CN109111516A - A method of extracting wool keratin - Google Patents
A method of extracting wool keratin Download PDFInfo
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- CN109111516A CN109111516A CN201811028704.4A CN201811028704A CN109111516A CN 109111516 A CN109111516 A CN 109111516A CN 201811028704 A CN201811028704 A CN 201811028704A CN 109111516 A CN109111516 A CN 109111516A
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- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/46—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates
- C07K14/47—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates from mammals
- C07K14/4701—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates from mammals not used
- C07K14/4741—Keratin; Cytokeratin
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Abstract
The present invention relates to wool keratins to extract field, disclose a kind of method for extracting wool keratin, reduction pretreatment is carried out to wool using sodium sulfite, after destroying scale layer, wool is dissolved under the action of ultrasound with 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid, 1- allyl -3- methylimidazole acetate ionic liquid and dimethyl sulfoxide mixed solution extracts keratin, by centrifugation, supernatant is taken to be dialysed and be freeze-dried to obtain pure wool keratin powder.Method provided by the invention is easy to operate, and recovery rate is high, and the wool keratin purity is high obtained.
Description
Technical field
The present invention relates to wool keratins to extract field more particularly to a kind of method for extracting wool keratin.
Background technique
The whole world has wool keratin of the number in terms of ten thousand tons to be landfilled every year, not only causes the huge waste of resource,
Result in serious problem of environmental pollution.Waste wool is a kind of important, cheap one of keratin resource, has high grind
Study carefully utility value.
Wool is a kind of animal origin, and protein content is about 99%, and wool keratin is made of 18 kinds of amino acid,
Middle cystine residue accounts for 12%.The structure of wool keratin is made of matrix between micro- fibril and fibre, and micro- fibril is by low-sulfur albumen structure
At the matrix between micro- fibril is made of High-sulphur protein and high sweet casein forms.Therefore it is to solve that dissolution wool, which extracts keratin,
The important means of shortage of resources and the wasting of resources.
Currently, the dissolving method of waste wool mainly has Mechanical Method, oxidizing process, reduction method, acid-base method, metal salt method etc.,
These methods extract often not enough thoroughly wool keratin, cannot extract completely the keratin in wool, therefore need
A kind of keratin that can be extracted completely as far as possible in wool is developed, the utilization rate of resource is improved.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of methods for extracting wool keratin.The present invention first adopts
Reduction pretreatment carried out to wool with sodium sulfite, after destroying scale layer, then with 1- ethyl-3-methylimidazole diethyl phosphate salt
Ionic liquid, 1- allyl -3- methylimidazole acetate ionic liquid and dimethyl sulfoxide mixed solution are under the action of ultrasound
It dissolves wool and extracts keratin, by centrifugation, supernatant is taken to be dialysed and be freeze-dried to obtain pure wool angle egg
White powder end.Method provided by the invention is easy to operate, the wool keratin purity is high of acquisition.
The specific technical proposal of the invention is: a kind of method for extracting wool keratin, in terms of g and mL, steps are as follows:
A) wool is taken to be added in ethyl alcohol, after stirring 1-3h, is rinsed and dried with deionized water.
B the wool for) taking 4-6g to dry is added in 9.6 buffer of CB with the bath raio of 1:18-20, and 1-1.4g sulfurous is added
Sour sodium reacts 25-35min at 55-65 DEG C, rinses 3-5 drying with deionized water.
The present invention carries out reduction pretreatment to wool using sodium sulfite, destroys scale layer, beats for the dissolution of subsequent wool
Open walk.
C step B) is taken) treated, and wool 1.8-2.2g immerses 18-22ml 1- ethyl-3-methylimidazole diethyl phosphate
In ionic liquid, the dimethyl sulfoxide of 20-25ml is added, is ultrasonically treated.
D 18-22ml 1- allyl -3- methylimidazole acetate ionic liquid) is added into step C) acquired solution, then
The dimethyl sulfoxide of 20-25ml is added, is ultrasonically treated.
Ionic liquid is a kind of green solvent, not can cause environmental pollution.The present invention uses two kinds of ionic liquids, 1- second
Base -3- methylimidazole diethyl phosphate ionic liquid and 1- allyl -3- methylimidazole acetate ionic liquid are able to
The hydrogen bond and disulfide bond in wool are efficiently opened, synergistic effect is played, to improve the recovery rate of wool keratin.
