CN104695046A - Preparation method of composite fiber with multilayer structure - Google Patents
Preparation method of composite fiber with multilayer structure Download PDFInfo
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- CN104695046A CN104695046A CN201310647438.4A CN201310647438A CN104695046A CN 104695046 A CN104695046 A CN 104695046A CN 201310647438 A CN201310647438 A CN 201310647438A CN 104695046 A CN104695046 A CN 104695046A
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Abstract
The invention relates to a preparation method of sheath core composite or multilayer structure fiber, and cellulose is cotton cellulose and wood cellulose with 400-800 of polymerization degree. The method comprises the following steps: dissolving chitin in a dilute sodium hydroxide solution to prepare a chitin spinning stock solution, dissolving cellulose in a mixing aqueous solution system of sodium hydroxide and urea to prepare a cellulose spinning stock solution, mixing two solutions to prepare a blended cortex spinning stock solution, wherein the cellulose spinning stock solution is taken as a core layer spinning stock solution, introducing the cellulose spinning stock solution from an inlet of the core layer of a sheath core composite spinning machine for coagulation bath spinning moulding, and obtaining chitin with a sheath core structure and cellulose composite fiber through a post-treatment process. The method has the advantages of reasonable route, high production efficiency, low cost and obvious antibiosis effect of the products, and is an ideal underwear raw material.
Description
Technical field:
The invention belongs to technical field of fiber preparation, relate to the preparation method of a kind of core-sheath or multiple structural fibre, particularly the preparation method of a kind of chitin and cellulose composite fiber.
Background technology:
Chitin is the product of crust deacetylate after concentrated base process.Chitin is by a kind of natural biological high polymer refined in the cell membrane of the shell of shrimp, crab etc. and mushroom, algae.In the year biosynthesis amount of occurring in nature chitin more than 10,000,000,000 tons, it is a kind of organic regenerative resource being only second to cellulosic reserves and very enriching.Chitin has the functions such as good biocompatibility, broad spectrum antibacterial and Immune enhancement activity, biological degradability.China has 300 Duo Ge chitin manufacturers at present, has become chitin and has produced and big export country, added the production of the downstream product of chitin and chitin, and China has in fact defined the new industry group of a chitin and chitin production.Prior art adopts chitin solution spun to become fiber, for medical application such as Absorbable rod operation sewing thread and artificial skin etc., but pure chitin fiber lacks the physical and mechanical properties of weaving required for aft-loaded airfoil, and cost is very high, expensive, its extensive popularization and application is restricted.
Cellulose fibre is as a kind of recyclability fiber, there is the advantages such as good sucting wet air permeability, snugness of fit be good, be widely used, in order to meet the multi-functional demand of people to fiber textile, can by adding the production that some functional components carry out practical function cellulose fibre in fibre spinning process.Conventional viscose is a kind of regenerated celulose fibre, but owing to having a large amount of waste water and waste gas to generate in process of production, seriously polluted.Cellulose carbamate is a kind of cellulose esters, is used for weaving as the upgraded product of cellulose sulfonate at present, solves the pollution of environment, achieve cellulosic making full use of.
At present, usually prepare by adding chitin or crust in cellulose fibre production process there is antibacterial viscose, adopt the composition such as chitin or chitin in the fiber prepared in this way to be uniformly distributed at fibrous inside, as patent CN01126469.1, a kind of health type viscose fiber with high wet modulus, a kind of health type viscose fiber with high wet modulus containing chitin is disclosed in Manufacturing approach and use, this fibrous outer surfaces is diluted to a great extent with the concentration of human body contact portion's chitin, be difficult to the biologically active playing chitin product, due sterilization is not reached to cause fiber, antibacterial functional realiey such as grade.Patent CN1120198C, chitin/cellulose blending film or fibrous material and method for making thereof and purposes disclose one and love and respect shell element and cellulose intermingling material and uses thereof and preparation method, the effects such as in the blended fiber prepared by the method, chitin is evenly distributed in fibrous inside, and it is antibacterial are also greatly affected.End is got up, and it is low that existing preparation fibre technology containing chitin and products thereof exists antibiotic effect, functional difference, and technology of preparing is complicated, the outstanding shortcoming of the unreasonable grade of production technology.
Summary of the invention:
The object of the invention is to overcome the shortcoming existed in prior art, seek the preparation method that a kind of sandwich construction composite fibre is provided, this fiber has core-skin type composite construction, described cortex is chitin and cellulosic mixture, sandwich layer is cellulose, there is excellent physical and mechanical properties, its composite fibre is owing to adopting core-sheath composite structure, in cortex, chitin content is higher and have good antibacterial, antipruritic, the health cares such as smelly eliminating, because cellulose composition in sandwich layer maintains the excellent textile garment wearability of cellulose fibre itself, can be used for preparing the various fabric with health care, especially underwear health-care textile material, its preparation method technique is not polluted, and is suitable for people and produces on a large scale chitin and cellulose composite fiber.
