CN101440574B - Oil solution for spandex spinning by dry method, and preparation and use thereof - Google Patents
Oil solution for spandex spinning by dry method, and preparation and use thereof Download PDFInfo
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- CN101440574B CN101440574B CN2008102072348A CN200810207234A CN101440574B CN 101440574 B CN101440574 B CN 101440574B CN 2008102072348 A CN2008102072348 A CN 2008102072348A CN 200810207234 A CN200810207234 A CN 200810207234A CN 101440574 B CN101440574 B CN 101440574B
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Abstract
The invention relates to a preparation agent for dry method urethane elastic fiber spinning. The preparation agent comprises the following components: silicone resin, methyl silicone oil, modification silicone oil, mineral oil and antistatic agent. The preparation method comprises the following steps: 1, silicane chain links(M, X, Y and Z) are mixed and evenly stirred, started, added with acid water at a temperature of 25 DEG C and reacted for 1 hour at the temperature of between 60 and 70 DEG C, stirring stops, after layering, the resin on the lower layer is separated out, the pH value of the resin is neutral by washing, and the resin is subjected to vacuum pumping, temperature rise and dewatering to prepare the silicone resin; and 2, the silicone resin, the methyl silicone oil, the polyether modification silicone oil, the mineral oil and the antistatic agent are placed in a stirring kettle, and evenly mixed at the temperature of between 10 and 50 DEG to obtain. The application of the preparation agent is as follows: the preparation agent is put in a storage tank and transferred to an oil nozzle or roller by an oil pump, and the urethane elastic fiber is directly contacted and oiled. The preparation agent for dry method urethane elastic fiber spinning is transparent liquid, does not contain solid particle components such as hard ester acid magnesium and the like, does not plug pipes and equipment in the oiling process, and does not need power-off cleaning, thereby improving production efficiency.
Description
Technical field
The invention belongs to the preparation field of fiber, particularly relate to a kind of oil solution for spandex spinning by dry and its production and application with finish.
Background technology
Polyurethane elastomeric fiber, i.e. spandex, because its excellent elasticity and good comprehensive performances, its production and application have obtained development fast in the several years in the past.National spandex output was above 200,000 tons in 2007.
Polyurethane elastomeric fiber, owing to have the carbamate polar group in its fibrous molecular structure, when giving the fibrous elasticity performance, also make between the spandex silk and easily stick together, if there is not good suitable oil solution for spandex spinning, bring serious problems then can for spandex fiber operation and processed and applied thereafter.Spandex fiber technology mainly contains dry spinning, melt spinning and wet spinning etc., and wherein dry spinning accounts for 80%.Spandex oil agent oils by atomizer or roller, forms layer protecting film on spandex silk fiber surface, prevents to produce adhesion between silk and the silk.The spinning cake forming that good finish is spun into after the spandex silk is oiled, silk thread has good flatness, convergence and antistatic behaviour, makes the easily unwinding in the process of back of spandex spinning cake, not fracture of wire, sliding limit, i.e. good processability simultaneously.
Present domestic spandex manufacturing enterprise, most for introducing technology in recent years and equipment, used finish is also accordingly based on imported product.The development of examination spandex oil agent, experienced following several stages technically: in the early stage of development, use similar other synthetic fiber finish, its component is essentially petrochemical industry class surfactant.The main finish composition that shows in the special public clear 44-8907 bulletin as Misshin Spinning Co., Ltd exploitation is mineral oil and fatty acid ester material, and its application result is that spinnability is poor, thread unwinding tension big and irregular one; Finish afterwards progressively begins to add silicone oil and modified silicon oil as the anti component, shown in the special public clear 57-128276 of Toyo Boseki K.K, its key component is mineral oil, silicone oil, polyether modified silicon oil, fatty acid ester material, although this type of finish quality has had large increase, but because the low surface tension of silicone oil, still there is an easily landing of silk, defective such as the inside and outside unwinding power difference of spinning cake is big; Patent (special public clear 41-286, special public clear 40-5557, publication number CN 1696395A etc.) report is also arranged, in finish, add the slaine of higher fatty acids, as magnesium stearate solid powder, as the antiseized component of spandex silk, but there is the sedimentation of magnesium stearate solid in the practical application and stops up problem such as finish pipeline.This shows, develop high-quality spandex fiber finish, especially oil solution for spandex spinning by dry,, promote that the development of spandex industry is significant for the quality that improves the spandex silk.
