CN1219750C - Industrial production of capsaicin with seed and skin of red hot pepper as material - Google Patents
Industrial production of capsaicin with seed and skin of red hot pepper as material Download PDFInfo
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- CN1219750C CN1219750C CN 01128110 CN01128110A CN1219750C CN 1219750 C CN1219750 C CN 1219750C CN 01128110 CN01128110 CN 01128110 CN 01128110 A CN01128110 A CN 01128110A CN 1219750 C CN1219750 C CN 1219750C
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Abstract
The present invention discloses an industrial method of production of capsaicin with seeds and skins of red hot peppers as raw material. The present invention overcomes the defect that the technology of the prior art is complicated. Through dry cleaning operation, powder milling operation, first extraction operation, separation operation, concentration operation, reaction operation, second extraction operation, separation operation, concentration operation, third extraction operation, concentration operation, separation operation, washing operation and crystal operation for the whole hot peppers, alcohol, ether or paraffin hydrocarbon is used as extracting agents, and capsaicin is prepared. The purity of the capsaicin prepared by the present invention can reach more than 99.8 %. The technology is simple, the control is convenient, the raw material is fully used, the product cost is low, the quality is high, the present invention is suitable for industrial production, and the integrated utilizing rate of the raw materials is high. Skins and seeds of hot peppers are used for preparing capsaicin. Main products are produced, and simultaneously, base material of red pigment of hot peppers, oil and fat of capsaicin, capsaicine, cayenne pepper and hot pepper paste can be obtained. The raw material is fully utilized. The purity of a product obtained by the present invention is high. The product can be used as medical novel material and green special marine paint. Alkali products which have different contents can be used for producing special paint, food additives, etc.
Description
Affiliated field: the present invention is that a kind of seed with chilli, leather powder are the industrial method of raw material production capsicine.
Background technology: the purity of the capsicine that abroad makes at present is low, the highest Japan reaches 80%, and complex technical process, with 11 split-phase methods, processing parameter is restive, product yield is low, the production cost height, price is higher, 58 dollars/g of U.S.'s quotation, also have 120 dollars/g, and purity is lower than 90%.The purity that China now makes capsicine is higher than external 80% level, and the report that has reaches 90% (Xiamen University), 99.6% (Tianjin Light Industry College), and purity does not reach 99.8% yet.It adopts four split-phase methods, though technology is simpler than external, has lost yield.Testing laboratory's product colour is pale yellow, below standard standard, and purifying repeatedly, technology is comparatively complicated, and the production cost height is unsuitable for large-scale production.Make a general survey of that to produce capsicine raw materials used both at home and abroad only be the capsicum skin, and rejected chilli seed, this is the waste to raw material.
Technology contents: the present invention is the deficiency that overcomes prior art, and it is simple to propose a kind of technology, the capsicine purity height of producing, the novel process that utilization rate of raw materials is high.The present invention is achieved in that seed, the leather powder with chilli is the industrial method of raw material production capsicine, its processing step is: (1), input red chilly powder granularity are the 10-120 order, add purity greater than 90% food grade ethanol, red chilly powder and alcoholic acid part by weight are 1: 8-10, stir quiet the soaking 3.5-4 hour in back, temperature is at 45-70 ℃, and this finishes single extraction; (2), behind the filter press sedimentation, add malleation P0.15-0.6Mpa/cm
2, make liquid go into return channel through filter screen; (3), slagging-off, collect residue, be used to make red chilly powder and sweet thick chilli sauce, spicy sauce; (4), evaporation, import concentration tank through the supernatant liquid of precipitation gained, temperature derives steam simultaneously at 75-85 ℃, reclaims ethanol through condenser, the single extraction agent is done in circulation.When temperature in the jar stops heating during at 90-100 ℃, can obtain concentrated solution; (5), separate, concentrated solution is imported separator, by the ratio adding separating agent of the 0.3-3% of concentrated solution, after stirring, left standstill 3 hours, layering after the liquid saponification, the upper strata is a capsanthin, lower floor is a capsaicine, open separator bottom row's mouth, derive capsaicine, the upper strata capsanthin can be cleaned repeatedly with ethanol, remove capsaicine, through solvent removed by evaporation at reduced pressure, obtain byproduct---the capsanthin of no pepper flavor then, be the phase-splitting first time.