CN100575336C - Extract the processing method of capsaicine crystals from chillies - Google Patents
Extract the processing method of capsaicine crystals from chillies Download PDFInfo
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- CN100575336C CN100575336C CN200710057643A CN200710057643A CN100575336C CN 100575336 C CN100575336 C CN 100575336C CN 200710057643 A CN200710057643 A CN 200710057643A CN 200710057643 A CN200710057643 A CN 200710057643A CN 100575336 C CN100575336 C CN 100575336C
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- capsicum
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Abstract
The present invention relates to extract the processing method of capsaicine crystals from chillies.The step that this technology comprises: with NaCl, NaHCO
3Form the modification ethanolic soln with the NaOH aqueous solution and ethanol, the capsicum rod layer that spray leaching chillies is made in the leacher of rotation, extracting solution another mistake stream lixiviate capsicum rod layer through spray-drip-dry-spray-drip-dry continuous countercurrent lixiviate, gets leach liquor, after concentrating, after the blender allotment with NaCl, sodium acetate and hydrochloric acid soln composition, use No. 6 solvent oil reflux extraction again, just obtained the capsicine crystalline mother solution, crystalline mother solution promptly obtains the high-purity capsaicin crystal through crystallization control.Processing step of the present invention is simple, can operate control.Be fit to scale operation high-purity natural capsaicine crystals.
Description
Technical field
The present invention relates to extract the processing method of capsaicine crystals from chillies.
Background technology
Natural capsicine has unique physiological function, extracts the at present existing a lot of reported in literature of technology of capsicine from chillies, and these processing methodes mainly comprise solvent extration, microwave reinforced extraction process, intensified by ultrasonic wave extraction process, supercritical CO
2Extraction process and column chromatography and ion-exchange method for refining etc.
Fact proved that microwave reinforced extraction is implemented to produce on a large scale also has a lot of difficulties.Though the intensified by ultrasonic wave extraction can realize small-scale suitability for industrialized production, heavy industrialization still has many problems.Supercritical CO
2Extraction process, facility investment is big.Column chromatography and ion-exchange method for refining technology are longer, and utility appliance is many, and the solvent for use kind is many.Therefore, the current solvent extration that remains that carries out suitability for industrialized production, the solvent extration extracting power is big, but the chilli extract that is extracted (lower concentration capsicine) foreign matter content height, refining difficulty is big.
Summary of the invention
The purpose of this invention is to provide a kind of processing method of from chillies, extracting capsaicine crystals, can overcome the deficiencies in the prior art.The present invention adopts adverse current leaching-allotment extraction-crystallization control technology, to producing the whole process of high-purity capsaicin crystalline, only uses two kinds of solvents from chillies, just obtains total alkali up to 95% above capsaicine crystals through crystallization control.Technology is simple, has suitability, is easy to large-scale industrial production.
The step that comprises from the processing method of chillies extraction capsaicine crystals provided by the invention:
With NaCl, NaHCO
3Form the modification ethanolic soln with the NaOH aqueous solution and ethanol, the capsicum rod layer that spray leaching chillies is made in the leacher of rotation, extracting solution another mistake stream lixiviate capsicum rod layer, through spray-drip-dry-spray-drip-dry continuous countercurrent lixiviate, get the leach liquor of suitable concentration, after concentrating, after the blender allotment with NaCl, sodium acetate and hydrochloric acid soln composition, use No. 6 solvent oil reflux extraction again, just obtained the capsicine crystalline mother solution, crystalline mother solution promptly obtains the high-purity capsaicin crystal through crystallization control.
The step that comprises from the processing method of chillies extraction capsaicine crystals provided by the invention:
1) in the leacher of rotation, with the NaCl, the NaHCO that give 40～55 ℃ of heat
3Make the capsicum rod layer that extraction agent spray chillies is made with the modification ethanolic soln of the NaOH aqueous solution and ethanol composition, leach liquor splashes into the susceptor of leacher.
2) by after the leach liquor drip-dry behind the spray capsicum rod layer, through pump the vat liquor in the susceptor is promoted and to spray capsicum rod layer again, proceed countercurrent spray, form the adverse current gradient leaching process of spray-drip-dry-spray-drip-dry, get leach liquor.
