CN106367816B - A kind of method of tussah silk high temperature and pressure acid degumming - Google Patents
A kind of method of tussah silk high temperature and pressure acid degumming Download PDFInfo
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- CN106367816B CN106367816B CN201611028318.6A CN201611028318A CN106367816B CN 106367816 B CN106367816 B CN 106367816B CN 201611028318 A CN201611028318 A CN 201611028318A CN 106367816 B CN106367816 B CN 106367816B
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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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Abstract
The invention discloses a kind of methods of tussah silk high temperature and pressure acid degumming, first mix acid, bleeding agent and water, obtain degumming liquid, and silk is immersed in degumming liquid, are 1.0~3.0MPa in pressure, temperature carries out degumming under conditions of being 100~140 DEG C.The present invention handles tussah silk using the method for high temperature and pressure acid degumming, improve the hydrolysis rate and protein peptide bond crack velocity of silk gum, usually time is short, and degumming rate can reach 13%, the ultimate strength of silk may remain in 620N or so after degumming, the strength loss of silk is small, realizes the fast degumming of tussah silk.
Description
Technical field
The present invention relates to a kind of technical field of textile fabric dyeing and finishing, more particularly to a kind of tussah silk high temperature and pressure acid degumming
Method.
Background technology
Tussah silk is one kind of tussah, and the tussah silk of China's specialty accounts for the 80% of whole world tussah.Its main feature is that machine
Tool intensity is high, acidproof and alkaline-resisting, is widely used in and weaves various silks and satins and knitwear.Tussah silk textiles are by fibroin and silk gum structure
At silk gum is present in fibroin periphery, plays protection and adhesive action to fibroin, colloid is not easy softening dissolving, silk in the hot water
The presence of glue can influence the performances such as gloss, feel and the dyeing and printing process of tussah silk textiles.Therefore, it is necessary to by the silk on silk surface
Glue carries out degumming process.
Degumming method commonly used in the prior art includes alkaline process degumming, sour degumming, high-temperature high pressure water degumming etc..Conventional acid,
Alkali degumming is to make silk gum puffing dissolving in acid or alkaline solution, concurrently gives birth to the amino acid that hydrolysis becomes soluble, from
And achieve the purpose that degumming, but acid, alkali degumming take longer, and silk loss of strength is larger；High-temperature high pressure water degumming be by
Silk is dipped in clear water, so that silk gum is hydrolyzed under conditions of high temperature and pressure, and high-temperature high pressure water degumming has the advantages that environmental protection, still
Usually time is longer, and degumming effect is general.
Invention content
In view of this, present invention aims at provide the tussah silk high temperature and pressure that a kind of usually time is short, degumming effect is good
The method of sour degumming realizes the fast degumming of tussah silk, reduces the discharge of waste water, and the ultimate strength loss of tussah silk is small.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of methods of tussah silk high temperature and pressure acid degumming, include the following steps：
Acid, bleeding agent and water are mixed, degumming liquid is obtained；
Tussah silk is immersed in degumming liquid, is 1.0~3.0MPa in pressure, temperature carries out under conditions of being 100~140 DEG C
Degumming；
Preferred acid is any one or a few the mixture in tartaric acid, citric acid and hydrochloric acid；
Sour a concentration of 0.1~0.5g/L in preferred degumming liquid；
Preferred bleeding agent is nonionic surfactant；
Preferred nonionic surfactant is fatty alcohol polyoxyethylene ether and/or alkyl polyoxyethylene ether；
A concentration of 0.1~0.5g/L of bleeding agent in preferred degumming liquid；
The bath raio of preferred tussah silk and degumming liquid is 1:20~40；
The time of preferred degumming is 20~50min；
The pressure of preferred degumming is 1.4~2.7MPa；The temperature of the degumming is 110~130 DEG C；
Further include after preferred degumming：Tussah silk after the degumming is washed and dried successively；Preferred washing
Temperature be 110~130 DEG C；Preferably dry temperature is 70~130 DEG C.
