CN101812802A - Method for preparing chitosan modified sizing agent used for sizing terylene super fine denier polyester filaments - Google Patents
Method for preparing chitosan modified sizing agent used for sizing terylene super fine denier polyester filaments Download PDFInfo
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Abstract
The invention relates to a method for preparing a chitosan modified sizing agent used for sizing terylene super fine denier polyester filaments. The method comprises the following steps of: (1) preparing persulfate solution; (2) adding chitosan into the persulfate solution to obtain a mixture; (3) adding glacial acetic acid liquid into the mixture, wherein the reaction system is refluxed in a closed mode and is placed in a water bath; heating the reaction system to the temperature of 90 DEG C; performing reaction by preserving heat; adding the chitosan; when the viscosity value is tested to be between 8 and 16 mPa.s, adding sodium sulfite solution; lowering the temperature to 30 DEG C; testing the pH value; regulating the pH value of reaction system solution to be 5 to 7 by using NaHCO3 solution; and adding a non-ionic surface active agent. The method is simple, has no pollution, and is suitable for industrial production; and the obtained chitosan modified sizing agent has the advantages of high adhesive force, high stability, convenient size mixing, and easy sizing operation.
Description
Technical field
The invention belongs to the preparation field of shitosan slurry, particularly relate to a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching.
Background technology
Dacron fine-denier long filament (multifilament) is in weaving process, and is powerful poor because number of fiber is few in the tow, is subjected to effects such as mechanical friction and adjacent yarn friction, the silk fiber fracture can take place, tangle phenomenon, causes and weaves and can't carry out.In order to make terylene super fine denier polyester filaments be processed into the vessel-like goods smoothly, need carry out starching to yarn.At present, domestic also being not used in washed a special sizing agent of woven blood vessel's shape thing, and not only there is the uncomfortable problem of sizing performance in common slurry, also exists destarch to influence artificial blood vessel serviceability problem not to the utmost.
At present, common type of stock is more, mainly contains materials such as starch, polyvinyl alcohol, polyacrylic and other polymer substance such as carboxymethyl cellulose, gelatin, polyoxyethylene ether.Starch size has abundant, renewable, the biodegradable characteristic in source, and cellulose fibre is had good adhesive force and film forming ability, but not enough to the polyster fibre adhesion, can not satisfy the starching requirement.The polyvinyl alcohol synthetic slurry is better to the polyster fibre adhesion, but biological degradability is poor, and environment is unfriendly, and destarch is also difficult.Polyacrylic is to terylene adhesion height, and sizing performance is good, but also belongs to synthetic slurry, and biological degradability is not as natural slurry.Other slurry, all some limits to separately aspect performance, source or environment, biocompatibility, can not accomplish the unification of sizing performance and biological safety simultaneously.
Shitosan derives from natural polymer, it is the abundant natural alkaline polysaccharide of unique existence, shitosan is nontoxic, good biocompatibility, biologically active and biodegradability are arranged, have effects such as antibiotic, anti-inflammatory, hemostasis, immunity, in aspect extensive uses such as artificial skin, operation suture thread, medical dressing, man-made organ, medical materials, performance has not had any query aspect security.
The terylene super fine denier multifilament forms the vessel-like goods by woven processing method and is used for medical treatment, and the slurry that is adopted during starching intends selecting to take into account sizing performance, biodegradability and security performance.Shitosan family macromolecule material, have above-mentioned fundamental characteristics, but, need carry out chemical modification chitosan molecule as terylene super fine denier multifilament slurry, make it to meet the slurry serviceability, keep characteristics such as the shitosan macromolecule is natural, antibiotic, degradable, safety again.
The polyester filament woven blood vessel is a blood vessel substitute main, that can enter clinical practice in artificial blood vessel research, is the primary study object of domestic artificial blood vessel.After washing a super fine denier multifilament starching, monofilament is starched with adhesives, parcel, and the collectivity of tow improves, and can resist the friction between mechanical friction and the yarn, can not tangle by fracture of wire, makes woven processing smooth, forms vessel-like fabric quality height.Therefore, slurry plays an important role in washing woven blood vessel's making.
