CN106676642A - Silk degumming/scouring agent, application and treatment method for degumming waste liquid - Google Patents
Silk degumming/scouring agent, application and treatment method for degumming waste liquid Download PDFInfo
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- CN106676642A CN106676642A CN201611142039.2A CN201611142039A CN106676642A CN 106676642 A CN106676642 A CN 106676642A CN 201611142039 A CN201611142039 A CN 201611142039A CN 106676642 A CN106676642 A CN 106676642A
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- degumming
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- scouring agent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C3/00—Treatment of animal material, e.g. chemical scouring of wool
- D01C3/02—De-gumming silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic System
Abstract
The invention discloses a silk degumming/scouring agent, an application and a treatment method for a degumming waste liquid. a calcium hydroxide water solution with the mass concentration of 0.01-1.0% is used for boiling degumming of silk or boiling refining of a silk floss sheet, silk spinning and grey silk as the silk degumming/scouring agent, and sericin of a fibroin fiber outer layer can be completely removed through boiling degumming/refining treatment for 10-60 minutes; the degumming rate reaches 28%, the injury to the degummed silk fiber is small, the original mechanical property of the fiber is basically kept; a calcium salt which is insoluble to water is generated by a lot of alkaline waste liquid obtained through degumming treatment through neutralization of a sulfuric acid or phosphoric acid for precipitation, a sericin protein solution is obtained after precipitation separation and spray drying is carried out to prepare sericin powder. According to the silk degumming/scouring agent, degumming/refining of silk can be carried out at low cost, all sericin protein and generated calcium salt can be recycled at high efficiency, and serious pollution to the environment and great waste of biological resources caused by a lot of alkaline degumming waste liquid can also be avoided.
Description
Technical field
The present invention relates to a kind of degumming silkworm cocoons agent or silk scouring agent, can be as a kind of cocoon shell or natural silk degumming agent and life
Silk, silk floss sheet, silk spinning and silk broadcloth blank scouring agent etc., at the same realize green, low cost, high efficiency reclaim sericin and
The purpose of calcium salt.
Background technology
Quick lime is commonly called as calcium oxide（CaO）, it is by lime stone（Also referred to as marble, main component is calcium carbonate CaCO3）Through
Cross the oxide generated after high-temperature calcination.Just reacted when quick lime runs into water, generate white lime, that is, the calcium hydroxide being commonly called as.
This white lime refers to just calcium hydroxide, and it is a kind of white powder, is slightly soluble in water.The aqueous solution of white lime is commonly called as white lime
Water, equivalent to the aqueous solution of calcium hydroxide.
All be with this limewash earliest in silkworm industry to sterilizations such as rearing instrument, silkworm rooms, with prevent various silkworms sick generation,
The pollution of germ.So, it be it is a kind of it is the most frequently used be also most cheap Disinfection in silkworm rearing agent.White lime i.e. calcium hydroxide as
NaOH etc. is equally a kind of highly basic, but different is its solubility very little in water, is slightly soluble in water；It is molten in its water
Xie Du is only 0.166 g/100g at 20 DEG C, and is that solubility reduces on the contrary as temperature is raised, and is at 100 DEG C
0.08g/100g water, half of solubility or so at only 20 DEG C.
Conventional degumming/the scouring agent such as silk cocoon, silk or silk floss sheet, raw silk, silk blank is mostly alkaline solution or alkali
Property material and surfactant mixture, what this sericin property for being mainly silk fiber outer layer was determined.Silk gum is a class
The mixture of various globular preteinses that molecular size range differs, is dissolved in hot water and is particularly very soluble in hot alkali water.In carbonic acid
It is the most frequently used Degumming method to carry out boiling degumming in the aqueous solution such as sodium, sodium acid carbonate, is also a kind of degumming very thoroughly method,
But can usually cause silk peptide chain break, fibroin fiber mechanical performance degradation.Because Sodium Hydroxide Alkaline is very strong, so
Typically carrying out silk without this aqueous solution boils degumming, and otherwise, not only silk gum hydrolysis, and fibroin fiber is also seriously hydrolyzed,
Therefore can be used for hydrolysis of the silk-fibroin including silk gum and fibroin fiber and be made acid hydrolysis thing.Document report is electrolysed with strong basicity
Water carries out the degumming of silk or silk cocoon, and the damage to fibroin fiber is smaller（Cao, T.-T., Wang, Y.-J. &
Zhang, Y.-Q. PLOS One, 2013. 8(6), e65654）.Certainly, with neutral soap lye or some surfactants etc.
