CN113913960A

CN113913960A - Morinda citrifolia filament yarn and preparation method thereof

Info

Publication number: CN113913960A
Application number: CN202111304229.0A
Authority: CN
Inventors: 黄金洪; 赵志远; 张静
Original assignee: YIBIN HUIMEI FIBER NEW MATERIAL CO Ltd
Current assignee: YIBIN HUIMEI FIBER NEW MATERIAL CO Ltd
Priority date: 2021-11-05
Filing date: 2021-11-05
Publication date: 2022-01-11
Anticipated expiration: 2041-11-05
Also published as: CN113913960B

Abstract

The invention provides noni filament and a preparation method thereof, belonging to the field of preparation of functional cellulose fibers. Taking noni extract and viscose as raw materials, and preparing noni filament yarn after blending, spinning, solidifying and post-processing; wherein, the weight ratio of the noni extract is 1-30%, and the ratio of the alpha fibers in the viscose is 70-99%. In the invention, substances in the noni extract are crosslinked and solidified in the nail fibers in the viscose through a specific preparation process, so that the functionalization of the filaments is realized.

Description

Morinda citrifolia filament yarn and preparation method thereof

Technical Field

The invention relates to a noni filament and a preparation method thereof, belonging to the field of preparation of functional cellulose fibers.

Background

The regenerated cellulose fiber is a degradable material which takes natural cellulose (such as cotton, hemp, bamboo, trees, shrubs and the like) as a raw material, and active hydroxyl in the natural cellulose molecule and a plurality of functional molecules are subjected to graft copolymerization in different production links to realize modification. Wherein, the physical structure of the natural cellulose is changed without changing the chemical structure, so as to manufacture regenerated cellulose fiber with better performance, such as: the fabric has good air permeability, good hygroscopicity, good elasticity, smooth and cool hand feeling, is not easy to generate static electricity, and has the softness of cotton, the luster of silk and the smoothness of hemp; easier coloring, good color fastness and the like.

Noni fruit is the fruit of morinda citrifolia, which is rich in the components of human cells (somatic cells). Noni juice has been found by experimental studies and epidemiological statistics to have various health benefits, such as: it has effects in improving physical fitness, improving overall health condition, relieving inflammation and pain, improving sleep, and improving allergic constitution. Noni fruit contains more than 150 nutrient elements such as siloenin, active ferment, beta-carotene, nicotine, protein, carbonate, folic acid, biotin, pantothenic acid, serotonin, dietary fiber, ferment, vitamin A, B group, C, D, E, K, calcium, iron, magnesium, zinc, iodine, phosphorus, copper, chromium, manganese, sulfur, sodium, potassium, selenium, germanium, molybdenum and the like.

In the prior art, "CN 201610781630.6 a noni extract emulsion and its preparation method and application" discloses that fresh noni is added into an ethanol aqueous solution containing a surfactant, stirred, and filtered after sufficient extraction to obtain the noni extract emulsion. The invention also provides application of the noni extract emulsion in preparing cosmetics or skin care products, and the noni extract emulsion has strong free radical clearing capability and good whitening and skin care effects. Wherein the surfactant comprises an ionic surfactant and a nonionic surfactant, and the ionic surfactant comprises hydroxypropyl methylcellulose. CN202010936638.1 noni fruit homopolysaccharide extraction and separation method and application disclose that noni fruit homopolysaccharide is used as a biological active component for inhibiting human liver cancer cells to be applied to preparation of antitumor drugs.

Disclosure of Invention

On the basis of the prior art, the invention provides a method for directly converting noni extract into fiber, using the fiber as a raw material of clothes, masks, sanitary materials and the like, and then blending the fiber with viscose to finally obtain noni filament, so that the functionalization of viscose is realized, and a new filament material is developed.