To achieve these goals, the core-sheath compound fibre with cortex and core structure that chitin of the present invention and cellulose composite fiber are made up of chitin and cellulose, the weight percentage of chitin than 2-50%, preferably 6-30%; Wherein the sandwich layer of composite fibre is cellulose, and fiber adopts the core-skin type of cortex and core structure; The molecular weight of chitin is 20-40 ten thousand, and deacetylation is 75%-95%; Described cellulose is one in the gossypin of degree of polymerization 400-800, lignose or two kinds.
Chitin is dissolved in the chitin spinning solution that diluted sodium hydroxide solution prepares 1-10% concentration by the preparation method of chitin of the present invention and cellulose composite fiber, cellulose is dissolved in NaOH and urea mixed aqueous solution system prepares the cellulose spin dope that concentration is 4-20%, by two kinds of solution mixing systems for blended cortex spinning solution, cellulose spin dope is as sandwich layer spinning solution; By cellulose spin dope by the sandwich layer entrance of core-sheath spinning machine, cellulose and chitin blending cortex spinning solution are entered coagulating bath spinning moulding by the cortex entrance of core-sheath spinning machine, and obtain chitin and the cellulose composite fiber of skin-core structure through postprocessing working procedures; Solidifying wherein adopts concentration to be the calcium chloride water of 1%-7% and concentration to be the aqueous sulfuric acid of 2%-10% to solidify for twice; Postprocessing working procedures comprises washing, oils, bleaches, oven dry etc.
The preparation of chitin spinning solution: be that the chitin of 20-40 ten thousand is immersed in the sodium hydrate aqueous solution of 40% in the ratio of 1:2-1:10 by molecular weight, low-temp reaction obtains the chitin that alkalizes, through techniques such as filtration, deaerations, and frozen water is utilized to regulate the chitin spinning solution obtaining 1.0-10.0%; Deacetylation is 75%-95%.
The preparation of cellulose spin dope: by one or both in the gossypin of degree of polymerization 400-800, lignose according to NaOH: urea: cellulose is the cellulose solution that the weight percent proportioning of 3-6:1-10:0.5-10 prepares 1-10%, obtains cellulose spin dope through techniques such as low-temp reaction dissolving, filtration, deaerations.
The preparation of blended cortex spinning solution: adopt chitin spinning solution and cellulose spin dope by volume for 1-1.5:1 is mixed to get blended cortex spinning solution, and the weight percent content controlling chitin in co-blended spinning stoste is 10-80%; Be NaOH (NaOH) solution of the chitin of 1-10% by percentage by weight be that the cellulosic NaOH of 1-10% and the solution of urea mix according to the weight ratio of 1:1-10 with percentage by weight, after filtration, deaeration technique obtains cortex spinning solution; Sandwich layer spinning solution is weight percentage as the aqueous solution of the cellulosic NaOH of 1-10% and urea obtains through filtration, deaeration technique.
The preparation of chitin and cellulose composite fiber: chitin and cellulose blending cortex spinning solution are delivered to cortex entrance measuring pump, cellulose spin dope is then delivered to sandwich layer entrance measuring pump by another road, enter in coagulating bath through first, second coagulating bath spinning moulding through core-skin type composite spinning, again through solidifying, washing, oil, bleach, the post processing such as oven dry, namely obtain finished product chitin and cellulosic type composite fibre; Adjustment cortex and sandwich layer two kinds of spinning solutions cortex entrance and sandwich layer entrance metering than adjustable cortex sandwich layer than and the content of chitin.
The present invention adopts the calcium chloride water of 2-8% as the first coagulating bath, 4-12% aqueous sulfuric acid as the second gelation, and through washing, oil, bleach, the post processing such as oven dry, namely obtain finished product chitin and cellulosic type composite fibre.
The cortex of the chitin content in the cortex of product of the present invention and in whole fiber and adjustment composite fibre and sandwich layer ratio, the content of chitin in whole composite fibre is reduced to increase the content of chitin in composite fibre cortex as much as possible, not only just in composite fibre with in the cortex of human contact, there is the chitin of higher concentration, thus make this composite fibre have stronger chitin bioactive functions and health-care function, effectively raise the biological action of composite fibre, reduce the production cost of composite fibre; Present invention process route is reasonable, and production efficiency is high, and cost is low, and product antibacterial action is obvious, is desirable underwear raw material.