Natural silk degumming is carried out, the influence to fibroin cellulose fiber is minimum, but has the disadvantage degumming inefficiency, degumming is often boiled repeatedly a lot of
Sericin outside secondary just inadequate removal silk surface；Industrially mostly made with surfactant mixed liquor with alkaline matter
It is degumming agent.The a large amount of alkaline natural silk degumming liquid that the above method is produced, is mostly difficult or at low cost by these alkaline degummings
Agent is separated with degumming liquid or sericin, does not reach the purpose that environmental protection and living resources make full use of.So, to being at present
Only also none of these methods both can completely remove sericin, and fibroin fiber mechanical performance degradation is not caused, generation
A large amount of degumming waste liquids do not cause environmental pollution again, cannot more realize fully reclaiming the side of a large amount of valuable living resources sericins
Method.
The content of the invention
The present invention is in view of the shortcomings of the prior art, there is provided a kind of to keep fibroin fiber performance, degumming efficiency high
Degumming agent, and environmental protection Degumming method and the method that is processed waste liquid and reclaimed silk gum.
Realize that the technical scheme of the object of the invention is to provide a kind of natural silk degumming/scouring agent, it be mass concentration 0.01~
1.0% calcium hydroxide aqueous solution.
Preferred scheme of the invention is that the mass concentration of calcium hydroxide aqueous solution is 0.01~0.025%.
Another technical scheme of the invention is the side of the application of natural silk degumming/scouring agent as described above, i.e. degumming/concise
Method includes：With mass concentration as 0.01~1.0% calcium hydroxide aqueous solution as degumming/scouring agent, boil degumming as silk,
Or silk floss sheet, silk spinning and greig boil it is concise, boil degumming/refining processing time be 10~60 min.
The preferred scheme of the application of natural silk degumming/scouring agent of the present invention is that the mass concentration of calcium hydroxide aqueous solution is
0.01~0.025%.Degumming/refining processing time is boiled for 20 min, is changed degumming/concise liquid and is repeated and boils degumming/concise
Process 20 min.
It is useless to degumming after degumming/concise that technical solution of the present invention also includes that natural silk degumming/scouring agent as described above is used for
The processing method of liquid, by mass concentration be 0.01~1.0% calcium hydroxide aqueous solution be used as silk boil degumming, or silk floss sheet,
Boiling for silk spinning and greig is concise, and the time for boiling degumming/refining processing is 10~60 min；After through degumming/refining processing
Sulfuric acid or phosphoric acid are added in the alkaline waste liquor for obtaining, neutralization reaction generates water insoluble calcium sulfate or calcium phosphate, by sediment
Sericin solution is obtained after separation, it is spray-dried to be made silk gum powder.
The preferred scheme of method for treating waste liquid is：The mass concentration of degumming/scouring agent calcium hydroxide aqueous solution be 0.01~
0.025%.Degumming/refining processing time is boiled for 20 min, is changed degumming/concise liquid and is repeated and boils degumming/refining processing 20
min.Concentration is carried out to alkaline waste liquor and puts solid content reaching 0.5~10%, adding sulfuric acid or phosphoric acid makes waste liquid in neutrality.
The purpose of the present invention be a kind of silk by the use of calcium hydroxide aqueous solution as environmental protection, sustainable development it is concise/it is de-
Jelly, is applied to a series of natural silk degummings or concise processing technology such as silk cocoon and natural silk degumming, raw silk and silk floss sheet is concise, thin,tough silk
Spin new technology and the new technologies such as concise, silk broadcloth blank is concise.By the middle hydroxide for adding sulfuric acid or phosphoric acid and degumming waste liquid
Calcium reaction generates water insoluble calcium salt and precipitates, and reaches the purpose that sericin and calcium salt are reclaimed entirely.The present invention develops one
Planting the Degumming method and accessory substance of the environmental protection that can substantially meet above-mentioned requirements includes the recovery technology of silk gum and calcium salt, utilizes
This strong basicity and the calcium hydroxide that is slightly soluble in water are carried out boiling degumming as silk cocoon or natural silk degumming agent, and fibroin can be kept substantially
The mechanical performance of fiber, and a large amount of alkalescence degumming waste liquids are neutralized by sulfuric acid or phosphoric acid, are not dissolved in calcium hydroxide reaction generation
The calcium precipitation of water, so that waste liquid exempts the purpose stained and reach and reclaim silk gum and calcium salt.