(6), concentrate, capsaicine solution concentrates under 75-85 ℃ temperature, transfers pH value=7-10 with the dilute hydrochloric acid or the acetic acid of 16-25% concentration; (7), reextraction, add ether toward concentrated solution, the ratio of concentrated solution and ether is 1: 10-20, temperature 30-40 ℃, leave standstill and get ether extraction liquid after 1.5-2 hour, (8), concentrate, concentrated solution and ether ratio are 1: 10-20 is placed in the vaporizer, temperature 50-90 ℃, time 1-2 hour, ether is reclaimed in condensation, recycles, and this is phase-splitting for the second time; (9), three extractions, concentrated solution is added the petroleum ether extraction agent, ratio 1: 10-20, time 1.5-2 hour, dwell temperature 20-40 ℃, winter was with 30-60 ℃ of I class sherwood oil, summer is with 60-90 ℃ of II class sherwood oil; (10), concentrate, condensation, return channel reclaims the condensation sherwood oil, in 40-60 ℃ of 60-90 ℃ of winter in summer, time 1-1.5 hour, concentrated solution made white crystals body capsicine through the ether purifying, phase-splitting for the third time gets finished product.The present invention makes capsicine purity up to more than 99.8%, general-purpose equipment, and technology simply is convenient to control, suitability for industrialized production.Raw material comprehensive utilization ratio height, capsicum skin and seed all are used to make the capsicum alkaloid, and produce major product and can obtain capsanthin simultaneously, the capsicine grease, capsaicine and red chilly powder, byproducts such as the base-material of hot sauce accomplish that raw material makes full use of low cost product.Products obtained therefrom purity height of the present invention can supply pharmaceutical novel material, green Specific marine paint or tear bomb raw material; The capsicine product of different content can be made green products such as specialized paint, termite repellant, foodstuff additive.
Embodiment 1: seed, leather powder with chilli are the industrial method of raw material production capsicine, with alcohols and ethers is extraction agent, and the process implementing process is as follows: dry-cleaning, get the 100kg chilli, press wind to go into the special-purpose dry cleaning machine of capsicum and add the green dry cleaning agent, clean and do whole green pepper; Oven dry, temperature is lower than 65 ℃, and moisture is less than 8-10%; Pulverize, with the special-purpose pulverizing mill of capsicum, seed, the equal powder process of skin, granularity 10-120 order, its processing step is: (1), to drop into the red chilly powder granularity be 120 orders adds purity and is 95% food grade ethanol, red chilly powder and alcoholic acid part by weight are 1: 8, stir quiet the soaking 3.5 hours in back, temperature is at 45 ℃, and this finishes single extraction; (2), press filtration, after the sedimentation, add malleation P at 0.6Mpa/cm
2, make liquid go into return channel through filter screen; (3), slagging-off, collect residue, be used to make red chilly powder and sweet thick chilli sauce, spicy sauce; (4), evaporation, import concentration tank through the supernatant liquid of precipitation gained, temperature derives steam at 85 ℃, reclaims ethanol through condenser, the single extraction agent is done in circulation.When temperature in the jar stops heating during at 90-100 ℃, can obtain concentrated solution, be the 1-10% of former clear liquid; (5), separate, concentrated solution is imported separator, 3% ratio in concentrated solution adds separating agent, be sherwood oil: NaOH=3: 1, NaOH concentration is to leave standstill 3 hours after 25% process stirs, layering after the liquid saponification, the upper strata is a capsanthin, and lower floor is a capsaicine, opens separator bottom row's mouth, derive capsaicine, the upper strata capsanthin can be cleaned repeatedly with ethanol, removes capsaicine, then through solvent removed by evaporation at reduced pressure, obtain byproduct---the capsanthin of no pepper flavor, be the phase-splitting first time.(6), concentrate, capsaicine solution concentrates under 85 ℃ temperature, with 16% concentration dilute hydrochloric acid adjusting pH value=7-10; (7), reextraction, add ether toward concentrated solution, the ratio of concentrated solution and ether is 1: 10-20, temperature 30-40 ℃, leave standstill and get ether extraction liquid after 1.5-2 hour, (8), concentrate, concentrated solution and ether ratio are 1: 10-20 is placed in the vaporizer, 50 ℃ of temperature, time 1-2 hour, ether is reclaimed in condensation, recycles, and this is phase-splitting for the second time; (9), three extractions, concentrated solution is added the petroleum ether extraction agent, ratio 1: 10, time 1.5-2 hour, 20 ℃ of dwell temperature, winter is with 30-60 ℃ of I class sherwood oil, summer is with 60-90 ℃ of II class; (11), concentrate, return channel reclaims the condensation sherwood oil, in 40-60 ℃ of 60-90 ℃ of winter in summer, time 1-1.5 hour, concentrated solution added 5500 milliliters of ether purifying and makes white crystals body capsicine 56g, phase-splitting for the third time gets finished product.In the ether purifying, concentrated solution is 1 with the ratio that adds ether: 10-20, and temperature is at 20-30 ℃, and time 2-3 hour, then at 40-60 ℃, evaporative condenser reclaimed ether and gets final product.
