 kinds of organic solvents, and all recyclable utilization.
3. the present invention adopts the molecular distillation washing technology, the quality product height that industrial production goes out, and its key technical indexes is as follows:
Capsaicine crystals: total alkali reaches more than 99%
Oleoresin capsicum: peppery cellulose content 8～40%
Total molten residual≤20mg/Kg
Capsanthin: look valency E
1cm 1%460nm:50～200
Peppery cellulose content :≤0.01%
Total molten residual≤20mg/Kg
4. the present invention adopts the molecular distillation washing technology, and whole process of production does not have the waste water,waste gas and industrial residue discharging substantially, the production technique cleaning.
The invention provides the commercial run of a kind of capsicum deep processing and comprehensive utilization, is that extraction separation from capsicum goes out high-purity capsaicine crystals with molecular distillation and washing technology, the industrial process of high-quality oleoresin capsicum and high-quality capsanthin.Production technique of the present invention is easy and simple to handle, extraction yield height, good separating effect, the equal no solvent residue of various products.
Embodiment
Embodiment 1:I scavenging agent and the manufacturing of II scavenging agent
(1) in dissolving jar, add water 1000Kg, after the moving stirring of liter, add various batchings in the following order:
MgCO
31.652Kg、CaCO
31.960Kg、ZnCO
32.458Kg、NaCl1.147Kg、Na
2CO
31.999Kg、NaOH0.784Kg.
After the stirring and dissolving 30 minutes, left standstill 1 hour, filter gained filtrate, be the I scavenging agent, weight concentration (solid content): 1%.
(2) in dissolving jar, add water 1000Kg, after the moving stirring of liter, add various batchings in the following order:
MgCl
25.064Kg, CaCl
26.392Kg, ZnCl
28.544Kg after the stirring and dissolving 30 minutes, left standstill 1 hour, to filter, gained filtrate is the II scavenging agent, weight concentration (solid content): 2%.
Embodiment 2
Take by weighing chilli fruit peel powder 400Kg (total look valency 400, every Kg look valency 10, peppery cellulose content 0.2%), drop in the lixiviate jar, vacuum sucks 1500 liters of 95% edible ethanols simultaneously, and temperature is 50 ℃ in the steam heating, controlling tank, and liter is moving to stir lixiviate 2 hours, press filtration.So similarity condition lixiviate twice again, filtrate is carried out concentrating under reduced pressure.Reclaim ethanol, get enriched material.
Enriched material carries out molecular distillation, control process parameters: vacuum tightness 10
-2～1Pa, 155 ℃ of distillation temperatures, enriched material flow velocity 0.5Kg/min, the condensing surface temperature: 27 ℃, knifing rotating speed 350rpm.
Gained effluent in the heavy phase receptor is squeezed in the washing tank, added I number purificationization agent 200Kg (concentration 0.5%), agitator treating 20 minutes divides the phase of anhydrating.Obtain 19Kg capsanthin product.
Press the GB10783-1996 method and detect, the result is as follows:
Look valency: look valency
Peppery cellulose content: 0.001%
Total organic molten residual: as not detect
The look valency rate of recovery: 95%
With gained overhead product in the light Phase Receiver device, squeeze into purification pot, add 90 liters of II scavenging agent (concentration 1%) 100Kg and No. 6 solvent oils, heat up 70 ℃, stirring and refluxing 30 minutes is told water.
Organic phase in stirred pot with the 30rpm speed drop to room temperature, get oleoresin capsicum product 2Kg, through high-pressure liquid phase chromatogram therapy determining, the peppery cellulose content of this product: 39%, total molten residual 15mg/Kg.
In crystallizer, produce capsaicine crystals product 0.12Kg, through high-pressure liquid phase chromatogram therapy determining, total alkali 99.5%.
Embodiment 3
Take by weighing chilli fruit peel powder 600Kg (per kilogram look valency 10, total look valency 6000, peppery cellulose content 0.2%), drop into the lixiviate jar, suck 1800 liters in acetone, heat up, temperature is 45 ℃ in the controlling tank, stirring and leaching press filtration in 1.5 hours.Similarity condition like this is the lixiviate secondary again, runs filtrate jointly, and evaporation concentration reclaims acetone.Enriched material is carried out molecular distillation, control process parameters: vacuum tightness 10
-2～1Pa, 150 ℃ of distillation temperatures, enriched material flow velocity 0.8Kg/min, 25 ℃ of condensing surface temperature, knifing rotating speed 300rpm.
The effluent of heavy phase receptor is added I scavenging agent 300Kg (concentration 1%), and agitator treating is 30 minutes in washing tank, tells water, obtains 32Kg capsanthin product, presses the GB10783-1996 method and detects, and the result is as follows:
Look valency: look valency
Peppery cellulose content: 0.0015%
Total molten residual: as not detect
The look valency rate of recovery: 97%
In purification pot, squeeze into light phase overhead product, add 140 liters of II scavenging agent 150Kg (concentration 1.5%) and No. 6 solvent oils.80 ℃ were refluxed 45 minutes, and told water.Organic phase drops to room temperature with the 30rpm rotating speed in stirred pot, tell oleoresin capsicum product 3.5Kg, through the peppery cellulose content 35% of high-pressure liquid chromatography, and total molten residual 12mg/Kg.
