CN104562665A - Preparation method of acid-alkali resistant flame-retardant silk - Google Patents
Preparation method of acid-alkali resistant flame-retardant silk Download PDFInfo
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- CN104562665A CN104562665A CN201410833633.0A CN201410833633A CN104562665A CN 104562665 A CN104562665 A CN 104562665A CN 201410833633 A CN201410833633 A CN 201410833633A CN 104562665 A CN104562665 A CN 104562665A
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Abstract
The invention discloses a preparation method of an acid-alkali resistant flame-retardant silk. The preparation method comprises the following steps: adding a silk to deionized water to obtain a mixture; heating the mixture and then cooling the heated mixture to a room temperature; adding 1mol/L of an NaOH solution; heating and stirring the mixture added with the NaOH solution, and adding the heated and stirred mixture to a barium chloride solution; heating and stirring the obtained mixture under a vacuum condition, adding the heated and stirred mixture to dimethyl phosphate, heating the obtained mixture to 40-50 DEG C and keeping the temperature for 50-80 minutes; taking out the silk, adding the silk to a mixture of boric acid double glyceride and isoamyl acetate, heating the mixture with the silk under a vacuum condition to 80-90 DEG C and keeping the temperature for 40-60 minutes; finally, taking out the silk, and drying the silk so as to obtain the acid-alkali resistant flame-retardant silk. The acid-alkali resistant flame-retardant silk provided by the invention has good performances, wherein the elongation at breaks is higher than 23%, the moisture regaining rate is within 7%, the prepared silk has normal acid resistance within 800h, and has normal alkali resistance within 500h, and a limit oxygen index is higher than 34.6%.
Description
Technical field
The invention belongs to chemical fibre product modification field, be specifically related to a kind of preparation method of acid and alkali-resistance flame-retardant silk.
Background technology
Silk is matured silkworm secreted silk liquid concretionary continuous fiber when cocooing, and also claiming natural silk, is a kind of natural fabric, is one of human use's animal fiber the earliest.According to archaeological discovery, before 4700, China has utilized silk to manufacture silk thread, braided wires silk cocoon silk band and simple silk goods.Shang and Zhou Dynasty silk knits the silk goods such as sieve processed, thin silk fabric, fine silk fabrics, yarn, crape, figured woven silk material, brocade, embroidery.Silkworm has silkworm, tussah, castor silkworm, cassava silkworm, willow silkworm and giant silkworm etc.The strand taken out by single silk cocoon claims silk.It borrows silk gum to bond coated forming by two filaments.During filature, the silk of several silk cocoon is extracted out, is bonded into strand by means of silk gum, be referred to as silk.The silk of removing silk gum, claims nett silk.What in silk, consumption was maximum is mulberry silk, is secondly tussah silk, and other silks do not form resource because of limited amount.Silk light weight and elongated, fabric sheen is good, comfortable and easy to wear, and feel is smooth plentiful, poor heat conductivity, and moisture absorption is breathed freely, 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 more than 90% of world wide production.
Current silk, in application process, because it belongs to inflammable articles, when carrying out testing vertical flammability, just burning up completely in igniting 15s, therefore how can carry out a large amount of research and development by fire-retardant needs for its needs for it.Meanwhile, silk is amphoteric compound, can act under certain condition with acid, again can with alkali effect, especially in the weak solution of highly basic, under normal temperature, also can there is the hydrolysis of fibroin albumen.This refining for silk and dyeing have larger impact, therefore need the performance of silk is carried out to research further and improved, and make it have more stable performance, thus are applied even more extensively with daily life.
Summary of the invention
The object of the invention is to the preparation method that a kind of acid and alkali-resistance flame-retardant silk is provided to overcome above the deficiencies in the prior art, improving acid-proof alkaline and the fire resistance of silk.
The present invention adopts following technological means to realize:
A preparation method for acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, joins silk in deionized water, is heated to 70-80 DEG C, keeps 30-40 minute, is down to room temperature, then adds the NaOH solution of 1mol/L, be heated to 50-60 DEG C, stirs 20-30 minute;
Step 2, silk step one obtained joins in barium chloride solution, is heated to 60-70 DEG C under vacuum, stirs 40-60 minute;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 40-50 DEG C, keeps 50-80 minute; Step 4, takes out the silk after step 3 process, joins in the mixture of boric acid double glyceride and isoamyl acetate, be heated to 80-90 DEG C under vacuum, keeps 40-60 minute;
Step 5, takes out the silk after step 4 process, 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 the 200-300 of silk quality times, and the quality adding NaOH solution can be the 10-20 of silk quality times.
The preparation method of described acid and alkali-resistance flame-retardant silk, the speed stirred in step one 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 preparation method of described acid and alkali-resistance flame-retardant silk, in the boric acid double glyceride described in step 4 and the mixture of isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate can be 1-3:3-5.
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 bake out temperature 60-80 DEG C, drying time 250-300 minute.
Acid and alkali-resistance flame-retardant silk provided by the invention has good performance, wherein elongation at break reaches more than 23%, regain reaches within 7%, it is without exception that acid resistance reaches 800h, it is without exception that alkali resistance reaches 500h, limited oxygen index reaches more than 34.6%, close to the fire-retardant index 35% of non-combustible matter.