3) leach liquor through concentrate chilli extract,
4) chilli extract after allocating, was used No. 6 solvent oils 50 ℃～65 ℃ following reflux extraction 0.5-2 hours with the blender of NaCl, sodium acetate and hydrochloric acid soln composition again, separated, and promptly obtained the capsicine crystalline mother solution.
5) with crystalline mother solution insulation 1～10 hour, can change crystallizer over to, carry out crystallization in (preferred 7～10 ℃) below 15 ℃, obtain capsaicine crystals.
The mass ratio of described capsicum rod and extraction agent: 1: 1.5～4.The mass ratio of each composition: 1～6%NaCl: 2～6%NaHCO in the described extraction agent
3: 0.5～2%NaOH: 95% ethanol=10～20: 8～15: 7～10: 55～75.
Described blender is by 8% sodium acetate (CH
3CONa:3H
2O), 10%NaCl 1.5% aqueous hydrochloric acid (quality) mixes formation.
The mass ratio of each composition in the described blender: 8% sodium acetate: 10%NaCl: 1.5% hydrochloric acid=4～8: 2～5: 1～2.
Described capsicum rod is that the pulverizing granulation forms after removing seed by chillies.
Described leacher rotating speed is controlled at 120min～240min/r.
Described extraction agent is by 2%～4%NaCl aqueous solution, 4～5%NaHCO
3The aqueous solution, 0.5～2%NaOH aqueous solution and 95% edible ethanol are formed.
Extracting the rotation leacher device that the processing method of capsaicine crystals uses from chillies mainly comprises: rotation leacher body, material are poor, wet slag jar, pump, leacher susceptor, sieve plate, screen cloth and spray header, it is poor that some material can be housed in the leacher body, the poor bottom of material band screen cloth, the poor below of material is a susceptor; Extraction agent is capsicum rod layer spray in material is poor, sees through the bed of material and splash into susceptor, and the vat liquor adverse current behind the spray enters the capsicum rod layer of material in poor again through pump and sprays formation spray-drip-dry-spray-drip-dry leaching process.
Provided by the inventionly extract the rotation leacher that uses the processing method of capsaicine crystals from chillies and rotate with-constant speed degree, leacher is by the interior 14-20 of being equipped with material poor (all not drawing among the figure), and the poor tail band screen cloth of material is a susceptor below material is poor.The rotation leacher of adverse current lixiviate-blending extraction-crystallization control technology is counterclockwise rotated and driven material by certain speed poor.The poor end of each material, be made up of screen cloth and porose sieve plate again.All be equipped with through removing seed in material is poor, pulverize and make the capsicum rod that material forms.Extraction agent one modification ethanolic soln sprays into material by jet pipe and is pickled with grains or in wine, and after the infiltration of the spray bed of material, splashes into susceptor through screen cloth, extract out by pump again and enter jet pipe, it is poor to spray into material, successively through repeatedly spraying the extraction agent of different concns, vat liquor concentration is improved constantly, obtained the suitable leach liquor of concentration at last, in leacher, extract out, and with new extraction agent modification ethanolic soln, at last the capsicum rod behind the spray, also unload after the drip-dry and leach mouth, thereby formed adverse current successive gradient leaching process.
Through the modification ethanol liquid evaporation concentration of said process with obtaining suitable concentration, reclaim ethanol, enriched material (chilli extract) adds the auxiliary tone agent in blending vat allocates, and gets mixed liquid.In extractor, squeeze into solvent oil earlier No. 6, heat up, slowly squeeze into mixed liquid, reflux extraction, tell extraction liquid the capsicine crystalline mother solution.Lower the temperature again after the insulation of capsicine crystalline mother solution and carry out crystallization.After filtration, vacuum-drying obtains capsaicine crystals.
Gained capsaicine crystals of the present invention reaches more than 95% through the high-performance liquid chromatogram determination total alkali.