At present, in silk wadding quilt process, first working procedure is that machine draws life under a large amount of NaOH hydrothermal solution drip washing
Silk floss sheet, two procedures are that these machines drawing silk floss sheet is placed in into substantial amounts of alkaline concise liquid to be lived including sodium carbonate, sodium metasilicate, surface
Property agent, carry out concise, the sericin outside removal fibroin fiber in bleaching agent etc. mixed solution, and fibroin fiber is carried out
Decolourize, soften, bleaching etc..After the technology of the present invention, added in first working procedure and two procedures and use together calcium hydroxide water
Solution boils the technique of degumming, can remove the sericin outside fibroin fiber, and the silk floss sheet of degumming can enter back into the 3rd road
Operation, that is, be added without carrying out silk decolouring in traditional scouring agent of alkaline matter, soften or bleaching, this 3rd road it is concise
Liquid is because can be with Reusability without sericin.And the alkaline degumming liquid that two procedures of above-mentioned insertion are produced can with sulfuric acid or
Phosphoric acid is neutralized, and is generated water insoluble calcium salt with calcium hydroxide reaction and is precipitated, so that a large amount of sericins in degumming liquid
Separated with the calcium salt for producing, sericin powder and calcium salt powder are made by methods such as spray drying, exempt traditional silk floss sheet
The severe contamination that concise liquid is caused to environment, and the largely huge waste of protein biology resource.
In the degummings such as silk spinning system silk floss, cocoon, dupion and silk broadcloth or the concise process of greig, it is also possible to as upper
State equally, make the technique that former mono bath degumming is processed into double baths, that is, increase the natural silk degumming bath of white lime water, the degumming after silk gum
Fiber enters the traditional concise bath for being not added with alkaline matter, the purpose is to improve silk fiber surface property, rather than concise degumming.
Same this concise liquid is because can be with Reusability, and in the degumming bath of slubbing in same use sulfuric acid or phosphoric acid without sericin
With, it is to avoid the waste of protein biology resource in a large amount of alkaline waste waters.
Meaning of the present invention is that China is Silk Industry big country, and what is produced in silk processing since changing thousands of years is a large amount of
Alkaline degumming liquid or scouring waste cannot reclaim substantial amounts of sericin and the severe contamination produced to environment.The present invention is provided
Technical scheme do not only have considerable economic benefit, also with significant social benefit, by traditional Silk Industry economy and silkworm
The sustainable development of silk industry produces active influence.
Compared with prior art, the beneficial effects of the present invention are：
1st, the sericin outside fibroin fiber can be completely sloughed, degumming rate reaches 28%, and the silk fiber after degumming is damaged
It is small, it is basic to keep the original mechanical performance of fiber.
2nd, during the degumming/scouring agent provided using the present invention carries out the waste liquid obtained after degumming process to silk etc., pass through
Add sulfuric acid or phosphoric acid to neutralize, generate water insoluble calcium salt with calcium hydroxide reaction and precipitate, by simple filtering or from
The heart just can by substantial amounts of sericin and formed calcium salt easily and lift it is separate, through spray drying etc. method be made calcium salt
Powder and sericin powder.The calcium salt of recovery can apply to fertilizer of plant culture etc., and sericin powder can be in work
The aspects such as industry product surface modifying material, cell culture substrate, healthy food, superior cosmetics or daily chemical product obtain extensively should
With.
Brief description of the drawings
Fig. 1 is to silk after degumming agent provided in an embodiment of the present invention and the degumming tech neutral soap lye traditional with use are processed
The contrast curve of cellulose fiber Effect of Thermal Performance；
Fig. 2 is degumming agent provided in an embodiment of the present invention and degumming tech de- with using what is obtained after traditional neutral soap lye treatment
The X-ray diffraction comparison diagram of collodion silk cellulose fiber；
Fig. 3 is that to waste liquid process the silk gum aqueous solution for obtaining using degumming agent provided in an embodiment of the present invention spray-dried
It is made the photo figure in kind of silk gum powder.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment is further described to technical solution of the present invention.
