CN101736440B - Manufacturing method of dyeable alginate fiber - Google Patents

Abstract

The invention discloses a method for manufacturing dyeable alginate fibers. Adding a water-soluble dendrimer compound into an alginate fiber spinning solution, and carrying out solidification, drafting, washing and post-treatment by adopting wet spinning equipment and technology to obtain the alginate fiber with excellent dyeing property, wherein the content of the dendrimer in the alginate fiber is 1-10%. Compared with the existing alginate fiber production technology, the method has the advantages that the prepared alginate fiber can be dyed by direct dyes and reactive dyes under the salt-free condition, has high dye uptake which can generally reach more than 80 percent, and is 10-15 times higher than that of the alginate fiber produced by the prior art. In addition, the alginate fiber prepared by the method has good color fastness, especially excellent wet processing fastness, and reaches more than grade 4.

Description

Manufacturing method of dyeable alginate fiber

technical field

The invention relates to a method for manufacturing dyeable alginate fibers, in particular to a method for manufacturing dyeable alginate fibers by wet spinning by adding a dendrimer dyeing modifier to a spinning solution.

Background technique

Alginate fiber is a new type of fiber obtained by wet spinning production process with polysaccharide extracted from natural seaweed as raw material and water-soluble metal salt solution as coagulation bath. Seaweed has accumulated rich minerals in the ocean, and contains carbohydrates, amino acids, fats and various vitamins, which can activate the metabolism of cells and have the functions of anti-inflammatory and anti-itching, making alginate fiber have a natural effect on human skin. It has the effects of maintenance, moisturizing, and beauty, and it also has special uses for skin disease treatment. In addition, alginate fiber also has good biodegradability, biocompatibility, excellent hygroscopicity, flame retardancy and electromagnetic shielding ability, making alginate fiber very suitable for the production of high-grade clothing and underwear fabrics, protective clothing As well as decorative textiles and medical textiles. However, alginate fiber is currently mainly used in the production of medical dressings. This is due to its poor salt and alkali resistance. Traditional dyeing processes are difficult to dye alginate fiber, which limits its application in many fields. Therefore, how to realize the dyeing of alginate fibers has become an urgent problem in the field of alginate fiber research, and there are few reports on this aspect at present.

Contents of the invention

The task of the present invention is to provide a kind of manufacture method of dyeable alginate fiber.

Its technical solutions are:

A kind of manufacturing method of dyeable alginate fiber, the step is to add water-soluble dendrimer compound to alginate aqueous solution, adopt wet spinning equipment and process, through coagulation, drafting, washing and post-treatment , to obtain dyeable alginate fiber.

The content of the above-mentioned water-soluble dendritic macromolecular compound in the dyeable alginate fiber is 1%-10%, calculated by weight percentage.

The above-mentioned water-soluble dendrimer compound is a polyamide-amine dendrimer compound, and the selected polyamide-amine dendrimer compound is preferably 1.0 generation to 4.0 generation polyamide-amine dendrimer compound any of the compounds.

The manufacture method of above-mentioned dyeable alginate fiber specifically comprises the following steps:

a Weigh an appropriate amount of polyamide-amine dendrimers and dissolve it in distilled water;

b Select an appropriate amount of alginate to dissolve in the polyamide-amine dendrimer aqueous solution obtained in step a to prepare an alginate fiber spinning solution with a concentration of 3% to 8% by mass; wherein, polyamide- The mass percentage of the amine dendrimer compound to the alginate is 1% to 10%;

c Select an appropriate amount of coagulant to dissolve in water to prepare an aqueous coagulant solution with a mass percent concentration of 2% to 10%, as a coagulation bath for spinning;

d. After filtering and defoaming the alginate fiber spinning solution prepared in step b, enter the coagulation bath prepared in step c under pressure to coagulate, and then draw, wash and dry to obtain dyeable alginic acid salt fiber.

In the above step b, the dissolution temperature of the alginate is 20° C. to 40° C., and mechanical stirring is performed at this temperature for 2 to 6 hours.