In order to achieve the technical purpose, the following technical scheme is proposed:

a Morinda citrifolia filament is prepared from Morinda citrifolia extract and viscose as raw materials by blending, spinning, coagulating, solidifying and post-treating; wherein, the weight ratio of the noni extract is 1-30%, and the ratio of the alpha fibers in the viscose is 70-99%;

the indexes of the prepared noni filament finished product are as follows:

the dry breaking strength is more than or equal to 1.85cN/dtex, the wet breaking strength is more than or equal to 0.85cN/dtex, and the dry breaking elongation is 17-24%.

Furthermore, the noni fruit content in the noni fruit extract is not less than 95%, and the viscose liquid takes serous fluid with alpha-cellulose content not less than 90%, hemicellulose not more than 15g/L and average polymerization degree of 700-1000 as raw material.

A preparation method of noni filament yarns comprises the following steps:

A. preparation of noni juice

1) Dissolving the noni extract in an ethanol water solution with the temperature of 50-90 ℃ and the concentration of 1-40%; adding hydroxypropyl methyl cellulose, fully stirring, and cooling to 30-40 ℃ to obtain a solution I;

wherein, the mass fraction of the noni extract dissolved in the ethanol water solution is 10-50%, the noni extract can be purchased directly, and the noni extract comprises silonin, active ferment, beta-carotene, nicotine, protein, carbonate and the like. The quality fraction is set to ensure the smooth and stable proceeding of the subsequent procedures, such as: when the mass fraction is less than the mass fraction, in order to ensure the quality of the final product, namely the morinda citrifolia filaments, during subsequent spinning, the amount of the morinda citrifolia solution is more, so that more water and ethanol are brought in, the viscosity of the viscose is reduced, and the spinning is not facilitated; similarly, if the addition amount of the noni fruit extract is too much, the viscosity of the solution is too high, the noni fruit solution is inconvenient to mix when being added into viscose, and the mixing is not uniform, so that the spinning process and the quality of the noni fruit filament are seriously affected;

ethanol is defined as a solvent, and the ethanol is mainly matched with the characteristics of substances in the noni extract to ensure the solubility of the substances in the noni extract, such as: part of the noni extract has low solubility in a simple aqueous solvent, and some precipitate-like insoluble substances are present. And setting the temperature of 50-90 ℃ and the concentration of 1-40% to ensure the solubility of substances in the noni fruit extract in ethanol, wherein if the temperature is too high, the ethanol in the solution can be quickly volatilized, so that the cost is wasted, and the concentration of the ethanol in the solution is reduced, but the theoretical solubility cannot be achieved; the temperature is too low, so that the substances in the noni extract are slowly dissolved, and the period of the whole preparation process is prolonged. Therefore, the mutual matching of the solvent ethanol, the concentration and the dissolving temperature thereof ensures the solubility of the substances in the noni fruit extract, thereby facilitating the subsequent processes;

wherein the mass fraction of the addition amount of the hydroxypropyl methyl cellulose is 1-5%, and the mass fraction specifically refers to: the mass fraction of hydroxypropyl methylcellulose in the total mixture of the noni fruit extract and the ethanol. The hydroxypropyl methylcellulose with the mass fraction promotes the dissolution of substances in the noni extract, disperses the solution, has the function of compatibilization, and is convenient for the dissolution of the noni extract and the stability of the solution;

after fully stirring, cooling to 30-40 ℃, ensuring that ethanol is not volatilized due to high temperature in the solution preparation process, and facilitating the addition of substances in subsequent processes (at the temperature);

2) adding caustic soda into the solution I obtained in the step 1), and adjusting the pH value to 8.5-9; slowly adding the cross-linking agent within 3 hours under the condition of continuously keeping the temperature at 30-40 ℃, and continuously stirring for 5-24 hours, so that the solution I and the cross-linking agent are uniformly mixed, and the self-crosslinking phenomenon is reduced, thereby obtaining a solution II;

wherein the cross-linking agent is 1,4 butanediol diglycidyl ether and/or ethylene glycol diglycidyl ether; the mass fraction of the addition amount of the cross-linking agent is 1-10%, and the mass fraction specifically refers to: the mass fraction of the crosslinking agent in the added solution;