Summary of the invention
Technical problem to be solved by this invention provides a kind of oil solution for spandex spinning by dry and its production and application, oil solution for spandex spinning by dry of the present invention is a colourless transparent liquid, do not contain solid particulate components such as magnesium stearate, the process that oils can blocking pipe and equipment, the dispense with parking cleaning, improved production efficiency, be applicable to multiple spandex spinning by dry technology, the inside and outside unwinding tension of spinning cake is even, antistatic property is good, be difficult for falling silk and fracture of wire, the comprehensive backing-off performance in the process of back is good.
A kind of oil solution for spandex spinning by dry of the present invention, its component comprises: methyl-silicone oil, modified silicon oil, mineral oil and the antistatic additive of organic siliconresin, viscosity 1～50mPa.s; Its mass ratio is: 1%～30%: 10%～60%: 1%～20%: 10%～60%: 0.5%～10%.
Described a kind of oil solution for spandex spinning by dry, wherein the mass ratio of organic siliconresin, methyl-silicone oil, modified silicon oil, mineral oil and antistatic additive is: 5%～20%: 20%～50%: 5%～15%: 20%～40%: 1%～5%;
Described oil solution for spandex spinning by dry is a water white transparency, does not have visible solid particle, viscosity 5～20mPa.s;
The general formula of described organic siliconresin compound is:
Me
2 Me
| |
[Si?O
1/2]
M[Si?O
2/2]
X[Si?O
3/2]
Y[Si?O
4/2]
Z (1)
| | |
R
1 R
2 R
3
Me is a methyl in the formula; R
1Be methyl, ethyl, phenyl or chloromethyl; R
2Be methyl, ethyl or phenyl; R
3Be methyl, ethyl, phenyl, hydroxyl or chain alkyl;
MXYZ in the described organic siliconresin compound general formula (1) is for forming the silane chain link of this resin, and its mol ratio is M: X: Y: Z=0.05～0.5: 0.05～0.5: 0.1～0.8: 0.1～0.8;
The structural formula of described organic siliconresin compound is:
Me
2 Me
| |
[Si?O
1/2]
0.3[Si?O
2/2]
0.2[Si?O
3/2]
0.2[Si?O
4/2]
0.3
| | |
Me Me Me
Me is a methyl in the formula;
Chain link M in the described organic siliconresin compound general formula (1) is trim,ethylchlorosilane, 3,5-dimethylphenyl chlorosilane, trimethyl methoxy silane or HMDO etc.;
X in the described organic siliconresin compound general formula (1) is dimethyldichlorosilane, dichloromethyl phenylsilane, dimethyldimethoxysil,ne, dimethyldiethoxysilane or aminomethyl phenyl diethoxy silane etc.;
Y in the described organic siliconresin compound general formula (1) is methyl trichlorosilane, phenyl trichlorosilane, MTMS, MTES or chain alkyl triethoxysilane etc.;
Z in the described organic siliconresin compound general formula (1) is silicon tetrachloride, methyl silicate or ethyl orthosilicate etc.;
Described organic siliconresin compound is a colourless transparent liquid, and viscosity is 100～100000mPa.s;
The viscosity of described methyl-silicone oil (commercially available) is 5～30mPa.s;
Described modified silicon oil (commercially available) is on the methyl-silicone oil molecular basis, and its molecular side chain is introduced the silicone oil behind the modification group, and the modification group is hydroxyl, amino, epoxy radicals or polyethers etc.;
Described mineral oil (commercially available) is water white transparency, tasteless refined mineral oil;
Described antistatic additive is CATION (as commercially available 1631,1831) or anionic antistatic agent (as commercially available phosphate kalium salt, phosphoric acid ester sodium);
The preparation method of a kind of oil solution for spandex spinning by dry of the present invention comprises:
(1) preparation of organic siliconresin: in molar ratio 0.05～0.5: 0.05～0.5: successively take by weighing chain link M at 0.1～0.8: 0.1～0.8, X, Y and Z silane, mix, begin to drip the sour water of forming by water and 30% concentration hydrochloric acid under 25 ℃, wherein the mass ratio of water and 30% concentration hydrochloric acid is 5: 1, add in 1 hour, reacting liquid temperature rises to 70 ℃, the reactant liquor color transfers oyster white to gradually by water white transparency, keeping reaction under 60 ℃～70 ℃ temperature after 1 hour, stop to stir, reactant liquor is divided into two layers, and lower-layer resin is isolated, with pure water resin is washed the neutrality to PH, moisture resin is reloaded in the reactor dehydration that under the condition of vacuumizing, heats up, 100 ℃～130 ℃ of dehydration temperaturres, 2～3 hours time, promptly;
