CN104562638B - A kind of preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation - Google Patents
A kind of preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation Download PDFInfo
- Publication number
- CN104562638B CN104562638B CN201410837132.XA CN201410837132A CN104562638B CN 104562638 B CN104562638 B CN 104562638B CN 201410837132 A CN201410837132 A CN 201410837132A CN 104562638 B CN104562638 B CN 104562638B
- Authority
- CN
- China
- Prior art keywords
- silkworm silk
- resistance
- fire
- oxidation
- silk
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses the preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, first silkworm silk is joined in ethanol solution, room temperature it is down to after heating, it is subsequently adding ethylenediamine, join in the mixed solution of LNBR and lecithin after continuing stirring, join after heated and stirred under vacuum in dimethyl phosphate aqueous solution, after reacting by heating, silkworm silk is taken out, add in hypo solution, silkworm silk after processing after heated and stirred under vacuum takes out, dry, obtain the fire-retardant toughened silkworm silk of resistance to oxidation.The resistance to oxidation fire-retardant toughened silkworm silk elongation at break that the present invention provides has reached more than 36%, within regain has reached 6%, it is without exception that oxidative resistance (in 5% hydrogen peroxide) has reached 500h, anti-flammability limited oxygen index has reached more than 34.8%, there is good pliability, oxidative resistance and anti-flammability, further expanded the range of silkworm silk.
Description
Technical field
The invention belongs to fibre preparing technical field, be specifically related to the preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation.
Background technology
Silkworm silk is the matured silkworm secreted concretionary continuous fiber of silk liquid, also referred to as natural silk when cocooing, and is a kind of natural
Fiber, is one of human use's animal fiber the earliest.According to archaeological discovery, about before 4700, China has utilized silkworm silk to manufacture
Silk thread, braided wires Bombyx bombycis silkworm silk band and simple silk.Shang and Zhou Dynasty silkworm silk knit sieve processed, thin silk fabric, fine silk fabrics, yarn, crape, figured woven silk material,
The silks such as brocade, embroidery.Silkworm has Bombyxmori Linnaeus, Antherea pernyi Guerin-Meneville, Semen Ricini silkworm, cassava silkworm, willow silkworm and giant silkworm etc..It is pumped by single Bombyx bombycis
Strand claims silk.It is borrowed sericin bonding cladding to form by two ultimate fibres.During filature, the silk of several Bombyx bombycis is extracted out, borrows
Sericin is bonded into strand, is referred to as silkworm silk.Remove the silkworm silk of sericin, claim nett silk.What in silkworm silk, consumption was maximum is mulberry silk,
Next to that tussah silk, other silkworm silks do not form resource because of limited amount.Silkworm silk light weight and elongated, fabric sheen is good, dress relax
Suitable, feel is smooth plentiful, poor heat conductivity, and moisture absorption is breathed freely, and is used for knitting the various silks and satins of system and knitwear, and for industry, national defence
And medicine and other fields.China, Japan, India, the former Soviet Union and Korea are main Chan Si states, and total output accounts for the 90% of world wide production
Above.
Silkworm silk is in application process at present, owing to it belongs to inflammable articles, when carrying out testing vertical flammability, in igniting 15s
Burn up the most completely, therefore how can fire-retardant need to carry out numerous studies and exploitation for it for its needs.Meanwhile, silkworm silk
Oxidative resistance poor, more sensitive to oxidant, the phenomenon of yellowing often can occur, thus have impact on the normal use of silkworm silk.
And improving constantly along with people's living standard, the requirement to silkworm silk based article is more and more higher, although natural silk has relatively
Good elasticity, but in use, owing to the Lars effect of machinery often makes silkworm silk rupture, thus have impact on silkworm silk
The planarization on surface, it is therefore desirable to improve further.
Summary of the invention
It is an object of the invention to provide the system of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation to overcome above the deficiencies in the prior art
Preparation Method, improves the resistance to oxidation of silkworm silk, fire-retardant and tensile toughness.
Technical scheme is as follows:
The preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, comprises the following steps:
Step one, joins silkworm silk in 10-15% ethanol solution, is heated to 50-60 DEG C, stirs 50-80 minute, is down to room temperature,
It is subsequently adding ethylenediamine, continues stirring 20-40 minute；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, under vacuum
It is heated to 70-80 DEG C, stirs 30-50 minute；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate aqueous solution, is heated to 40-50 DEG C, keeps 40-50
Minute；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in hypo solution, is heated under vacuum
50-60 DEG C, stir 60-100 minute；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, obtains the fire-retardant toughened silkworm silk of resistance to oxidation.