caustic soda is used as an acid-base regulator, so that the cost is low, the caustic soda is also a commonly used reagent in the textile industry, the source is wide (the caustic soda can be directly purchased and can also be recovered from a spinning process), and the related waste liquid treatment process is mature;

regarding the adjustment of the pH value, the raw material viscose is alkaline, so that the solution I is adjusted to be alkaline (if the solution I is acidic, the acid-base neutralization reaction in the subsequent blending can affect the spinning solution and can not carry out normal spinning), and the smooth and stable operation of the subsequent spinning process is ensured; in addition, when the pH value is too high, substances such as protein, silonin and the like in the noni fruit extract lose activity, and the quality of a final product cannot be guaranteed;

the heat preservation temperature is set to be 30-40 ℃, so that the temperature reduction temperature in the step 1) is met, the activity of substances such as protein, silonin and the like in the noni extract is kept, and the volatilization of ethanol is reduced;

the addition of the cross-linking agent enables most of substances in the noni liquid to be combined with the nail fibers when the noni liquid and the viscose are blended; meanwhile, in subsequent post-treatment, the primary filament product is dried and then subjected to ultraviolet radiation so as to be crosslinked again, and the crosslinking effect is ensured. The noni liquid is slowly added within 3 hours, so that the noni liquid is convenient to stir and uniformly disperse; meanwhile, the limitation of the feeding mode of 'slow feeding' can prevent the heat release generated in the dissolving process and reduce the self-crosslinking phenomenon;

3) standing the obtained solution II for more than 24h to precipitate part of insoluble substances in the solution II, and removing the insoluble substances by using a centrifugal machine or a filter to obtain noni liquid;

B. blending of

Defoaming the obtained noni liquid and viscose respectively, then carrying out static mixing, and then defoaming to obtain a blended liquid;

in static mixing, the mass ratio of the noni liquid is 1-30%, and the mass ratio of the alpha fibers in the viscose liquid is 70-99%;

wherein the viscose takes serum containing more than or equal to 90 percent of alpha-cellulose, less than or equal to 15g/L of hemicellulose and an average polymerization degree of 700-1000 as a raw material;

compared with the raw material pulp for producing common viscose staple fibers, the pulp for producing filaments requires high purity of the initial raw material, high content of alpha-cellulose in the pulp and small fluctuation range; low hemicellulose and other impurities are required, such as: if the content of hemicellulose in the pulp is high, the technical processes of impregnation, ageing, yellowing, alkali liquor recovery and the like are difficult to occur, the quality of viscose is influenced, and the physical and mechanical properties of finished silk are reduced finally; the average polymerization degree is ensured to be moderate and to be uniformly distributed, the fluctuation range of the distribution is small, and the like.

During static mixing, the ratio of the noni liquid to the viscose is limited, so that subsequent spinning is guaranteed, and the quality of a final product is guaranteed. Such as: if the noni liquid accounts for a large proportion, spinning is not facilitated, and spinning forming is not good; if the noni liquid is low in proportion, the obtained functional filament has unobvious characteristics;

C. spinning

Spinning by adopting a continuous method;

feeding the blended liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blended liquid into the spinning machine through a metering pump, filtering particle impurities by using a candle filter, feeding the filtered blended liquid into a spinning nozzle assembly through a curved pipe, and allowing the blended liquid to pass through spinning holes under pressure to form viscose trickle;

the related spinning process specifically comprises the processes of pre-spinning filtration, a metering pump, a spinning nozzle, a spinning glass tube, a drafting disc, a processing roller, a drying roller, an oiling roller, ring spindle winding and the like;