The present invention provides a kind of methods of tussah silk high temperature and pressure acid degumming, first mix acid, bleeding agent and water, obtain
To degumming liquid；By tussah silk immerse degumming liquid in, pressure be 1.0~3.0MPa, temperature be 100~140 DEG C under conditions of into
Row degumming.The present invention carries out sour degumming under conditions of high temperature and pressure, and hydrolysis rate and the protein peptide bond for improving silk gum are disconnected
Split speed, usually time is short, and wastewater discharge is small, and in scouring processes tussah silk strength loss it is small.The experimental results showed that making
Degumming is carried out to tussah silk with method provided by the invention, degumming rate can reach 13%, the ultimate strength of tussah silk after degumming
620N or so is may remain in, ultimate strength loss is small, realizes the fast degumming of tussah silk.
Specific implementation mode
The present invention provides a kind of methods of tussah silk high temperature and pressure acid degumming, include the following steps：
Acid, bleeding agent and water are mixed, degumming liquid is obtained；
Tussah silk is immersed in degumming liquid, is 1.0~3.0MPa in pressure, temperature carries out under conditions of being 100~140 DEG C
Degumming.
The present invention mixes acid, bleeding agent and water, obtains degumming liquid.In the present invention, the acid is preferably tartaric acid, lemon
The mixture of one or more of lemon acid and hydrochloric acid；Preferably 2 kinds of sour mixtures, more preferably wine in the mixture of the acid
The mixture of the mixture or tartaric acid and hydrochloric acid of stone acid and citric acid.In the present invention, when it is described acid be preferably tartaric acid and
When citric acid, the molar ratio of the tartaric acid and citric acid is preferably 1~1.2:1, more preferably 1.1:1；When the acid is preferred
For tartaric acid and hydrochloric acid when, the molar ratio of the tartaric acid and hydrochloric acid is preferably 1~1.2:1, more preferably 1.1:1.In this hair
In bright, sour concentration is preferably 0.1~0.5g/L in the degumming liquid, more preferably 0.3~0.4g/L；The present invention utilizes acidity
Solution makes that sericin is puffing, hydrolysis, soluble amino acid is generated, to achieve the purpose that degumming, simultaneously because fibroin is not
Soluble, acid-fast ability is stronger, thus is had an impact to the ultimate strength of fibroin smaller.
In the present invention, the bleeding agent is preferably nonionic surfactant, more preferably polyethenoxy ether class it is non-from
Sub- surfactant, most preferably fatty alcohol polyoxyethylene ether and/or alkyl polyoxyethylene ether.In specific embodiments of the present invention
In, JFC-1 (sec-octyl alcohol polyoxyethylene ether), JFC-e (isomeric alcohol polyethenoxy ether), paregal O series of products (alkane can be selected
Base polyoxyethylene ether) in any one or a few mixture.In the present invention, the concentration of bleeding agent is excellent in the degumming liquid
It is selected as 0.1~0.5g/L, more preferably 0.3~0.4g/L.The present invention reduces the surface tension of silk tussah fibre using bleeding agent,
The infiltration for promoting degumming liquid makes degumming liquid uniformly, adequately be contacted with silk gum, improves degumming effect, while reducing tussah silk
Fibre damage.
In the present invention, the amount of water is the concentration in order to make said components reach restriction, in specific embodiments of the present invention
In, the amount of water can be determined according to the specific concentration of said components.
After obtaining degumming liquid, the present invention immerses tussah silk in degumming liquid, is 1.0~3.0MPa, temperature 100 in pressure
Degumming is carried out under conditions of~140 DEG C.In the present invention, the tussah silk belongs to protein fibre, and main component is fibroin, silk
Glue, natural pigment and ash grade impurity；The mass content of fibroin in tussah silk (water reeled silk) is about 85%, the quality of silk gum
Content is about 13%, and the mass content of natural pigment and impurity is about 2%.
In the present invention, the bath raio of the tussah silk and degumming liquid is preferably 1:20~40；More preferably 1:25~35, most
Preferably 1:30.
In the present invention, the pressure of the degumming is preferably 1.4~2.7MPa, more preferably 1.5~2.5MPa；It is described de-
The temperature of glue is preferably 110~130 DEG C, more preferably 115~125 DEG C；The time of the degumming is preferably 20~50min, more
Preferably 30~40min.Present invention preferably uses autoclaves to carry out degumming.It is de- that the present invention carries out acid under conditions of high temperature and pressure
Glue promotes hydrolysis of the sericin in acid solution using the condition of high temperature and pressure, improves hydrolysis rate, accelerate in acidic environment
The fracture of middle sericine peptide bond, realizes the fast degumming of tussah silk.