Washing a characteristic of thin dawn multifilament is that fiber surface is smooth, hydrophobic, monofilament is thin, powerful low, as the blood vessel substitute, also needs safe and harmless, for this reason, slurry therewith should have characteristics such as adhesiveness is good, convergence increase, film tough and hard wear resistant, the quick also biodegradable of destarch.Analyze in view of the above, wash a super fine denier multifilament and should have following two main features with slurry: (1) has ecology, safe, biodegradable, this is that the operating characteristic of artificial blood vessel determines, although slurry does not enter final products as processing aid, can destarch remove, but security reliability is improved.(2) have convenience for size mixing, starching is easy, the rate of sizing is high, serous coat is pliable and tough, ABRASION RESISTANCE is good, can significantly improve weavability, the easy characteristics of destarch.
According to These characteristics, on the pluses and minuses basis of understanding natural and synthetic high polymer slurry, be that the master makes the woven slurry of using of polyester filament artificial blood vessel with shitosan class material, be reasonable selection.At present, shitosan raw material and the product supplied on the market can not be as slurries, because it does not meet size performance, i.e. and starching and destarch performance demands.
Chitin modified slurrying material, weave the artificial blood vessel slurry especially for the terylene super fine denier multifilament, domestic relevant document is less at present, only there are 2006, the bio-modification research of sizing performance when the chitin that the Chen Yan of Donghua University etc. deliver on the weaving Leader is made slurry, it is mainly studied is with the enzyme process viscosity reduction, improve chitin water soluble to be used for textile sizing, and enzyme operating position more complicated, performance are also unstable.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching, and this method is simple, and is pollution-free, is suitable for suitability for industrialized production; It is easy that the chitin modified slurry of gained has adhesion height, good stability, convenience for size mixing, slashing operation.
A kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching of the present invention comprises:
(1) the preparation mass percent is 0.4～0.6% persulfate solution;
(2) get shitosan and add in the above-mentioned persulfate solution, add while stirring, get mixed solution;
(3) add glacial acetic acid liquid in above-mentioned mixed solution, stir, the airtight backflow of reaction system, place water-bath, reaction system heats up, temperature to 90 ℃, insulation reaction; Add the shitosan with step weight such as (2) 1-3 time, insulation reaction to solution flows like water, during tested viscosity value to 8～16mPa.s, every hectogram solution adds 5% mass percentage concentration sodium sulfite solution, 2.5 grams, cooling cooling reaction system to 30 ℃, test pH value is the NaHCO of 5%-10% with mass percentage concentration
3Solution conditioned reaction system solution pH value adds non-ionic surface active agent to 5-7, takes out promptly.
Persulfate in the described step (1) is sodium peroxydisulfate, potassium peroxydisulfate or ammonium persulfate.
Deacetylating degree of chitosan in the described step (2) is 70～85%, and consumption is 1.5～6% of a mixed solution quality, preferred amounts 3～5%.
Deacetylating degree of chitosan in the described step (3) is 70～85%.
Glacial acetic acid liquid addition in the described step (3) is 3～5% of a mixed solution quality, after glacial acetic acid liquid adds, when being stirred to thickness and not flowing, stirs and suspends.
Reaction system in the described step (3) heats up with 2～4 ℃ of speed of per minute.
Reaction maximum temperature in the described step (3) is at 90 ℃, and insulation reaction is controlled 90 ℃ of reactant liquor viscosity numbers at 8～16mPa.s.
The method of testing of described step (3) viscosity number is, in reactor or take out 100 milliliters of liquid, with NDJ-1 type rotation viscometer tested viscosity value.
After being reflected at viscosity and meeting the requirements in the described step (3), use the sodium sulfite solution conditioned reaction, with about NaHCO3 solution conditioned reaction system solution pH value to 6.
