CN1199115A - Process for preparation of hydroxyethylated chitin fibre - Google Patents
Process for preparation of hydroxyethylated chitin fibre Download PDFInfo
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- CN1199115A CN1199115A CN 98110869 CN98110869A CN1199115A CN 1199115 A CN1199115 A CN 1199115A CN 98110869 CN98110869 CN 98110869 CN 98110869 A CN98110869 A CN 98110869A CN 1199115 A CN1199115 A CN 1199115A
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- chitin
- hydroxyethylation
- preparation
- alkali
- fiber according
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Abstract
A process for preparing hydroxyethylated chitin fibre includes etherification reaction of polyacetamidoglucose with epoxy ethylane in alkaline condition to produce hydroxyethylated chitin, dissolving it in diluted alkali solution to obtain spinning dope, spinning jet and coagulating in coagulation bath, and features less used amount of epoxy ethylane as etherifying agent, no corrosion of apparatus, simple process and low cost.
Description
The present invention relates to a kind of preparation of spinning.
Chitin (chemical name: chitin) extensively be present in arthropodan shell (as shrimp, crab) and the insect shell, also be present in the cell membrane of mushroom, algae and higher plant.Day disclosure clear and 58-183169 patent, it is dissolved in chitin in the mixed solvent of dimethylacetylamide and lithium chloride, the price of this solvent is very high, solvent load is big, so production cost is high.As solvent, and trichloroacetic acid is very big to the corrosivity of equipment, causes the rising of production cost equally with trichloroacetic acid for EP051421.
The object of the present invention is to provide a kind of preparation method of hydroxyethylation chitin fiber of low production cost.
Technical scheme of the present invention is: a kind of preparation method of hydroxyethylation chitin fiber, it comprises following operation
(1). chitin and oxirane are carried out etherification reaction under the alkali condition, generate the hydroxyethylation chitin;
(2). described hydroxyethylation chitin is dissolved in is made into spinning slurry in the dilute alkaline soln;
(3). with described spinning slurry spray silk, the silk of ejection solidifies the formation fiber in coagulating bath.
The present invention compared with prior art has following advantage:
(1). etherifying agent oxirane of the present invention is low-consuming, but complete reaction can be omitted solvent recovery process of the prior art, and technology is simple.
(2). because etherification reaction is complete, do not have waste gas to produce in process of production, to not corrosion of equipment, the cost of etherifying agent is also low, so work simplification, and is with low cost.
Embodiment: a kind of preparation method of hydroxyethylation chitin fiber, it comprises following operation
(1). chitin and oxirane are carried out etherification reaction under the alkali condition, generate the hydroxyethylation chitin;
(2). described hydroxyethylation chitin is dissolved in is made into spinning slurry in the dilute alkaline soln;
(3). with described spinning slurry spray silk, the silk of ejection solidifies the formation fiber in coagulating bath.Described etherification reaction is to put into chitin and high alkali liquid in container, it at container (vacuum is 600 millimetress of mercury) injection ring oxidative ethane in container under the condition of vacuum, after the oxirane gasification, stirring makes it carry out gas-solid phase reaction and generates the alkaline soluble glycol chitin under 20～50 ℃ temperature.The weight proportion of described chitin, oxirane, alkali is: alkali is 10～30% of chitin, and oxirane is 5～60% of chitin.Described alkali is NaOH or potassium hydroxide or calcium hydroxide, and described alkali is preferably NaOH.Consisting of of described spinning slurry
Hydroxyethylation chitin 6～15%
NaOH 4～20%
Zinc oxide 2～8%
All the other are water.In order to dissolve the hydroxyethylation chitin, the method that can adopt twin-screw to mediate can limit dissolving, limit deaeration, limit spinning move continuously, needs only 15 minutes to wire vent from advancing screw rod, shortens dramatically than the diel of the formula of the retouching stirring and dissolving of routine.