In the above step c, the coagulant is any one or a combination of calcium chloride, barium chloride, aluminum chloride, and copper sulfate reagents.

In the above step d: the defoaming process of the alginate fiber spinning solution is vacuum defoaming for 12-24 hours or standing for defoaming for 24-36 hours; the temperature of the coagulation bath is 25°C-60°C; Sectional drawing process, each section is drawn 1.1 to 2.2 times; the fiber washing temperature is 20°C to 50°C, and the drying temperature is 40°C to 80°C.

In the above step b, the alginate is preferably sodium alginate or potassium alginate.

The beneficial technical effect of the present invention is:

1. The invention realizes the dyeing of alginate fibers, which not only helps to promote the application of alginate fibers in the field of clothing and decorative textiles, but also develops various functional textile garments to meet the diversified needs of people's lives; Moreover, it will help accelerate the product upgrading and replacement of my country's textile industry, improve the added value and market competitiveness of products, and promote the sustainable development of my country's textile industry.

2. The aqueous solution of alginate is prepared by dissolving alginate in water. In the prior art, it can be directly used as an alginate fiber spinning solution, and then treated with wet spinning equipment and processes to obtain alginate fiber, but the dyeing performance of the alginate fiber prepared by this method is poor. The present invention creatively adds a dendritic macromolecular dyeing modifier to the alginate fiber spinning solution, and utilizes the existing production process of the alginate fiber to manufacture the alginate fiber with excellent dyeing performance. The method is simple and easy, and the operation process is controllable, and the dosage of the dyeing modifier can be adjusted according to the requirements of the fiber dyeing process.

3. The alginate fiber produced by the present invention has a very high dye uptake rate, which can generally reach more than 80%, which is 10-15 times higher than that of the alginate fiber produced in the prior art. In addition, the color fastness of the fiber is good, especially the wet fastness is excellent, reaching above grade 4.

4. The dyeable alginate fibers manufactured by the present invention are dyed with direct dyes or reactive dyes. Compared with the traditional dyeing process, the dyeing of the alginate fibers manufactured by the present invention does not need to use salt to promote dyeing and alkali agent to fix the color, shortening the process flow.

Detailed ways

The present invention will be further described below in conjunction with specific examples.

Example 1

Weigh 1.2 grams of polyamidoamine dendrimers of the second generation (2.0 generations) and dissolve them in 960 ml of distilled water, then add 40 grams of sodium alginate, and mechanically stir at 25° C. for 4 hours to obtain a concentration of 4% by mass. The sodium alginate fiber spinning solution was filtered and defoamed under reduced pressure for 14 hours to obtain the sodium alginate fiber spinning solution. Under the action of pressure, the sodium alginate spinning stock solution enters the coagulation bath of calcium chloride aqueous solution with a temperature of 30°C and a concentration of 4% by mass through the metering pump and spinneret, and then it is drawn after solidification, and the fiber The drafting adopts three-stage drafting process, and each stage is drawn by 1.5 to 1.8 times, and then washed and dried to obtain dyeable sodium alginate fibers. In the above steps, the fiber washing temperature is 40°C, and the drying temperature is 60°C.

Example 2

Take by weighing the polyamide-amine dendrimer compound of the second generation (2.0 generation) of 2.0 grams, be dissolved in 950ml distilled water, obtain polyamide-amine dendrimer aqueous solution, then add polyamide-amine dendrimer aqueous solution Add 50 grams of sodium alginate to the mixture, stir mechanically at 30°C for 3.5 hours to obtain a sodium alginate fiber spinning solution with a concentration of 5% by mass, filter the above-mentioned sodium alginate fiber spinning solution, and defoam under reduced pressure for 16 hours to obtain seaweed Sodium acid fiber spinning dope. Under the action of pressure, the sodium alginate fiber spinning stock solution enters the coagulation bath of barium chloride aqueous solution with a temperature of 40°C and a concentration of 5% by mass through the metering pump and spinneret, and then is drawn, washed, and dried in sequence. Then get dyeable sodium alginate fiber. In the above steps, the fiber is drawn using a three-stage drawing process, and each stage is drawn by 1.6 to 1.9 times. The fiber washing temperature is 40°C, and the drying temperature is 60°C.