Non-ionic surface active agent in the described step (3) is 50～53% APG, and for commercially available, consumption is 0.6～1.0% of a solution quality.
Described chitin modified slurries, chitosan molecule contain the amino of some and the carboxyl that oxidation forms, and contain surfactant in the slurries, and viscosity, concentration, pH value meet the starching claimed range.
The chitin modified slurry of usefulness of the present invention is as follows to the method for terylene super fine denier polyester filaments warp sizing:
Sizing technique method one: made chitin modified slurries are heated to 50～60 ℃, on the monofilament Sizing machines, 30D/12F is carried out the starching of dacron fine-denier multifilament, the rate of sizing 12～14%, the dewaxing of slurry after waxing animal and plant fat, the amount of waxing accounts for slurry yarn quality 0.4～0.6%.
Sizing technique method two: get made chitin modified slurries, viscosity is 6～8mPa.s polyacrylate grafting modified starch, both dry weight ratios are 1: 1, be heated to 85 ℃, mashing off half an hour, on the monofilament Sizing machines, 30D/12F is carried out the starching of dacron fine-denier multifilament, the rate of sizing 12～14%, the dewaxing of slurry after waxing animal and plant fat, the amount of waxing accounts for slurry yarn quality 0.6～0.8%.
Have certain carboxyl and amino on the chitin modified slurry molecular structure that the present invention makes, have acidic-group and basic group simultaneously, have the Amphiphatic high polymer electrolyte property, certain dissolubility is arranged in the pH relative broad range, desizability might as well in the hot water.Because unit structure is hydrophilic, it is also big that film properties improves again, and this material is during to warp sizing, directly uses or the water dilution is used, and slurries are stable, and sizing wear resistant is good, slurry biological degradability, security are good.With Polyacrylamide Grafted modified starch, animal and plant fat after waxing combination, has good effect.
The processing performance that textile sizing needs has: adhesiveness, viscosity, film forming, water-soluble.Adhesiveness be the starching engineering by main performance, make slurry bonding between fiber, strengthening the ability of warp thread opposing friction and other mechanisms, between adhesion property and starch finishing effect and the sizing quality confidential relation is arranged, is an important parameter of sizing technique.Many hydroxyls and amino are arranged on the chitosan molecule, soda acid base interaction force and the hydrogen bond action power certain with the intermolecular formation of polyster fibre, the further modification of chitosan molecule can make molecular structure submissive, and interfacial interaction is stronger.Infiltration, the coating characteristic of viscosity decision slurries, suitable viscosity are to guarantee that slurry is distributed in the inside and outside reasonably prerequisite of multifilament, and too high, low excessively viscosity is all bad to sizing performance, therefore, when chitin modified slurrying material, need control product viscosity simultaneously.Film forming is meant the film forming ability of slurry molecule self interphase interaction, the interleaving effect repeatedly of weaving requires serous coat that certain pliability is arranged, just can bear mechanism such as stretching, bending and do not break, slurry does not fall, by modification, connect flexible group, reduce the serous coat vitrification point, the modification of chitosan molecule is made slurry and can be met the demands.Water cheapness, safe, harmless, other solvent type method for sizing can't be compared with it, therefore the textile sizing great majority use aqueous solution starching method at present, aqueous solution destarch method is also used in destarch, so it is water-soluble that the starching disposed slurry all should have destarch, water-soluble high-molecular compound must contain hydrophilic radical, as hydroxyl, carboxyl, amide groups etc.Chitosan molecule can obtain better water solubility by modification, the control of molecular size appropriateness, and simultaneously, group can make serous coat that the certain space structure is arranged, and helps pliable and toughization of rigidity serous coat, is beneficial to and weaves.Based on the above-mentioned theory analysis, preparation is used for the chitin modified slurry that the terylene super fine denier multifilament is weaved usefulness.