(2) with above-mentioned organic siliconresin, methyl-silicone oil, modified silicon oil, mineral oil and antistatic additive by mass ratio 1%～30%: 10%～60%: 1%～20%: 10%～60%: 0.5%～10% adds in the stirred tank successively, under 10～50 ℃ of temperature, fully mix, promptly get water white oil solution for spandex spinning by dry.
The application of a kind of oil solution for spandex spinning by dry of the present invention, comprise: finish is contained in the storage tank, by oil pump finish is transported to atomizer or roller, direct and spandex wire connection is touched and is oiled, use this finish, the finish storage tank need not to stir, and according to spinning technique, the scope of the last oil mass of control silk is 3～6%.
In the oil solution for spandex spinning by dry of the present invention, the organic siliconresin compound is as the key component of compound finish, its microscopic dimensions is the nanoscale microparticle, between the spandex silk, form the particle buffer action, can avoid the adhesion between the spandex silk effectively, this resin has quite high viscosity again simultaneously, and good convergence is provided, help the spinning cake moulding and prevent the silk thread landing, and this organic siliconresin compound and methyl-silicone oil, mineral oil have good intermiscibility; In other components, methyl-silicone oil has excellent flatness, release property and high-low temperature resistant characteristic; And modified silicon oil can play anti, reduces the effects such as coefficient of friction of silk; Mineral oil is as one of basic components of finish, for spinning provides certain smoothness properties with finish; Select CATION or anionic antistatic agent at last, usually the antistatic property of anionic antistatic agent is better than CATION and nonionic.
Beneficial effect
(1) organic siliconresin compound provided by the invention, form the particle buffer action between the spandex silk, can avoid the adhesion between the spandex silk effectively, this resin has quite high viscosity again simultaneously, good convergence is provided, helps the spinning cake moulding and prevent the silk thread landing;
(2) oil solution for spandex spinning by dry of the present invention is a colourless transparent liquid, does not contain solid particulate components such as magnesium stearate, and the process that oils can blocking pipe and equipment, and the dispense with parking cleaning has improved production efficiency;
(3) of the present inventionly be suitable for multiple spandex spinning by dry technology with finish, the inside and outside unwinding tension of spinning cake is even, and antistatic property is good, is difficult for falling silk and fracture of wire, and the comprehensive backing-off performance in the process of back is good.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
In three mouthfuls of glass reactors of 500ml, add 32.4g HMDO, 29.6g dimethyldiethoxysilane, 35.6g MTES, 250g ethyl orthosilicate successively, mix, begin to drip the sour water of forming by 50g water and 10g30% concentration hydrochloric acid under 25 ℃, add in 1 hour, reacting liquid temperature rises to 70 ℃, and the reactant liquor color transfers oyster white to gradually by water white transparency.Keeping reaction under 60 ℃～70 ℃ temperature after 1 hour, stopping to stir, reactant liquor is divided into two layers.Isolate lower-layer resin, resin is washed the neutrality to PH with pure water.Moisture resin is reloaded in the glass reactor, the dehydration that under the condition of vacuumizing, heats up, 100 ℃～130 ℃ of dehydration temperaturres, 2～3 hours time is to the resin water white transparency with meet the requirements of viscosity, end operation.
