CN104073904B - A kind of spandex waste silk that utilizes prepares the method for hygienic material with thick dawn spandex fibre - Google Patents
A kind of spandex waste silk that utilizes prepares the method for hygienic material with thick dawn spandex fibre Download PDFInfo
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Abstract
The invention belongs to field of material preparation, relate to the preparation method of thick dawn spandex fibre, be specifically related to a kind of spandex waste silk that utilizes and prepare the method for hygienic material with thick dawn spandex fibre, its step comprises: (1), preliminary treatment; (2), prepolymerization; (3), be polymerized; (4), spinning.The present invention is in the preparation process of spandex fibre, to spandex waste silk, cosolvent, desiliconization oil assistant and catalyst is adopted to process respectively, make greatly to improve the stationary phase of prepared polymer solution (being greater than 20 days), improve the mobility of polymer dope prepared by spandex waste silk, reduce the gel in polymer dope, improve the spinnability of polymer dope, in the spandex fibre strand that method of the present invention is obtained hard segment and soft chain segment in order regular.
Description
Technical field
The invention belongs to field of material preparation, relate to the preparation method of thick dawn spandex fibre, be specifically related to a kind of spandex waste silk that utilizes and prepare the method for hygienic material with thick dawn spandex fibre.
Background technology
Spandex is widely used in the fields such as weaving, bio-medical with its excellent elasticity and Physical Mechanical.Rapidly, the output of China's spandex is more than 600,000 tons/year in polyurethane fibre industry development in recent years.
Meanwhile, in the manufacture and usage process of spandex, a large amount of waste silk is also created.The method of burying and burning is taked to process at present for these waste silks---not only waste a large amount of industrial chemicals, also can cause land wastage and atmosphere pollution, do not meet Global Sustainable Development strategy.
Along with people are to the pay attention to day by day of environmental issue, the particularly raising of Consciousness of Sustainable Development, eliminate white pollution, realize the Appropriate application of resource, but because its output only accounts for very little proportion in the extended familys of polyurethane products, therefore the recycling of spandex waste silk is never drawn attention in the past, and the technical barrier that spandex waste silk reclaims is a lot, spandex is linear block polymers of polyurethane, although theoretically, spandex waste silk can carry out secondary dissolving, again spinning solution is made, but experiment finds, again spinning solution stability is made very poor by spandex waste silk, mobility also can reduce, very easily generate gel and cannot spinning,
In addition, in the process of first time spinning, in order to the needs of fiber process, surface is the spinning oil of attachment containing amino silicone wet goods composition often, is convenient to the smooth performance increasing fiber and the electrostatic eliminated in procedure of fibre production.But these compositions all can accelerate the degradation speed of spandex waste silk stoste, make the abnormal fracture of spandex waste silk polyurethane molecular chain in secondary course of dissolution, range of molecular weight distributions is wider, causes its machinability poorer than normal stoste.
The poor stability of spinning solution shows two aspects, on the one hand can accelerated degradation, and macromolecular chain destroys serious, reacts for apparent viscosity is too low, in polymer dope spinning process, can from spinneret orifice and spinning shaft Fracture, and it is shaping to be difficult to Continuous maching; In addition, part group can carry out cross-linking reaction, and produce the gel particle that can not be dissolved in system, these particles have elasticity, in spinning process process, under certain pressure effect, can filter be passed through, enter in the spinneret component of spinning, through the spinneret orifice of spinnerets, spinneret orifice can be blocked, cause polymer dope to stop, it is shaping to be difficult to Continuous maching equally.
Summary of the invention
Goal of the invention: the present invention is directed to above-mentioned prior art Problems existing and make improvements, namely the invention provides a kind of spandex waste silk that utilizes and prepares the method for hygienic material with thick dawn spandex fibre.
