CN102199650A - Instant sericin powder and preparation method thereof - Google Patents
Instant sericin powder and preparation method thereof Download PDFInfo
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- CN102199650A CN102199650A CN2008103049315A CN200810304931A CN102199650A CN 102199650 A CN102199650 A CN 102199650A CN 2008103049315 A CN2008103049315 A CN 2008103049315A CN 200810304931 A CN200810304931 A CN 200810304931A CN 102199650 A CN102199650 A CN 102199650A
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Abstract
The invention relates to sericin powder, in particular to sericin powder instantly soluble in water and a preparation method thereof. The sericin powder can be prepared from husks, waste silk, light defective cocoons and the like. The method comprises the following steps of: purifying sericin solution obtained after silk is degummed, decolorizing, degrading, classifying, concentrating, deodorizing, and spray-drying to obtain instant sericin powder. The instant sericin powder has high dissolubility in cold water, and is quite different from sericin of cocoon silk. By the technical scheme, the instant sericin powder with high purity can be extracted from the discharged sericin solution, so that the pollution of sericin sewage to the environment can be effectively prevented; and specifically the instant sericin powder serving as a nutrition additive for high-grade cosmetics has broad development prospect.
Description
Technical field
The present invention relates to a kind of sericin powder, sericin powder and manufacture method thereof that particularly a kind of speed is water-soluble, this sericin powder can adopt husks, waste silk, light defective cocoon etc. to make for raw material.
Background technology
The main body of silk fiber is a fibroin, and silk gum is coated on the fibroin periphery, and fibroin is played provide protection and adhesive action, and it can prevent that because of weaving the damage of friction to silky fibre therefore, general silk weaving article will be to dyeing, just silk gum all being purified when putting in order.The sericin that in the concise liquid sewage of silk white silk dye-works and silk spinning factory, contains very high concentrations, in the sewage that the cocoon cooking and the misty silk workshop of misty Silk Mill give off, also contain a large amount of silk gum, allow it flow into the dissolved oxygen of river course in can mass consumption water, make water body forfeiture self-purification capacity, destroy the environmental ecology balance.Simultaneously, in sewing silk, weaving process, also produce a large amount of husks (the sleave thread of silk cocoon periphery), waste silk, light defective cocoon etc., can only be as low-grade silk spinning raw material, its added value is not high.
Silk gum is a kind of fine protein, if can reclaim rightly but on the other hand,, can be used for playing effects such as health care, skin care, therefore in food, makeup even the medicine, people begin one's study recovery, the utilization of silk gum, and be not only as Pollution abatement.In this process, run into following problems: the one, existing Degumming method mainly is the High Temperature High Pressure method for degumming, because the temperature of coming unstuck is higher than 100 ℃, needs to adopt pressurized vessel, has increased facility investment and technology cost; Another kind of is to adopt the hot solution of alkaline substance such as soap, soda ash to realize coming unstuck, and its shortcoming is that salt is more in last product, causes the ash content of product big, can not be applicable to food, makeup.Second problem is that silk gum is a kind of globular proteins of macromolecule, more easily dissolves in hot water, but separates than indissoluble in cold water, forms a kind of jellylike gel when temperature is low easily, and is water-soluble relatively poor, the feasible relatively difficulty of using.Moreover, because environmental pollution at present is more serious, the residual amount of various objectionable impuritiess is more in the silk silk gum, the silk gum quality that makes with ordinary method is lower, the particularly content of heavy metal lead, mercury and objectionable impurities arsenic and bacterium index exceeding standard do not meet the healthy requirement of food, makeup, medicine material.The sericin powder that existing technology makes exists that purity is not high, color and luster is dark, solvability extreme difference in the cold water, and harmful substance contents is more, does not meet the defective of healthy requirement.
