CN1219118C - Quick dissolving sericin powder and its making method - Google Patents

Quick dissolving sericin powder and its making method Download PDF

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Publication number
CN1219118C
CN1219118C CNB031506526A CN03150652A CN1219118C CN 1219118 C CN1219118 C CN 1219118C CN B031506526 A CNB031506526 A CN B031506526A CN 03150652 A CN03150652 A CN 03150652A CN 1219118 C CN1219118 C CN 1219118C
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China
Prior art keywords
sericin powder
sericin
instant capacity
silk
silk gum
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Expired - Fee Related
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CN1493722A (en
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盛家镛
沈新琦
胡汉清
陈义璋
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AOTESI BIOCHEMISTRY IND Co Ltd HUZHOU
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AOTESI BIOCHEMISTRY IND Co Ltd HUZHOU
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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Abstract

The present invention relates to a quick dissolving sericin powder and a manufacturing method thereof. A sericin solution after silk degumming is purified, decolorized, degraded, condensed and dried by spraying to manufacture the quick dissolving sericin powder with good solubility in cooling water and obvious differences from cocoon silk sericin. By adopting the technical scheme, the quick dissolving sericin powder with high purity can be extracted from the discharged sericin solution, and the environmental pollution caused by sericin sewage can be effectively prevented. The quick dissolving sericin powder can be used for after-treating coating of health-care textiles, nutrition additives of cosmetics for facial beautification, antioxidants for oil and fat food and raw materials of medicine, and the quick dissolving sericin powder has wide developing prospect.

