CN108219027A - A kind of method that sisal hemp pectin is prepared using sisal hemp waste residue - Google Patents
A kind of method that sisal hemp pectin is prepared using sisal hemp waste residue Download PDFInfo
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- CN108219027A CN108219027A CN201611154804.2A CN201611154804A CN108219027A CN 108219027 A CN108219027 A CN 108219027A CN 201611154804 A CN201611154804 A CN 201611154804A CN 108219027 A CN108219027 A CN 108219027A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
- C08B37/0048—Processes of extraction from organic materials
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Abstract
The invention discloses a kind of methods that pectin is prepared using sisal hemp waste residue, specifically comprise the following steps：A, boiling enzyme deactivation：The dry slag of sisal hemp is taken to carry out boiling enzyme deactivation, obtains the sisal hemp wet slag after enzyme deactivation；B, sisal hemp wet slag addition calgon is extracted, obtains extract liquor；C, removal of impurities decoloration：It is filtered after the extract liquor is added in diatomite stirring and adsorbing, obtains filtrate, the upper K15 particle charcoal posts of the filtrate, flow velocity is 0.8 1.2L/min, obtains upper prop liquid；D, except sodium decolourizes again：By the upper prop liquid, then upper 732 cationic resin column, flow velocity is 0.3 0.6L/min, obtains twin columns liquid；E, the twin columns liquid is concentrated under reduced pressure, alcohol is analysed, is washed, is pressed dry, dry, screening, mixing, packaging obtain sisal hemp pectin.The sisal hemp pectin color and luster that the preparation method of the present invention is produced is good, and calcination ash content index is less than Customer Standard.
Description
Technical field
The invention belongs to technical field of plant extraction, more particularly to a kind of side that sisal hemp pectin is prepared using sisal hemp waste residue
Method.
Background technology
Sisal hemp is abounded in Guangdong, Guangxi, sisal fiber sisal hemp waste residue remaining after preparing, as offal treatment, seriously
Local ecological environment is polluted, sisal hemp waste residue can obtain sisal hemp pectin, sisal hemp pectin is as natural after biotechnology is handled
Low-fat pectin there is very vast market prospect, however the ash content after the product color of sisal hemp pectin and calcination is relatively difficult to
It is up to standard.A small number of producers only at present can use old technique productions, and products obtained therefrom all encounters above-mentioned two indexs cannot be up to standard
Situation, the backwardness of production technology, it has also become the bottleneck of sisal hemp pectin industry development.
The old technique of tradition of sisal hemp pectin production is：A, boiling enzyme deactivation；B, calgon extracts；C, diatomite, which is crossed, filters out
It is miscellaneous；D, it is concentrated under reduced pressure；E, alcohol is analysed；F, it centrifuges, is broken, washing, squeezing；G, drying, crushing, screening, mixing, packaging.Its
In, calgon can partly be precipitated to remain in pectin wet product when alcohol is analysed, dry finished product as sisal hemp pectin extractant
It can inevitably cause calcination ash content higher；Using diatomite filtering and impurity removing, part magazine and pigment be not divisible, is eventually brought into
Product, can occur enzymatic browning after drying, finished product color and luster is relatively deep poor, it is impossible to meet the quality requirement of client.
Invention content
In view of the problems of the above-mentioned prior art, the purpose of the present invention is to propose to a kind of pectin is prepared using sisal hemp waste residue
Method.Sisal hemp pectin product color and luster prepared by this method is true qualities, off-white color solid powder, and calcination ash content index effectively drops
It is low, less than Customer Standard.
The purpose of the present invention will be achieved by the following technical programs：
A kind of method that sisal hemp pectin is prepared using sisal hemp waste residue, is specifically comprised the following steps：A, boiling enzyme deactivation：Take sisal hemp
Dry slag carries out boiling enzyme deactivation, obtains the sisal hemp wet slag after enzyme deactivation；B, sisal hemp wet slag addition calgon is extracted, obtained
Extract liquor；C, removal of impurities decoloration：It is filtered after the extract liquor is added in diatomite stirring and adsorbing, obtains filtrate, the filtrate is K15 upper
Grain charcoal post, flow velocity 0.8-1.2L/min obtain upper prop liquid；D, except sodium decolourizes again：By the upper prop liquid, then upper 732 cation tree
Fat column, flow velocity 0.3-0.6L/min obtain twin columns liquid；E, the twin columns liquid is concentrated under reduced pressure, alcohol is analysed, is washed, is pressed dry, do
Dry, screening, mixing, packaging, obtain sisal hemp pectin.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, the temperature control for the decoloration that cleans in step c
For system at 65 ± 1 DEG C, the upper prop liquid is clear liquid, and transmitance >=80% and pH value are 7~8.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, diatomite and step described in step c
The mass volume ratio of extract liquor described in b is 2.5~3.5: 1000, and the diatomite stirring and adsorbing time is 15 minutes.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, twin columns liquid transmitance described in step d
>=90% and pH value be 3~4.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, the boiling enzyme deactivation further includes as follows
Step：Deionization exchanged water is first added in, 75 DEG C of temperature is slow added into the dry slag of the sisal hemp, is continuously heating to 88~92 DEG C, protects
Temperature 30 minutes.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, the dry slag of sisal hemp with it is described go from
The mass volume ratio of sub- exchanged water is 1kg: 15L.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, step b further includes following steps：Claim
Ion exchange water is removed, is warming up to 75 DEG C, the sisal hemp wet slag being slowly added to after the calgon, the enzyme deactivation is warming up to
85-89 DEG C, heat preservation extraction obtains the extract liquor.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, calgon described in step b with
The mass volume ratio of the deionization exchanged water is 1kg: 200L.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, the sisal hemp described in step b after enzyme deactivation
Wet slag weight is in terms of the dry slag of sisal hemp, and the mass volume ratio of the dry slag of sisal hemp and deionization exchanged water described in step b is 1:
20~25.