In the present invention, the tussah silk is immersed in degumming liquid again after preferably soaking in water；The temperature of the wetting is excellent
It is selected as room temperature, without being heated and being cooled down；Ensure that tussah silk can when immersing degumming liquid by first soaking tussah silk
Uniform absorption degumming liquid.
After the degumming, the tussah silk after the degumming is preferably washed and is dried successively by the present invention.In the present invention
In, the temperature of the washing is preferably 110~130 DEG C, more preferably 115~125 DEG C；The number of the washing is preferably 2~5
It is secondary, more preferably 3~4 times.In the present invention, the temperature of the drying is preferably 70~130 DEG C, more preferably 80~120 DEG C,
Most preferably 90~110 DEG C, the time of the drying is preferably 1~3h, more preferably 1.5~2.5h.
The method of tussah silk high temperature and pressure acid degumming provided by the invention is described in detail with reference to embodiment,
But they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Tartaric acid, penetrating agent JFC -1 and water are mixed, degumming liquid, a concentration of 0.2g/L of mesotartaric acid, infiltration are prepared
A concentration of 0.1g/L of agent JFC-1；
It is immersed in degumming liquid after tussah silk is soaked in water, the bath raio for controlling tussah silk and degumming liquid is 1:30, in height
Degumming process, control pressure 1.4MPa are carried out in pressure kettle, temperature is 140 DEG C, handles 30min；
The tussah silk after degumming is taken out, tussah silk is washed 3 times at 110 DEG C, later by tussah silk under the conditions of 70 DEG C
Drying.
Detect the degumming rate (fabric before degumming rate=(fabric weight after fabric weight-degumming before degumming)/degumming of tussah silk textiles
Weight), it is 11.5% that can obtain degumming rate；
The ultimate strength of tussah silk textiles is detected using electronic fabric strength tester, it is 550N that can obtain ultimate strength.
Embodiment 2
Tartaric acid, penetrating agent JFC-e and water are mixed, degumming liquid, a concentration of 0.1g/L of mesotartaric acid, infiltration are prepared
A concentration of 0.1g/L of agent JFC-e；
It is immersed in degumming liquid after tussah silk is soaked in water, the bath raio for controlling tussah silk and degumming liquid is 1:35, in height
Degumming process, control pressure 1.0MPa are carried out in pressure kettle, temperature is 130 DEG C, handles 40min；
The tussah silk after degumming is taken out, tussah silk is washed 3 times at 130 DEG C, later by tussah silk under the conditions of 110 DEG C
Drying.
The degumming rate and ultimate strength of tussah silk are detected according to the method for embodiment 1, can obtain degumming rate is
12.8%, ultimate strength 590N.
Embodiment 3
Citric acid, bleeding agent paregal O -8 and water are mixed, degumming liquid, the wherein a concentration of 0.3g/ of citric acid are prepared
L, a concentration of 0.3g/L of bleeding agent paregal O -8；
It is immersed in degumming liquid after tussah silk is soaked in water, the bath raio for controlling tussah silk and degumming liquid is 1:30, in height
Degumming process, control pressure 3.0MPa are carried out in pressure kettle, temperature is 120 DEG C, handles 30min；
The tussah silk after degumming is taken out, tussah silk is washed 3 times at 120 DEG C, later by tussah silk under the conditions of 130 DEG C
Drying.
The degumming rate and ultimate strength of tussah silk are detected according to the method for embodiment 1, can obtain degumming rate is
13.0%, ultimate strength 620N.
Embodiment 4
Citric acid, bleeding agent paregal O -8 and water are mixed, degumming liquid, the wherein a concentration of 0.5g/ of citric acid are prepared
L, a concentration of 0.1g/L of bleeding agent paregal O -8；
It is immersed in degumming liquid after tussah silk is soaked in water, the bath raio for controlling tussah silk and degumming liquid is 1:40, in height
Degumming process, control pressure 2.7MPa are carried out in pressure kettle, temperature is 100 DEG C, handles 50min；
The tussah silk after degumming is taken out, tussah silk is washed 3 times at 110 DEG C, later by tussah silk under the conditions of 80 DEG C
Drying.