Embodiment 1：
Compound concentration be 0.025% calcium hydroxide aqueous solution for degumming liquid, by silkworm cocoon with 1：60（g/mL）Bath raio, agitation bar
The min of degumming process 20 is boiled under part, degumed silk is then taken out, then is changed fresh identical degumming liquid and continue to stir, boil degumming
Process 20 min.Take out 2 times treatment degumed silks, rinsed repeatedly with running water, 100 DEG C drying 2 h, obtain the fibroin after degumming
Fiber.
In the present embodiment, degumming process is carried out to silkworm cocoon with various concentrations calcium hydroxide aqueous solution, and calculates silk cocoon
Degumming rate.Calcium hydroxide aqueous solution is configured to 0.01,0.025,0.05,0.075 and 0.10% 5 kind of concentration, 5.0 g silk cocoons
Shell is with 1：60（g/mL）Bath raio is immersed in the calcium hydroxide aqueous solution of above-mentioned five kinds of concentration respectively, and 5,10,20,40 and are boiled respectively
60 min, then take out degumed silk, after being cleaned repeatedly with running water, are placed in 100 DEG C of h of oven for drying 2, and taking-up is positioned over room temperature
Under overnight balance be re-weighed, calculate silkworm cocoon degumming rate, each sample in triplicate, calculate average value and its standard deviation（±
SD）, usually time and calcium hydroxide aqueous solution concentration to degumming silkworm cocoons rate influence result ginseng be shown in Table 1.
Table 1
Numerical value degumming rate % ± SD are represented in table 1；There is the value that " * " is marked too high for degumming rate, reason is in this concentration
Boiled in calcium hydroxide aqueous solution the specified time, fibroin is seriously broken and hydrolyzes, short fibroin fiber is lost in during cleaning, therefore degumming rate
It is higher.
Embodiment 2：
The present embodiment carries out the experiment and analysis of retting function with baryta water as comparative example.
The present embodiment prepared calcium hydroxide aqueous solution concentration in the same manner as in Example 1 carry out silk boil degumming examination
Test.Result shows：20 min are boiled in 0.025% baryta water, then change identical fresh solution and boil 20 min,
The glue glue rate of its silk cocoon layer is 25.63%.Concrete outcome ginseng is shown in Table 2.
Table 2
The silk cocoon amount of each sample is 5g in table 2, repeats experiment 3.
Embodiment 3：
The present embodiment to calcium hydroxide aqueous solution, observe by the situation of change of pH value before and after silk cocoon layer degumming is carried out, to implementing
Acid-base property of the calcium hydroxide aqueous solution pH meter of the various various concentrations that example 1 is provided to degumming liquid after solution before degumming or degumming
It is measured, as a result referring to table 3.
Table 3
Degumming silkworm cocoons treatment, cocoon quality (g) and degumming liquid (mL) are carried out in the calcium hydroxide aqueous solution of the prescribed concentration of table 3
Bath raio 1：60.From table 3, the pH value of five kinds of calcium hydroxide aqueous solutions of various concentrations before degumming is with the rising of its concentration
And raise, the pH value of solution is 11.60 during 0.01% concentration, be have decreased to by its degumming liquid pH value after 5.0 g degumming silkworm cocoons
PH8.77, about have dropped 3 points；And solution ph drops to pH9.57 from 12.37 during with 0.025% slightly higher concentration of concentration,
Have dropped close to 3 points；With the rising of calcium hydroxide aqueous solution concentration, the value that pH value declines after this degumming also subtracts therewith
Few, pH have dropped 2.5 when 0.05%, and about 2.3 are only have dropped to pH when 0.1%.These results illustrate calcium hydroxide aqueous solution pH value
With the rising of its concentration, alkalescence is significantly increased, and pH value after effect is boiled with sericin in silk cocoon layer in degumming liquid is still
In alkalescence, this alkalescence is also to have strengthened with the raising of original content.
Embodiment 4：
By the technical scheme that embodiment 1 is provided, the min of degumming process 20 is carried out with 0.025% calcium hydroxide aqueous solution, renewed fresh de-
Glue same degumming 1 time again, the temperature of degumming process is different, influence of the observation degumming temperature to degumming silkworm cocoons rate.Ordinary circumstance
Under, the degumming rate of silk cocoon layer or silk in various solution or medium can all rise with the raising of its treatment temperature.Degumming
Influence of the temperature to degumming silkworm cocoons rate can be found in table 4.
