CN102425014B - Method for preparing loofah sponge viscose fibers - Google Patents

Abstract

The invention provides a method for preparing loofah sponge viscose fibers. The method comprises the following processes of: residue removal, crushing, degumming, digestion, bleaching, acid treatment, pulping, squeezing, crushing, ageing, sulfonating, grinding, dissolving, filtering, defoaming, filtering, spinning, drafting, cutting, post treatment, drying and packing, wherein a biological-chemical combined degumming method is adopted in the degumming process. Compared with the conventional degumming process, the method has the advantage that: the performance indexes such as residual gum rate, dry breaking strength, dry breaking elongation, moisture regain, whiteness and the like of the loofah sponge viscose fibers prepared by adopting the degumming method are further improved.

Description

A kind of preparation method of loofah sponge viscose fibers

Technical field

The present invention relates to man-made cellulose fibers technical field, relate in particular to a kind of preparation method of loofah sponge viscose fibers.

Background technology

In textile industry, the development of textile raw material is the basis of whole Chinese Textile Industry.Various fibrous raw materials have different character and feature.For by the textile fabric of various different classes of, different performances, make all-purpose high-quality finished product; For the raw material with limited, be processed into how better textiles; In order to open up the new raw material sources that textile industry is used that are suitable for, increase production various textiless to meet the people and national each side needs, must carry out to textile fiber material the research work of each side.Therefore, the research of textile material is the research of a permanence.

Along with the raising day by day of people's living standard and the impact of world energy sources crisis; people recognize the advantage of natural environmental-protective shaped material gradually; especially increasing to the demand of clothing natural environmental-protective shaped material, and the viscose that wherein fabric can natural degradation after discarded just accounts for sizable ratio.At present people to be used for producing the main raw material of viscose pulp be leaf wood, needlebush or cotton linter.But along with developing rapidly of viscose fibre industry and paper industry in recent years, the demand of leaf wood, needlebush or cotton linter is increased greatly, cause the raw material for producing viscose pulp unprecedentedly nervous, imbalance between supply and demand is outstanding.Therefore, in order to develop viscose fibre industry, must the new raw material field of developing.

Sponge gourd is that Curcurbitaceae is climbed up by holding on to herbaceous plant, all has both at home and abroad and distributes and cultivation.When sponge gourd is ripe, the reticular fibre of the inside claims luffa, can replace sponge to be used as and scrub kitchen range and furniture; Also can hyoscine, the effect of have refrigerant, diuresis, invigorating blood circulation, stimulate the menstrual flow, detoxifying.Luffa has another name called sponge gourd net, melon network, Si Gua Pro, cries plant sponge abroad, is the vascular bundle of cucurbitaceous plant sponge gourd dry mature fruit, be oval tubular or spindle shape, surperficial white or yellow-white, be interwoven by the thread vascular bundle of multilayer, body footpath, matter is tough and tensile, not frangibility.All the time, luffa mainly and the clean a pot value that washes the dishes medicinal take it be familiar with and utilize as people.

In recent years, along with scientific and technological development and the raising of people's living standard, luffa, through scientific development, develops into dairy industry field from field of medicaments.Handicraft take luffa as raw material, the favor that commodity are subject to people just day by day, as Luffa slipper, luffa pillowcase and pillow etc.Luffa industry has realized the standardization of plantation, processing, product quality and sale, scientific, standardization and modernization gradually, the opened international market of luffa product, more than 50 countries and regions such as situation of selling well Southeast Asia, America and Europe, wherein luffa goods in Cixi City of Zhejiang Province just account for 80% of world market share.

From literature search situation, people mainly concentrate on sewage treatment area for the research of luffa at present.As Liu Yinfeng, the people such as Mao Jinhao disclose a kind of preparation method of etherized luffa and the application in adsorption of metal ions thereof in patent CN101239306.The method is that natural loofah is mixed with appropriate NaOH ethanolic solution, alkalization at 25～80 ℃, or alkalize with microwave intermittent radiation; Then in water bath with thermostatic control, reflux, washing, suction filtration, oven dry; Use NaOH Solution Dispersion, react with the alcoholic solution of chloroacetic acid, suction filtration, washing, oven dry, obtain etherized luffa.Etherized luffa wide material sources, biodegradable, and treatment process is relatively simple, can partly substitute synthesized polymer material, and have advantages of environment protection aspect sewage disposal.