D. solidification and solidification

And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a nascent strand silk;

wherein the coagulating bath comprises 260-340g/L sodium sulfate, 125-135g/L sulfuric acid, 10-25g/L zinc sulfate and 8-25g/L auxiliary agent, the circulating amount of the acid bath is 35-45L/ingot minute, the immersion length is 2.4-3.5m, the specific gravity of the coagulating bath and the viscose trickle is 1.25-1.32, the temperature of the coagulating bath is 40-60 ℃, and the forming of the viscose trickle can be better ensured. Viscose spinning is a very violent process, and the temperature of the coagulating bath is limited so as not to be too violent, thereby ensuring the fiber forming and being beneficial to the CS produced in the reaction process₂Can be recycled as much as possible. The decomposition reaction of cellulose sulfonate is accelerated due to the increase of the temperature, the forming is not sufficient due to the excessively fast reaction, and simultaneously, the added noni extract cannot be effectively retained on the fiber, so that the loss of a large amount of noni extract is caused, and the quality of a filament finished product cannot be ensured;

and (3) curing: after passing through a godet, bundling and stretching the nascent filaments in a curing bath; in a curing bath, the primary strand silk is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure shaping and the performance of the fiber are stable, and a fiber bundle is obtained;

E. post-treatment

Carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, tertiary water washing, oiling, dehydration, drying and tube forming on the obtained fiber bundle to obtain a noni filament primary product;

and radiating the obtained noni filament primary product for 1-10min by adopting ultraviolet rays with the wavelength of 280-400nm to obtain a noni filament finished product.

The noni extract and cellulose molecules can be better solidified, namely solidified and crosslinked, by adopting ultraviolet radiation; simultaneously; the bactericidal effect is also realized.

By adopting the technical scheme, the beneficial technical effects brought are as follows:

1) the invention takes noni extract and viscose as raw materials, and obtains noni filament yarn after blending, spinning, solidifying and post-processing, and the indexes of the noni filament yarn finished product are as follows:

The obtained noni filament has excellent functions of resisting oxidation, removing free radicals, whitening and the like;

2) in the invention, the prepared noni liquid can be directly used as raw materials of clothes, masks, sanitary materials and the like, when the noni liquid is blended with viscose, noni filament yarns are finally obtained, the functionalization of viscose is realized, and a new filament material is further developed;

3) in the invention, in order to match with the preparation process of the filament and ensure the product quality, a specific raw material noni liquid (specifically: noni fruit content in noni fruit extract is more than or equal to 95 percent, solvent types and concentration thereof, control conditions and the like), selecting specific raw material viscose (the viscose takes serum with alpha-cellulose content more than or equal to 90 percent, hemicellulose less than or equal to 15g/L and average polymerization degree of 700-1000 as raw materials), further limiting the proportional relationship of the two, crosslinking and curing substances in the noni fruit extract in alpha fibers in the viscose, realizing the functionalization of filaments, and further ensuring the stability, controllability, continuity and standardization of the functionalized fiber/filament preparation process.

Detailed Description

In the following, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

This embodiment provides a morinda citrifolia filament, which is prepared from morinda citrifolia extract and viscose as raw materials through blending, spinning, solidifying, curing and post-treatment; wherein, the weight ratio of the noni extract is 1-30%, and the ratio of the alpha fibers in the viscose is 70-99%;

the indexes of the prepared noni filament finished product are as follows:

The noni extract contains noni not less than 95%, and the viscose liquid takes serous cypress liquid with alpha-cellulose content not less than 90%, hemicellulose not more than 15g/L and average polymerization degree of 700-1000 as raw material.

Example 2

This example provides a method for preparing a morinda citrifolia filament yarn, including the following steps:

A. preparation of noni juice

the mass fraction of the noni extract dissolved in the ethanol water solution is 10-50%, and the mass fraction of the added amount of hydroxypropyl methyl cellulose is 1-5%;

wherein the cross-linking agent is 1,4 butanediol diglycidyl ether and/or ethylene glycol diglycidyl ether; the mass fraction of the added amount of the cross-linking agent is 1-10%;

B. blending of

C. spinning

Spinning by adopting a continuous method;