Beneficial effect
(1) preparation method of the present invention is simple, and is pollution-free, is suitable for suitability for industrialized production;
(2) the chitin modified slurry that makes of the present invention has adhesion height, good stability, convenience for size mixing, slashing operation and is easy to characteristics, and last sizing ABRASION RESISTANCE is good, slurry desizability, good, the human safety advantages of higher of biological degradability.
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
Join that to get mass percentage concentration be 450 milliliters of 0.6% sodium peroxydisulfate solution; Take by weighing shitosan raw material 16.67 grams, 16.67 gram shitosans are added in the sodium peroxydisulfate solution, add while stirring, shitosan and solution are mixed; get 25 milliliters of glacial acetic acid liquid and evenly add; stir, reaction system is airtight, have reflux, reaction system to place water-bath with 3 ℃ of speed heat temperature raisings of per minute; to 90 ℃; insulation reaction 5min., take by weighing shitosan raw material 16.67 grams, add reactant liquor; stir; insulation reaction to solution flows like water, take by weighing shitosan raw material 16.66 grams in addition again, add in the reactant liquor equably; Treat that the chitosan solution kinematic viscosity is in 8～16mPa.s, add 5% mass percentage concentration sodium sulfite solution 12.5 gram, cooling, cooling reaction system to 30 ℃, test pH value is 10% NaHCO with mass percentage concentration
3About solution conditioned reaction system solution pH value to 6; Add non-ionic surface active agent APG 3 gram of 50% quality percentage composition, stirred 15 minutes, the taking-up reacting slurry, the slurries of mass percentage concentration 10%.
Embodiment 2
The preparation mass percentage concentration is that 720 milliliters of 0.6% potassium persulfate solutions are stand-by; Take by weighing two parts of shitosan raw material 40 grams, 40 gram shitosans are added in the potassium persulfate solution, add while stirring, shitosan and solution are mixed, get glacial acetic acid liquid and evenly add for 32 milliliters, stir, reaction system is airtight, reflux is arranged, and reaction system places water-bath with 2 ℃ of speed heat temperature raisings of per minute, to 90 ℃, insulation reaction., treat that solution flows like water, the shitosan that adds second part stirs insulation reaction, treat that the chitosan solution kinematic viscosity is in 8～16mPa.s, add 5% mass percentage concentration sodium sulfite solution 20 gram, cooling, cooling reaction system to 30 ℃, testing the pH value, is 5% NaHCO with mass percentage concentration
3About solution conditioned reaction system solution pH value to 6; Add non-ionic surface active agent APG 4.8 gram of 50% quality percentage composition, stirred 15 minutes, the taking-up reacting slurry, the slurries of mass percentage concentration 10%.
Embodiment 3
The preparation mass percentage concentration is that 920 milliliters of 0.4% ammonium persulfate solutions are stand-by; Take by weighing shitosan raw material 80 grams, be divided into three equal parts, every part 26.67 gram is standby, 26.67 gram shitosans being added in the ammonium persulfate solutions, add while stirring, shitosan and solution are mixed; get glacial acetic acid liquid and evenly add for 30 milliliters; stir, reaction system is airtight; reflux is arranged, and reaction system places water-bath with 3 ℃ of speed heat temperature raisings of per minute; to 90 ℃; insulation reaction, and the shitosan that adds second part stirs, and insulation reaction to solution flows like water; be operated to shitosan equally and add; insulation reaction, treat that the chitosan solution kinematic viscosity is in 8～16mPa.s, add 5% mass percentage concentration sodium sulfite solution, 25 grams; lower the temperature; cooling reaction system to 30 ℃, test the pH value, is 5% NaHCO with mass percentage concentration
3About solution conditioned reaction system solution pH value to 6; Add non-ionic surface active agent APG 10 gram of 50% quality percentage composition, stirred 15 minutes, the taking-up reacting slurry, the slurries of mass percentage concentration 8%.
