CN104562665B - A kind of preparation method of acid and alkali-resistance flame-retardant silk - Google Patents
A kind of preparation method of acid and alkali-resistance flame-retardant silk Download PDFInfo
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- CN104562665B CN104562665B CN201410833633.0A CN201410833633A CN104562665B CN 104562665 B CN104562665 B CN 104562665B CN 201410833633 A CN201410833633 A CN 201410833633A CN 104562665 B CN104562665 B CN 104562665B
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Abstract
The invention discloses the preparation method of a kind of acid and alkali-resistance flame-retardant silk, first silkworm silk is joined in deionized water, room temperature it is down to after heating, it is subsequently adding the NaOH solution of 1mol/L, join after heated and stirred in barium chloride solution, heated and stirred joins in dimethyl phosphate after processing under vacuum, it is heated to 40 50 DEG C, keep 50 80 minutes, then silkworm silk is taken out, join in the mixture of boric acid double glyceride and isoamyl acetate, it is heated to 80 90 DEG C under vacuum, keep 40 60 minutes, finally silkworm silk is taken out, dry, obtain acid and alkali-resistance flame-retardant silk.The acid and alkali-resistance flame-retardant silk that the present invention provides has good performance, and wherein elongation at break has reached more than 23%, and within regain has reached 7%, it is without exception that acid resistance has reached 800h, and it is without exception that alkali resistance has reached 500h, and limited oxygen index has reached more than 34.6%.
Description
Technical field
The invention belongs to chemical fibre product modification field, be specifically related to the preparation method of a kind of acid and alkali-resistance flame-retardant silk.
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,
It it is one of human use's animal fiber the earliest.According to archaeological discovery, about before 4700 China utilized silkworm silk 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, brocade,
The silks such as embroidery.Silkworm has Bombyxmori Linnaeus, Antherea pernyi Guerin-Meneville, Semen Ricini silkworm, cassava silkworm, willow silkworm and giant silkworm etc..The strand being pumped by single Bombyx bombycis
Claim silk.It is borrowed sericin bonding cladding to form by two ultimate fibres.During filature, the silk of several Bombyx bombycis is extracted out, by means of sericin
It 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, secondly
Being tussah silk, other silkworm silks do not form resource because of limited amount.Silkworm silk light weight and elongated, fabric sheen is good, comfortable and easy to wear,
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 doctor
The fields such as medicine.China, Japan, India, the former Soviet Union and Korea are main Chan Si states, and total output accounts for more than the 90% of world wide production.
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
It is amphoteric compound, under certain condition can be with acid effect, again can be with alkali effect, especially in the weak solution of highly basic, often
The hydrolysis of fibroin albumen also can occur under temperature.This has large effect for refine and the dyeing of silkworm silk, it is therefore desirable to silkworm silk
Performance study further and improve so that it is there is more stable performance, thus be applied even more extensively the day with people
Often in life.
Summary of the invention
It is an object of the invention to provide the preparation side of a kind of acid and alkali-resistance flame-retardant silk to overcome above the deficiencies in the prior art
Method, improves acid-proof alkaline and the fire resistance of silkworm silk.
The present invention is to use techniques below means to realize:
The preparation method of a kind of acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silkworm silk in deionized water, is heated to 70-80 DEG C, keeps 30-40 minute, is down to room temperature, then adds
Enter the NaOH solution of 1mol/L, be heated to 50-60 DEG C, stir 20-30 minute；
Step 2, silkworm silk step one obtained joins in barium chloride solution, is heated to 60-70 DEG C under vacuum, stirring
40-60 minute；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 40-50 DEG C, keeps 50-80 minute；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate,
Heated under vacuum, to 80-90 DEG C, keeps 40-60 minute；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, obtains acid and alkali-resistance flame-retardant silk.
The preparation method of described acid and alkali-resistance flame-retardant silk, the quality of the deionized water added in step one can be silk quality
200-300 times, the quality adding NaOH solution can be 10-20 times of silk quality.
The preparation method of described acid and alkali-resistance flame-retardant silk, in step one, the speed of stirring can be 100-120 rev/min.
The preparation method of described acid and alkali-resistance flame-retardant silk, the mass fraction of barium chloride solution described in step 2 can be
10-15%.
The preparation method of described acid and alkali-resistance flame-retardant silk, in step 2, the vacuum of vacuum condition can be 0.02-0.05MPa.
The mixing of the preparation method of described acid and alkali-resistance flame-retardant silk, the boric acid double glyceride described in step 4 and isoamyl acetate
In thing, boric acid double glyceride can be 1-3:3-5 with the mass ratio of isoamyl acetate.