In addition, the present invention mixes dimethyl sulfoxide with ionic liquid, ion liquid system viscosity is advantageously reduced, is promoted
Wool dissolution, while the cost of ionic liquid can be reduced.
The present invention is ultrasonically treated dissolution system, increases the effect of physical shear, so that wool keratin be promoted to exist
Dissolution time is shortened in the dissolution of ionic liquid.
E) by step D) acquired solution centrifugal treating, centrifugation rate 7000-8000r/min, centrifugation time 8-
12min takes supernatant liquor.
F supernatant) is packed into bag filter dialysis, is freeze-dried, grinding obtains wool keratin.
Preferably, step A) in, it weighs 8-12g wool and is added in 180-200ml ethyl alcohol, stir 2h at 40 DEG C
Afterwards, 3-5 drying is rinsed with deionized water.
Preferably, step C) in, the preparation method of 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid are as follows:
N- methylimidazole and triethyl phosphate are mixed to join in round-bottomed flask by 1:1.1 molar ratio, heats and stirs at 130-150 DEG C
Reaction 10-15h is mixed, products therefrom is washed repeatedly with ether and separated with separatory funnel, lower layer's liquid phase is revolved with Rotary Evaporators
It is dried in vacuo 1-3 days after steaming 3-5h.
Preferably, step D) in, the preparation method of 1- allyl -3- methylimidazole acetate ionic liquid are as follows: by N-
Methylimidazole and allyl chloride are mixed by 1:1.2 molar ratio, in a nitrogen environment 50-60 DEG C of heating water bath reflux, while mechanical
Stir 1h, with acetone washing three times after, 0.8-1.2h is rotated at 65-75 DEG C, is finally dried in vacuo 1-3 days at 75-85 DEG C.
Preferably, step C) and step D) in, ultrasonic power 260-300W, ultrasonic time 25-30min.
Preferably, step F) in, the molecule interception of bag filter is 4000, and every 5-7h changes a water in dialysis procedure,
Dialysis 2-3 days.
It is compared with the prior art, the beneficial effects of the present invention are:
(1) present invention carries out reduction pretreatment with sodium sulfite to it when extracting wool keratin, destroys scale layer, is subsequent
Wool dissolution open channel.
(2) present invention uses two kinds of ionic liquids, 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid and 1-
Allyl -3- methylimidazole acetate ionic liquid is able to efficiently open the hydrogen bond and disulfide bond in wool, plays collaboration
Effect, to improve the recovery rate of wool keratin.
(3) present invention is ultrasonically treated wool dissolution system, increases the effect of physical shear, to promote wool angle
Albumen shortens dissolution time in the dissolution of ionic liquid.
(4) ionic liquid that the present invention uses is a kind of green solvent, environmentally friendly, may be recovered recycling.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1:
A method of extracting wool keratin, comprising the following steps:
A it) weighs 8g wool to be added in 180ml ethyl alcohol, after stirring 2h at 40 DEG C, rinses 3 drying with deionized water.
B) take 5g step A) in dry wool be added in 9.6 buffer of CB with the bath raio of 1:18, be added 1g sulfurous
Sour sodium reacts 25min at 60 DEG C, rinses 3 drying with deionized water.
C) take step B) in treated wool 1.8g immerse 20ml 1- ethyl-3-methylimidazole diethyl phosphate salt from
Sub- liquid adds the dimethyl sulfoxide of 20ml, is ultrasonically treated, ultrasonic power 260W, ultrasonic time 25min.
Wherein, the preparation of 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid: by N- methylimidazole and tricresyl phosphate
Ethyl ester is mixed to join in round-bottomed flask by 1:1.1 molar ratio, and heating stirring reacts 12h, products therefrom ether at 140 DEG C
Washing is multiple and is separated with separatory funnel, is dried in vacuo two days after lower layer's liquid phase is rotated 4h with Rotary Evaporators.
D 20ml 1- allyl -3- methylimidazole acetate ionic liquid) is added in acquired solution in step C), is added
The dimethyl sulfoxide of 20ml, is ultrasonically treated, ultrasonic power 260W, ultrasonic time 25min.
Wherein, the preparation of 1- allyl -3- methylimidazole acetate ionic liquid: N- methylimidazole and allyl chloride are pressed
The mixing of 1:1.2 molar ratio, 55 DEG C of heating water bath reflux in a nitrogen environment, while mechanical stirring 1h, with acetone washing three times after,
0.8h is rotated at 70 DEG C, is finally dried in vacuo two days at 80 DEG C.