Summary of the invention
The purpose of this invention is to provide a kind of production high purity, solvability is fabulous in cold water, meets food, makeup, medicine material healthy requirement, and molecular weight is comparatively concentrated, does not have the manufacture method of the instantly-soluble sericin powder of enzyme stink.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
The manufacture method of instantly-soluble sericin powder is characterized in that, comprises the following steps: successively
(1) purify, come unstuck: with husks, waste silk, light defective cocoon is raw material, earlier to its removal of impurities, rinsing and silk gum swelling, adding degumming agent again comes unstuck, described degumming agent is the organic degumming agent of weakly alkaline, the pH value of degumming agent is 8～10, temperature is 90～100 ℃, and usually time is 100～200 minutes, obtains come unglued liquid;
(2) purify: in the solution that step 1 obtains, add the appropriate amount of acid neutralization, with ultra-fine filter desalination and once concentration;
(3) degraded adopts Sumizyme MP that silk gum solution is carried out enzymolysis, and enzyme dosage is 800～1000 unit of activity/milliliters, and hydrolysis temperature is 40～45 ℃, and the pH value is controlled at 10～10.5,45～60 minutes time;
(4) Jiang Xie product is by membrane separation plant, isolates molecular weight successively and be more than 40000, the parting liquid of 20000～40000,10000～20000,4000～10000 (dalton);
(5) be concentrated into 10% above percentage concentration respectively;
(6) respectively with concentrated solution by containing the filtration unit of orange peel powder;
(7) spraying drying obtains the instantly-soluble sericin powder.
As preferably, described husks, waste silk or light defective cocoon before coming unstuck, dipping 20 to 40 minutes in 30～35 ℃ dilute alkaline soln earlier, the abundant drip washing of water again makes the abundant swelling of silk gum on the husks.
As preferably, described degumming agent is organic amine or quaternary amine.
As preferably, between described step 2 and the step 3, can decolour to silk gum solution, described decolouring is, adds silk gum liquid and weighs 1～3% gac, and water temperature is controlled between 80～85 ℃, bleaching time 30～40 minutes is removed gac with the filter press device then.Wherein, the filter press device forms with diatomite earlier and helps filtering layer, is example with 15 square metres of pressure filters, and diatomaceous consumption is 15～25 kilograms.
As preferably, be coated with in the filter press device that is adopted by what diatomite formed and help filtering layer.
As preferably, the weight of orange peel powder is 0.1～2% of concentrated solution weight in the step 4.
As preferably, the described filtration unit of step 4 is the exchange resin column that contains described orange peel powder.
Sericin powder by aforesaid method obtains can get particle diameter less than 20 microns, and molecular weight is 2000～8000 dalton, total nitrogen content with the kilogram restatement greater than 14%.
As preferably, solubleness is greater than 18 grams in 8 ℃ cold water for above-mentioned sericin powder, and the solubleness in 100 ℃ hot water is greater than 96 grams.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. because the present invention has adopted the separating and filtering device processes that original molecular weight distribution product very extensive, that added value of product is lower has been become comparatively high-grade product, promoted the annex value of product;
2. because the present invention has adopted special orange peel powder as reodorant, removed in the product because the oxidized smell of enzyme has improved the quality of products obtained therefrom of the present invention as cosmetics of super quality raw material;
3. because the present invention carries out degradation treatment to silk gum, the sericin powder molecular weight distribution that obtains is 2000～8000 dalton, most of particle diameter is 10～15 microns, thereby the solubleness in cold water (8 ℃) is bigger more than 10 times than indissoluble sericin powder, has fabulous solvability;
4. the present invention adopts the organic degumming agent of weakly alkaline to the husks processing of coming unstuck, and the salt content in the final product is low, thereby the ash content that makes product is less than 4%;
5. the sericin powder that obtains of the present invention, because husks has been carried out pre-treatment, arsenic, plumbous equal size are low, are suitable for food, makeup and medicine material and use;
6. adopt technical scheme of the present invention, can from discharging silk gum waste liquid, extract highly purified instantly-soluble sericin powder, can effectively prevent of the pollution of silk gum sewage to environment, can be applied to the antioxidant and the medicine material of arrangement coating and makeup beautifying nourishing additive and lipid food behind the health-care textile thing again, have the wide development prospect.
Specific embodiment
This specific embodiment only is an explanation of the invention; it is not a limitation of the present invention; those skilled in the art can make the modification that does not have creative contribution to present embodiment as required after reading this specification sheets, but as long as all are subjected to the protection of patent law in claim scope of the present invention.
Embodiment: a kind of manufacture method of instantly-soluble sericin powder comprises the following steps: successively
(1) husks removal of impurities, rinsing and silk gum swelling thereof: the husks that peels from cocoon-peeling machine is open-textured silk floss and opens, before coming unstuck, the impurity that is adhering to must be removed husks, in order to remove the adherent dust of husks extexine, husks can be cleaned earlier in cold water, for impelling the abundant swelling dissolving of silk gum on the husks, can be immersed in 30～35 ℃ the dilute alkaline soln 30 minutes before husks comes unstuck, the abundant drip washing of water again can make the abundant swelling of silk gum on the husks.