Detailed description of the invention:
The content that the invention is further illustrated by the following examples.
Embodiment 1:
By molecular weight be 300,000 chitin 100 grams be immersed in the ratio of 1:4 in the sodium hydrate aqueous solution of 400 gram 40%, low-temp reaction obtain alkalize chitin, through filtration, deaeration technique, and utilize frozen water regulate obtain 2% chitin spinning solution.
By the gossypin 1000 grams of the degree of polymerization 600,1200 grams, urea, 1500 grams, NaOH is dissolved in 183000 grams of deionized waters, and through fully stirring, low-temp reaction obtains the cellulose spin dope of 22000 gram 4.5%.
By chitin spinning solution/cellulose spin dope using 1.5:1.0(V/V) ratio mixing as cortex spinning solution, enter cortex entrance measuring pump through prefilter.Cellulose spin dope directly enters sandwich layer entrance measuring pump by prefilter.The rotating speed of cortex entrance measuring pump and sandwich layer entrance measuring pump is 1.0:1.25.The composite spinning stoste extruded through core-skin type composite spinneret enters 35 DEG C of 3% calcium chloride water, then the aqueous sulfuric acid entering 35 DEG C 6% carries out solidifying for twice, again by washing, oil, bleach, the post processing such as oven dry, namely obtain finished product chitin and cellulosic type composite fibre.
The dry fracture strength of fiber is 1.80cN/dtex, and dry elongation at break is 15.3%, and whiteness is 65.3%, and Chinese People's Anti-Japanese Military and Political College's enterobacteria rate is 99.8%.
Embodiment 2:
Repeat above-mentioned course of dissolution, by chitin spinning solution/cellulose spin dope using 1.4:1.0(V/V) ratio mixing as cortex spinning solution, enter cortex entrance measuring pump through prefilter.Cellulose spin dope directly enters sandwich layer entrance measuring pump by prefilter.The rotating speed of cortex entrance measuring pump and sandwich layer entrance measuring pump is 1.0:1.25.The composite spinning stoste extruded through core-skin type composite spinneret enters 35 DEG C of 3% calcium chloride water, then the aqueous sulfuric acid entering 35 DEG C 6% carries out solidifying for twice, further by washing, oil, bleach, the post processing such as oven dry, namely obtain finished product chitin and cellulosic type composite fibre.
The dry fracture strength of fiber is 1.92cN/dtex, and dry elongation at break is 16.2%, and whiteness is 66.0%, and Chinese People's Anti-Japanese Military and Political College's enterobacteria rate is 99.8%.
Embodiment 3:
Repeat above-mentioned course of dissolution, by chitin spinning solution/cellulose spin dope using 1.0:1.0(V/V) ratio mixing as cortex spinning solution, enter cortex entrance measuring pump through prefilter.Cellulose spin dope directly enters sandwich layer entrance measuring pump by prefilter.The rotating speed of cortex entrance measuring pump and sandwich layer entrance measuring pump is 1.0:1.25.The composite spinning stoste extruded through core-skin type composite spinneret enters 35 DEG C of 3% calcium chloride water, then the aqueous sulfuric acid entering 35 DEG C 6% carries out solidifying for twice, further by washing, oil, bleach, the post processing such as oven dry, namely obtain finished product chitin and cellulosic type composite fibre.
The dry fracture strength of fiber is 1.95cN/dtex, and dry elongation at break is 17.0%, and whiteness is 66.1%, and Chinese People's Anti-Japanese Military and Political College's enterobacteria rate is 99.6%.
Comparative examples:
Repeat above-mentioned course of dissolution, by chitin spinning solution/cellulose spin dope using 0:1.0(V/V) ratio mixing as cortex spinning solution, enter cortex entrance measuring pump through prefilter.Cellulose spin dope directly enters sandwich layer entrance measuring pump by prefilter.The rotating speed of cortex entrance measuring pump and sandwich layer entrance measuring pump is 1.0:1.0.The composite spinning stoste extruded through core-skin type composite spinneret enters 35 DEG C of 3% calcium chloride water, then the aqueous sulfuric acid entering same temperature 6% carries out solidifying for twice, further by washing, oil, bleach, the post processing such as oven dry, namely obtain finished product chitin and cellulosic type composite fibre.
The dry fracture strength of fiber is 2.2cN/dtex, and dry elongation at break is 16.0%, and whiteness is 67.0%, and Chinese People's Anti-Japanese Military and Political College's enterobacteria rate is 0%.