Technical scheme: a kind of spandex waste silk that utilizes prepares the method for hygienic material with thick dawn spandex fibre, and its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is carried out sorting and impurities removing;
(12) the described spandex waste silk after step (11) being sorted is organized into waste silk bundle;
(13) described for step (12) waste silk bundle is switched to the staple fibre of 3 ~ 10cm;
(14) according to volume ratio water: desiliconization oil assistant=100:(1 ~ 5) configuration cleaning fluid, by step (13) described staple fibre described cleaning fluid cleaning 30 ~ 80min, the mass ratio of described staple fibre and described cleaning fluid is 1:5 ~ 1:20;
(15) staple fibre after step (14) described cleaning being dried extremely moisture mass percent is 0.01% ~ 2%;
(2), prepolymerization: according to the ratio of 10 ~ 45 parts, spandex waste silk staple fibre, polar solvent 55 ~ 90 parts and cosolvent 1 ~ 5 part, the spandex waste silk staple fibre described in step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 35 ~ 40 DEG C, and the reaction time is 30 ~ 60min;
(3), polymerization: first add catalyst in step (2) described prepolymerization product, the consumption of described catalyst is 1% ~ 5% of described prepolymerization product quality; Described prepolymerization product is transplanted on polymerization in polymerization reaction kettle again and forms polymer dope, the reaction temperature of polymerisation is 30 ~ 80 DEG C, and the reaction time of polymerisation is 150 ~ 180min;
(4), spinning: adopt dry-spinning silk method to make hygienic material thick dawn spandex fibre polymer dope obtained for step (3).
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: step (14) described desiliconization oil assistant component is: DDAO 8 ~ 12 parts, modification cocoanut fatty acid diethanolamide 3 ~ 5 parts, sodium xylene sulfonate 2 ~ 4 parts, EDTA5 ~ 8 part and deionized water 77.5 parts as utilizing spandex waste silk in the present invention.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: step (14) described desiliconization oil assistant component is: DDAO 8 ~ 12 parts, modification cocoanut fatty acid diethanolamide 3 ~ 5 parts, sodium xylene sulfonate 2 ~ 4 parts, NTA5 ~ 8 part and deionized water 77.5 parts as utilizing spandex waste silk in the present invention.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: step (2) described cosolvent is one or more in urethanes, urea, formamide, acetamide as utilizing spandex waste silk in the present invention.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: polar solvent described in step (2) is one or more in DMAc, DMF, DMSO, NMP as utilizing spandex waste silk in the present invention.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: step (2) described prepolymerization product apparent viscosity at 20 DEG C is 2000 ~ 8000poise as utilizing spandex waste silk in the present invention.
Prepare a kind of preferred version of hygienic material by the method for thick dawn spandex fibre as utilizing spandex waste silk in the present invention: step (3) described catalyst be dibutyl tin dilaurate, stannous octoate one or both.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: step (3) described polymer dope is 3000 ~ 12000poise the apparent viscosity of 20 DEG C as utilizing spandex waste silk in the present invention.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: in step (4), the technological parameter of dry spin processes is: spinneret temperature is 210 ~ 300 DEG C, and spinning speed is 300 ~ 750m/min as utilizing spandex waste silk in the present invention.
A kind of preferred version of hygienic material by the method for thick dawn spandex fibre is prepared: described in step (1), baking temperature is 120 ~ 250 DEG C, and drying time is 180 ~ 260min as utilizing spandex waste silk in the present invention.
Beneficial effect: in the process that 1, the present invention is dissolved at spandex waste silk secondary, in conjunction with chemical method, adopt cosolvent, desiliconization oil assistant and catalyst, make greatly to improve the stationary phase of prepared polymer dope (being greater than 20 days);
2, for the shortcoming of waste silk stoste poor fluidity, the present invention, by adding the mode of cosolvent, makes the sex change of waste silk stoste in the course of the polymerization process, improves its mobility, reduces the gel in polymer dope, improves the spinnability of polymer dope.The polymer solids level obtained after polymerisation controls 10% ~ 45%, and polymer dope apparent viscosity is 3000 ~ 12000poise 20 DEG C time, makes it meet the requirement of spinning process completely;
3, the character of the spandex fibre that obtains of method of the present invention and conventional spandex fibre has bigger difference, although soft section of part of macromolecular main chain is identical with conventional spandex, but make hard section in strand more in order regular by adding the additives such as cosolvent, catalyst, desiliconization oil assistant, improve polymer dope stability, rheological characteristic, processability, ensure that soft section easily larger deformation occurs under effect of stress, fiber has lower modulus, thus gives the characteristic of the good low stress of fiber.