Detailed description of the invention
Embodiment 1
A preparation method for acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, silk is joined in deionized water, be heated to 70 DEG C, keep 30 minutes, be down to room temperature, then the NaOH solution of 1mol/L is added, be heated to 50 DEG C, stir 20 minutes, mixing speed is 100 revs/min, the quality of the deionized water wherein added is 200 times of silk quality, and the quality adding NaOH solution is 10 times of silk quality;
Step 2, silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 10%, is heated to 60 DEG C under vacuum is 0.02MPa condition, stirs 40 minutes;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 40 DEG C, keeps 50 minutes;
Step 4, silk after step 3 process is taken out, join in the mixture of boric acid double glyceride and isoamyl acetate, 80 DEG C are heated under vacuum is 0.01MPa condition, keep 40 minutes, in the mixture of its mesoboric acid double glyceride and isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate is 1:3;
Step 5, takes out the silk after step 4 process, and dry, wherein bake out temperature 60 DEG C, drying time 250 minutes, obtains acid and alkali-resistance flame-retardant silk.
Embodiment 2
A preparation method for acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, silk is joined in deionized water, be heated to 72 DEG C, keep 35 minutes, be down to room temperature, then the NaOH solution of 1mol/L is added, be heated to 53 DEG C, stir 24 minutes, mixing speed is 108 revs/min, the quality of the deionized water wherein added is 230 times of silk quality, and the quality adding NaOH solution is 12 times of silk quality;
Step 2, silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 12%, is heated to 65 DEG C under vacuum is 0.03MPa condition, stirs 48 minutes;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 45 DEG C, keeps 60 minutes;
Step 4, silk after step 3 process is taken out, join in the mixture of boric acid double glyceride and isoamyl acetate, 84 DEG C are heated under vacuum is 0.02MPa condition, keep 45 minutes, in the mixture of its mesoboric acid double glyceride and isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate is 2:3;
Step 5, takes out the silk after step 4 process, and dry, wherein bake out temperature 66 DEG C, drying time 270 minutes, obtains acid and alkali-resistance flame-retardant silk.
Embodiment 3
A preparation method for acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, silk is joined in deionized water, be heated to 76 DEG C, keep 37 minutes, be down to room temperature, then the NaOH solution of 1mol/L is added, be heated to 55 DEG C, stir 27 minutes, mixing speed is 112 revs/min, the quality of the deionized water wherein added is 260 times of silk quality, and the quality adding NaOH solution is 17 times of silk quality;
Step 2, silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 13%, is heated to 68 DEG C under vacuum is 0.04MPa condition, stirs 52 minutes;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 45 DEG C, keeps 70 minutes;
Step 4, silk after step 3 process is taken out, join in the mixture of boric acid double glyceride and isoamyl acetate, 88 DEG C are heated under vacuum is 0.04MPa condition, keep 55 minutes, in the mixture of its mesoboric acid double glyceride and isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate is 1:1;
Step 5, takes out the silk after step 4 process, and dry, wherein bake out temperature 78 DEG C, drying time 280 minutes, obtains acid and alkali-resistance flame-retardant silk.
Embodiment 4
A preparation method for acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, silk is joined in deionized water, be heated to 80 DEG C, keep 40 minutes, be down to room temperature, then the NaOH solution of 1mol/L is added, be heated to 58 DEG C, stir 27 minutes, mixing speed is 120 revs/min, the quality of the deionized water wherein added is 280 times of silk quality, and the quality adding NaOH solution is 17 times of silk quality;
Step 2, silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 14%, is heated to 70 DEG C under vacuum is 0.04MPa condition, stirs 58 minutes;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 46 DEG C, keeps 75 minutes;
Step 4, silk after step 3 process is taken out, join in the mixture of boric acid double glyceride and isoamyl acetate, 90 DEG C are heated under vacuum is 0.04MPa condition, keep 56 minutes, in the mixture of its mesoboric acid double glyceride and isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate is 1:5;
Step 5, takes out the silk after step 4 process, and dry, wherein bake out temperature 75 DEG C, drying time 300 minutes, obtains acid and alkali-resistance flame-retardant silk.
Embodiment 5
A preparation method for acid and alkali-resistance flame-retardant silk, comprises the following steps:
Step one, silk is joined in deionized water, be heated to 80 DEG C, keep 40 minutes, be down to room temperature, then the NaOH solution of 1mol/L is added, be heated to 60 DEG C, stir 30 minutes, mixing speed is 120 revs/min, the quality of the deionized water wherein added is 300 times of silk quality, and the quality adding NaOH solution is 20 times of silk quality;
Step 2, silk step one obtained joins in barium chloride solution, and the mass fraction of barium chloride solution is 15%, is heated to 70 DEG C under vacuum is 0.05MPa condition, stirs 60 minutes;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 50 DEG C, keeps 80 minutes;
Step 4, silk after step 3 process is taken out, join in the mixture of boric acid double glyceride and isoamyl acetate, 90 DEG C are heated under vacuum is 0.04MPa condition, keep 60 minutes, in the mixture of its mesoboric acid double glyceride and isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate is 3:5;
Step 5, takes out the silk after step 4 process, and dry, wherein bake out temperature 80 DEG C, drying time 300 minutes, obtains acid and alkali-resistance flame-retardant silk.