Obtaining 160g, water white transparency, range of viscosities is the organic siliconresin of 5000～8000mPa.s, concrete molecular structure as the formula (2):
Me
2 Me
| |
[Si?O
1/2]
0.2[Si?O
2/2]
0.1[Si?O
3/2]
0.1[Si?O
4/2]
0.6 (2)
| | |
Me Me Me
Me is a methyl in the formula.
Embodiment 2
In three mouthfuls of glass reactors of 500ml, add 48.6g HMDO, 48g dimethyldimethoxysil,ne, 54.4g MTMS, 125g ethyl orthosilicate successively, mix, begin to drip the sour water of forming by 45g water and 9g30% concentration hydrochloric acid under 25 ℃, add in 1 hour, reacting liquid temperature rises to 65 ℃, and the reactant liquor color transfers oyster white to gradually by water white transparency.Keeping reaction under 60 ℃～70 ℃ temperature after 1 hour, stopping to stir, reactant liquor is divided into two layers.Isolate lower-layer resin, resin is washed the neutrality to PH with pure water.Moisture resin is reloaded in the glass reactor, the dehydration that under the condition of vacuumizing, heats up, 100 ℃～130 ℃ of dehydration temperaturres, 2～3 hours time is to the resin water white transparency with meet the requirements of viscosity, end operation.
Obtaining 145g, water white transparency, range of viscosities is the organic siliconresin of 3000～5000mPa.s, concrete molecular structure as the formula (3):
Me
2 Me
| |
[Si?O
1/2]
0.3[Si?O
2/2]
0.2[Si?O
3/2]
0.2[Si?O
4/2]
0.3 (3)
| | |
Me Me Me
Me is a methyl in the formula.
Embodiment 3
The percentage composition of the composition of oil solution for spandex spinning by dry and each component in the present embodiment:
Organic siliconresin (structural formula 2) 10%
Methyl-silicone oil 40%
Polyether modified silicon oil 5%
Mineral oil 43%
Antistatic additive 2%
Said components is added in the stirred tank successively, under 20～40 ℃, fully mix, promptly get water white oil solution for spandex spinning by dry of the present invention.
The main performance of finish:
Outward appearance: water white transparency.
Viscosity: 10mPa.s.
PH value: 6～7
Fugitive constituent: 0.5% (100 ℃, 1hr)
Finish is at semi-continuous polymerization, and the application result in the dry-spinning process is as shown in table 1 below:
Table 1
In the present embodiment, add the organic siliconresin compound 10% of molecular formula (2) expression, the unwinding tension of spandex spinning cake is reduced in the 1g, and the unwinding tension of the top layer of spinning cake, middle level and internal layer changes little; Under the same terms, as not adding the organic siliconresin compound of molecular formula (2) expression, and the consumption of methyl-silicone oil is brought up to 50%, then the unwinding tension of spandex spinning cake is greater than 2g, and the unwinding tension undulating value of top layer and internal layer has more than the 0.5g approximately.
Embodiment 4
The percentage composition of the composition of oil solution for spandex spinning by dry and each component in the present embodiment:
Organic siliconresin (structural formula 2) 15%
Methyl-silicone oil 35%
Polyether modified silicon oil 5%
Mineral oil 43%
Antistatic additive 2%
Said components is added in the stirred tank successively, under 20～40 ℃, fully mix, promptly get water white oil solution for spandex spinning by dry of the present invention.
The main performance of finish:
Outward appearance: water white transparency.
Viscosity: 11mPa.s.
PH value: 6～7
Fugitive constituent: 0.4% (100 ℃, 1hr)
Finish is at semi-continuous polymerization, and the application result in the dry-spinning process is as shown in table 2 below:
Table 2
In an embodiment, increased the consumption of organic siliconresin, correspondingly reduce the consumption of methyl-silicone oil, but keep total organosilicon material constituent content constant, can find by table 2 data, the few of variation of physical index of the spandex silk that spins, but the silk unwinding tension obviously descend, the ectonexine unwinding tension is more even.The organic siliconresin compound that includes general formula (1) expression in the finish is described, between the spandex silk, forms the particle buffer action, can avoid the adhesion between the spandex silk effectively, improve the back processing characteristics of silk.
