CN103242440A

CN103242440A - Sericin extracting method

Info

Publication number: CN103242440A
Application number: CN2013101591004A
Authority: CN
Inventors: 潘大东
Original assignee: GUANGXI LI SHENG COCOON SILK CO Ltd
Current assignee: GUANGXI LI SHENG COCOON SILK CO Ltd
Priority date: 2013-05-03
Filing date: 2013-05-03
Publication date: 2013-08-14
Anticipated expiration: 2033-05-03
Also published as: CN103242440B

Abstract

The invention is applicable to the field of compound extraction, and provides a sericin extracting method. The method comprises the following steps of: filtering silk wastewater, adjusting the temperature and PH value of the filtered solution, adding polyacrylamide powder into the filtered solution, fully stirring the obtained mixture, and standing the obtained mixture so as to generate a flocculate; stirring the flocculate for dissolving by using distilled water, removing polyacrylamide through reduced-pressure distillation, and obtaining coarse sericin powder by using a spray drying method; adding deionized water and anhydrous ethanol pre-cooled at a temperature of minus 15 DEG C in the coarse sericin powder, fully stirring the obtained mixture, and standing the mixture; carrying out centrifugation on the mixture so as to obtain a precipitate, dissolving the precipitate by using distilled water, and removing ethanol through reduced pressure distillation; carrying out freeze drying on the obtained product so as to obtain pure sericin powder. According to the invention, silk wastewater is precipitated by using polyacrylamide, so that the required cost for wastewater concentration is saved; an organic solvent is reacted under low-temperature conditions, so that the biological activity of sericin protein is not destroyed; and the method is simple, easy to operate, environment-friendly, and high in sericin recovery rate and purity.

Description

A kind of silk gum extracting method

Technical field

The present invention is applicable to that compound extracts the field, relates in particular to a kind of silk gum extracting method.

Background technology

Organic solvent method is to extract one of silk gum method commonly used from silk waste water, and it mainly is to add ethanol or acetone and other organic solvent in waste water, destroys protein water body hydration layer on every side with this, makes it take off steady sedimentation.

The silk broadcloth degumming waste water water yield is very big in the prior art, isolate silk gum under the effect of organic solvent, at first will remove most moisture, make concentrated solution.Adopt general concentrate drying method, treatment capacity is big, the time is long, and its cost consumption also can increase greatly, and industrial applicibility is not strong.So, a kind of method that effectively concentrates silk gum waste water must be arranged, could reduce organic solvent method and extract the cost of silk gum aspect suitability for industrialized production.

Summary of the invention

The invention provides a kind of silk gum extracting method, be intended to solve the rate of recovery of silk gum in the prior art and the cost height of purity and extraction silk gum, the problem that industrial applicibility is not strong.

The embodiment of the invention provides a kind of silk gum extracting method, said method comprising the steps of:

Filter silk waste water, and regulate temperature and the pH value that filters back solution, add the polyacrylamide powder, fully stir, leave standstill the back and generate throw out;

Described throw out is fused with the distilled water stirring, remove polyacrylamide and obtain the silk gum coarse meal with spray-drying process by underpressure distillation;

In described silk gum coarse meal, add deionized water, under-15 ℃ of temperature the dehydrated alcohol of pre-freeze, leave standstill after fully stirring;

Centrifugal back produces throw out, with described throw out dissolved in distilled water, removes ethanol by underpressure distillation;

Lyophilize obtains pure silk gum powder.

The embodiment of the invention makes the silk wastewater sedimentation by utilizing polyacrylamide, saved the required cost of concentrated waste water, organic solvent reacts under low-temperature condition, and the biological activity of sericin is not destroyed, simple, the easy to operate and environmental protection of this method, all very high for the rate of recovery and the purity of silk gum.

Description of drawings

Fig. 1 represents the method flow diagram of the extraction silk gum that the embodiment of the invention provides.

Embodiment

In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explaining the present invention, and be not used in restriction the present invention.

Fig. 1 shows the method flow of the extraction silk gum that the embodiment of the invention provides, and details are as follows:

In step S101, filter silk waste water, and regulate temperature and the pH value that filters back solution, add the polyacrylamide powder, fully stir, leave standstill the back and generate throw out;

In an embodiment of the present invention, be 50-80 ℃ with the temperature regulation of filtering back solution, pH value is adjusted to 7-9.