In crystallizer, obtain capsaicine crystals product 0.25Kg, through high-pressure liquid chromatography, total alkali is 99.0%.
Claims (6)
1, a kind of commercial run of production of natural capsaicin crystal by molecular distilling and washing is characterized in that it comprises the steps:
1) peel powder of hot pepper adds 3～5 times of volume organic solvents (W/V, Kg/ liter) in the lixiviate jar, and 45～70 ℃, stirring and leaching 1.5～4 hours repeats lixiviate 3～4 times, merges vat liquor, and concentrating under reduced pressure reclaims solvent, gets enriched material;
2) enriched material carries out molecular distillation, and control process parameters is as follows: vacuum tightness 10
-2～1Pa, 150～170 ℃ of distillation temperatures, material flow 1～2Kg/min, 20～28 ℃ of condensing surface temperature, knifing rotating speed 250～400rpm;
3) molecular distillation gained heavy phase effluent liquid adding solid content is 0.5～1% I scavenging agent, and agitator treating is 30～60 minutes in washing tank, tells water, obtains the capsanthin product; Said I scavenging agent is MgCO
3, CaCO
3, ZnCO
3, Na
2CO
3, NaOH and NaCl mixture aqueous solution;
4) the light phase overhead product adding of molecular distillation gained solid content is II scavenging agent and No. 6 solvent oils of 0.5～2%, in purification pot, heats up 60～80 ℃, and stirring and refluxing 30～50 minutes is divided and removed water; Organic phase stirs with the 30rpm rotating speed in stirred pot, cools to room temperature naturally, tells the oleoresin capsicum product, obtains the high-purity capsaicin crystal product in crystallizer; Said II scavenging agent is MgCl
2, Ca
2CO
3With ZnCl
2Mixture aqueous solution.
2, according to the commercial run of the said production of natural capsaicin crystal by molecular distilling and washing of claim 1, it is characterized in that: said solvent is No. 6 solvent oils, ethanol or acetone.
3, according to the commercial run of the said production of natural capsaicin crystal by molecular distilling and washing of claim 1, it is characterized in that: said heavy phase effluent liquid: I scavenging agent=1: 4～10, W/V, Kg/ liter.
4, according to the commercial run of the said production of natural capsaicin crystal by molecular distilling and washing of claim 1, it is characterized in that: said I scavenging agent composition proportion is: MgCO
3: CaCO
3: ZnCO
3: Na
2CO
3: NaOH: NaCl=10: 5: 1: 30: 10: 20, mol ratio.
5, according to the commercial run of the said production of natural capsaicin crystal by molecular distilling and washing of claim 1, it is characterized in that: said II scavenging agent composition proportion is: MgCl
2: Ca
2CO
3: ZnCl
2=4: 1: 2, mol ratio.
6, according to the commercial run of the said production of natural capsaicin crystal by molecular distilling and washing of claim 1, it is characterized in that: said light phase overhead product: II scavenging agent=1: 100～200, W/V, the Kg/ liter, said light phase overhead product: No. 6 solvent oil=1: 80～100, W/V, the Kg/ liter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100130754A CN1315784C (en) | 2005-01-07 | 2005-01-07 | Industrial production of natural capsaicin crystal by molecular distilling and washing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100130754A CN1315784C (en) | 2005-01-07 | 2005-01-07 | Industrial production of natural capsaicin crystal by molecular distilling and washing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1680285A true CN1680285A (en) | 2005-10-12 |
| CN1315784C CN1315784C (en) | 2007-05-16 |
Family
ID=35067147
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057660B (en) * | 2007-05-28 | 2010-05-19 | 天津神农种业有限责任公司 | Technique method for producing capsicine crystal from capsicum oleoresin |
| CN102603554A (en) * | 2011-12-15 | 2012-07-25 | 武城县英潮经贸有限公司 | New process for extracting capsaicin crystal substances |
| CN104629487A (en) * | 2013-11-15 | 2015-05-20 | 李锦梁 | Method for extracting capsanthin by using ethanol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176904C (en) * | 2002-07-18 | 2004-11-24 | 中山大学 | Molecular distilling process for enriching and purifying capsaicin |
-
2005
- 2005-01-07 CN CNB2005100130754A patent/CN1315784C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057660B (en) * | 2007-05-28 | 2010-05-19 | 天津神农种业有限责任公司 | Technique method for producing capsicine crystal from capsicum oleoresin |
| CN102603554A (en) * | 2011-12-15 | 2012-07-25 | 武城县英潮经贸有限公司 | New process for extracting capsaicin crystal substances |
| CN102603554B (en) * | 2011-12-15 | 2013-12-11 | 武城县英潮经贸有限公司 | New process for extracting capsaicin crystal substances |
| CN104629487A (en) * | 2013-11-15 | 2015-05-20 | 李锦梁 | Method for extracting capsanthin by using ethanol |
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| Publication number | Publication date |
|---|---|
| CN1315784C (en) | 2007-05-16 |
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Granted publication date: 20070516 Termination date: 20100208 |