Embodiment 5
The percentage composition of the composition of oil solution for spandex spinning by dry and each component in the present embodiment:
Organic siliconresin (structural formula 3) 12%
Methyl-silicone oil 38%
Polyether modified silicon oil 5%
Mineral oil 42%
Antistatic additive 3%
Said components is added in the stirred tank successively, under 20～40 ℃, fully mix, promptly get water white oil solution for spandex spinning by dry of the present invention.
The main performance of finish:
Outward appearance: water white transparency.
Viscosity: 10.5mPa.s.
PH value: 6～7
Fugitive constituent: 0.5% (100 ℃, 1hr)
Finish spins the spandex technology in Japan, and the application result in the dry-spinning process is as shown in table 3 below:
Table 3.
In the present embodiment, keep total organosilicon material constituent content constant, the antistatic ingredient consumption is increased to 3%, can be found by table 3 data, the fricative under the same conditions static of institute's spandex silk that spins can be reduced to 400V.Can satisfy the peak demand to antistatic property when using of spandex silk fully.
Claims (8)
1. oil solution for spandex spinning by dry, its component comprises: methyl-silicone oil, modified silicon oil, mineral oil and the antistatic additive of organic siliconresin, viscosity 1～50mPa.s, and its mass ratio is: 1%～30%: 10%～60%: 1%～20%: 10%～60%: 0.5%～10%;
Wherein, the general formula of described organic siliconresin compound is:
Me is a methyl in the formula; R
1Be methyl, ethyl, phenyl or chloromethyl; R
2Be methyl, ethyl or phenyl; R
3Be methyl, ethyl, phenyl, hydroxyl or chain alkyl; MXYZ is for forming the silane chain link of this resin, and its mol ratio is M: X: Y: Z=0.05～0.5: 0.05～0.5: 0.1～0.8: 0.1～0.8.
2. a kind of oil solution for spandex spinning by dry according to claim 1 is characterized in that: the mass ratio of described organic siliconresin, methyl-silicone oil, modified silicon oil, mineral oil and antistatic additive is: 5%～20%: 20%～50%: 5%～15%: 20%～40%: 1%～5%.
3. a kind of oil solution for spandex spinning by dry according to claim 1 is characterized in that: described oil solution for spandex spinning by dry is a water white transparency, does not have visible solid particle, viscosity 5～20mPa.s.
4. a kind of oil solution for spandex spinning by dry according to claim 1 is characterized in that: the structural formula of described organic siliconresin compound is:
Me is a methyl in the formula.
5. a kind of oil solution for spandex spinning by dry according to claim 1 is characterized in that: the chain link M in the described organic siliconresin compound general formula (1) is trim,ethylchlorosilane, 3,5-dimethylphenyl chlorosilane, trimethyl methoxy silane or HMDO; X is dimethyldichlorosilane, dichloromethyl phenylsilane, dimethyldimethoxysil,ne, dimethyldiethoxysilane or aminomethyl phenyl diethoxy silane; Y is methyl trichlorosilane, phenyl trichlorosilane, MTMS, MTES or chain alkyl triethoxysilane; Z is silicon tetrachloride, methyl silicate or ethyl orthosilicate.
6. a kind of oil solution for spandex spinning by dry according to claim 1 is characterized in that: described organic siliconresin compound is a colourless transparent liquid, and viscosity is 100～100000mPa.s.