A kind of above-mentioned method that sisal hemp pectin is prepared using sisal hemp waste residue, wherein, the extract liquor includes 1 He of extract liquor
Extract liquor 2, the extract liquor 1 are that the liquid of dry gained, the extract liquor 2 is the washing pressure that is soaked in water for squeezing after heat preservation extracts
It squeezes to the liquid obtained by dry filter cake.
Compared with prior art, a kind of method that pectin is prepared using sisal hemp waste residue provided by the invention, the technology reached
Effect is：(1) activated carbon is directly mixed with sisal hemp pectin extract liquor, after heating decoloration, due to the material characteristic of pectin, after decoloration
Activated carbon is difficult that separation is clean, often forms leakage charcoal phenomenon, the present invention is using the directly upper K15 of the extract liquor after diatomite filtering
Granulated carbon (or fiber charcoal) column controls corresponding upper prop flow velocity to obtain fine decolorizing effect, products obtained therefrom color and luster is light beige；
(2) extract liquor on after particle charcoal post, then upper cationic 732 exchange resin columns, control appropriate column flow quantity to remove to greatest extent
Sodium ion to the greatest extent in extract liquor, further remove impurity and pigment, and products obtained therefrom color further improves namely sisal hemp pectin
True qualities, off-white color solid powder, the ash content index of pectin product is well below Customer Standard；(3) new process of the present invention relative to
The old technique of tradition, increases two critical operations, thoroughly solves two big technical barriers in sisal hemp pectin production, product quality
It is greatly improved, the quality requirement of current client can not only be met, the quality for also having reached customer is looked forward to for sisal hemp pectin
The production and application of the later scale high standard of industry provide strong technical guarantee.
Below just in conjunction with the embodiments, the embodiment of the present invention is described in further detail, so that technical solution is more
It should be readily appreciated that, grasp.
Specific embodiment
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.In following embodiments
The experimental method is conventional method unless otherwise specified；The reagent and material, unless otherwise specified, can be from business
Approach obtains, and example below is not to limit the scope of the claims of the invention, all equivalence enforcements without departing from carried out by the present invention
Or change, it is intended to be limited solely by the scope of this patent.
Embodiment 1 prepares sisal hemp pectin
A, boiling enzyme deactivation：It is accurate to measure 150L deionization exchanged waters, be added in 200L glassed steel reaction vessels, open steam and
Stirring, treats that material temperature in kettle to 75 DEG C, is slow added into the dry slag of 10kg sisal hemps, is continuously heating to 88 DEG C, heat preservation, boiling enzyme deactivation
After 30 minutes, blowing is squeezed to doing, and obtains sisal hemp wet slag 28Kg；
B, 200L deionization exchanged waters are accurately measured, 200L glassed steel reaction vessels is added to, opens steam and stirring, treat in kettle
Temperature of charge rises to 75 DEG C, the sisal hemp wet slag 28kg being slow added into after 1kg calgons and the above-mentioned enzyme deactivation of boiling squeezing,
85 DEG C are continuously heating to, after heat preservation extracts 3 hours, blowing squeezes to dry and obtains extract liquor, and the filter cake after squeezing uses suitable quantity of water again
Washing by soaking is primary, and washing lotion is incorporated to extract liquor, amounts to extract liquor 220L or so；
C, removal of impurities decoloration：Extract liquor is pumped into 300L reaction kettles, opens steam and stirring, treats material temperature in kettle to 65 DEG C
When, it adds in 600g diatomite stirring and adsorbing 15 minutes, is then pumped into diatomite filter again and filters, K15 particle charcoal posts on filtrate,
Flow control in 1L/min,
Wherein, upper prop liquid be clear liquid, transmitance be 83% (721 spectrophotometer), pH value between 7.5,
Particle charcoal post is renewable, Reusability；
D, except sodium ion decolourizes again：By above-mentioned upper prop liquid, then upper 732 cationic resin column, flow control in 0.5L/min,
Obtain twin columns liquid.Twin columns liquid is supernatant liquid, almost colourless liquid, and transmitance is 94% (721 spectrophotometer), and pH value exists
Between 3.5, twin columns liquid product 240L；
If twin columns liquid cannot meet above-mentioned two index of central control (pH value and transmitance), must again on regeneration treatment it is good not
Once the 732 cation trees used refer to column；
E, the twin columns liquid for having gone up twin columns is concentrated under reduced pressure again, volume be reduced to original a quarter or so namely
During 60L, then add the edible alcohol of 95% concentration of 100L, cooling crystallization in motion 3~4 hours is squeezed to dry, filtrate distillation reuse, filter cake
Impregnated, washed, pressed dry with the edible alcohol of 80~85% concentration again, repetitive operation twice, filter cake dry crushing, drying, screening,
Mixing, packaging obtain sisal hemp pectin finished product 1.2kg, and washing lotion is incorporated to alcohol recycle liquid, distills reuse.