Polyacrylamide is high molecular weight water soluble polymer, is insoluble to most of organic solvents, has good flocculence, can reduce the frictional resistance between the liquid.Polyacrylamide itself and hydrolysis body thereof do not have toxicity, and the toxicity of polyacrylamide is from its residual monomer acrylamide (AN).Acrylamide is the agent of nervosa intoxicating, and neural system is had damaging action, and it is unable to show human body after the poisoning, symptoms such as ataxia.Therefore all there is residual acrylamide content in the regulation polyacrylamide Industrial products in various countries hygiene department, is generally 0.5%-0.05%.When polyacrylamide is used for the purifying treatment aspect of industry and municipal effluent, generally allow acrylamide content below 0.2%, when being used for the direct drinking water processing, acrylamide content needs below 0.05%.

As a preferred embodiment of the present invention, the polyacrylamide powder of adding accounts for and filters back silk gum wastewater quality 0.5-0.8%, fully stirs 15-20 minute, leaves standstill afterwards and produces throw out in 2-5 hour.

In step S102, throw out is fused with the distilled water stirring, remove polyacrylamide and obtain the silk gum coarse meal with spray-drying process by underpressure distillation;

Take out throw out, add distilled water and mix, mixing the back strength of solution is about 30%, and polyacrylamide is soluble in water, uses distillation under vacuum that it is removed.

In step S103, in the silk gum coarse meal, add deionized water, under-15 ℃ of temperature the dehydrated alcohol of pre-freeze, leave standstill after fully stirring;

In an embodiment of the present invention, the mass ratio of the dehydrated alcohol of adding, deionized water and silk gum coarse meal is 70: 250: 25, fully stirs fusedly, rests in-15 ℃ the environment 12-24 hour then.

In step S104, centrifugal back produces throw out, with the throw out dissolved in distilled water, removes ethanol by underpressure distillation;

In an embodiment of the present invention, solution is through centrifugal 30 seconds of 5000 rev/mins of refrigerated centrifuges, and using then with silk gum coarse meal mass ratio is 8: 25 dissolved in distilled water precipitation, and then ethanol is removed in underpressure distillation.

In step S105, lyophilize obtains pure silk gum powder.

Embodiment one:

1. with silk waste water 100Kg strainer filtering;

2. the solution temperature after will filtering is adjusted to 70 ℃, and pH value is adjusted to 8, adds the polyacrylamide powder of 0.5kg, fully stirs 20 minutes, leaves standstill then 3 hours;

3. the throw out that forms in the taking-up waste water adds distilled water and fully stirs, and the allotment strength of solution is about 30%;

4. with the polyacrylamide in the distillation under vacuum removal solution, make silk gum coarse meal 8.42kg with spray-drying process then;

5. in the silk gum coarse meal, add the dehydrated alcohol 23.7kg of pre-freeze under deionized water 85kg ,-15 ℃ of environment, stirred 15 minutes, rest in-15 ℃ the environment 12 hours then;

6. solution produced precipitation in centrifugal 30 seconds through refrigerated centrifuge 5000r/min, and with the dissolved in distilled water precipitation of 2.8kg, then ethanol is removed in underpressure distillation then;

7. the solution lyophilize is made pure silk gum powder 7.46kg.

More than the silk gum extraction rate reached to 85%.With polyacrylamide precipitation silk waste water, again with the dry silk gum coarse meal that produces of spray-drying process, its production cost will be well below existing method behind the formation throw out.So the inventive method all is fit to be applied to suitability for industrialized production on no matter still being the angle of efficient from cost.

The embodiment of the invention makes the silk wastewater sedimentation by utilizing polyacrylamide, has saved the required cost of concentrated waste water; Organic solvent reacts under low-temperature condition, and the biological activity of sericin is not destroyed.The inventive method technology does not simply pollute again.The silk gum rate of recovery is higher, and silk gum purity height, the good water solubility extracted.

The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims

1. a silk gum extracting method is characterized in that, said method comprising the steps of:

Lyophilize obtains pure silk gum powder.

2. the method for claim 1 is characterized in that, the temperature that back solution is filtered in described adjusting is 50-80 ℃, and pH value is 7-9.

3. the method for claim 1 is characterized in that, the polyacrylamide of described adding accounts for the 0.5-0.8% of water body quality.

4. the method for claim 1 is characterized in that, the mass ratio of the dehydrated alcohol of described adding, deionized water and silk gum coarse meal is 70: 250: 25.

5. the method for claim 1 is characterized in that, described solution is centrifugal 30 seconds through 5000 rev/mins of refrigerated centrifuges.

6. the method for claim 1 is characterized in that, the described distilled water that adds during with dissolved in distilled water and the mass ratio of silk gum coarse meal are 8: 25.