E) by gained mixed solution centrifugal treating in step D), centrifugation rate 7000r/min, centrifugation time 8min,
Take supernatant liquor.
F the supernatant in step E)) is packed into the bag filter that molecule interception is 4000, every 5h is changed once in dialysis procedure
Water is dialysed 2 days.Sample after drying is ground, wool keratin powder is obtained.
Embodiment 2:
A method of extracting wool keratin, comprising the following steps:
A it) weighs 10g wool to be added in 190ml ethyl alcohol, after stirring 2h at 40 DEG C, rinses 4 drying with deionized water.
B) take 5g step A) in dry wool be added in 9.6 buffer of CB with the bath raio of 1:19, be added 1.2g sulfurous
Sour sodium reacts 30min at 60 DEG C, rinses 4 drying with deionized water.
C) take step B) in treated wool 2g immerse 20ml 1- ethyl-3-methylimidazole diethyl phosphate salt ion
Liquid adds the dimethyl sulfoxide of 23ml, is ultrasonically treated, ultrasonic power 280W, ultrasonic time 27min.
Wherein, the preparation of 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid: by N- methylimidazole and tricresyl phosphate
Ethyl ester is mixed to join in round-bottomed flask by 1:1.1 molar ratio, and heating stirring reacts 12h, products therefrom ether at 140 DEG C
Washing is multiple and is separated with separatory funnel, is dried in vacuo two days after lower layer's liquid phase is rotated 4h with Rotary Evaporators.
D 20ml 1- allyl -3- methylimidazole acetate ionic liquid) is added in acquired solution in step C), is added
The dimethyl sulfoxide of 23ml, is ultrasonically treated, ultrasonic power 280W, ultrasonic time 27min.
Wherein, the preparation of 1- allyl -3- methylimidazole acetate ionic liquid: N- methylimidazole and allyl chloride are pressed
The mixing of 1:1.2 molar ratio, 55 DEG C of heating water bath reflux in a nitrogen environment, while mechanical stirring 1h, with acetone washing three times after,
1h is rotated at 70 DEG C, is finally dried in vacuo two days at 80 DEG C.
E) by gained mixed solution centrifugal treating in step D), centrifugation rate 7500r/min, centrifugation time 10min,
Take supernatant liquor.
F the supernatant in step E)) is packed into the bag filter that molecule interception is 4000, every 6h is changed once in dialysis procedure
Water is dialysed 2.5 days.Sample after drying is ground, wool keratin powder is obtained.
Embodiment 3:
A method of extracting wool keratin, comprising the following steps:
A it) weighs 12g wool to be added in 200ml ethyl alcohol, after stirring 2h at 40 DEG C, rinses 5 drying with deionized water.
B) take 5g step A) in the wool dried be added in 9.6 buffer of CB with the bath raio of 1:20, it is sub- that 1.4g is added
Sodium sulphate reacts 35min at 60 DEG C, rinses 5 drying with deionized water.
C) take step B) in treated wool 2.2g immerse 20ml 1- ethyl-3-methylimidazole diethyl phosphate salt from
Sub- liquid adds the dimethyl sulfoxide of 25ml, is ultrasonically treated, ultrasonic power 300W, ultrasonic time 30min.
Wherein, the preparation of 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid: by N- methylimidazole and tricresyl phosphate
Ethyl ester is mixed to join in round-bottomed flask by 1:1.1 molar ratio, and heating stirring reacts 12h, products therefrom ether at 140 DEG C
Washing is multiple and is separated with separatory funnel, is dried in vacuo two days after lower layer's liquid phase is rotated 4h with Rotary Evaporators.
D 20ml 1- allyl -3- methylimidazole acetate ionic liquid) is added in acquired solution in step C), is added
The dimethyl sulfoxide of 25ml, is ultrasonically treated, ultrasonic power 300W, ultrasonic time 30min.
Wherein, the preparation of 1- allyl -3- methylimidazole acetate ionic liquid: N- methylimidazole and allyl chloride are pressed
The mixing of 1:1.2 molar ratio, 55 DEG C of heating water bath reflux in a nitrogen environment, while mechanical stirring 1h, with acetone washing three times after,
1.2h is rotated at 70 DEG C, is finally dried in vacuo two days at 80 DEG C.