The present invention compared with prior art has following characteristics from the commercial run of chillies extraction capsaicine crystals:
1. on the capsicum rod of the material of extraction agent modification ethanolic soln at the bottom of in poor layer with the concentration gradient solution spraying of formation in service band screen cloth in rotating leacher, in the successive processes that spray-drip-dry-spray-drip-dry is leached, it is more complete that capsicine is extracted, and the capsicine extraction yield can reach more than 95%.
2. extraction agent modification ethanolic soln has the height specificity to capsicine, repel the degree of mixing in the capsicum and be not extracted, thereby after this extraction agent extraction, gained chilli extract impurity is few, refining easily purifying.
3. through the chilli extract of blender allotment, can force capsicine to enter solvent oil No. 6, and be detained impurity, thereby obtain the capsicine crystalline mother solution.
4. crystalline mother solution forms the sufficient quantity crystal seed through control, and crystallization is finished in the control crystal growth, makes gained capsaicine crystals total alkali up to more than 95%.
5. with adverse current lixiviate-allotment extraction-crystallization control technology, extract capsaicine crystals from chillies, technology is simple, and is smooth and easy, and easy operation control can realize the high-purity capsaicine crystals of scale operation.
Description of drawings
Fig. 1 is that the rotation leacher device that the present invention uses launches the section partial schematic diagram.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Fig. 1 is that the rotation leacher device that the present invention uses launches the section partial schematic diagram.Rotation leacher device mainly comprises: the 1st, and new extraction agent inlet, the 2nd, the sense of rotation of rotation leacher body, the 3rd, the wet slag jar, the 4th, pump, 5 leacher susceptors, the 6th, the gradient leach liquor, the 7th, sieve plate, the 8th, screen cloth, the 9th, material is poor, and the 10th, capsicum rod, the 11st, spray header.Leacher rotates with certain speed, and 14 to 20 material poor (all not drawing among the figure) are housed in the leacher, the poor tail band screen cloth of material, and the poor below of material is a susceptor.The capsicum rod of packing in material is poor is used by NaCl, NaHCO
3Make extraction agent with the modification ethanolic soln of the NaOH aqueous solution and ethanol composition, give heat earlier after 40～55 ℃, capsicum rod layer spray in material is poor sees through the bed of material and splashes into susceptor again.Form the adverse current gradient leaching process of " spray-drip-dry-spray-drip-dry ".Leach liquor is through concentrating the gained chilli extract, with NaCl, sodium acetate (CH
3COONa3H
2O) and the blender formed of hydrochloric acid soln, after allocating, use No. 6 solvent oil reflux extraction at a certain temperature again, separate, promptly obtain the capsicine crystalline mother solution.After crystalline mother solution kept certain hour at a certain temperature, can change crystallizer over to,, obtain capsaicine crystals in carrying out crystallization below 15 ℃.
Embodiment 1: the preparation of extraction agent modification ethanolic soln
Claim 4kgNaCl soluble in water and towards rare to 100kg, obtain the 4%NaCl aqueous solution; Take by weighing 5kgNaHCO
3Soluble in water and towards rare to 100kg, obtain 5%NaHCO
3The aqueous solution; Take by weighing 1kgNaOH soluble in water and towards rare to 100kg, the 1%NaOH aqueous solution.
With the 100kg4%NaCl aqueous solution, the 60kg 5%NaHCO3 aqueous solution and the 40kgl%NaOH aqueous solution, in the dissolving cylinder, stir miscible after, under agitation squeeze into 300kg 95% edible ethanol gradually, stirring and dissolving 10min～20min promptly obtains extraction agent modification ethanolic soln.
Embodiment 2: the preparation of blender
Take by weighing sodium acetate (CH
3COONa3H
2O) 8kg water-soluble and towards rare to 100kg, 8% sodium acetate solution; Take by weighing NaCl 10kg water-soluble and towards rare to 100kg, 10%NaCl solution; Take by weighing 35% concentrated hydrochloric acid 4.3kg water towards rare 100kg of arriving, get 1.5% aqueous hydrochloric acid.
In the dissolving cylinder, stir down, add 100kg 8% sodium acetate solution, 50kg 10%NaCl solution and 20kg 1.5% aqueous hydrochloric acid, add after miscible water towards rare to 1000kg, promptly obtain blender after being mixed.