Description

Instant capacity sericin powder and manufacture method thereof
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 protective effect and adhesive action, and it can prevent that because of weaving the damage of friction to silk fiber 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 filature workshop of reeling mill give off, also contain a large amount of silk gum, allow it flow into the dissolved oxygen of river course in can a large amount of consume water, make water body forfeiture self-purification capacity, destroy the environmental ecology balance.
Simultaneously, in filature, 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 protein of high-quality, if can reclaim rightly but on the other hand,, can be used for playing effects such as health care, skin care, therefore in food, cosmetics even the medicine, people begin one's study recovery, the utilization of silk gum, and be not only as pollution control.
In this process, run into following problems: the one, existing Degumming method mainly is the High Temperature High Pressure degumming method, because the temperature of coming unstuck is higher than 100 ℃, needs to adopt pressure vessel, has increased equipment investment and technology cost; Another kind of is to adopt the hot solution of basic species 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, cosmetics.Second problem is that silk gum is a kind of globular protein of macromolecule, more easily dissolves in hot water, but separates than indissoluble in cold water, forms a kind of gel that freezes shape 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 harmful substances is more in the silk silk gum, the silk gum quality that makes with conventional method is lower, the particularly content of heavy metal lead, mercury and harmful substance arsenic and bacterium index exceeding standard do not meet the healthy requirement of food, cosmetics, medicine material.
Thus, the sericin powder that existing technology makes exists that purity is not high, color and luster is dark, dissolubility 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 instant capacity sericin powder of the purpose of this invention is to provide a kind of high-purity, dissolubility is fabulous in cold water meets food, cosmetics, medicine material healthy requirement; Another object of the present invention provides the manufacture method of this sericin powder.
For achieving the above object, the technical solution used in the present invention is: a kind of manufacture method of instant capacity sericin powder comprises the following steps: successively
(1) be raw material with husks, waste silk, light defective cocoon, earlier to its removal of impurities, rinsing and silk gum swelling, add degumming agent again and come unstuck that the condition of coming unstuck is, the pH value of degumming agent is 8~10, and temperature is 90~100 ℃, and usually time is 100~200 minutes, the acquisition degumming baths;
(2) purify, in the solution that step 1 obtains, add the appropriate amount of acid neutralization, with ultrafilter desalination and once concentration;
(3) degraded adopts alkali protease 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) be concentrated into 10% above percent concentration;
(5) spray drying obtains the instant capacity sericin powder.
In the technique scheme, spray-dired EAT is at 200~250 ℃, and leaving air temp is at 70~80 ℃.
In the technique scheme, described husks 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.
In the technique scheme, preferred degumming agent is the organic degumming agent of alkalescent, for example, and organic amine or quaternary amine.
In the technique scheme, for avoiding color problem, 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% active carbon, and water temperature is controlled between 80~85 ℃, bleaching time 30~40 minutes, remove active carbon with the plate compression device, wherein, the plate compression device forms with diatomite earlier and helps filtering layer, with 15 square metres of pressure filters is example, and diatomaceous consumption is 15~25 kilograms.
Utilize a kind of instant capacity sericin powder of the method acquisition of technique scheme, 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%.
Solubility is greater than 18 grams in 8 ℃ cold water for described sericin powder, and the solubility 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 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 solubility in cold water (8 ℃) is bigger more than 10 times than indissoluble sericin powder, has fabulous dissolubility.
2. the present invention adopts the organic degumming agent of alkalescent to the husks processing of coming unstuck, and the salt content in the end product is low, thereby the ash content that makes product is less than 4%.
3. the sericin powder that obtains of the present invention, because husks has been carried out preliminary treatment, arsenic, plumbous equal size are low, are suitable for food, cosmetics and medicine material and use.
4. adopt technical scheme of the present invention, can from discharging silk gum waste liquid, extract highly purified instant capacity 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 cosmetics beautifying nourishing additive and grease based food behind the health-care textile thing again, have the wide development prospect.
The specific embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one: a kind of manufacture method of instant capacity 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 dust that the husks extexine adheres to, 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 degumming baths and cleaning solution merge, and obtain slightly solubility 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 ultrafilter, desalination and once concentration;
(4) decolouring of silk gum solution: add silk gum liquid and weigh 1~3% active carbon, water temperature is controlled between 80~85 ℃, bleaching time 30 minutes, on the plate compression device, help filtering layer earlier with a small amount of diatomite formation, and then remove active carbon with the plate compression device, with 15 square metres pressure filters is example, and diatomaceous consumption is 15~25 kilograms.
(5) degraded of sericine: for the molecular weight that makes the instant capacity sericin powder is controlled at 2000~8000 dalton, adopt alkali protease 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 spray drying smoothly for making silk gum solution, the silk gum solution concentration must be adopted thin film concentrator, make the concentrate of the above percent concentration of silk gum solution concentration to 10%;
(7) spray drying: adopt hig h-speed centrifugal spray drying device drying, EAT is at 200~250 ℃, and leaving air temp obtains the instant capacity sericin powder at 70~80 ℃.
The instant capacity 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%.
Solubility is greater than 18 grams in 8 ℃ cold water, and the solubility in 100 ℃ hot water is greater than 96 grams.
With instant capacity sericin powder and the contrast of indissoluble sericin powder that present embodiment obtains, the indissoluble sericin powder is directly the silk gum in the degumming baths to be made through concentrate drying, and its color and luster is lark, and impurity content is higher, and is water-soluble relatively poor; And instant capacity sericin powder appearance character be oyster white to micro-yellow powder, fabulous dissolubility is arranged in cold water, the content of lead, mercury, arsenic meets the healthy requirement of food, cosmetics, pharmaceutical raw material.
See table, as seen, the solubility of instant capacity 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 instant capacity sericin powder has fabulous dissolubility in cold water, will bring great convenience to use.
The solubility of table 1 instant capacity sericin powder and indissoluble sericin powder relatively
The silk gum kind Cold water (8 ℃) solubility (g) Hot water (100 ℃) solubility (g)
Instant capacity sericin powder indissoluble sericin powder 18.05 1.80 96.25 23.15
By analysis, causing the instant capacity 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.
In addition, particle shape from electron microscope observation to the instant capacity sericin powder is spherical, overwhelming majority particle diameter is 10~15 microns, the largest particles 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 solubility that one of reason of notable difference is arranged.
The molecular weight ratio of table 2 instant capacity sericin powder and indissoluble sericin powder
(gel filtration)
The silk gum kind Mean molecule quantity (dalton) Molecular weight distribution (dalton)
Instant capacity sericin powder indissoluble sericin powder 5500 76000 2000~8000 60000~98000