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, in step one, the quality of ethanol solution is silkworm silk
300-350 times of quality, adds 5-10 times that quality is silk quality of ethylenediamine.
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, LNBR described in step 2 and ovum
The mass ratio of phospholipid is 1-3:2-5.
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, the vacuum of vacuum condition described in step 2
For 0.01-0.05MPa.
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, the matter of dimethyl phosphate aqueous solution in step 3
Amount mark is 10-15%.
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, the hypo solution described in step 4
Mass fraction is 8-15%.
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, in step 4, the vacuum of vacuum condition is
0.01-0.05MPa。
Further, the preparation method of the fire-retardant toughened silkworm silk of described resistance to oxidation, the drying condition of step 5 is for drying temperature
80 DEG C, drying time 200-250 minute.
The present invention provide resistance to oxidation fire-retardant toughened silkworm silk elongation at break reached more than 36%, regain reached 6% with
In, it is without exception that oxidative resistance (in 5% hydrogen peroxide) has reached 500h, and anti-flammability limited oxygen index has reached more than 34.8%,
There is good pliability, oxidative resistance and anti-flammability, further expanded the range of silkworm silk.
Detailed description of the invention
Embodiment 1
The preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, comprises the following steps:
Step one, joins silkworm silk in 10% ethanol solution, is heated to 50 DEG C, stirs 50 minutes, is down to room temperature, is subsequently adding
Ethylenediamine, continues stirring 20 minutes, and wherein the quality of ethanol solution is 300 times of silk quality, adds the quality of ethylenediamine
For silk quality 5 times；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, wherein nitrile (HTBN)
The mass ratio of rubber and lecithin is 1:2, is heated to 70 DEG C under conditions of vacuum is 0.01MPa, stirs 30 minutes；
Step 3, the silkworm silk after step 2 being processed joins in the dimethyl phosphate aqueous solution that mass fraction is 10%, is heated to
40 DEG C, keep 40 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in the hypo solution that mass fraction is 8%, in vacuum
For being heated to 50 DEG C under conditions of 0.01MPa, stir 60 minutes；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 80 DEG C, drying time 200 minutes, obtains
To the fire-retardant toughened silkworm silk of resistance to oxidation.
Embodiment 2
The preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, comprises the following steps:
Step one, joins silkworm silk in 12% ethanol solution, is heated to 53 DEG C, stirs 55 minutes, is down to room temperature, is subsequently adding
Ethylenediamine, continues stirring 25 minutes, and wherein the quality of ethanol solution is 310 times of silk quality, adds the quality of ethylenediamine
For silk quality 6 times；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, wherein nitrile (HTBN)
The mass ratio of rubber and lecithin is 1:2, is heated to 73 DEG C under conditions of vacuum is 0.02MPa, stirs 36 minutes；
Step 3, the silkworm silk after step 2 being processed joins in the dimethyl phosphate aqueous solution that mass fraction is 12%, is heated to
43 DEG C, keep 42 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in the hypo solution that mass fraction is 10%, in vacuum
Degree, for being heated to 55 DEG C under conditions of 0.02MPa, stirs 70 minutes；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 80 DEG C, drying time 210 minutes, obtains
To the fire-retardant toughened silkworm silk of resistance to oxidation.
Embodiment 3
The preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, comprises the following steps:
Step one, joins silkworm silk in 13% ethanol solution, is heated to 58 DEG C, stirs 65 minutes, is down to room temperature, is subsequently adding
Ethylenediamine, continues stirring 30 minutes, and wherein the quality of ethanol solution is 320 times of silk quality, adds the quality of ethylenediamine
For silk quality 7 times；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, wherein nitrile (HTBN)
The mass ratio of rubber and lecithin is 1:1, is heated to 76 DEG C under conditions of vacuum is 0.03MPa, stirs 40 minutes；
Step 3, the silkworm silk after step 2 being processed joins in the dimethyl phosphate aqueous solution that mass fraction is 13%, is heated to
48 DEG C, keep 46 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in the hypo solution that mass fraction is 12%, in vacuum
Degree, for being heated to 58 DEG C under conditions of 0.03MPa, stirs 80 minutes；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 80 DEG C, drying time 230 minutes, obtains
To the fire-retardant toughened silkworm silk of resistance to oxidation.