Example 3

Weigh 3.6 grams of the second-generation (2.0 generation) polyamide-amine dendrimers and dissolve them in 940 mL of distilled water, then add 60 grams of sodium alginate, and stir mechanically at 35° C. for 3.5 hours to obtain a polyamide-amine dendrimer with a mass percentage concentration of 6%. The sodium alginate fiber spinning solution was filtered and defoamed under reduced pressure for 18 hours to obtain the sodium alginate fiber spinning solution. Under the action of pressure, the sodium alginate fiber spinning stock solution enters the coagulation bath of aluminum chloride aqueous solution with a temperature of 45°C and a mass percentage concentration of 6% through a metering pump and a spinneret, and is obtained after coagulation, drawing, washing and drying. Sodium alginate fiber can be dyed. In the above steps, the fiber is drawn using a three-stage drawing process, each stage is drawn 1.7 to 2.0 times, the fiber washing temperature is 45°C, and the drying temperature is 65°C.

Example 4

Weigh 5.6 grams of the second-generation (2.0 generation) polyamide-amine dendrimers and dissolve them in 930 mL of distilled water, then add 70 grams of sodium alginate, and stir mechanically at 40°C for 3 hours to obtain seaweed with a mass percentage concentration of 7%. sodium alginate fiber spinning solution, and then filtered and defoamed under reduced pressure for 19 hours to obtain the sodium alginate fiber spinning solution. Under the action of pressure, the sodium alginate fiber spinning dope enters the coagulation bath of calcium chloride aqueous solution with a temperature of 50°C and a mass percentage concentration of 7% through a metering pump and a spinneret, and is obtained after coagulation, drawing, washing and drying. Sodium alginate fiber can be dyed. In the above steps, the fiber is drawn using a three-stage drawing process, each stage is drawn 1.8 to 2.1 times, the fiber washing temperature is 50°C, and the drying temperature is 70°C.

Example 5

Weigh 8 grams of the second-generation (2.0 generation) polyamide-amine dendrimers and dissolve them in 920 mL of distilled water, then add 80 grams of sodium alginate, and stir mechanically at 40°C for 4 hours to obtain seaweed with a mass percentage concentration of 8%. sodium alginate fiber spinning solution, and then filtered and defoamed under reduced pressure for 22 hours to obtain the sodium alginate fiber spinning solution. Under the action of pressure, the sodium alginate fiber spinning stock solution enters the coagulation bath of calcium chloride aqueous solution with a temperature of 50 °C and a mass percentage concentration of 8% through a metering pump and a spinneret, and is obtained after coagulation, drawing, washing and drying. Sodium alginate fiber can be dyed. In the above steps, the fiber is drawn using a three-stage drawing process, each stage is drawn 1.8 to 2.2 times, the fiber washing temperature is 50°C, and the drying temperature is 80°C.

In the above-mentioned embodiment, we select the second generation (2.0 generation) polyamide-amine dendrimers for use, of course, we can also select the first generation (1.0 generation), the third generation (3.0 generation) or the fourth generation ( 4.0 generation) polyamide-amine dendrimers to achieve the same or similar technical effects.

In the above examples, the order of adding the polyamide-amine dendrimer compound and sodium alginate can also be changed, that is, first add sodium alginate to distilled water to prepare a sodium alginate aqueous solution, and then add water-soluble sodium alginate to the sodium alginate aqueous solution. non-toxic polyamide-amine dendrimers.

In the above-mentioned embodiments, the degassing process can be degassed under reduced pressure for 12-24 hours, or left standing for 24-36 hours.