Embodiment 2: seed, leather powder with the 150kg chilli are the industrial method of raw material production capsicine, and the process implementing process is as follows: dry-cleaning, and press wind to go into the special-purpose dry cleaning machine of capsicum and clean dried whole green pepper, add the green dry cleaning agent; Oven dry then, temperature is lower than 65 ℃, and moisture is less than 8%; Pulverize, with the special-purpose pulverizing mill of capsicum, seed, the equal powder process of skin, granularity 10-100 order; Its processing step is: (1), to drop into the red chilly powder granularity be 60 orders, adding purity and be 90% food grade ethanol, red chilly powder and alcoholic acid part by weight are 1: 10, stir quiet the soaking 4 hours in back, and temperature is at 70 ℃, and this finishes single extraction; (2), press filtration, after the sedimentation, adding malleation P is 0.15Mpa/cm
2, make liquid go into return channel through filter screen; (3), slagging-off, collect residue, be used to make red chilly powder and sweet thick chilli sauce, spicy sauce; (4), evaporation, import concentration tank through the supernatant liquid of precipitation gained, temperature derives steam at 75 ℃, reclaims ethanol through condenser, the single extraction agent is done in circulation.When temperature in the jar stops heating during at 90-100 ℃, can obtain concentrated solution, be 10% of former clear liquid.(5), separate, concentrated solution is imported separator, 0.3% ratio in concentrated solution adds separating agent, be sherwood oil: NaOH=1.5: 1, NaOH concentration is to leave standstill 3 hours after 16% process stirs, layering after the liquid saponification, the upper strata is a capsanthin, and lower floor is a capsaicine, opens separator bottom row's mouth, derive capsaicine, the upper strata capsanthin can be cleaned repeatedly with ethanol, removes capsaicine, then through solvent removed by evaporation at reduced pressure, obtain byproduct---the capsanthin of no pepper flavor, be the phase-splitting first time.(6), concentrate, capsaicine solution concentrates under 75 ℃ temperature, transfers pH value=7-10 with dilute hydrochloric acid 25% concentration; (7), reextraction, add ether toward concentrated solution, the ratio of concentrated solution and ether is 1: 10-20, temperature 30-40 ℃, leave standstill after 1.5-2 hour ether extraction liquid, (8), concentrate, concentrated solution and ether ratio are 1: 20, be placed in the vaporizer, temperature 50-90 ℃, time 1-2 hour, ether was reclaimed in condensation, recycle, this is phase-splitting for the second time; (9), three extractions, concentrated solution is added the petroleum ether extraction agent, ratio 1: 10-20, time 1.5-2 hour, 40 ℃ of dwell temperature, winter is with 30-60 ℃ of I class sherwood oil, summer is with 60-90 ℃ of II class sherwood oil; (10), concentrate, return channel reclaims the condensation sherwood oil, in 40-60 ℃ of 60-90 ℃ of winter in summer, time 1-1.5 hour, concentrated solution made white crystals body capsicine through the sherwood oil purifying, phase-splitting for the third time gets finished product capsicine 85g.Concentrated solution is 1 with the ratio that adds sherwood oil: 10-20, and temperature is at 30-40 ℃, and time 2-3 hour, then at 50-90 ℃, evaporative condenser reclaimed sherwood oil and gets final product.