Detailed description of the invention:
Below the specific embodiment of the present invention is described in detail.
Specific embodiment 1
Utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre, its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is carried out sorting and impurities removing;
(12) spandex waste silk after step (11) being sorted is organized into waste silk bundle (waste silk is entwined in the same way);
(13) step (12) spandex bundle is switched to the staple fibre of about 3cm;
(14) according to volume ratio water: desiliconization oil assistant=100:5 configures cleaning fluid, the staple fibre cleaning fluid of step (13) is cleaned 30min, the mass ratio of staple fibre and cleaning fluid is 1:5;
(15) drying to moisture mass percent by the staple fibre after cleaning in step (14) is 0.01%, and baking temperature is 250 DEG C, and drying time is 260min;
(2), prepolymerization: according to the ratio of 10 parts, spandex waste silk staple fibre, DMAc (polar solvent) 90 parts and urethanes (cosolvent) 1 part, the spandex waste silk staple fibre of step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 35 DEG C, reaction time is 60min, and prepolymerization product apparent viscosity at 20 DEG C is 8000poise;
(3), polymerization: first add dibutyl tin dilaurate (catalyst) in step (2) prepolymerization product, the consumption of dibutyl tin dilaurate is 1% of the quality of prepolymerization product; Again prepolymerization product (with catalyst) is transplanted on polymerization in polymerization reaction kettle and forms polymer dope, the reaction temperature of polymerisation is 30 DEG C, the reaction time of polymerisation is 180min, and the apparent viscosity of polymer dope is 12000poise at 20 DEG C;
(4), spinning: adopt dry-spinning silk method to make hygienic material thick dawn spandex fibre polymer dope obtained for step (3), technological parameter is: spinneret temperature is 300 DEG C, and spinning speed is 750m/min.
Step (14) desiliconization oil assistant component is: DDAO 8 parts, modification cocoanut fatty acid diethanolamide 3 parts, sodium xylene sulfonate 2 parts, EDTA5 part and deionized water 77.5 parts.
Specific embodiment 2
Utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre, its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is carried out sorting and impurities removing;
(12) spandex waste silk after step (11) being sorted is organized into waste silk bundle (waste silk is entwined in the same way);
(13) step (12) spandex bundle is switched to the staple fibre of about 10cm;
(14) according to volume ratio water: desiliconization oil assistant=100:1 configures cleaning fluid, step (13) staple fibre cleaning fluid is cleaned 80min, the mass ratio of staple fibre and cleaning fluid is 1:10;
(15) drying to moisture mass percent by the staple fibre after cleaning in step (14) is 2%, and baking temperature is 120 DEG C, and drying time is about 180min;
(2), prepolymerization: according to the ratio of 45 parts, spandex waste silk staple fibre, DMF (polar solvent) 55 parts and 5 parts, urea (cosolvent), the spandex waste silk staple fibre of step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 40 DEG C, reaction time is 30min, and prepolymerization product apparent viscosity at 20 DEG C is 2000poise;
(3), polymerization: first add stannous octoate (catalyst) in step (2) prepolymerization product, the consumption of stannous octoate is 5% of the quality of prepolymerization product; Again prepolymerization product (with catalyst) is transplanted on polymerization in polymerization reaction kettle and forms polymer dope, the reaction temperature of polymerisation is 80 DEG C, the reaction time of polymerisation is 150min, and the apparent viscosity of polymer dope is 3000poise at 20 DEG C;
(4), spinning: adopt dry-spinning silk method to make hygienic material thick dawn spandex fibre polymer dope obtained for step (3), technological parameter is: spinneret temperature is 210 DEG C, and spinning speed is 300m/min.
Step (14) desiliconization oil assistant component is: DDAO 12 parts, modification cocoanut fatty acid diethanolamide 5 parts, sodium xylene sulfonate 4 parts, EDTA5 part and deionized water 77.5 parts.