Embodiment 2 prepares sisal hemp pectin
A, boiling enzyme deactivation：It is accurate to measure 150L deionization exchanged waters, be added in 200L glassed steel reaction vessels, open steam and
Stirring, treats that material temperature in kettle to 75 DEG C, is slow added into the dry slag of 10kg sisal hemps, is continuously heating to 90 DEG C, keeps the temperature (90 DEG C ± 2
DEG C), after boiling enzyme deactivation 30 minutes, blowing is squeezed to dry, obtains sisal hemp wet slag 27Kg；
B, 200L deionization exchanged waters are accurately measured, 200L glassed steel reaction vessels is added to, opens steam and stirring, treat in kettle
Temperature of charge rises to 75 DEG C, the sisal hemp wet slag 27Kg being slow added into after 1kg calgons and the above-mentioned enzyme deactivation of boiling squeezing,
87 DEG C are continuously heating to, after heat preservation extracts 3 hours, blowing squeezes to dry and obtains extract liquor, and the filter cake after squeezing uses suitable quantity of water again
Washing by soaking is primary, and washing lotion is incorporated to extract liquor, amounts to extract liquor 225L or so；
C, removal of impurities decoloration：Extract liquor is pumped into 300L reaction kettles, opens steam and stirring, treats material temperature in kettle to 65 DEG C
When, it adds in 700g diatomite stirring and adsorbing 15 minutes, is then pumped into diatomite filter again and filters, K15 particle charcoal posts on filtrate,
Flow control is in 1.2L/min；
Wherein, upper prop liquid be clear liquid, transmitance be 83% (721 spectrophotometer), pH value between 7.5,
Particle charcoal post is renewable, Reusability；
D, except sodium ion decolourizes again：By above-mentioned upper prop liquid, then upper 732 cationic resin column, flow control in 0.4L/min,
Obtain twin columns liquid；Twin columns liquid is more clarifies, and almost colourless liquid, transmitance are 95% (721 spectrophotometer), and pH value exists
Between 3.5, twin columns liquid product 260L；
Wherein, as efflux cannot meet above-mentioned two index of central control (pH value and transmitance), must again on regeneration treatment
The good spare tree not used refers to column；
E, the twin columns liquid for having gone up twin columns is concentrated under reduced pressure again, when volume reduces 60L, then adds 95% concentration of 100L
Edible alcohol, cooling crystallization in motion 3~4 hours are squeezed to dry, and filtrate goes distillation reuse, filter cake eating with 80~85% concentration again
Alcohol is impregnated, washs, is pressed dry, and twice, filter cake is dried, crushes, dries, sieves, mixes, packed for repetitive operation, obtains sisal hemp pectin
Finished product 1.4kg, washing lotion are incorporated to alcohol recycle liquid, distill reuse.
Embodiment 3 chooses the sisal hemp pectin of the preparation of embodiment 1 according to the quality standard and detection method of GB25533-2010
It is detected, the results are shown in Table 1.