Embodiment 3: seed, leather powder with chilli are the industrial method of raw material production capsicine, with the alkanes is extraction agent, and the process implementing process is as follows: dry-cleaning, get the 200kg chilli, press wind to go into the special-purpose dry cleaning machine of capsicum and clean dried whole green pepper, add the green dry cleaning agent; Oven dry, temperature is lower than 65 ℃, and moisture is less than 8-10%; Pulverize, with the special-purpose pulverizing mill of capsicum, seed, the equal powder process of skin, granularity 10-120 order; Its processing step is: (1), to drop into the red chilly powder granularity be 10 orders, adding purity greater than 90% food grade ethanol, red chilly powder and alcoholic acid part by weight are 1: 9, stir quiet the soaking 3.8 hours in back, and temperature is at 60 ℃, and this finishes single extraction; (2), press filtration, after the sedimentation, adding malleation P is 0.1Mpa/cm
2, make liquid go into return channel through filter screen; (3), slagging-off, collect residue, be used to make red chilly powder and sweet thick chilli sauce, spicy sauce; (4), evaporation, import concentration tank through the supernatant liquid of precipitation gained, temperature derives steam simultaneously at 80 ℃, reclaims ethanol through condenser, recycles, and does single extraction.When temperature in the jar stops heating during at 90-100 ℃, can obtain concentrated solution, be 6% of former clear liquid; (5), separate, concentrated solution is imported separator, 1% ratio in concentrated solution adds separating agent, be sherwood oil: NaOH=2: 1, NaOH concentration is 20%, after stirring, left standstill 3 hours, layering after the liquid saponification, the upper strata is a capsanthin, lower floor is a capsaicine, open separator bottom row's mouth, derive capsaicine, the upper strata capsanthin can be cleaned repeatedly with ethanol, remove capsaicine, through solvent removed by evaporation at reduced pressure, obtain byproduct---the capsanthin of no pepper flavor then, be the phase-splitting first time.(6), concentrate, capsaicine solution concentrates under 75-85 ℃ temperature, with the dilute hydrochloric acid accent pH value=7-10 of 20% concentration; (7), reextraction, add ether toward concentrated solution, the ratio of concentrated solution and ether is 1: 15, temperature 30-40 ℃, leave standstill after 1.5 hours ether extraction liquid.(8), concentrate, concentrated solution and ether ratio are to be placed on vaporizer at 1: 15,70 ℃ of temperature, time 1-2 hour, ether was reclaimed in condensation, recycled, this is the phase-splitting second time; (9), three extractions, concentrated solution is added the petroleum ether extraction agent, ratio 1: 15,1.8 hours time, 30 ℃ of dwell temperature, winter is with 30-60 ℃ of I class sherwood oil, summer is with 60-90 ℃ of II class; (10), concentrate, return channel reclaims the condensation sherwood oil, in 40-60 ℃ of 60-90 ℃ of winter in summer, 1.2 hours time, concentrated solution adds 8000 milliliters of normal butane purifying and makes white crystals body capsicine 111g, phase-splitting for the third time gets finished product., concentrated solution is 1 with the ratio that adds normal butane: 10-20, and temperature is at 30-40 ℃, and time 2-3 hour, then at 50-70 ℃, evaporative condenser reclaimed normal butane and gets final product.