Specific embodiment 3
Utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre, its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is carried out sorting and impurities removing;
(12) spandex waste silk after step (11) being sorted is organized into waste silk bundle (waste silk is entwined in the same way);
(13) step (12) spandex bundle is switched to the staple fibre of about 5cm;
(14) according to volume ratio water: desiliconization oil assistant=100:3 configures cleaning fluid, the staple fibre cleaning fluid of step (13) is cleaned 50min, the mass ratio of staple fibre and cleaning fluid is 1:20;
(15) drying to moisture mass percent by the staple fibre after cleaning in step (14) is 1%, and baking temperature is 150 DEG C, and drying time is about 200min;
(2), prepolymerization: according to the ratio of 30 parts, spandex waste silk staple fibre, DMSO (polar solvent) 70 parts and formamide (cosolvent) 3 parts, the spandex waste silk staple fibre of step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 38 DEG C, reaction time is 45min, and prepolymerization product apparent viscosity at 20 DEG C is 5000poise;
(3), polymerization: first add stannous octoate (catalyst) in step (2) prepolymerization product, the consumption of stannous octoate is 3% of the quality of prepolymerization product; Again prepolymerization product (with catalyst) is transplanted on polymerization in polymerization reaction kettle and forms polymer dope, the reaction temperature of polymerisation is 50 DEG C, the reaction time of polymerisation is 165min, and the apparent viscosity of polymer dope is 6000poise at 20 DEG C;
(4), spinning: adopt dry-spinning silk method to make hygienic material thick dawn spandex fibre polymer dope obtained for step (3), technological parameter is: spinneret temperature is 250 DEG C, and spinning speed is 450m/min.
Step (14) desiliconization oil assistant component is: DDAO 10 parts, modification cocoanut fatty acid diethanolamide 4 parts, sodium xylene sulfonate 3 parts, EDTA6 part and deionized water 77.5 parts.
Specific embodiment 4
With specifically to implement 1 roughly the same, distinguish and be only:
1, the polar solvent in step (2) is NMP, and cosolvent is acetamide;
2, step (14) desiliconization oil assistant component is: DDAO 8 parts, modification cocoanut fatty acid diethanolamide 3 parts, sodium xylene sulfonate 2 parts, NTA5 part and deionized water 77.5 parts.
Specific embodiment 5
With specifically to implement 1 roughly the same, distinguish and be only:
1, the polar solvent in step (2) is NMP and DMF, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
2, the cosolvent in step (2) is urethanes and urea, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
3, step (14) desiliconization oil assistant component is: DDAO 12 parts, modification cocoanut fatty acid diethanolamide 5 parts, sodium xylene sulfonate 4 parts, NTA5 part and deionized water 77.5 parts.
Specific embodiment 6
With specifically to implement 1 roughly the same, distinguish and be only:
1, the polar solvent in step (2) is NMP and DMSO, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
2, the cosolvent in step (2) is urethanes and formamide, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
3, step (14) desiliconization oil assistant component is: DDAO 10 parts, modification cocoanut fatty acid diethanolamide 4 parts, sodium xylene sulfonate 3 parts, EDTA6 part and deionized water 77.5 parts.
Specific embodiment 7
With specifically to implement 1 roughly the same, distinguish and be only:
1, the polar solvent in step (2) is NMP and DMAc, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
2, the cosolvent in step (2) is urethanes and acetamide, its mass ratio 1:1 (its ratio can be allocated arbitrarily).
Specific embodiment 8
With specifically to implement 1 roughly the same, distinguish and be only:
1, the polar solvent in step (2) such as is at DMAc, DMF, DMSO, the NMP (its ratio can be allocated arbitrarily) of mass ratio;
3, the cosolvent in step (2) such as is at urethanes, urea, formamide, the acetamide (its ratio can be allocated arbitrarily) of mass ratio.
According to the mixture composition that number is stated in specific embodiment, be all mass fraction without being prescriptive.Such as 10 ~ 45 parts, spandex waste silk staple fibre, polar solvent 55 ~ 90 parts and cosolvent 1 ~ 5 part, all refer to mass fraction when specifically not indicating.