They disclose a kind of luffa alkalization modifying method and the application in adsorption of metal ions thereof simultaneously in patent CN101239303.The method is that natural loofah is mixed with appropriate NaOH ethanolic solution, alkalization at 25～80 ℃, or with microwave intermittent radiation 1～10min alkalization, then in water bath with thermostatic control, reflux, washing, suction filtration, oven dry, obtain alkali treatment luffa.Luffa wide material sources, biodegradable, and treatment process is relatively simple, can partly substitute synthesized polymer material, and have advantages of environment protection aspect sewage disposal.

Li Huizhi, Xu Chongjuan discloses a kind of hydrosulphonyl functionalized loofah preparation method and application technology in patent CN101670273.In the triangular flask of tool plug, add by mass percentage TGA, oxolane, the luffa of alkalization, the concentrated sulfuric acid, jump a queue, in 40 ℃ of constant temperature, place 48h, then with deionized water, wash, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 35 ℃ of baking ovens dry, the hydrosulphonyl functionalized loofah obtaining is large to the adsorbance of metal ion, there is sulfydryl characteristic, the directly absorption to each metal ion species in water body and wash-out, adsorption efficiency is high, the speed of absorption is fast, selective strong, desorption performance is good, there are good physical and chemical stability and excellent mechanical stability, can within the scope of wider soda acid, use, hydrosulphonyl functionalized loofah has power of regeneration simultaneously.

Liu Yinfeng, the people such as Yang Hong disclose a kind of preparation method of esterified vegetable sponge and at organic matter in patent CN101664671, the especially application in Adsorption of Organic in aqueous systems.The method be by natural loofah with after appropriate NaOH/ alcohol solution dipping, microwave intermittent radiation alkalization then refluxes in water bath with thermostatic control, washing, dries; With acetic anhydride immersion, then under microwave condition, carry out intermittent reaction, washing, oven dry, obtain esterified vegetable sponge.The treatment process of esterified vegetable sponge is relatively simple, the performance of absorption organic pollution increases compared with natural loofah, aspect sewage disposal, can partly substitute synthesized polymer material, and there is the features such as environmental friendliness, wide material sources, cheap, biodegradable and environmental friendliness.

Yin Jingbo, Yu Zhen sun waits people to disclose a kind of polylactic acid/vegetable sponge fiber composite and preparation method thereof in patent CN101177523.This novel totally biodegradable composite can obviously improve the heat resistance of PLA, has good mechanical performance, and has reduced the cost of raw material, is conducive to PLA and applies widely.This composite, using PLA as main body raw material, adds through organically-modified luffa staple fibre and a small amount of lubricant, heat stabilizer.The totally biodegradable composite of being made by above-mentioned raw materials and auxiliary material thereof has better mechanical performance, good heat resistance, antibacterial, the features such as humidity and lower cost, can be applicable to pack the every field such as parcel, engineering construction, interior decoration, automotive trim, solve the environmental problem that white pollution brings.

Along with the attention of people to environmental problem and the ecological demand to textiles, natural fabric is extremely paid attention to its environmentally safe and the compatibility to human skin, and the green environmental protection of loofah fiber is subject to people's favor especially.For loofah sponge viscose fibers, what people generally adopted is conventional technology of preparing, comprise slagging-off, pulverize, come unstuck, boiling, bleaching, acid treatment, manufacture paper with pulp, squeeze, the technical process such as pulverizing, experienced, sulfonation, grinding, dissolving, filtration, deaeration, filtration, spinning, drawing-off, cut-out, post processing, dry, packing.Especially degumming tech, owing to adopting conventional chemical Degumming technology, causes the waste water generating in production process many, poor product quality etc.

Summary of the invention

The object of this invention is to provide a kind of preparation method of loofah sponge viscose fibers.

For achieving the above object, technical scheme provided by the invention is:

A kind of preparation method of loofah sponge viscose fibers, comprise slagging-off, pulverize, come unstuck, boiling, bleaching, acid treatment, manufacture paper with pulp, squeeze, pulverizing, experienced, sulfonation, grinding, dissolving, filtration, deaeration, filtration, spinning, drawing-off, cut-out, post processing, dry and packing, what described degumming tech adopted is biological-chemical combination degumming method:

(1) biological degumming: add biology enzyme in the luffa adopting after the pre-poach-pickling-washing of common process, carry out biological degumming, control biology enzyme 4-15g/l in the process of coming unstuck, pH value 3.5-5.5, temperature 40-60 ℃, time 3-10 hour, bath raio 1: 10-1: 30;

(2) chemical Degumming: step (1) gained luffa is washed-beaten after fibre, carry out soda boiling, soda boiling condition is NaOH 5-20g/l, Na ₂sO ₃1-10g/l, Na ₅p ₃o ₁₀1-5g/l, bath raio 1: 10-1: 30, time 2-5h.