The preparation method of described acid and alkali-resistance flame-retardant silk, in step 4, the vacuum of vacuum condition can be 0.01-0.04MPa.
The preparation method of described acid and alkali-resistance flame-retardant silk, the drying condition of step 5 can be to dry temperature 60-80 DEG C, dries
250-300 minute time.
The acid and alkali-resistance flame-retardant silk that the present invention provides has good performance, and wherein elongation at break has reached more than 23%, returns
Within tide rate has reached 7%, it is without exception that acid resistance has reached 800h, and it is without exception that alkali resistance has reached 500h, limited oxygen index
Reach more than 34.6%, close to the fire-retardant index 35% of non-combustible matter.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silkworm silk in deionized water, is heated to 70 DEG C, keeps 30 minutes, is down to room temperature, is subsequently adding 1mol/L
NaOH solution, be heated to 50 DEG C, stir 20 minutes, mixing speed is 100 revs/min, the deionization wherein added
The quality of water is 200 times of silk quality, adds quality is silk quality 10 times of NaOH solution；
Step 2, silkworm silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 10%, very
Reciprocal of duty cycle is to be heated to 60 DEG C under the conditions of 0.02MPa, stirs 40 minutes；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 40 DEG C, keeps 50 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate,
Vacuum is to be heated to 80 DEG C under the conditions of 0.01MPa, keeps 40 minutes, its mesoboric acid double glyceride and isoamyl acetate
In mixture, boric acid double glyceride is 1:3 with the mass ratio of isoamyl acetate；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 60 C, drying time 250 minutes, obtains
To acid and alkali-resistance flame-retardant silk.
Embodiment 2
The preparation method of a kind of acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silkworm silk in deionized water, is heated to 72 DEG C, keeps 35 minutes, is down to room temperature, is subsequently adding 1mol/L
NaOH solution, be heated to 53 DEG C, stir 24 minutes, mixing speed is 108 revs/min, the deionization wherein added
The quality of water is 230 times of silk quality, adds quality is silk quality 12 times of NaOH solution；
Step 2, silkworm silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 12%, very
Reciprocal of duty cycle is to be heated to 65 DEG C under the conditions of 0.03MPa, stirs 48 minutes；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 45 DEG C, keeps 60 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate,
Vacuum is to be heated to 84 DEG C under the conditions of 0.02MPa, keeps 45 minutes, its mesoboric acid double glyceride and isoamyl acetate
In mixture, boric acid double glyceride is 2:3 with the mass ratio of isoamyl acetate；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 66 DEG C, drying time 270 minutes, obtains
To acid and alkali-resistance flame-retardant silk.
Embodiment 3
The preparation method of a kind of acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silkworm silk in deionized water, is heated to 76 DEG C, keeps 37 minutes, is down to room temperature, is subsequently adding 1mol/L
NaOH solution, be heated to 55 DEG C, stir 27 minutes, mixing speed is 112 revs/min, the deionization wherein added
The quality of water is 260 times of silk quality, adds quality is silk quality 17 times of NaOH solution；
Step 2, silkworm silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 13%, very
Reciprocal of duty cycle is to be heated to 68 DEG C under the conditions of 0.04MPa, stirs 52 minutes；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 45 DEG C, keeps 70 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate,
Vacuum is to be heated to 88 DEG C under the conditions of 0.04MPa, keeps 55 minutes, its mesoboric acid double glyceride and isoamyl acetate
In mixture, boric acid double glyceride is 1:1 with the mass ratio of isoamyl acetate；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 78 DEG C, drying time 280 minutes, obtains
To acid and alkali-resistance flame-retardant silk.
Embodiment 4
The preparation method of a kind of acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silkworm silk in deionized water, is heated to 80 DEG C, keeps 40 minutes, is down to room temperature, is subsequently adding 1mol/L
NaOH solution, be heated to 58 DEG C, stir 27 minutes, mixing speed is 120 revs/min, the deionization wherein added
The quality of water is 280 times of silk quality, adds quality is silk quality 17 times of NaOH solution；
Step 2, silkworm silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 14%, very
Reciprocal of duty cycle is to be heated to 70 DEG C under the conditions of 0.04MPa, stirs 58 minutes；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 46 DEG C, keeps 75 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate,
Vacuum is to be heated to 90 DEG C under the conditions of 0.04MPa, keeps 56 minutes, its mesoboric acid double glyceride and isoamyl acetate
In mixture, boric acid double glyceride is 1:5 with the mass ratio of isoamyl acetate；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 75 DEG C, drying time 300 minutes, obtains
To acid and alkali-resistance flame-retardant silk.