(2) come unstuck: take by weighing 10 kilograms of husks, 100 kilograms in water, 0.1～0.2 kilogram of degumming agent, the pH value of adjusting degumming agent is 8～10, and the temperature of coming unstuck is 95～100 ℃, heats to come unstuck in 150 minutes, described degumming agent can adopt organic amine, husks reusable heat clear water after will coming unstuck soaks, and come unglued liquid and washings merge, and obtain insoluble silk gum solution;
(3) purification of silk gum solution adds the appropriate amount of acid neutralization in the solution that obtained in last step, make in the alkaline agent that comes unstuck and salify after, by a ultra-fine filter, desalination and once concentration;
(4) decolouring of silk gum solution: add silk gum liquid and weigh 1～3% gac, water temperature is controlled between 80～85 ℃, bleaching time 30 minutes, on the filter press device, help filtering layer earlier with a small amount of diatomite formation, and then remove gac with the filter press device, with skilful square metre pressure filter is example, and diatomaceous consumption is 15～25 kilograms.
(5) degraded of sericine: for the molecular weight control that makes the instantly-soluble sericin powder 2000～8000 dalton, adopt Sumizyme MP that silk gum solution is carried out enzymolysis, enzyme dosage is 800～1000 unit of activity/milliliters, hydrolysis temperature is 40～45 ℃, the pH value is controlled at 10～10.5,45～60 minutes time; (6) concentrating of silk gum solution: carry out spraying drying smoothly for making silk gum solution, must be with the silk gum solution concentration, adopt thin film concentrator, make the concentrated solution of the above percentage concentration of silk gum solution concentration to 10%: (7) spraying drying: adopt hig h-speed centrifugal spray drying device drying, inlet temperature is at 200～250 ℃, air outlet temperature obtains the instantly-soluble sericin powder at 70～80 ℃.
The instantly-soluble sericin powder that present embodiment obtains, particle diameter is less than 20 microns, and molecular weight is 2000～8000 dalton, and total nitrogen content is to do grammes per square metre greater than 14%.
Solubleness is greater than 18 grams in 8 ℃ cold water, and the solubleness in 100 ℃ hot water is greater than 96 grams.With instantly-soluble sericin powder and the contrast of indissoluble sericin powder that present embodiment obtains, the indissoluble sericin powder is directly the silk gum in the come unglued liquid to be made through concentrate drying, and its color and luster is lark, and foreign matter content is higher, and is water-soluble relatively poor; And instantly-soluble sericin powder appearance character be oyster white to micro-yellow powder, fabulous solvability is arranged in cold water, the content of lead, mercury, arsenic meets the healthy requirement of food, makeup, pharmaceutical raw material.See table, as seen, the solubleness of instantly-soluble sericin powder in cold water (8 ℃) is bigger more than 10 times than indissoluble sericin powder, wants big more than 4 times in hot water (100 ℃), the instantly-soluble sericin powder has fabulous solvability in cold water, will bring great convenience to use.
The solubleness of table 1 instantly-soluble sericin powder and indissoluble sericin powder relatively
By analysis, causing the instantly-soluble sericin powder that a fabulous deliquescent reason is arranged in cold water, is that its silk gum molecular weight is less, and it is as shown in table 2 to record the silk gum molecular weight with gel filtration method.In addition, particle form from electron microscope observation to the instantly-soluble sericin powder is spherical, overwhelming majority particle diameter is 10～15 microns, the largest particle diameter is no more than 20 microns, and indissoluble sericin powder average particulate diameter is 20～30 microns, and this also is to cause two kinds of silk gum solubleness that one of reason of notable difference is arranged.