Embodiment 4
The preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, comprises the following steps:
Step one, joins silkworm silk in 14% ethanol solution, is heated to 58 DEG C, stirs 70 minutes, is down to room temperature, is subsequently adding
Ethylenediamine, continues stirring 36 minutes, and wherein the quality of ethanol solution is 345 times of silk quality, adds the quality of ethylenediamine
For silk quality 8 times；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, wherein nitrile (HTBN)
The mass ratio of rubber and lecithin is 3:2, is heated to 78 DEG C under conditions of vacuum is 0.04MPa, stirs 47 minutes；
Step 3, the silkworm silk after step 2 being processed joins in the dimethyl phosphate aqueous solution that mass fraction is 14%, is heated to
50 DEG C, keep 50 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in the hypo solution that mass fraction is 14%, in vacuum
Degree, for being heated to 58 DEG C under conditions of 0.04MPa, stirs 80 minutes；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 80 DEG C, drying time 240 minutes, obtains
To the fire-retardant toughened silkworm silk of resistance to oxidation.
Embodiment 5
The preparation method of the fire-retardant toughened silkworm silk of a kind of resistance to oxidation, comprises the following steps:
Step one, joins silkworm silk in 15% ethanol solution, is heated to 60 DEG C, stirs 80 minutes, is down to room temperature, is subsequently adding
Ethylenediamine, continues stirring 40 minutes, and wherein the quality of ethanol solution is 350 times of silk quality, adds the quality of ethylenediamine
For silk quality 10 times；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, wherein nitrile (HTBN)
The mass ratio of rubber and lecithin is 1:5, is heated to 80 DEG C under conditions of vacuum is 0.05MPa, stirs 50 minutes；
Step 3, the silkworm silk after step 2 being processed joins in the dimethyl phosphate aqueous solution that mass fraction is 15%, is heated to
50 DEG C, keep 50 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in the hypo solution that mass fraction is 15%, in vacuum
Degree, for being heated to 60 DEG C under conditions of 0.05MPa, stirs 100 minutes；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 80 DEG C, drying time 250 minutes, obtains
To the fire-retardant toughened silkworm silk of resistance to oxidation.
The fire-retardant toughened silkworm silk of resistance to oxidation preparing above example carries out performance test, and result is as follows:
From above result of the test it can be seen that the resistance to oxidation fire-retardant toughened silkworm silk elongation at break that the present invention provides has reached 36%
Above, within regain has reached 6%, it is without exception that oxidative resistance (in 5% hydrogen peroxide) has reached 500h, the anti-flammability limit
Oxygen index (OI) has reached more than 34.8%, has good pliability, oxidative resistance and anti-flammability, has further expanded silkworm silk
Range.
Claims (8)
1. the preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation, it is characterised in that comprise the following steps:
Step one, joins silkworm silk in 10-15% ethanol solution, is heated to 50-60 DEG C, stirs 50-80 minute, is down to room temperature, is subsequently adding ethylenediamine, continues stirring 20-40 minute；
Step 2, silkworm silk step one obtained joins in the mixed solution of LNBR and lecithin, is heated to 70-80 DEG C under vacuum, stirs 30-50 minute；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate aqueous solution, is heated to 40-50 DEG C, keeps 40-50 minute；
Step 4, the silkworm silk after step 3 being processed takes out, and adds in hypo solution, is heated to 50-60 DEG C under vacuum, stirs 60-100 minute；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, obtains the fire-retardant toughened silkworm silk of resistance to oxidation.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that in step one, the quality of ethanol solution is 300-350 times of silk quality, adds 5-10 times that quality is silk quality of ethylenediamine.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that the mass ratio of LNBR described in step 2 and lecithin is 1-3:2-5.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that the vacuum of vacuum condition described in step 2 is 0.01-0.05MPa.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that in step 3, the mass fraction of dimethyl phosphate aqueous solution is 10-15%.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that the mass fraction of the hypo solution described in step 4 is 8-15%.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that in step 4, the vacuum of vacuum condition is 0.01-0.05MPa.
The preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation the most according to claim 1, it is characterised in that the drying condition of step 5 is for drying temperature 80 DEG C, drying time 200-250 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410837132.XA CN104562638B (en) | 2014-12-29 | 2014-12-29 | A kind of preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410837132.XA CN104562638B (en) | 2014-12-29 | 2014-12-29 | A kind of preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104562638A CN104562638A (en) | 2015-04-29 |
| CN104562638B true CN104562638B (en) | 2017-01-04 |
Family
ID=53079660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410837132.XA Active CN104562638B (en) | 2014-12-29 | 2014-12-29 | A kind of preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104562638B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107164963A (en) * | 2017-05-31 | 2017-09-15 | 句容市恒鑫遮阳科技有限公司 | A kind of fire-retardant uvioresistant window curtain fabric and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5311682A (en) * | 1976-05-26 | 1978-02-02 | Aoyama Kk | Material for artificral flower |
| CN1990533A (en) * | 2005-12-28 | 2007-07-04 | 上海日之升新技术发展有限公司 | Halogen-free flame-proof toughening polypropylene composition and preparation process thereof |
| CN102966803A (en) * | 2012-12-05 | 2013-03-13 | 青岛鑫万通塑业发展有限公司 | High strength PVC (Polyvinyl Chloride) tube |
| CN103572395B (en) * | 2013-11-14 | 2015-08-12 | 东华大学 | A kind of activeness and quietness regenerated silk fiber and preparation method thereof |
-
2014
- 2014-12-29 CN CN201410837132.XA patent/CN104562638B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104562638A (en) | 2015-04-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101229117B1 (en) | Manufacturing method of ramie-reinforced natural yarns | |
| CN105420926A (en) | Anti-radiation fabric | |
| CN104562638B (en) | A kind of preparation method of the fire-retardant toughened silkworm silk of resistance to oxidation | |
| CN107099089A (en) | A kind of graphene master batch with antistatic behaviour and its preparation method and application | |
| CN106958139A (en) | A kind of antipilling fabric and preparation method thereof | |
| CN104562665B (en) | A kind of preparation method of acid and alkali-resistance flame-retardant silk | |
| CN103653318A (en) | Woolen sweater and production method thereof | |
| CN103132327B (en) | Sizing agent applied to constant SiC (Silicon Carbide) fiber and preparation method and application thereof | |
| CN103382660A (en) | Dyeing and finishing process for protein garment materials | |
| CN108589296A (en) | A kind of flame-proof antibiotic high performance garment fabric and preparation method thereof | |
| CN110699963B (en) | Waterproof and scratch-resistant baby stroller bag hanging fabric and preparation method thereof | |
| CN205741416U (en) | One washs fiber crops blending multifunction sofa fabric | |
| CN106498707A (en) | A kind of preparation method of simple conductive silk fiber | |
| CN103451839A (en) | Moisture-absorption moisture-transfer comfortable and cool knitted fabric | |
| CN105951258A (en) | Radiation-proof garment fabric | |
| CN109868547A (en) | The high-elastic high reply of one kind is with the elastic plain weave fabric of idea weft knitting | |
| CN104611865B (en) | A kind of dyeing silk pre-treating technology | |
| CN107142550B (en) | A kind of preparation method of the fiber of thread sliding underwear fabric | |
| CN108342785B (en) | Application of graphene in preparation of soybean protein fiber and fabric thereof | |
| CN208151580U (en) | A kind of acetate fiber Silk knitting fabric | |
| CN113119549A (en) | Antistatic radiation-proof graphene modified fiber fabric and preparation process thereof | |
| CN105926297A (en) | Preparation technology of anti-static underwear fabric | |
| CN112137186A (en) | Volcanic self-heating trousers and production process thereof | |
| CN106757675A (en) | A kind of children are next to the skin to perspire ventilative cotton face fabric | |
| CN110359172A (en) | A kind of far infrared deodorization knitted side preparation method for material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 214011 Jiangsu province Wuxi chonganou mount a horse Pier Road No. 18 building 1201 room A Patentee after: Wuxi silkworm charm Biotechnology Co., Ltd. Address before: 214011 Jiangsu province Wuxi chonganou mount a horse Pier Road No. 18 building 1201 room A Patentee before: WUXI CANMEI TECHNOLOGY CO., LTD. |