Embodiment 3:
Each material poor (totally 16 material are poor) adds 250kg capsicum rod (the capsicum rod is that the pulverizing granulation forms after removing seed by chillies) in leacher, regulate and leach mouthful rotating speed to 180min/r (whenever circling 180 minutes), extraction agent 500kg is given heat earlier to 45 ℃ ± 2 ℃ in giving hot device, leach to the poor capsicum rod layer spray of material again, by expecting that poor bottom screen cloth splashes into susceptor, extract out by pump again, by the capsicum rod layer spray of jet pipe in the material that forwards to is poor.Operate extraction agent according to this by " spray-drip-dry-spray-drip-dry " process, concentration improves gradually, forms the gradient lixiviate, finally obtains the leach liquor of suitable concentration.
In as above leaching process, the material that new capsicum rod raw material is housed is poor by dense extraction agent spray, and the capsicum rod of new extraction agent spray becomes material slag (wet slag) to unload leacher after the drip-dry, thereby has formed the successive processes that adverse current leaches.
Leach liquor with the lixiviate of adverse current gradient obtains by rising the thin-film evaporator of film and falling liquid film, reclaims ethanol, obtains the peppery smart 25kg of enriched material (for 250kg capsicum rod).
Peppery smart 25kg is squeezed in the blending vat, start stirring, add blender 100kg, normal temperature is allocated 30 minutes down, must allocate solution.
In the extraction cylinder, squeeze into solvent oil 125kg No. 6, be warmed up to 55 ℃, rise moving the stirring, mixed liquid 125kg squeezed into the extraction cylinder with 15kg/min speed, add mixed liquid after, be warmed up to 60 ℃ ± 2 ℃, after the reflux extraction 45 minutes, be discharged in the insulation standing separation device, after 50 ℃ ± 2 ℃ insulations are left standstill 50 minutes, branch vibration layer, the capsicine crystalline mother solution of No. 6 solvent phase of acquisition.
Crystalline mother solution is placed 30 ℃ ± 2 ℃, be incubated after 2 hours, move in the crystallizer, after the cooling, carry out crystallization under 8 ℃ naturally, filter, vacuum-drying obtains capsaicine crystals 250g.Through high-performance liquid chromatogram determination, total alkali is 96.60%.
Wherein: capsicine content: 59.70%
Dihydrocapsaicin content: 34.80%
Class capsicine content: 2.10%.
Embodiment 4:
Except that following condition variation, equally carry out adverse current gradient spray with embodiment 3 and leach, be 50 ℃ ± 2 ℃ to 250kg capsicum rod with extraction agent 600kg and temperature, the rotating speed 210min/r of leacher.
Get 28kg (to 250kg capsicum rod) chilli extract after leach liquor concentrates and add blender 120kg, get mixed liquid 148kg.
In the extraction cylinder, add No. 6 solvent oil 150kg, add the 148kg mixed liquid, 55 ℃ ± 2 ℃ reflux extraction 40 minutes, obtain the capsicine crystalline mother solution and place 25 ℃ ± 2 ℃ insulations after 4 hours, move in the crystallizer, naturally after the cooling, place and carry out crystallization under 10 ℃, filter, vacuum-drying obtains capsaicine crystals 260g.
Through high-performance liquid chromatogram determination, total alkali is 95.85%.
Wherein: capsicine content: 60.10%
Dihydrocapsaicin content: 33.50%
Class capsicine content: 2.25%.
Claims (10)
1. the processing method from chillies extraction capsaicine crystals is characterized in that the step that this technology comprises: with NaCl, NaHCO
3Form the modification ethanolic soln with the NaOH aqueous solution and ethanol, the capsicum rod of making by chillies in spray leaching material in the leacher of rotation is poor layer, extracting solution another mistake stream lixiviate capsicum rod layer, through spray-drip-dry-spray-drip-dry continuous countercurrent lixiviate, got the leach liquor of suitable concentration, after concentrating, after the blender allotment with NaCl, sodium acetate and hydrochloric acid soln composition, use No. 6 solvent oil reflux extraction again, just obtained the capsicine crystalline mother solution, crystalline mother solution promptly obtains the high-purity capsaicin crystal through crystallization control.