The degumming rate and ultimate strength of tussah silk are detected according to the method for embodiment 1, can obtain degumming rate is
12.5%, ultimate strength 615N.
Embodiment 5
Hydrochloric acid, bleeding agent paregal O -9 and water are mixed, preparation degumming liquid, the wherein a concentration of 0.5g/L of citric acid,
A concentration of 0.5g/L of bleeding agent paregal O -9；
It is immersed in degumming liquid after tussah silk is soaked in water, the bath raio for controlling tussah silk and degumming liquid is 1:35, in height
Degumming process, control pressure 2.0MPa are carried out in pressure kettle, temperature is 110 DEG C, handles 30min；
The tussah silk after degumming is taken out, tussah silk is washed 3 times at 110 DEG C, later by tussah silk under the conditions of 90 DEG C
Drying.
The degumming rate and ultimate strength of tussah silk are detected according to the method for embodiment 1, can obtain degumming rate is
12.0%, ultimate strength 603N.
As seen from the above embodiment, the method degumming speed for the high temperature and pressure acid degumming that scheme of the present invention is provided
Soon, processing time is short, and degumming rate is high, the ultimate strength loss of tussah silk is small, realizes the fast degumming of tussah silk.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of method of tussah silk high temperature and pressure acid degumming, which is characterized in that include the following steps：
Acid, bleeding agent and water are mixed, degumming liquid is obtained；It is described acid be tartaric acid, citric acid and hydrochloric acid in any one or
Several mixtures；
Tussah silk is immersed in degumming liquid, is 1.0~3.0MPa in pressure, temperature is taken off under conditions of being 100~140 DEG C
Glue.
2. according to the method described in claim 1, it is characterized in that, a concentration of 0.1~0.5g/L sour in the degumming liquid.
3. according to the method described in claim 1, it is characterized in that, the bleeding agent is nonionic surfactant.
4. according to the method described in claim 3, it is characterized in that, the nonionic surfactant is aliphatic alcohol polyethenoxy
Ether and/or alkyl polyoxyethylene ether.
5. according to the method described in claim 1,3 or 4, which is characterized in that a concentration of the 0.1 of bleeding agent in the degumming liquid~
0.5g/L。
6. according to the method described in claim 1, it is characterized in that, the bath raio of the tussah silk and degumming liquid is 1:20~40.
7. according to the method described in claim 1, it is characterized in that, the time of the degumming is 20~50min.
8. according to the method described in claim 1,6 or 7, which is characterized in that the pressure of the degumming is 1.4~2.7MPa；Institute
The temperature for stating degumming is 110~130 DEG C.
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| CN107325303B (en) * | 2017-07-31 | 2020-11-24 | 安徽工程大学 | Degumming-free silk fiber solution, preparation method and application thereof |
| CN108179481A (en) * | 2018-02-07 | 2018-06-19 | 苏州先蚕丝绸生物科技有限公司 | A kind of method of refining of natural colorful silk |
| CN112401598B (en) * | 2020-10-27 | 2022-04-19 | 广西时宜农业科技有限公司 | Preparation method of silk quilt |
| CN112981647B (en) * | 2021-02-07 | 2022-07-19 | 康宝莱(宁波)织造有限公司 | Wild tussah silk napping yarn and preparation method thereof |
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| CN103739691B (en) * | 2013-12-11 | 2016-04-20 | 浙江大学 | The method of silk fibroin powder is prepared in a kind of environmental protection |
| CN103774246B (en) * | 2014-01-20 | 2016-08-17 | 丹东中天柞蚕生物科技有限公司 | Tussah cocoon case degumming malleation preprocessing technical method |
| CN104532365B (en) * | 2015-01-15 | 2016-04-27 | 武汉纺织大学 | A kind of preparation method of silk nanofiber |
| CN104693297A (en) * | 2015-02-15 | 2015-06-10 | 浙江大学 | Preparation method of camphor silkworm regenerated fibroin |
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