It must be pointed out that the above-mentioned embodiments are only used to further illustrate the present invention, and should not be interpreted as limiting the protection scope of the present invention. Those skilled in the art will make some non-essential aspects of the present invention according to the guidance of the above-mentioned content of the invention. Improvements and adjustments still belong to the protection scope of the present invention.

The properties of common alginate fibers and the dyeable alginate fibers obtained in Examples 1, 2, 3, 4, and 5 are shown in Table 1.

Table 1 Properties of ordinary and dyeable alginate fibers

Note: 1. The fiber dyeing process is as follows:

Weigh 0.04 g of reactive dyes (reactive brilliant red K-2G, reactive yellow K-RN, reactive brilliant blue P-3R) into 100 g of water, stir and dissolve, add 2 g of alginate fiber at 60°C, and dye for 30 minutes. Then boil and wash in 90°C water for 10 minutes, then wash in cold water for 5 minutes, and dry at 80°C or dry in the air.

2. Refer to the national standard "GB/T 3921-2008 Textile Color Fastness Test Color Fastness to Soaping" to test the color fastness to washing of the fiber. The color fastness to soaping of the alginate fibers obtained in Examples 1, 2, 3, 4 and 5 to reactive brilliant red K-2G, reactive yellow K-RN and reactive brilliant blue P-3R all reached or exceeded grade 4.

Claims (7)

1. the manufacturing approach of a stainable alginate fibers; It is characterized in that: water miscible dendrimer compound is added in the alginate aqueous solution; Adopt wet spinning equipment and technology, through solidify, drawing-off, washing and post processing, obtain stainable alginate fibers;

The content of above-mentioned water miscible dendrimer compound in stainable alginate fibers is 1%～10%, by weight percentage;

The dendritic macromole compound that above-mentioned water miscible dendrimer compound is the polyamide-amide class.

2. the manufacturing approach of stainable alginate fibers according to claim 1 is characterized in that the polyamide-amide class dendritic macromole compound of being selected for use is any one in the 1.0 generation～4.0 generation polyamide-amide dendrimer compounds.

3. the manufacturing approach of stainable alginate fibers according to claim 2 is characterized in that may further comprise the steps:

A takes by weighing an amount of polyamide-amide dendrimer compound, and it is dissolved in the distilled water;

B chooses an amount of alginate and is dissolved in the polyamide-amide dendrimer aqueous solution that step a obtained, and makes mass percent concentration and be 3%～8% alginate fibre spinning solution; Wherein, polyamide-amide dendrimer compound is 1%～10% to the mass percent of alginate;

It is 2%～10% aqueous coagulant solution that c chooses an amount of coagulating agent mass percent concentration that makes soluble in water, uses coagulating bath as spinning;

The alginate fibre spinning solution that d produces step b through filter and deaeration after, get under pressure in the coagulating bath that step c produces and solidify, after drawing-off, washing and drying, obtain stainable alginate fibers again.

4. the manufacturing approach of stainable alginate fibers according to claim 3 is characterized in that among the step b, and the solution temperature of alginate is 20 ℃～40 ℃, and under this temperature mechanical agitation 2～6 hours.

5. the manufacturing approach of stainable alginate fibers according to claim 3 is characterized in that among the step c, and said coagulating agent is any one or a few the combination in calcium chloride, barium chloride, aluminium chloride, the copper sulphate reagent.

6. the manufacturing approach of stainable alginate fibers according to claim 3, it is characterized in that in the said steps d: the deaeration technology of alginate fibre spinning solution is vacuum deaerator 12～24h or standing and defoaming 24～36h; The temperature of coagulating bath is 25 ℃～60 ℃; Three sections draft process are adopted in the drawing-off of fiber, 1.1～2.2 times of every section drawing-offs; The washing temperature of fiber is 20 ℃～50 ℃, and bake out temperature is 40 ℃～80 ℃.

7. the manufacturing approach of stainable alginate fibers according to claim 3 is characterized in that among the step b, and said alginate is sodium alginate or potassium alginate.