Claims (7)

1. the manufacture method of an instant capacity sericin powder is characterized in that, comprises the following steps: successively
(1) is raw material with husks, waste silk, light defective cocoon,, adds degumming agent again and come unstuck earlier to its removal of impurities, rinsing and silk gum swelling, described degumming agent is the organic degumming agent of alkalescent, and the pH value of degumming agent is 8~10, and temperature is 90~100 ℃, usually time is 100~200 minutes, obtains degumming baths;
(2) purify, in the solution that step 1 obtains, add the appropriate amount of acid neutralization, with ultrafilter desalination and once concentration;
(3) degraded adopts alkali protease 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) be concentrated into 10% above percent concentration;
(5) spray drying obtains the instant capacity sericin powder.
2. the manufacture method of instant capacity sericin powder according to claim 1, it is characterized in that: described husks, waste silk or light defective cocoon are before coming unstuck, flooded 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.
3. the manufacture method of instant capacity sericin powder according to claim 1 is characterized in that: described degumming agent is organic amine or quaternary amine.
4. the manufacture method of instant capacity sericin powder according to claim 1, it is characterized in that: between described step 2 and the step 3, can decolour to silk gum solution, described decolouring is, add silk gum liquid and weigh 1~3% active carbon, water temperature is controlled between 80~85 ℃, and bleaching time 30~40 minutes is removed active carbon with the plate compression device then.
5. the manufacture method of instant capacity sericin powder according to claim 4 is characterized in that: be coated with in the plate compression device that is adopted by what diatomite formed and help filtering layer.
6. instant capacity 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%.
7. instant capacity sericin powder according to claim 7 is characterized in that: solubility is greater than 18 grams in 8 ℃ cold water for described sericin powder, and the solubility in 100 ℃ hot water is greater than 96 grams.
CNB031506526A 2003-08-29 2003-08-29 Quick dissolving sericin powder and its making method Expired - Fee Related CN1219118C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100376170C (en) * 2006-04-06 2008-03-26 浙江省农业科学院 Edible watural silk protein powder and preparation method of natural silk extract
CN102250995A (en) * 2011-03-25 2011-11-23 兴化市大地蓝绢纺有限公司 Method for degumming from silk spinning raw material and recovering sericin

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999545B (en) * 2007-01-12 2010-09-08 东华大学 Process of recovering sericine by ion exchanging
CN101849605B (en) * 2010-05-17 2012-07-18 湖州澳特丝生物科技有限公司 Preparation method of silkworm pupa high zinc protein powder
CN102559824B (en) * 2012-01-11 2014-10-22 湖州南方生物科技有限公司 Sericin for biological material and preparation method thereof
CN103262912B (en) * 2013-06-15 2014-10-15 杭州鹏龙科技有限公司 Process for producing novel nutrient health-care edible oil
CN103627367B (en) * 2013-11-29 2016-03-30 郝飞麟 A kind of environment-protective adhesive and its preparation method and application

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100376170C (en) * 2006-04-06 2008-03-26 浙江省农业科学院 Edible watural silk protein powder and preparation method of natural silk extract
CN102250995A (en) * 2011-03-25 2011-11-23 兴化市大地蓝绢纺有限公司 Method for degumming from silk spinning raw material and recovering sericin
CN102250995B (en) * 2011-03-25 2012-07-04 兴化市大地蓝绢纺有限公司 Method for degumming from silk spinning raw material and recovering sericin

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