7. the preparation method of a kind of oil solution for spandex spinning by dry according to claim 1 comprises:
(1) preparation of organic siliconresin: in molar ratio 0.05～0.5: 0.05～0.5: successively take by weighing chain link M at 0.1～0.8: 0.1～0.8, X, Y and Z, mix, begin to drip the sour water of forming by water and 30% concentration hydrochloric acid under 25 ℃, wherein the mass ratio of water and 30% concentration hydrochloric acid is 5: 1, add in 1 hour, reacting liquid temperature rises to 70 ℃, the reactant liquor color transfers oyster white to gradually by water white transparency, keeping reaction under 60 ℃～70 ℃ temperature after 1 hour, stop to stir, reactant liquor is divided into two layers, and lower-layer resin is isolated, wash neutrality with the pure water resin to PH, moisture resin is reloaded in the glass reactor dehydration that under the condition of vacuumizing, heats up, 100 ℃～130 ℃ of dehydration temperaturres, 2～3 hours time, promptly;
(2) with above-mentioned organic siliconresin, methyl-silicone oil, modified silicon oil, mineral oil and antistatic additive by mass ratio 1%～30%: 10%～60%: 1%～20%: 10%～60%: 0.5%～10% adds in the stirred tank successively, under 10～50 ℃ of temperature, fully mix, promptly get water white oil solution for spandex spinning by dry.
8. the application of a kind of oil solution for spandex spinning by dry according to claim 1, it is characterized in that: finish is contained in the storage tank, by oil pump finish is transported to atomizer or roller, direct and spandex wire connection is touched and is oiled, use this finish, the finish storage tank need not to stir, and according to spinning technique, the scope of the last oil mass of control silk is 3～6%.
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|---|---|---|---|
| CN2008102072348A CN101440574B (en) | 2008-12-18 | 2008-12-18 | Oil solution for spandex spinning by dry method, and preparation and use thereof |
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|---|---|---|---|
| CN2008102072348A CN101440574B (en) | 2008-12-18 | 2008-12-18 | Oil solution for spandex spinning by dry method, and preparation and use thereof |
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| CN101440574B true CN101440574B (en) | 2011-01-05 |
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| CN101824752B (en) * | 2010-04-19 | 2012-05-02 | 北京中纺海天染织技术有限公司 | Polyurethane fiber dry spinning oil agent and preparation method thereof |
| CN103014922A (en) * | 2011-09-22 | 2013-04-03 | 中国科学院化学研究所 | Organosilicon spinning oil agent used for preparing polyacrylonitrile-based carbon fiber, and preparation method thereof |
| CN102619091B (en) * | 2012-03-22 | 2013-07-31 | 上海罗洋新材料科技有限公司 | Spinning finish for polyvinyl alcohol fiber for toughening cement concrete |
| CN102877296B (en) * | 2012-10-30 | 2014-08-27 | 佛山市顺德区德美瓦克有机硅有限公司 | High-unwinding-tension spandex oil preparation |
| CN103806131A (en) * | 2012-11-06 | 2014-05-21 | 中国科学院化学研究所 | Organosilicon spinning oil agent for preparing polyacrylonitrile-based carbon fibers |
| CN103074774A (en) * | 2013-01-28 | 2013-05-01 | 天津工业大学 | Spinning oil for fine-denier melt-spun spandex fiber |
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| CN106930104A (en) * | 2017-03-01 | 2017-07-07 | 烟台锐泽化学品有限公司 | A kind of polyurethane fiber dry spinning oil agent without organosilicon and preparation method thereof |
| CN107164962B (en) * | 2017-07-06 | 2018-04-24 | 江苏宇道生物科技有限公司 | A kind of spinning oil and preparation method thereof |
| CN109722907B (en) * | 2018-12-27 | 2021-04-30 | 北京光华纺织集团有限公司 | Polyurethane spinning oil containing fatty acid modified silicone oil and preparation method thereof |
| KR102137274B1 (en) * | 2019-01-07 | 2020-07-23 | (주) 정산인터내셔널 | Thermoplastic elastomer yarn with improved unwinding, weaving and yarn shrinking property, and manufacturing method thereof |
| CN110746607B (en) * | 2019-11-26 | 2021-07-30 | 山东大易化工有限公司 | Auxiliary product applied to spandex spinning oil agent and having effects of isolating and adjusting friction |
| JP6887039B1 (en) * | 2020-03-27 | 2021-06-16 | 松本油脂製薬株式会社 | Treatment agents for synthetic fibers and their use |
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| CN101440574A (en) | 2009-05-27 |
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