Claims (7)
1. a preparation method for sandwich construction composite fibre, is characterized in that the core-sheath compound fibre with cortex and core structure be made up of chitin and cellulose, and the content of chitin is 2-50%; The molecular weight of chitin is 20-40 ten thousand, and deacetylation is 75%-95%; Cellulose is one or both in the gossypin of degree of polymerization 400-800, lignose.
2. the preparation method of a kind of sandwich construction composite fibre according to claim 1, it is characterized in that chitin being dissolved in the chitin spinning solution that diluted sodium hydroxide solution prepares 1-10% concentration, cellulose is dissolved in NaOH and urea mixed aqueous solution system prepares the cellulose spin dope that concentration is 4-20%, by two kinds of solution mixing systems for blended cortex spinning solution, cellulose spin dope is as sandwich layer spinning solution; By cellulose spin dope by the sandwich layer entrance of core-sheath spinning machine, cellulose and chitin blending cortex spinning solution are entered coagulating bath spinning moulding by the cortex entrance of core-sheath spinning machine, and obtain chitin and the cellulose composite fiber of skin-core structure through postprocessing working procedures; Solidifying wherein adopts concentration to be the calcium chloride water of 1%-7% and concentration to be the aqueous sulfuric acid of 2%-10% to solidify for twice; Postprocessing working procedures comprises washing, oils, bleaches, dries.
3. the preparation method of sandwich construction composite fibre according to claim 2, it is characterized in that the preparation of chitin spinning solution: be immersed in the sodium hydrate aqueous solution of 40% by chitin in the ratio of 1:2-1:10, low-temp reaction obtains the chitin that alkalizes, through filtering, deaeration technique utilize frozen water to regulate to obtain the chitin spinning solution of 1.0-10.0%.
4. the preparation method of sandwich construction composite fibre according to claim 2, it is characterized in that the preparation of cellulose spin dope: by one or both in the gossypin of degree of polymerization 400-800, lignose according to NaOH: urea: cellulose is the cellulose solution that the weight percent proportioning of 3-6:1-10:0.5-10 prepares 1-10%, dissolve through low-temp reaction, filter, deaeration technique obtains cellulose spin dope.
5. the preparation method of sandwich construction composite fibre according to claim 2, it is characterized in that the preparation of blended cortex spinning solution: adopt chitin spinning solution and cellulose spin dope by volume for 1-1.5:1 is mixed to get blended cortex spinning solution, the weight percent content controlling chitin in co-blended spinning stoste is 10-80%; Be the sodium hydroxide solution of the chitin of 1-10% by percentage by weight be that the cellulosic NaOH of 1-10% and the solution of urea mix according to the weight ratio of 1:1-10 with percentage by weight, after filtration, deaeration technique obtains cortex spinning solution; Sandwich layer spinning solution is weight percentage as the aqueous solution of the cellulosic NaOH of 1-10% and urea obtains through filtration, deaeration technique.
6. the preparation method of sandwich construction composite fibre according to claim 2, it is characterized in that the preparation of chitin and cellulose composite fiber: chitin and cellulose blending cortex spinning solution are delivered to cortex entrance measuring pump, cellulose spin dope is delivered to sandwich layer entrance measuring pump, enter in coagulating bath through first, second coagulating bath spinning moulding through core-skin type composite spinning, again through solidifying, washing, oil, bleach, dry post processing, namely obtain finished product chitin and cellulosic type composite fibre; Adjustment cortex and sandwich layer two kinds of spinning solutions cortex entrance and sandwich layer entrance metering than adjustable cortex sandwich layer than and the content of chitin.
7. the preparation method of sandwich construction composite fibre according to claim 2, it is characterized in that adopting the calcium chloride water of 2-8% as the first coagulating bath, 4-12% aqueous sulfuric acid is as the second gelation.
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| CN201310647438.4A CN104695046A (en) | 2013-12-04 | 2013-12-04 | Preparation method of composite fiber with multilayer structure |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106400201A (en) * | 2016-09-26 | 2017-02-15 | 嘉兴学院 | Preparation method of chitosan/hydroxyapatite composite fibers |
| CN111118695A (en) * | 2019-08-26 | 2020-05-08 | 张昌录 | Cool multifunctional elastic fabric |
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2013
- 2013-12-04 CN CN201310647438.4A patent/CN104695046A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106400201A (en) * | 2016-09-26 | 2017-02-15 | 嘉兴学院 | Preparation method of chitosan/hydroxyapatite composite fibers |
| CN106400201B (en) * | 2016-09-26 | 2018-10-02 | 嘉兴学院 | The preparation method of chitosan/hydroxyapatite composite fibre |
| CN111118695A (en) * | 2019-08-26 | 2020-05-08 | 张昌录 | Cool multifunctional elastic fabric |
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Application publication date: 20150610 |