D. solidification and solidification

wherein the coagulating bath comprises 260-340g/L sodium sulfate, 125-135g/L sulfuric acid, 10-25g/L zinc sulfate and 8-25g/L auxiliary agent, the circulating amount of the acid bath is 35-45L/ingot minute, the immersion length is 2.4-3.5m, the specific gravity of the coagulating bath and the viscose trickle is 1.25-1.32, the temperature of the coagulating bath is 40-60 ℃, and the forming of the viscose trickle can be better ensured. Viscose spinning is a very violent process, and the temperature of the coagulating bath is limited so as not to be too violent, thereby ensuring the fiber forming and being beneficial to the CS produced in the reaction process₂Can be recycled as much as possible. The decomposition reaction of cellulose sulfonate is accelerated due to the temperature rise, the too fast reaction leads to insufficient forming, and the added noni fruit extract cannot be effectively retainedOn the fiber, the noni extract is greatly lost, and the quality and quality of the filament finished product cannot be ensured;

E. post-treatment

and (3) radiating the obtained noni filament primary product for 1-10min by adopting ultraviolet rays with the wavelength of 280-400nm to realize solidification between the noni extract and the fiber, so as to obtain a noni filament finished product.

Example 3

This example illustrates the production of 3kg of finished Morinda citrifolia filament yarn for further illustration of the present invention.

The method specifically comprises the following steps:

A. preparation of noni juice

1) Dissolving Morinda citrifolia extract in 30% ethanol water solution at 70 deg.C; adding hydroxypropyl methyl cellulose, fully stirring, and cooling to 30 ℃ to obtain a solution I;

the mass fraction of the noni extract dissolved in the ethanol water solution is 30 percent, and the mass fraction of the addition amount of the hydroxypropyl methyl cellulose is 4 percent;

2) adding caustic soda into the solution I obtained in the step 1), and adjusting the pH value to 8.5; slowly adding the cross-linking agent within 3 hours under the condition of continuously keeping the temperature at 30 ℃, and continuously stirring for 6 hours, so that the solution I and the cross-linking agent are uniformly mixed, and the self-crosslinking phenomenon is reduced to obtain a solution II;

wherein the cross-linking agent is one or two of 1,4 butanediol diglycidyl ether/ethylene glycol diglycidyl ether; the mass fraction of the added amount of the cross-linking agent is 6 percent;

B. blending of

Defoaming the obtained noni liquid and viscose respectively, then carrying out static mixing, and then defoaming to obtain a blended liquid; in static mixing, the mass ratio of the noni liquid is 15%, and the mass ratio of the nail fiber in the viscose liquid is 85%; wherein the viscose takes serum containing more than or equal to 90 percent of alpha-cellulose, less than or equal to 15g/L of hemicellulose and an average polymerization degree of 700-1000 as a raw material;

C. spinning

Spinning by adopting a continuous method;

the spinning process comprises pre-spinning filtration, a metering pump, a spinning nozzle, a spinning glass tube, a drafting disc, a processing roller, a drying roller, an oiling roller and ring spindle winding. The blended liquid is fed into a spinning machine through a glue supply pipeline, is quantitatively fed by a metering pump, is filtered by a candle filter to remove particle impurities, and is fed into a spinning nozzle assembly through a bent pipe, and the blended liquid passes through spinning holes under pressure to form viscose trickle;

D. solidification and solidification

And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a strand silk;

wherein the coagulating bath comprises 260g/L sodium sulfate, 100g/L sulfuric acid, 15g/L zinc sulfate and 12g/L auxiliary agent, the circulating amount of the acid bath is 35 liters/ingot minute, the immersion length is 3.5m, the specific gravity of the coagulating bath and the viscose trickle is 1.28, the temperature of the coagulating bath is 55 ℃, and the forming of the viscose trickle can be better ensured. Viscose spinning is a very violent process, and the temperature of the coagulating bath is limited so as not to be too violent, thereby ensuring the fiber forming and being beneficial to the CS produced in the reaction process₂Can be recycled as much as possible. The decomposition reaction of cellulose sulfonate is accelerated due to the increase of the temperature, the forming is not sufficient due to the excessively fast reaction, and simultaneously, the added noni extract cannot be effectively retained on the fiber, so that the loss of a large amount of noni extract is caused, and the quality of a filament finished product cannot be ensured;

and (3) curing: after passing through a godet, bundling and stretching the nascent filaments in a curing bath; in a curing bath, the primary strand silk is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure shaping and the performance of the fiber are stable, and the tows are obtained;