Table 4
| Temperature | 60℃ | 70℃ | 80℃ | 90℃ | 100℃ | 120℃* |
| Degumming rate (%) | 3.13 | 4.90 | 6.83 | 10.74 | 27.89 | 29.99 |
| ±SD | ±0.67 | ±0.91 | ±0.28 | ±0.35 | ±1.02 | ±0.36 |
Data are represented with " * " and process 30 under 120 DEG C of HTHPs in the calcium hydroxide aqueous solution of same concentration in table 4
min.It can be found that temperature influences very big on degumming rate from table 4, the min of degumming process 40 only removes 3% at 60 DEG C, rises to
Degumming rate, when 100 DEG C of double risings of its degumming rate are risen to, reaches 27.89% also only proximate to 11% at 90 DEG C.When with HTHP
Increase the temperature to 120 DEG C treatment after, its natural silk degumming rate almost do not raise again how much.Result shows in 0.025% calcium hydroxide
20 min × 2 are boiled in the aqueous solution can remove the sericin of fibroin periphery.
Embodiment 5：
By the technical scheme that embodiment 1 is provided, change degumming bath ratio, observation degumming bath compares the influence of degumming silkworm cocoons rate.
The min of degumming process 20 is boiled in 0.025% calcium hydroxide aqueous solution, 20 min for the treatment of are boiled again after renewing fresh degumming liquid.Bath raio
Influence to degumming silkworm cocoons rate is referring to table 5.
Table 5
Numerical value is to boil min × 2 of degumming 20 with 0.025% calcium hydroxide aqueous solution in table 5.The result of table 5 shows that bath raio is to silk cocoon
The degumming rate influence of shell is little, is fluctuated up and down between 25% to 29%, and degumming rate changes and is no more than 4%.So, in testing afterwards
Degumming bath ratio generally all uses 1 in addition to special instruction：60.
Embodiment 6：
After the present embodiment using calcium hydroxide aqueous solution to carrying out degumming process, the mechanical performance of fibroin fiber is observed and surveyed
Examination.
Fibroin fiber is almost no impact using conventional neutral soap lye degumming, and in 0.5% aqueous sodium carbonate
Middle degumming influences very big on fibroin fiber, causes serious fibroin Fragmentation, mechanical stretching performance degradation.The present embodiment
In, using two kinds of fibroin fibers being obtained using neutral soap lye and sodium carbonate liquor degumming as control, as a result referring to accompanying drawing 1, Fig. 1
It has been shown that, boils the min of degumming 40 in 0.01% calcium hydroxide aqueous solution, its ultimate strength and elongation at break are almost de- with neutral soap
The fibroin fiber of glue is similar, and the ultimate strength and elongation at break of its fibroin monfil are respectively reached close to 6.0 cN and 27%.
With the rising of calcium hydroxide aqueous solution concentration, its tensile property significantly decreases；When concentration reaches 0.025%, its monofilament is fine
The ultimate strength and elongation at break of dimension are declined slightly about 10%；When calcium hydroxide aqueous solution concentration is increased to 0.05%, these refer to
Mark decline becomes apparent from；When concentration reaches 0.1%, the ultimate strength and elongation at break of its monfil drop to concentration 0.01%
When half be less than, respectively 2.748 cN and 7.762%.It is further noted that boiling degumming in 0.1% calcium hydroxide aqueous solution
Fibroin fiber mechanical performance than 0.5% concentration degumming is worse, the tensile property of 0.05% calcium hydroxide aqueous solution degumed silk with
0.5% aqueous sodium carbonate degumed silk is similar.So, it is believed that 0.01% calcium hydroxide aqueous solution degumming from these results
Seemingly, but its degumming rate is too low for fiber tensile property and neutral soap liquid phase, and just explanation sericin is not sloughed completely.And 0.025%
Calcium hydroxide aqueous solution degumming its tensile property can also keep the ninety percent of original fiber, and fibroin fiber can be also reacted from its degumming rate
The sericin of outside has been removed.The tensile property of degumming fibroin fiber compares referring to table 6.