Embodiment 5
The preparation method of a kind of acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silkworm silk in deionized water, is heated to 80 DEG C, keeps 40 minutes, is down to room temperature, is subsequently adding 1mol/L
NaOH solution, be heated to 60 DEG C, stir 30 minutes, mixing speed is 120 revs/min, the deionization wherein added
The quality of water is 300 times of silk quality, adds quality is silk quality 20 times of NaOH solution；
Step 2, silkworm silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 15%, very
Reciprocal of duty cycle is to be heated to 70 DEG C under the conditions of 0.05MPa, stirs 60 minutes；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 50 DEG C, keeps 80 minutes；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate,
Vacuum is to be heated to 90 DEG C under the conditions of 0.04MPa, keeps 60 minutes, its mesoboric acid double glyceride and isoamyl acetate
In mixture, boric acid double glyceride is 3:5 with the mass ratio of isoamyl acetate；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, and wherein dries temperature 80 DEG C, drying time 300 minutes, obtains
To acid and alkali-resistance flame-retardant silk.
The acid and alkali-resistance flame-retardant silk preparing above example carries out performance test, and result is as follows:
By the result in upper table it is known that the acid and alkali-resistance flame-retardant silk that the present invention provides has good performance, wherein rupture
Percentage elongation has reached more than 23%, and within regain has reached 7%, it is without exception that acid resistance has reached 800h, and alkali resistance reaches
500h is without exception, and limited oxygen index has reached more than 34.6%, close to the fire-retardant index 35% of non-combustible matter.
Claims (7)
1. the preparation method of an acid and alkali-resistance flame-retardant silk, it is characterised in that comprise the following steps:
Step one, joins silkworm silk in deionized water, is heated to 70-80 DEG C, keeps 30-40 minute, is down to room temperature, be subsequently adding the NaOH solution of 1mol/L, is heated to 50-60 DEG C, stirs 20-30 minute；
Step 2, silkworm silk step one obtained joins in barium chloride solution, is heated to 60-70 DEG C under vacuum, stirs 40-60 minute；
Step 3, the silkworm silk after step 2 being processed joins in dimethyl phosphate, is heated to 40-50 DEG C, keeps 50-80 minute；
Step 4, the silkworm silk after step 3 being processed takes out, and joins in the mixture of boric acid double glyceride and isoamyl acetate, is heated to 80-90 DEG C under vacuum, keeps 40-60 minute；
Step 5, the silkworm silk after step 4 being processed takes out, and dries, obtains acid and alkali-resistance flame-retardant silk；
Wherein the mass fraction of barium chloride solution described in step 2 is 10-15%.
The preparation method of acid and alkali-resistance flame-retardant silk the most according to claim 1, it is characterised in that 200-300 times that quality is silk quality of the deionized water added in step one, adds 10-20 times that quality is silk quality of NaOH solution.
The preparation method of acid and alkali-resistance flame-retardant silk the most according to claim 1, it is characterised in that in step one, the speed of stirring is 100-120 rev/min.
The preparation method of acid and alkali-resistance flame-retardant silk the most according to claim 1, it is characterised in that in step 2, the vacuum of vacuum condition is 0.02-0.05MPa.
The preparation method of acid and alkali-resistance flame-retardant silk the most according to claim 1, it is characterised in that the boric acid double glyceride described in step 4 is with the mixture of isoamyl acetate, and boric acid double glyceride is 1-3:3-5 with the mass ratio of isoamyl acetate.
The preparation method of acid and alkali-resistance flame-retardant silk the most according to claim 1, it is characterised in that in step 4, the vacuum of vacuum condition is 0.01-0.04MPa.
The preparation method of acid and alkali-resistance flame-retardant silk the most according to claim 1, it is characterised in that the drying condition of step 5 is for drying temperature 60-80 DEG C, drying time 250-300 minute.
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| CN109235020A (en) * | 2018-08-17 | 2019-01-18 | 安徽三利丝绸集团有限公司 | A kind of processing method improving the acidproof alkali ability of mulberry silk |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS61192791A (en) * | 1985-02-22 | 1986-08-27 | Kuraray Co Ltd | Flame retardant composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1191905A (en) * | 1998-04-09 | 1998-09-02 | 俞祥根 | Silk fibre pretreating process and product |
| CN1923090A (en) * | 2006-09-11 | 2007-03-07 | 潘新平 | Manufacturing method of washable mulberry silk quilt |
| CN101381959A (en) * | 2008-09-01 | 2009-03-11 | 林德方 | Method for producing flame-retardant silk |
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| CN103061122A (en) * | 2012-12-28 | 2013-04-24 | 苏州市华智顾纺织有限公司 | Method for producing flame retardant silk fabric |
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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. |
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