Above embodiments of the present invention are elaborated.But the present invention is not limited to above-mentioned embodiment, in the ken that art those of ordinary skill possesses, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (7)
1. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre, comprise the following steps:
(1), preliminary treatment:
(11) spandex waste silk is carried out sorting and impurities removing;
(12) the described spandex waste silk after step (11) being sorted is organized into waste silk bundle;
(13) described for step (12) waste silk bundle is switched to the staple fibre of 3 ~ 10cm;
(14) according to volume ratio water: desiliconization oil assistant=100:(1 ~ 5) configuration cleaning fluid, by step (13) described staple fibre described cleaning fluid cleaning 30 ~ 80min, the mass ratio of described staple fibre and described cleaning fluid is 1:5 ~ 1:20;
(15) staple fibre after step (14) described cleaning being dried extremely moisture mass percent is 0.01% ~ 2%;
(2), prepolymerization: according to the ratio of 10 ~ 45 parts, spandex waste silk staple fibre, polar solvent 55 ~ 90 parts and cosolvent 1 ~ 5 part, the spandex waste silk staple fibre described in step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 35 ~ 40 DEG C, and the reaction time is 30 ~ 60min;
(3), polymerization: first add catalyst in step (2) described prepolymerization product, the consumption of described catalyst is 1% ~ 5% of the quality of described prepolymerization product; Described prepolymerization product is transplanted on polymerization in polymerization reaction kettle again and forms polymer dope, the reaction temperature of polymerisation is 30 ~ 80 DEG C, and the reaction time of polymerisation is 150 ~ 180min;
(4), spinning: adopted by polymer dope obtained for step (3) dry-spinning silk method to make the thick dawn spandex fibre of hygienic material,
Step (2) described cosolvent is one or more in urethanes, urea, formamide, acetamide,
Polar solvent described in step (2) is one or more in DMAc, DMF, DMSO, NMP,
Step (3) described catalyst be dibutyl tin dilaurate, stannous octoate one or both.
2. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre as claimed in claim 1, it is characterized in that, step (14) described desiliconization oil assistant component is: DDAO 8 ~ 12 parts, modification cocoanut fatty acid diethanolamide 3 ~ 5 parts, sodium xylene sulfonate 2 ~ 4 parts, EDTA5 ~ 8 part and deionized water 77.5 parts.
3. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre as claimed in claim 1, it is characterized in that, step (14) described desiliconization oil assistant component is: DDAO 8 ~ 12 parts, modification cocoanut fatty acid diethanolamide 3 ~ 5 parts, sodium xylene sulfonate 2 ~ 4 parts, NTA5 ~ 8 part and deionized water 77.5 parts.
4. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre as claimed in claim 1, it is characterized in that, step (2) described prepolymerization product apparent viscosity at 20 DEG C is 2000 ~ 8000poise.
5. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre as claimed in claim 1, it is characterized in that, the apparent viscosity of the described polymer dope of step (3) 20 DEG C is 3000 ~ 12000poise.
6. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre as claimed in claim 1, it is characterized in that, the technological parameter in step (4) is: spinneret temperature is 210 ~ 300 DEG C, and spinning speed is 300 ~ 750m/min.
7. utilize spandex waste silk to prepare the method for hygienic material with thick dawn spandex fibre as claimed in claim 1, it is characterized in that, described in step (1), baking temperature is 120 ~ 250 DEG C, and drying time is 180 ~ 260min.
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| CN107099873A (en) * | 2017-06-15 | 2017-08-29 | 淮安侨新新材料科技有限公司 | Spandex waste silk regenerates the preparation method of false proof spandex fibre |
| CN110885538A (en) * | 2019-12-08 | 2020-03-17 | 周佩珍 | Flame-retardant high-temperature-resistant electric wire and manufacturing method thereof |
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Address after: No. 60 Huaian leoch 211699 city of Jiangsu province Jinhu County Road Patentee after: Huaian overseas Chinese New Mstar Technology Ltd Address before: No. 60 leoch Road Economic Development Zone 211600 Huaian city Jiangsu County of Jinhu Province Patentee before: JIANGSU QIAOXIN FIBER CO., LTD. |