Carry out performance test to the acid and alkali-resistance flame-retardant silk that above embodiment prepares, result is as follows:
Can be learnt by the result in upper table, acid and alkali-resistance flame-retardant silk provided by the invention has good performance, wherein elongation at break reaches more than 23%, regain reaches within 7%, it is without exception that acid resistance reaches 800h, it is without exception that alkali resistance reaches 500h, and limited oxygen index reaches more than 34.6%, close to the fire-retardant index 35% of non-combustible matter.
Claims (8)
1. a preparation method for acid and alkali-resistance flame-retardant silk, is characterized in that, comprises the following steps:
Step one, joins silk in deionized water, is heated to 70-80 DEG C, keeps 30-40 minute, is down to room temperature, then adds the NaOH solution of 1mol/L, be heated to 50-60 DEG C, stirs 20-30 minute;
Step 2, silk step one obtained joins in barium chloride solution, is heated to 60-70 DEG C under vacuum, stirs 40-60 minute;
Step 3, joins in dimethyl phosphate by the silk after step 2 process, is heated to 40-50 DEG C, keeps 50-80 minute;
Step 4, takes out the silk after step 3 process, joins in the mixture of boric acid double glyceride and isoamyl acetate, be heated to 80-90 DEG C under vacuum, keeps 40-60 minute;
Step 5, takes out the silk after step 4 process, dries, obtains acid and alkali-resistance flame-retardant silk.
2. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, the quality of the deionized water added in step one is 200-300 times of silk quality, and the quality adding NaOH solution is 10-20 times of silk quality.
3. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, the speed stirred in step one is 100-120 rev/min.
4. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, the mass fraction of barium chloride solution described in step 2 is 10-15%.
5. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, in step 2, the vacuum of vacuum condition is 0.02-0.05MPa.
6. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, in the boric acid double glyceride described in step 4 and the mixture of isoamyl acetate, the mass ratio of boric acid double glyceride and isoamyl acetate is 1-3:3-5.
7. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, in step 4, the vacuum of vacuum condition is 0.01-0.04MPa.
8. the preparation method of acid and alkali-resistance flame-retardant silk according to claim 1, is characterized in that, the drying condition of step 5 is bake out temperature 60-80 DEG C, drying time 250-300 minute.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61192791A (en) * | 1985-02-22 | 1986-08-27 | Kuraray Co Ltd | Flame retardant composition |
| CN1191905A (en) * | 1998-04-09 | 1998-09-02 | 俞祥根 | Silk fiber pretreatment process and product thereof |
| 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 |
| CN101613935A (en) * | 2009-08-05 | 2009-12-30 | 辽宁恒星精细化工（集团）有限公司 | Organic boron antiflaming finishing agent for fabrics and preparation method thereof |
| CN102560696A (en) * | 2011-11-29 | 2012-07-11 | 湖州市农业科学研究院 | Production method of natural colorful mulberry silk floss |
| CN102660868A (en) * | 2012-04-10 | 2012-09-12 | 浙江好运来集团有限公司 | Silkworm silk flame retardant aid and flame retardation arrangement method |
| 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 |
| CN103061132A (en) * | 2012-12-28 | 2013-04-24 | 苏州市华智顾纺织有限公司 | Method for manufacturing flame retardant silk fabric |
| CN103061121A (en) * | 2013-01-28 | 2013-04-24 | 达利(中国)有限公司 | Environmental-friendly flame-retardant finishing technology of real silk or real silk cellulosic fiber interwoven fabric |
-
2014
- 2014-12-29 CN CN201410833633.0A patent/CN104562665B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61192791A (en) * | 1985-02-22 | 1986-08-27 | Kuraray Co Ltd | Flame retardant composition |
| CN1191905A (en) * | 1998-04-09 | 1998-09-02 | 俞祥根 | Silk fiber pretreatment process and product thereof |
| 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 |
| CN101613935A (en) * | 2009-08-05 | 2009-12-30 | 辽宁恒星精细化工（集团）有限公司 | Organic boron antiflaming finishing agent for fabrics and preparation method thereof |
| CN102560696A (en) * | 2011-11-29 | 2012-07-11 | 湖州市农业科学研究院 | Production method of natural colorful mulberry silk floss |
| CN102660868A (en) * | 2012-04-10 | 2012-09-12 | 浙江好运来集团有限公司 | Silkworm silk flame retardant aid and flame retardation arrangement method |
| 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 |
| CN103061132A (en) * | 2012-12-28 | 2013-04-24 | 苏州市华智顾纺织有限公司 | Method for manufacturing flame retardant silk fabric |
| CN103061121A (en) * | 2013-01-28 | 2013-04-24 | 达利(中国)有限公司 | Environmental-friendly flame-retardant finishing technology of real silk or real silk cellulosic fiber interwoven fabric |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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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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