The molecular weight ratio of table 2 instantly-soluble sericin powder and indissoluble sericin powder
(gel filtration method)
Claims (9)
1. the manufacture method of instantly-soluble sericin powder is characterized in that, comprises the following steps: successively
(1) purify, come unstuck: with husks, waste silk, light defective cocoon is raw material, earlier to its removal of impurities, rinsing and silk gum swelling, adding degumming agent again comes unstuck, described degumming agent is the organic degumming agent of weakly alkaline, the pH value of degumming agent is 8～10, temperature is 90～100 ℃, and usually time is 100～200 minutes, obtains come unglued liquid;
(2) purify: in the solution that step 1 obtains, add the appropriate amount of acid neutralization, with ultra-fine filter desalination and once concentration;
(3) degraded adopts Sumizyme MP that silk gum solution is carried out enzymolysis, and enzyme dosage is 800～1000 unit of activity/milliliters, and hydrolysis temperature is 40～45 ℃, and the pH value is controlled at 10～10.5,45～60 minutes time;
(4) Jiang Xie product is by membrane separation plant, isolates molecular weight successively and be more than 40000, the parting liquid of 20000～40000,10000～20000,4000～10000 (dalton);
(5) be concentrated into 10% above percentage concentration respectively;
(6) respectively with concentrated solution by containing the filtration unit of orange peel powder;
(7) spraying drying obtains the instantly-soluble sericin powder.
2. the manufacture method of instantly-soluble sericin powder according to claim 1 is characterized in that:
Described husks, waste silk or light defective cocoon flooded 20 to 40 minutes in 30～35 ℃ dilute alkaline soln earlier before coming unstuck, and the abundant drip washing of water again makes the abundant swelling of silk gum on the husks.
3. the manufacture method of instantly-soluble sericin powder according to claim 1 is characterized in that:
Described degumming agent is organic amine or quaternary amine.
4. the manufacture method of instantly-soluble sericin powder according to claim 1 is characterized in that:
Between described step 2 and the step 3, can decolour to silk gum solution, described decolouring is, adds silk gum liquid and weighs 1～3% gac, and water temperature is controlled between 80～85 ℃, and bleaching time 30～40 minutes is removed gac with the filter press device then.
5. the manufacture method of instantly-soluble sericin powder according to claim 4 is characterized in that: be coated with in the filter press device that is adopted by what diatomite formed and help filtering layer.
6. the manufacture method of instantly-soluble sericin powder according to claim 1 is characterized in that: the weight of orange peel powder is 0.1～2% of concentrated solution weight in the step 4.
7. the manufacture method of instantly-soluble sericin powder according to claim 1 is characterized in that: the described filtration unit of step 4 is the exchange resin column that contains described orange peel powder.
8. instantly-soluble sericin powder is characterized in that: obtained by the described method of claim 1, particle diameter is less than 20 microns, and molecular weight is 2000～8000 dalton, and total nitrogen content is to do grammes per square metre greater than 14%.
9. instantly-soluble sericin powder according to claim 8 is characterized in that: solubleness is greater than 18 grams in 8 ℃ cold water for described sericin powder, and the solubleness in 100 ℃ hot water is greater than 96 grams.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008103049315A CN102199650A (en) | 2008-10-15 | 2008-10-15 | Instant sericin powder and preparation method thereof |
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| CN2008103049315A CN102199650A (en) | 2008-10-15 | 2008-10-15 | Instant sericin powder and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301033A (en) * | 2013-05-30 | 2013-09-18 | 南通缘生堂生物科技有限公司 | Preparation method of ultramicro silk fibroin powder |
| CN105331661A (en) * | 2015-11-24 | 2016-02-17 | 浙江汇能生物股份有限公司 | Method for preparing sericin polypeptides with aqueous enzymatic method |
| CN108047322A (en) * | 2017-12-19 | 2018-05-18 | 上海祁稷新材料发展有限公司 | A kind of preparation method and application of sericin |
| CN108440662A (en) * | 2017-12-14 | 2018-08-24 | 重庆尚奕辉生物科技有限公司 | Sericin preparation process and application thereof |
-
2008
- 2008-10-15 CN CN2008103049315A patent/CN102199650A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301033A (en) * | 2013-05-30 | 2013-09-18 | 南通缘生堂生物科技有限公司 | Preparation method of ultramicro silk fibroin powder |
| CN103301033B (en) * | 2013-05-30 | 2015-03-25 | 南通缘生堂生物科技有限公司 | Preparation method of ultramicro silk fibroin powder |
| CN105331661A (en) * | 2015-11-24 | 2016-02-17 | 浙江汇能生物股份有限公司 | Method for preparing sericin polypeptides with aqueous enzymatic method |
| CN108440662A (en) * | 2017-12-14 | 2018-08-24 | 重庆尚奕辉生物科技有限公司 | Sericin preparation process and application thereof |
| CN108047322A (en) * | 2017-12-19 | 2018-05-18 | 上海祁稷新材料发展有限公司 | A kind of preparation method and application of sericin |
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Open date: 20110928 |