Present embodiment to chitinous index request is: logarithmic viscosity number＞4.5, and ash＜0.5%, nitrogen＜7%, moisture content＜5%, color and luster is white.The coagulation bath of present embodiment is an acidic liquid, based on sulfuric acid, during concrete prescription is every liter in the coagulation bath: sulfuric acid 70 grams, vulcanized sodium 220 grams, zinc sulphide 15 grams.In order to strengthen solidifying, also want every liter to add sodium chloride 30 grams in the body lotion.Fiber drawn after solidifying, washing, dry the fiber that promptly becomes, also can carry out chemical interlinkage in case of necessity to fiber, purpose is the hygroscopicity of regulating fiber, improves and does wet strength, and cross linking agent can adopt (NH4) 2SO4, MgCL2, urethanes, mela mine-formaldehyde resin, glyoxal etc.
For example: the usefulness logarithmic viscosity number is mixed with high alkali liquid (NaOH) greater than 4.5 chitin, generate the alkali chitin, the concentration of described high alkali liquid be greater than: 250 the gram alkali/liter, the alkali chitin that generates is through pulverizing, under vacuum condition, carry out gas-solid phase reaction with etherifying agent oxirane, generate the hydroxyethylation chitin, the etherifying agent consumption is that decision hydroxyethylation chitin is alkali solubility or water miscible key, the consumption of etherifying agent of the present invention is chitinous 10～15% for well, crossing low or too high is not dissolve in sig water, and what obtain exactly is water miscible hydroxyethylation chitin, 35～50 ℃ of etherification temperatures, 1～5 hour time, here to point out that according to the size of chitin logarithmic viscosity number, the etherifying agent consumption will be done when adjusting, so far, the hydroxyethylation chitin is a kind of intermediate, and this intermediate must can be dissolved in rare sodium hydroxide solution, is made into spinning slurry, it is described above proportioning components, viscosity 20 to 80.
Claims (7)
1. the preparation method of a hydroxyethylation chitin fiber, it is characterized in that: it comprises following operation
(1). chitin and oxirane are carried out etherification reaction under the alkali condition, generate the hydroxyethylation chitin;
(2). described hydroxyethylation chitin is dissolved in is made into spinning slurry in the dilute alkaline soln;
(3). with described spinning slurry spray silk, the silk of ejection solidifies the formation fiber in coagulating bath.
2. the preparation method of hydroxyethylation chitin fiber according to claim 1, it is characterized in that: described etherification reaction is to put into chitin and high alkali liquid in container, at container be under the condition of vacuum in container the injection ring oxidative ethane, after the oxirane gasification, stirring makes it carry out gas-solid phase reaction and generates the alkaline soluble glycol chitin under 20～50 ℃ temperature.
3. the preparation method of hydroxyethylation chitin fiber according to claim 2, it is characterized in that: the weight proportion of described chitin, oxirane, alkali is: alkali is 10～30% of chitin, and oxirane is 5～60% of chitin.
4. the preparation method of hydroxyethylation chitin fiber according to claim 1 is characterized in that: described alkali is NaOH or potassium hydroxide or calcium hydroxide.
5. the preparation method of hydroxyethylation chitin fiber according to claim 1 is characterized in that: described alkali is NaOH.
6. the preparation method of hydroxyethylation chitin fiber according to claim 1 is characterized in that: the consisting of of described spinning slurry
Hydroxyethylation chitin 6～15%
NaOH 4～20%
Additive: zinc oxide 2～8%
All the other are water.
7. the preparation method of hydroxyethylation chitin fiber according to claim 1 is characterized in that: the method that described dissolving hydroxyethylation chitin adopts twin-screw to mediate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98110869 CN1199115A (en) | 1998-05-22 | 1998-05-22 | Process for preparation of hydroxyethylated chitin fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98110869 CN1199115A (en) | 1998-05-22 | 1998-05-22 | Process for preparation of hydroxyethylated chitin fibre |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1199115A true CN1199115A (en) | 1998-11-18 |
Family
ID=5220885
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98110869 Pending CN1199115A (en) | 1998-05-22 | 1998-05-22 | Process for preparation of hydroxyethylated chitin fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1199115A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368328B (en) * | 2008-08-04 | 2011-11-09 | 东华大学 | Preparation method for hydroxyethyl group chitosan fiber |
-
1998
- 1998-05-22 CN CN 98110869 patent/CN1199115A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368328B (en) * | 2008-08-04 | 2011-11-09 | 东华大学 | Preparation method for hydroxyethyl group chitosan fiber |
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