E. post-treatment

the obtained Morinda citrifolia filament yarn primary product is subjected to ultraviolet (wavelength of 280 nm) radiation for 3min to realize solidification between Morinda citrifolia extract and fiber, and 3kg of Morinda citrifolia filament yarn finished product is obtained.

Wherein, the indexes of the finished noni filament are as follows: dry breaking strength 2.15 cN/dtex, wet breaking strength 1.11cN/dtex, dry elongation at break 18.7%.

Example 4

This example differs from example 3 in that:

the mass fraction of the noni juice is 20%, and the rest steps are the same as those in example 3.

Example 5

This example differs from example 3 in that:

the mass fraction of the hydroxypropyl methylcellulose added was 2%, and the remaining method steps were the same as in example 3.

Example 6

This example differs from example 3 in that:

in the static mixing, the mass ratio of the noni juice was 8%, and the remaining process steps were the same as in example 3.

Example 7

This example differs from example 3 in that:

the mass ratio of the crosslinking agent was 2%, and the remaining steps were the same as in example 3.

Combining the noni filament products obtained in examples 3-7 above, the results shown in Table 1 below were obtained.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.

Claims

1. A noni filament yarn is characterized in that noni extract and viscose are used as raw materials and are prepared by blending, spinning, solidifying and post-processing; wherein, the weight ratio of the noni extract is 1-30%, and the ratio of the alpha fibers in the viscose is 70-99%;

the indexes of the prepared noni filament finished product are as follows:

2. The noni filament as claimed in claim 1, wherein the noni extract contains noni at a content of 95% or more, and the viscose is prepared from a pulp-cypress liquid containing alpha-cellulose at a content of 90% or more, hemicellulose at 15g/L or less, and an average degree of polymerization of 700-1000.

3. A process for preparing a Morinda citrifolia filament according to any one of claims 1-2, comprising the steps of:

A. preparation of noni juice

2) adding caustic soda into the solution I obtained in the step 1), and adjusting the pH value to 8.5-9; slowly adding a cross-linking agent within 3 hours under the condition of continuously keeping the temperature at 30-40 ℃, and continuously stirring for 5-24 hours to obtain a solution II;

3) standing the obtained solution II for more than 24h, and removing impurities to obtain noni fruit liquid;

B. blending of

C. spinning

Spinning by adopting a continuous method;

D. solidification and solidification

wherein the coagulating bath comprises 260-340g/L sodium sulfate, 125-135g/L sulfuric acid, 10-25g/L zinc sulfate and 8-25g/L auxiliary agent, the circulating amount of the acid bath is 35-45L/ingot minute, the immersion length is 2.4-3.5m, the specific gravity of the coagulating bath and the viscose trickle is 1.25-1.32, and the temperature of the coagulating bath is 40-60 ℃;

E. post-treatment

4. A process for producing a Morinda citrifolia filament according to claim 3, wherein in step 1), the Morinda citrifolia extract is added in an amount of 8 to 30% by mass and the hydroxypropyl methylcellulose is added in an amount of 1 to 5% by mass.

5. A process for producing noni filaments according to claim 3, wherein in step 2), the crosslinking agent is 1, 4-butanediol diglycidyl ether and/or ethylene glycol diglycidyl ether.

6. A process for producing a noni filament according to claim 3, wherein in the step 2), the amount of the crosslinking agent added is 1 to 10% by mass.

7. The method of claim 3, wherein in step B, the viscose is prepared from a pulp containing at least 90% of alpha-cellulose, at least 15g/L of hemicellulose and an average degree of polymerization of 700-1000.