Claims (7)
1, a kind of seed with chilli, leather powder are the industrial method of raw material production capsicine, with alcohols and ethers is extraction agent, its processing step is: (1), input red chilly powder granularity are the 10-120 order, add purity greater than 90% food grade ethanol, red chilly powder and alcoholic acid part by weight are 1: 8-10, stir quiet the soaking 3.5-4 hour in back, temperature is at 45--70 ℃, and this finishes single extraction; (2), press filtration, after the sedimentation, adding malleation P is 0.15-0.6Mpa/cm
2, make liquid go into return channel through filter screen; (3), slagging-off, collect residue, be used to make red chilly powder and sweet thick chilli sauce, spicy sauce; (4), evaporation, import concentration tank through the supernatant liquid of precipitation gained, temperature derives steam simultaneously at 75-85 ℃, reclaims ethanol through condenser, recycles, and does single extraction.When temperature in the jar stops heating during at 90-100 ℃, can obtain concentrated solution; (5), separate, concentrated solution is imported separator, by the ratio adding separating agent of the 0.3-3% of concentrated solution, after stirring, left standstill 3 hours, layering after the liquid saponification, the upper strata is a capsanthin, lower floor is a capsaicine, open separator bottom row's mouth, derive capsaicine, the upper strata capsanthin can be cleaned repeatedly with ethanol, remove capsaicine, through solvent removed by evaporation at reduced pressure, obtain byproduct---the capsanthin of no pepper flavor then, be the phase-splitting first time.(6), concentrate, capsaicine solution concentrates under 75-85 ℃ temperature, transfers pH value=7-10 with the dilute hydrochloric acid or the acetic acid of 16-25% concentration; (7), reextraction, add ether toward concentrated solution, the ratio of concentrated solution and ether is 1: 10-20, temperature 30-40 ℃, leave standstill after 1.5-2 hour ether extraction liquid.(8), concentrate, concentrated solution and ether ratio are 1: 10-20, be placed in the vaporizer, temperature 50--90 ℃, time 1-2 hour, ether was reclaimed in condensation, recycled, this is the phase-splitting second time; (9), three extractions, concentrated solution is added the petroleum ether extraction agent, ratio 1: 10-20, time 1.5-2 hour, dwell temperature 20--40 ℃, winter was with 30-60 ℃ of I class sherwood oil, summer is with 60-90 ℃ of II class; (10), concentrate, condensation, return channel reclaims the condensation sherwood oil, in 40-60 ℃ of 60-90 ℃ of winter in summer, time 1-1.5 hour, concentrated solution made white crystals body capsicine through the ether purifying, phase-splitting for the third time gets finished product.
2, the seed with chilli according to claim 1, leather powder are the industrial method of raw material production capsicine, it is characterized in that: can also alkanes be extraction agent.
3, the seed with chilli according to claim 1, leather powder are the industrial method of raw material production capsicine, it is characterized in that: the proportioning of described separating agent is sherwood oil: NaOH=1.5-3: 1, and NaOH concentration is 16-25%.
4, the seed with chilli according to claim 1, leather powder are the industrial method of raw material production capsicine, it is characterized in that: concentrate, in the condensing steps, concentrated solution is 1 with the ratio that adds ether: 10-20, temperature is at 20-30 ℃, time 2-3 hour, at 40-60 ℃, evaporative condenser reclaims ether and gets final product then.
5, the seed with chilli according to claim 1, leather powder are the industrial method of raw material production capsicine, it is characterized in that: concentrate, in the condensing steps, the also available sherwood oil of purifying, concentrated solution is 1 with the ratio that adds sherwood oil: 10-20, temperature is at 30-40 ℃, and time 2-3 hour, then at 50-90 ℃, evaporative condenser reclaims sherwood oil and gets final product.
6, the seed with chilli according to claim 1, leather powder are the industrial method of raw material production capsicine, it is characterized in that: concentrate, in the condensing steps, the also available normal butane of purifying, concentrated solution is 1 with the ratio that adds normal butane: 10-20, temperature is at 30-40 ℃, and time 2-3 hour, then at 50-70 ℃, evaporative condenser reclaims normal butane and gets final product.
7, seed, the leather powder of doing with red pepper according to claim 1 is the industrial method of raw material production capsicine, and it is characterized in that: the concentrated solution that obtains in evaporation step is the 1-10% of former clear liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01128110 CN1219750C (en) | 2001-08-29 | 2001-08-29 | Industrial production of capsaicin with seed and skin of red hot pepper as material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01128110 CN1219750C (en) | 2001-08-29 | 2001-08-29 | Industrial production of capsaicin with seed and skin of red hot pepper as material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1406928A CN1406928A (en) | 2003-04-02 |
| CN1219750C true CN1219750C (en) | 2005-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 01128110 Expired - Fee Related CN1219750C (en) | 2001-08-29 | 2001-08-29 | Industrial production of capsaicin with seed and skin of red hot pepper as material |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739511A (en) * | 2013-12-20 | 2014-04-23 | 白城艾高食品有限公司 | Method for extracting capsaicin |
| CN105566142A (en) * | 2015-12-29 | 2016-05-11 | 云南宏绿辣素有限公司 | Process for extracting chili with high capsaicin content |
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- 2001-08-29 CN CN 01128110 patent/CN1219750C/en not_active Expired - Fee Related
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| CN1406928A (en) | 2003-04-02 |
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