Table 6
In table 6, three kinds of silk cocoons first unify reel silk from cocoons raw silk with common single cocoon reeling silk reeling method, are with 100 times during every cocoon filature
One, the sequence notation from the beginning to the end by the 1st, 2,3 ..., 12 strands ... takes the 3rd of cocoon the, 4 and 5 strands every, by three methods in table
Totally seven groups carry out degumming or concise respectively, then, 20 5 cm monofilament long are randomly selected in per share concise fibroin fiber fine
Dimension, is placed on the universal testing machine of INSTRON companies of the U.S. 3365 and determines, and the average of this 20 monfil is drawn respectively
Value, then the 3rd, 4 and 5 strands are carried out, finally repeatedly 3 values of cocoon are average again, and statistical analysis draws the average value and mark that 3 cocoons are repeated
It is accurate poor.
Embodiment 7
The present embodiment using the fibroin fiber after technical solution of the present invention degumming process to carrying out thermal performance test.
The method that degumming process is provided by embodiment 1, with neutral soap and Na2CO3The aqueous solution boils degumming for comparative example, right
The hot property of these three degumming fibroin fibers is analyzed.Its result is referring to accompanying drawing 1, as seen from Figure 1, neutral soap solution degumming
Fibroin fiber heat decomposition temperature is 327.84 DEG C, and is with the fibroin fiber heat decomposition temperature of 0.025% aqua calcis degumming
321.86 DEG C are slightly better than sodium carbonate, and the degumed silk compared with neutral soap will differ from 6 DEG C.
Embodiment 8：
The fibroin fiber that the technical scheme provided by embodiment 1 is obtained carries out X-ray diffraction analysis, determines 0.025% hydroxide
Calcium solution boils influence of the degumming to the crystal structure of fibroin fiber.Equally boiled with neutral soap and 0.5% aqueous sodium carbonate de-
The fibroin fiber of glue is compared, and the crystallinity of these three degumming fibroin fibers is analyzed with X-ray diffraction analyzer.Knot
Referring to accompanying drawing 2, Fig. 2 shows fruit, and 0.025% aqua calcis boils degumming to the crystal structure of fibroin fiber and other two kinds
Degumming is similar, and obvious influence is not produced on crystal structure.
Embodiment 9：
The present embodiment provides a kind of recovery method of sericin in alkaline degumming waste liquid.
By the technical scheme that embodiment 1 is provided, the degumming waste liquid obtained after degumming is boiled using calcium hydroxide aqueous solution and is entered
Row concentration, when obtaining 0.5~10% solid content, adds sulfuric acid or phosphoric acid to be adjusted to degumming liquid in neutrality, with calcium hydroxide reaction
Produce, the generation precipitation such as calcium sulfate or calcium phosphate, through filtering or centrifugal treating after, separated with silk gum solution, sediment is through drying
After obtain calcium salt, can be recycled as phosphate fertilizer etc..Degumming waste liquid obtains the silk gum aqueous solution after treatment, can be direct
It is spray-dried, is made silk gum powder, its product, can be in healthy food, surface industrial material surface modifying referring to accompanying drawing 3
The fields such as agent, cell culture additive, bio-medical material are recycled.
Claims (9)
1. a kind of natural silk degumming/scouring agent, it is characterised in that：It is the calcium hydroxide aqueous solution of mass concentration 0.01~1.0%.
2. a kind of natural silk degumming/scouring agent according to claim 1, it is characterised in that：The quality of calcium hydroxide aqueous solution
Concentration is 0.01~0.025%.
3. a kind of application of natural silk degumming/scouring agent as claimed in claim 1, it is characterised in that the method bag of degumming/concise
Include：With mass concentration as 0.01~1.0% calcium hydroxide aqueous solution as degumming/scouring agent, boil degumming, or silk as silk
Boiling for continuous piece, silk spinning and greig is concise, and the time for boiling degumming/refining processing is 10~60 min.
4. the application of a kind of natural silk degumming/scouring agent according to claim 3, it is characterised in that：Calcium hydroxide aqueous solution
Mass concentration be 0.01~0.025%.
5. the application of a kind of natural silk degumming/scouring agent according to claim 3 or 4, it is characterised in that：Boil degumming/essence
It is 20 min to practice process time, changes degumming/concise liquid and repeats and boils the min of degumming/refining processing 20.