E) by gained mixed solution centrifugal treating, centrifugation rate 8000r/min, centrifugation time 8- in step D)
12min takes supernatant liquor.
F the supernatant in step E)) is packed into the bag filter that molecule interception is 4000, every 5-7h changes one in dialysis procedure
Secondary water is dialysed 3 days.Sample after drying is ground, wool keratin powder is obtained.
Comparative example 1(uses single ionic liquid: 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid)
A method of extracting wool keratin, comprising the following steps:
A it) weighs 8g wool to be added in 180ml ethyl alcohol, after stirring 2h at 40 DEG C, rinses 3 drying with deionized water.
B) take 5g step A) in dry wool be added in 9.6 buffer of CB with the bath raio of 1:18, be added 1g sulfurous
Sour sodium reacts 25min at 60 DEG C, rinses 3 drying with deionized water.
C) take step B) in treated wool 1.8g immerse 40ml 1- ethyl-3-methylimidazole diethyl phosphate salt from
Sub- liquid adds the dimethyl sulfoxide of 40ml, is ultrasonically treated, ultrasonic power 260W, ultrasonic time 50min.
Wherein, the preparation of 1- ethyl-3-methylimidazole diethyl phosphate ionic liquid: by N- methylimidazole and tricresyl phosphate
Ethyl ester is mixed to join in round-bottomed flask by 1:1.1 molar ratio, and heating stirring reacts 12h, products therefrom ether at 140 DEG C
Washing is multiple and is separated with separatory funnel, is dried in vacuo two days after lower layer's liquid phase is rotated 4h with Rotary Evaporators.
D) by gained mixed solution centrifugal treating in step C), centrifugation rate 7000r/min, centrifugation time 8min,
Take supernatant liquor.
E the supernatant in step D)) is packed into the bag filter that molecule interception is 4000, every 5h is changed once in dialysis procedure
Water is dialysed 2 days.Sample after drying is ground, wool keratin powder is obtained.
Comparative example 2(uses single ionic liquid: 1- allyl -3- methylimidazole acetate ionic liquid)
A method of extracting wool keratin, comprising the following steps:
A it) weighs 8g wool to be added in 180ml ethyl alcohol, after stirring 2h at 40 DEG C, rinses 3 drying with deionized water.
B) take 5g step A) in dry wool be added in 9.6 buffer of CB with the bath raio of 1:18, be added 1g sulfurous
Sour sodium reacts 25min at 60 DEG C, rinses 3 drying with deionized water.
C) take step B) in treated wool 1.8g immerse 40ml 1- allyl -3- methylimidazole acetate ion liquid
Body adds the dimethyl sulfoxide of 40ml, is ultrasonically treated, ultrasonic power 260W, ultrasonic time 50min.
Wherein, the preparation of 1- allyl -3- methylimidazole acetate ionic liquid: N- methylimidazole and allyl chloride are pressed
The mixing of 1:1.2 molar ratio, 55 DEG C of heating water bath reflux in a nitrogen environment, while mechanical stirring 1h, with acetone washing three times after,
0.8h is rotated at 70 DEG C, is finally dried in vacuo two days at 80 DEG C.
D) by gained mixed solution centrifugal treating in step C), centrifugation rate 7000r/min, centrifugation time 8min,
Take supernatant liquor.
E the supernatant in step D)) is packed into the bag filter that molecule interception is 4000, every 5h is changed once in dialysis procedure
Water is dialysed 2 days.Sample after drying is ground, wool keratin powder is obtained.
Recovery rate comparison:
It is 81.2% that embodiment 1 and the wool keratin extract powder of comparative example 1-2, which are respectively as follows: embodiment 1,；Comparative example 1 is
62.2%；Comparative example 2 is 71.6%.
By comparing it is found that the recovery rate of embodiment 1 achieves significant progress relative to comparative example 1-2.The present inventor
Know, in the prior art, using other as solvent can obtain higher recovery rate, but using the advantage of ionic liquid is more
Added with conducive to the subsequent processing of keratin, modified, regeneration.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (6)
1. a kind of method for extracting wool keratin, which is characterized in that in terms of g and mL, steps are as follows:
A) wool is taken to be added in ethyl alcohol, after stirring 1-3h, is rinsed and dried with deionized water；
B the wool for) taking 4-6g to dry is added in 9.6 buffer of CB with the bath raio of 1:18-20, and 1-1.4g sulfurous acid is added
Sodium reacts 25-35min at 55-65 DEG C, rinses 3-5 drying with deionized water；
C) take step B) treated wool 1.8-2.2g immerse 18-22ml 1- ethyl-3-methylimidazole diethyl phosphate salt from
In sub- liquid, the dimethyl sulfoxide of 20-25ml is added, is ultrasonically treated；
D 18-22ml 1- allyl -3- methylimidazole acetate ionic liquid) is added into step C) acquired solution, adds
The dimethyl sulfoxide of 20-25ml, is ultrasonically treated；
E) by step D) acquired solution centrifugal treating, centrifugation rate 7000-8000r/min, centrifugation time 8-12min are taken
Supernatant liquor；
F supernatant) is packed into bag filter dialysis, is freeze-dried, grinding obtains wool keratin.