Embodiment 4
Embodiment 1～3 made chitin modified slurries are heated to 50 ℃, on the monofilament Sizing machines, 30D/12F is carried out the starching of dacron fine-denier multifilament, the rate of sizing is controlled at 12～14% of multifilament quality, the dewaxing of slurry after waxing animal and plant fat, the amount of waxing are controlled at and account for 0.4～0.6% of slurry yarn quality, are woven into tube knitting on the pipe machine, tube boils 30min. at pH5.5,95 ℃, 1: 50 hot water of bath raio, take out, destarch is finished in 95 ℃ of clear water rinsings three times.
Embodiment 5
Get embodiment 1～3 made chitin modified slurries, viscosity is 6～8mPa.s polyacrylate grafting modified starch, both dry weight ratios are 1: 1, being mixed with solid content is that mass percent is 10% solution, be heated with stirring to 85 ℃, mashing off half an hour, on the monofilament Sizing machines 30D/12F is carried out the starching of dacron fine-denier multifilament, the rate of sizing is controlled at 12～14% of multifilament quality, the dewaxing of slurry after waxing animal and plant fat, the amount of waxing accounts for slurry yarn quality 0.6～0.8%, be woven into tube knitting on the pipe machine, tube is at pH5.5,95 ℃; 1: 50 hot water of bath raio boils 30min., take out; 95 ℃ of clear water rinsings three times, finish destarch.
The performance data of the dacron fine-denier multifilament starching of embodiment 4 and embodiment 5 is as shown in table 1 below, method of testing is measured by textile industry starching detection method commonly used, the data of table 1 show that starching can weave in the role smoothly to the dacron fine-denier multifilament, brute force is not a principal element, because with not starching polyester multifilament comparison, the increase of starching silk brute force is not remarkable.Starch finishing effect is mainly reflected in boundling, the slurry silk is wear-resisting not loose, when monolateral friction 30 times, the slurry silk anti-wear performance of pure chitosan slurry sizing is better than mixed pulp, from the adhesion data of the pure terylene rove of starching gained as can be known, than higher, adhesion property is outstanding to the polyster fibre adhesion for the shitosan slurry.
Table 1 invention slurry is to the sizing performance of dacron fine-denier multifilament
| Numbering | ??1 | ??2 | ??3 | ?4 | ??5 | ?6 |
| Pulp components | Embodiment 1 slurry (shitosan) | Embodiment 2 slurries (shitosan) | Embodiment 3 slurries (shitosan) | Embodiment 1 slurry (shitosan)+graft starch | Embodiment 2 slurries (shitosan)+graft starch | Embodiment 3 slurries (shitosan)+graft starch |
| The pulp components ratio | ??100％ | ??100％ | ??100％ | ?1∶1 | ??1∶1 | ?1∶1 |
| Slurry viscosity (mPa.s) | ??17 | ??17 | ??16 | ?15 | ??15 | ?15 |
| The rate of sizing (%) | ??12 | ??13 | ??12 | ?13 | ??13 | ?13 |
| Sizing tow ABRASION RESISTANCE (monolateral friction 30 times) | There is not loose phenomenon | There is not loose phenomenon | There is not loose phenomenon | Bunch fiber is little to scatter | Bunch fiber is little to scatter | Bunch fiber is little to scatter |
| Slurry silk ultimate strength (cN) | ??151 | ??151 | ??150 | ?149 | ??148 | ?148 |
| Slurry silk elongation at break (%) | ??28 | ??28 | ??28 | ?29 | ??29 | ?29 |
| Starch the adhesion (N) of pure terylene rove | ??146 | ??147 | ??145 | ?143 | ??144 | ?144 |
Annotate: precursor ultimate strength 145cN, elongation at break 27%.