6. a kind of natural silk degumming/scouring agent is used for after degumming/concise the processing method to degumming waste liquid, it is characterised in that：By matter
Amount concentration be 0.01~1.0% calcium hydroxide aqueous solution be used as silk boil degumming, or silk floss sheet, silk spinning and greig boil
Concise, the time for boiling degumming/refining processing is 10~60 min；In the alkaline waste liquor obtained after through degumming/refining processing
Sulfuric acid or phosphoric acid are added, neutralization reaction generates water insoluble calcium sulfate or calcium phosphate, silk gum egg is obtained after sediment is separated
White solution, it is spray-dried to be made silk gum powder.
7. a kind of natural silk degumming/scouring agent according to claim 6 is used for the treatment side of degumming/concise rear gained waste liquid
Method, it is characterised in that：The mass concentration of calcium hydroxide aqueous solution is 0.01~0.025%.
8. a kind of natural silk degumming/scouring agent according to claim 6 is used for the treatment side of degumming/concise rear gained waste liquid
Method, it is characterised in that：Degumming/refining processing time is boiled for 20 min, is changed degumming/concise liquid and is repeated and boils degumming/essence
Practice 20 min for the treatment of.
9. a kind of natural silk degumming/scouring agent according to claim 6 is used for the treatment side of degumming/concise rear gained waste liquid
Method, it is characterised in that：Concentration is carried out to alkaline waste liquor and puts solid content reaching 0.5~10%, adding sulfuric acid or phosphoric acid makes to give up
Liquid is in neutrality.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385383A (en) * | 2018-02-07 | 2018-08-10 | 嘉兴市桑田新材料科技有限公司 | A kind of silk is scouringed and bleaching degumming tech |
| CN109402743A (en) * | 2018-12-29 | 2019-03-01 | 阳城县禹珈豪丝业有限公司 | A kind of dried cocoon silk reeling method |
| CN112826286A (en) * | 2021-01-07 | 2021-05-25 | 浙江蚕缘家纺股份有限公司 | Washable silk quilt |
| CN113150307A (en) * | 2021-04-30 | 2021-07-23 | 苏州大学 | Glycosylated sericin, preparation method and application thereof |
| CN113604890A (en) * | 2021-07-30 | 2021-11-05 | 苏州家和蚕业生物科技有限公司 | Combined production method of fibroin and white steam filature |
| CN115637502A (en) * | 2022-09-09 | 2023-01-24 | 温州穆清生物科技有限公司 | Method for removing sericin |
| WO2023242849A1 (en) * | 2022-06-16 | 2023-12-21 | Yeda Research And Development Co. Ltd. | Method for degumming silk fibers |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385383A (en) * | 2018-02-07 | 2018-08-10 | 嘉兴市桑田新材料科技有限公司 | A kind of silk is scouringed and bleaching degumming tech |
| CN109402743A (en) * | 2018-12-29 | 2019-03-01 | 阳城县禹珈豪丝业有限公司 | A kind of dried cocoon silk reeling method |
| CN112826286A (en) * | 2021-01-07 | 2021-05-25 | 浙江蚕缘家纺股份有限公司 | Washable silk quilt |
| CN112826286B (en) * | 2021-01-07 | 2023-12-05 | 浙江蚕缘家纺股份有限公司 | Silk quilt capable of being washed |
| CN113150307A (en) * | 2021-04-30 | 2021-07-23 | 苏州大学 | Glycosylated sericin, preparation method and application thereof |
| CN113150307B (en) * | 2021-04-30 | 2023-01-31 | 苏州大学 | Glycosylated sericin, preparation method and application thereof |
| CN113604890A (en) * | 2021-07-30 | 2021-11-05 | 苏州家和蚕业生物科技有限公司 | Combined production method of fibroin and white steam filature |
| CN113604890B (en) * | 2021-07-30 | 2023-11-17 | 苏州家和蚕业生物科技有限公司 | Combined production method of fibroin and white silk |
| WO2023242849A1 (en) * | 2022-06-16 | 2023-12-21 | Yeda Research And Development Co. Ltd. | Method for degumming silk fibers |
| CN115637502A (en) * | 2022-09-09 | 2023-01-24 | 温州穆清生物科技有限公司 | Method for removing sericin |
| WO2024050915A1 (en) * | 2022-09-09 | 2024-03-14 | 温州穆清生物科技有限公司 | Sericin removal method |
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