2. processing method of extracting capsaicine crystals from chillies: it is characterized in that the step that this technology comprises:
1) in the leacher of rotation, with the NaCl, the NaHCO that give 40～55 ℃ of heat
3Make the capsicum rod layer that extraction agent spray chillies is made with the modification ethanolic soln of the NaOH aqueous solution and ethanol composition, leach liquor splashes into the susceptor of leacher;
2) by after the leach liquor drip-dry behind the spray capsicum rod layer, through pump the vat liquor in the susceptor is promoted and to spray capsicum rod layer again, proceed countercurrent spray, form the adverse current gradient leaching process of spray-drip-dry-spray-drip-dry, get leach liquor;
3) leach liquor through concentrate chilli extract;
4) after chilli extract is allocated with the blender of NaCl, sodium acetate and hydrochloric acid soln composition, use No. 6 solvent oils again 50 ℃～65 ℃ following reflux extraction 0.5-2 hours, separate, promptly obtain the capsicine crystalline mother solution;
5) crystalline mother solution is incubated 1～10 hour again, can changes crystallizer over to,, obtain capsaicine crystals in carrying out crystallization below 15 ℃.
3, extract the capsaicine crystals processing method according to claim 2 is described from chillies, it is characterized in that the mass ratio of described capsicum rod and extraction agent: 1: 1.5～4.
4, extract the capsaicine crystals processing method according to claim 2 is described from chillies, it is characterized in that the mass ratio of each composition in the described extraction agent: 1～6%NaCl: 2～6%NaHCO
3: 0.5～2%NaOH: 95% ethanol=10～20: 8～15: 7～10: 55～75.
5, extract the capsaicine crystals processing method according to claim 2 is described from chillies, it is characterized in that described blender is that 8% sodium acetate, 10%NaCl mix formation with the solution of 1.5% hydrochloric acid.
6, extract the capsaicine crystals processing method according to claim 4 is described from chillies, it is characterized in that the mass ratio of each composition in the described blender: 8% sodium acetate: 10%NaCl: 1.5% hydrochloric acid=4～8: 2～5: 1～2.
7, extract the capsaicine crystals processing method according to claim 2 is described from chillies, it is characterized in that described leacher rotating speed is controlled at 120min～240min/r.
8, extract the capsaicine crystals processing method according to claim 2 is described from chillies, it is characterized in that described extraction agent is by 2%～4%NaCl aqueous solution, 4～5%NaHCO
3The aqueous solution, 0.5～2%NaOH aqueous solution and 95% edible ethanol are formed.
9, a kind of claim 1 or the 2 described rotation leacher devices that extract the processing method use of capsaicine crystals from chillies, it is characterized in that it mainly comprises: rotation leacher body, material are poor, wet slag jar, pump, leacher susceptor, sieve plate, screen cloth and spray header, it is poor that some material can be housed in the leacher body, material poor bottom band screen cloth and sieve plate, the poor below of material is a susceptor; Extraction agent is capsicum rod layer spray in material is poor, sees through the bed of material and splash into susceptor, and the vat liquor adverse current behind the spray enters the capsicum rod layer of material in poor again through pump and sprays formation spray-drip-dry-spray-drip-dry leaching process.
10, according to the described rotation leacher of claim 9 device, it is poor to it is characterized in that being equipped with in the described rotation leacher body 14 to 20 material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710057643A CN100575336C (en) | 2007-06-15 | 2007-06-15 | Extract the processing method of capsaicine crystals from chillies |
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|---|---|---|---|
| CN200710057643A CN100575336C (en) | 2007-06-15 | 2007-06-15 | Extract the processing method of capsaicine crystals from chillies |
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| CN101070289A CN101070289A (en) | 2007-11-14 |
| CN100575336C true CN100575336C (en) | 2009-12-30 |
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| CN108276301A (en) * | 2018-02-11 | 2018-07-13 | 常德金德新材料科技股份有限公司 | A method of extraction capsaicine |
| CN108850982A (en) * | 2018-06-25 | 2018-11-23 | 南昌大学 | A kind of spicy fresh powder, preparation method thereof |
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