The test result of 1 sisal hemp pectin of table
| Detection project | Quality standard | Experimental result |
| Degree of gelation | >=100 (US-SAG methods) | 105 |
| Esterification degree | 25%-35% | 26% |
| Gala furfural | >=65% | 90% |
| Appearance | Yellow powder | Off-white color |
| PH (1% aqueous solution) | 5±0.5 | 5.1 |
| Moisture content | ＜ 12% | 10% |
| Ash content | ＜ 5% | 0.2% |
| Granularity | 60 mesh of ＜ | It is qualified |
| Acid-insoluble ash | ＜ 1% | 0.05% |
| Sulfur dioxide | ＜ 5ppm | 2ppm |
| Heavy metal | ＜ 5ppm | 2ppm |
Several preferred embodiments of the present invention have shown and described in above description, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations,
Modification and environment, and the above teachings or related fields of technology or knowledge can be passed through in the scope of the invention is set forth herein
It is modified.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be in this hair
In the protection domain of bright appended claims.
Claims (10)
- A kind of 1. method that sisal hemp pectin is prepared using sisal hemp waste residue, which is characterized in that specifically comprise the following steps：A, boiling is gone out Enzyme：The dry slag of sisal hemp is taken to carry out boiling enzyme deactivation, obtains the sisal hemp wet slag after enzyme deactivation；B, by the sisal hemp wet slag add in calgon into Row extraction, obtains extract liquor；C, removal of impurities decoloration：It is filtered after the extract liquor is added in diatomite stirring and adsorbing, obtains filtrate, the filter K15 particles charcoal post on liquid, flow velocity 0.8-1.2L/min obtain upper prop liquid；D, except sodium decolourizes again：By the upper prop liquid, then upper 732 Cationic resin column, flow velocity 0.3-0.6L/min obtain twin columns liquid；E, the twin columns liquid is concentrated under reduced pressure, alcohol analysis, washed It washs, press dry, dry, screening, mixing, packaging obtain sisal hemp pectin.
- A kind of 2. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 1, which is characterized in that step c The temperature of middle removal of impurities decoloration is controlled at 65 ± 1 DEG C, and the upper prop liquid is clear liquid, and transmitance >=80% and pH value are 7 ~8.
- A kind of 3. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 2, which is characterized in that step c Described in the mass volume ratio of extract liquor described in diatomite and step b be 2.5~3.5: 1000, the diatomite stirring and adsorbing Time is 15 minutes.
- A kind of 4. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 1, which is characterized in that step d Described in twin columns liquid transmitance >=90% and pH value be 3~4.
- A kind of 5. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 1, which is characterized in that the steaming It boils enzyme deactivation and further includes following steps：Deionization exchanged water is first added in, 75 DEG C of temperature is slow added into the dry slag of the sisal hemp, continues 88~92 DEG C are warming up to, keeps the temperature 30 minutes.
- A kind of 6. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 5, which is characterized in that the sword The mass volume ratio of the dry slag of fiber crops and the deionization exchanged water is 1kg: 15L.
- A kind of 7. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 3, which is characterized in that step b Further include following steps：Deionization exchanged water is measured, 75 DEG C are warming up to, after being slowly added to the calgon, the enzyme deactivation Sisal hemp wet slag, be warming up to 85-89 DEG C, heat preservation extraction obtains the extract liquor.
- A kind of 8. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 7, which is characterized in that step b Described in the mass volume ratio of calgon and the deionization exchanged water be 1kg: 200L.
- A kind of 9. method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 8, which is characterized in that step b Described in sisal hemp wet slag weight after enzyme deactivation be in terms of the dry slag of sisal hemp, the dry slag of sisal hemp is exchanged with deionization described in step b The mass volume ratio of water is 1: 20~25.
- 10. a kind of method that sisal hemp pectin is prepared using sisal hemp waste residue according to claim 7, which is characterized in that described Extract liquor includes extract liquor 1 and extract liquor 2, and the extract liquor 1 is to be squeezed after heat preservation extracts to the liquid of dry gained, the extraction Liquid 2 is the liquid being soaked in water obtained by wash press to dry filter cake.
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| CN110959785A (en) * | 2019-08-03 | 2020-04-07 | 黄振翠 | Sisal hemp pectin-containing beverage and preparation method thereof |
| CN110973431A (en) * | 2019-08-03 | 2020-04-10 | 黄振翠 | Sisal hemp pectin solid beverage and preparation method thereof |
| CN113680102A (en) * | 2021-08-27 | 2021-11-23 | 湖南绿蔓生物科技股份有限公司 | Method for preparing plant extract without exogenous pollutant |
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| CN110959785A (en) * | 2019-08-03 | 2020-04-07 | 黄振翠 | Sisal hemp pectin-containing beverage and preparation method thereof |
| CN110973431A (en) * | 2019-08-03 | 2020-04-10 | 黄振翠 | Sisal hemp pectin solid beverage and preparation method thereof |
| CN113680102A (en) * | 2021-08-27 | 2021-11-23 | 湖南绿蔓生物科技股份有限公司 | Method for preparing plant extract without exogenous pollutant |
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Application publication date: 20180629 |