Claims (7)
1. preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching comprises:
(1) the preparation mass percent is 0.4～0.6% persulfate solution;
(2) get shitosan and add in the above-mentioned persulfate solution, add while stirring, get mixed solution;
(3) add glacial acetic acid liquid in above-mentioned mixed solution, stir, the airtight backflow of reaction system, place water-bath, reaction system heats up, temperature to 90 ℃, insulation reaction; Add the shitosan with step weight such as (2) 1-3 time, insulation reaction to solution flows like water, during tested viscosity value to 8～16mPa.s, every hectogram solution adds 5% mass percentage concentration sodium sulfite solution, 2.5 grams, cooling cooling reaction system to 30 ℃, test pH value is the NaHCO of 5%-10% with mass percentage concentration
3Solution conditioned reaction system solution pH value adds non-ionic surface active agent to 5-7, takes out promptly.
2. a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching according to claim 1 is characterized in that: the persulfate in the described step (1) is sodium peroxydisulfate, potassium peroxydisulfate or ammonium persulfate.
3. a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching according to claim 1 is characterized in that: the deacetylating degree of chitosan in the described step (2) is 70～85%, and consumption is 1.5～6% of a mixed solution quality.
4. according to claim 1 or 3 described a kind of preparation methods that are used for the chitin modified slurry of terylene super fine denier polyester filaments starching, it is characterized in that: the chitosan dosage in the described step (2) is 3～5% of a mixed solution quality.
5. a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching according to claim 1 is characterized in that: the glacial acetic acid liquid addition in the described step (3) is 3～5% of a mixed solution quality.
6. a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching according to claim 1 is characterized in that: the reaction system in the described step (3) heats up with 2～4 ℃ of speed of per minute.
7. a kind of preparation method who is used for the chitin modified slurry of terylene super fine denier polyester filaments starching according to claim 1, it is characterized in that: the non-ionic surface active agent in the described step (3) is 50～53% APG, and consumption is 0.6～1.0% of a solution quality.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102330341A (en) * | 2011-07-26 | 2012-01-25 | 吴江市瑞丰织造有限公司 | Biodegradable cotton fiber slurry |
| CN103103762A (en) * | 2012-12-11 | 2013-05-15 | 宜兴市军达浆料科技有限公司 | Fatigue-resistant hydroxyethyl high-performance modified starch |
| CN103225207A (en) * | 2013-04-28 | 2013-07-31 | 徐州众恒淀粉科技有限公司 | Chitosan grafted copolymer slurry formula and preparation method thereof |
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| JP2001081027A (en) * | 1999-09-09 | 2001-03-27 | Ichimaru Pharcos Co Ltd | Antibacterial-antiseptic agent |
| US20070178125A1 (en) * | 2003-05-21 | 2007-08-02 | Aki Laine | Process for the preparation of carnitine esters and their use |
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- 2010-03-11 CN CN2010101222839A patent/CN101812802B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001081027A (en) * | 1999-09-09 | 2001-03-27 | Ichimaru Pharcos Co Ltd | Antibacterial-antiseptic agent |
| US20070178125A1 (en) * | 2003-05-21 | 2007-08-02 | Aki Laine | Process for the preparation of carnitine esters and their use |
Non-Patent Citations (2)
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| 《全国浆料和浆纱技术2006年会》 20061231 陈燕等 壳聚糖的生物改性及其在浆料应用上的研究 第65-72页 1-7 , 2 * |
| 《纺织学报》 20031231 黄立新 细旦高密涤纶短纤织物的上浆工艺研究 第357-358页 1-7 第24卷, 第4期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102330341A (en) * | 2011-07-26 | 2012-01-25 | 吴江市瑞丰织造有限公司 | Biodegradable cotton fiber slurry |
| CN103103762A (en) * | 2012-12-11 | 2013-05-15 | 宜兴市军达浆料科技有限公司 | Fatigue-resistant hydroxyethyl high-performance modified starch |
| CN103103762B (en) * | 2012-12-11 | 2015-01-21 | 宜兴市军达浆料科技有限公司 | Fatigue-resistant hydroxyethyl high-performance modified starch |
| CN103225207A (en) * | 2013-04-28 | 2013-07-31 | 徐州众恒淀粉科技有限公司 | Chitosan grafted copolymer slurry formula and preparation method thereof |
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| CN101812802B (en) | 2012-01-11 |
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