2. a kind of method for extracting wool keratin as described in claim 1, which is characterized in that step A) in, weigh 8-
12g wool is added in 180-200ml ethyl alcohol, after stirring 2h at 40 DEG C, rinses 3-5 drying with deionized water.
3. a kind of method for extracting wool keratin as described in claim 1, which is characterized in that step C) in, 1- ethyl-
The preparation method of 3- methylimidazole diethyl phosphate ionic liquid are as follows: N- methylimidazole and triethyl phosphate rub by 1:1.1
You are mixed to join in round-bottomed flask ratio, and heating stirring reacts 10-15h at 130-150 DEG C, and products therefrom is washed more with ether
It is secondary and separated with separatory funnel, it is dried in vacuo 1-3 days after lower layer's liquid phase is rotated 3-5h with Rotary Evaporators.
4. a kind of method for extracting wool keratin as described in claim 1, which is characterized in that step D) in, 1- allyl
The preparation method of base -3- methylimidazole acetate ionic liquid are as follows: mix N- methylimidazole and allyl chloride by 1:1.2 molar ratio
Close, in a nitrogen environment 50-60 DEG C of heating water bath reflux, while mechanical stirring 1h, with acetone washing three times after, at 65-75 DEG C
Lower revolving 0.8-1.2h is finally dried in vacuo 1-3 days at 75-85 DEG C.
5. a kind of method for extracting wool keratin as described in claim 1, which is characterized in that step C) and step D) in,
Ultrasonic power is 260-300W, ultrasonic time 25-30min.
6. a kind of method for extracting wool keratin as described in claim 1, which is characterized in that step F) in, bag filter
Molecule interception is 4000, and every 5-7h changes a water in dialysis procedure, is dialysed 2-3 days.
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| CN201811028704.4A CN109111516B (en) | 2018-09-05 | 2018-09-05 | Method for extracting wool keratin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110106706A (en) * | 2019-05-23 | 2019-08-09 | 叶盛 | A kind of preparation method of modified protein UV resistance finishing agent |
| CN114318865A (en) * | 2021-12-30 | 2022-04-12 | 江南大学 | Wool pretreatment liquid and application thereof |
| CN114456253A (en) * | 2022-03-01 | 2022-05-10 | 上海天同纺织科技有限公司 | Waste wool dissolving and keratin extracting process |
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| CN105399809A (en) * | 2015-12-28 | 2016-03-16 | 嘉兴学院 | Wool keratin extraction method |
| CN105970346A (en) * | 2016-05-26 | 2016-09-28 | 中国科学院过程工程研究所 | Method for preparing spinning solutions by dissolving animal hair and polymer assistants simultaneously with heterocyclic and dicyclic ionic liquid |
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| CN105399809A (en) * | 2015-12-28 | 2016-03-16 | 嘉兴学院 | Wool keratin extraction method |
| CN105970346A (en) * | 2016-05-26 | 2016-09-28 | 中国科学院过程工程研究所 | Method for preparing spinning solutions by dissolving animal hair and polymer assistants simultaneously with heterocyclic and dicyclic ionic liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106706A (en) * | 2019-05-23 | 2019-08-09 | 叶盛 | A kind of preparation method of modified protein UV resistance finishing agent |
| CN114318865A (en) * | 2021-12-30 | 2022-04-12 | 江南大学 | Wool pretreatment liquid and application thereof |
| CN114318865B (en) * | 2021-12-30 | 2022-12-27 | 江南大学 | Wool pretreatment liquid and application thereof |
| CN114456253A (en) * | 2022-03-01 | 2022-05-10 | 上海天同纺织科技有限公司 | Waste wool dissolving and keratin extracting process |
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