Preferably, described biology enzyme is pectase or hemicellulase.

Compared with traditional degumming tech, adopt the performance indications such as residual gum content, dry fracture strength, dry elongation at break, regain and whiteness of loofah sponge viscose fibers prepared by Degumming method of the present invention to be all further improved.

The specific embodiment

Embodiment 1:

(1) slagging-off: the sulfuric acid solution of 35 ℃ soaks, and concentration is 6g/L, and the time is 24h;

(2) biological-chemical combination degumming: controlling pectase concentration in biological degumming process is 4g/l, pH value 3.5,40 ℃ of temperature, 3 hours time, bath raio 1: 10; In chemical Degumming process, soda boiling condition is NaOH 5g/l, Na ₂sO ₃10g/l, Na ₅p ₃o ₁₀5g/l, bath raio 1: 10, time 2h;

(3) boiling: alkali charge be in NaOH to oven dry stock amount 25%, liquor ratio is 1: 3, the heating-up time is 100min, holding temperature is 150 ℃, temperature retention time is 180min.

(4) bleaching: chlorine dosage to oven dry stock 3%, 40 ℃ of temperature, the time is 60min.

(5) acid treatment: by acid amount to oven dry stock 4%, temperature is normal temperature, the time is 60min.

(6) squeezing: the fine content 30% of first, sodium hydrate content 14%.

(7) experienced: temperature is 16 ℃.

(8) sulfonation: 30% of the relative first fibre of CS2 addition, the time is 90min, sulfonation final temperature is 30 ℃.

(9) spinning: acid bath liquid consists of: sulfuric acid 120g/L, sodium sulphate 270g/L, zinc sulfate 10g/L, temperature is 50 ℃.

(10) prepared end product quality: dry fracture strength 2.54CN/dtex, wet breaking strength 1.46CN/dtex, dry elongation at break 20.4%, line density deviation ratio+0.72%, length variation rate-2.5%, overcut fibre 0.4%, over-length fibre 3.5mg/100g, residual sulfur content 7.6mg/100g, fault 3.0mg/100g, the dry strong coefficient of variation 12.4%, whiteness 77.4%, regain 11.4%.

Embodiment 2:

(2) biological-chemical combination degumming: controlling hemicellulose enzyme concentration in biological degumming process is 15g/l, pH value 5.5, temperature 60 C, 10 hours time, bath raio 1: 30; In chemical Degumming process, soda boiling condition is NaOH 20g/l, Na ₂sO ₃1g/l, Na ₅p ₃o ₁₀1g/l, bath raio 1: 30, time 5h;

Other step is with embodiment 1.

Embodiment 3

(2) biological-chemical combination degumming: controlling hemicellulose enzyme concentration in biological degumming process is 8g/l, pH value 4.0, temperature 45 C, 5 hours time, bath raio 1: 15; In chemical Degumming process, soda boiling condition is NaOH 15g/l, Na ₂sO ₃8g/l, Na ₅p ₃o ₁₀2g/l, bath raio 1: 15, time 2h;

Other step is with embodiment 1.

Embodiment 4

(2) biological-chemical combination degumming: controlling pectase concentration in biological degumming process is 12g/l, pH value 4.5,55 ℃ of temperature, 8 hours time, bath raio 1: 25; In chemical Degumming process, soda boiling condition is NaOH 10g/l, Na ₂sO ₃4g/l, Na ₅p ₃o ₁₀4g/l, bath raio 1: 25, time 4h;

Other step is with embodiment 1.

Comparative example 1

(2) chemical Degumming: adopt the sodium hydroxide solution immersion containing the cationic surfactant of 0.2 weight portion, temperature is 40 ℃, and naoh concentration is 6g/l, and the time is 24h.

Other step is with embodiment 1.

Comparative example 2

(2) chemical Degumming: adopt the sodium hydroxide solution immersion containing the anion surfactant of 0.4 weight portion, temperature is 45 ℃, and naoh concentration is 7g/L, and the time is 20h.

Other step is with embodiment 1.

Residual gum content, fineness, filament intensity, length, regain and the whiteness of embodiment 1-4 and comparative example 1-2 gained loofah sponge viscose fibers are tested, the results are shown in Table shown in 1.

The quality index of the loofah sponge viscose fibers that the different Degumming methods of table 1 obtain

Test event	Embodiment 1	Embodiment 2	Embodiment 3	Embodiment 4	Comparative example 1	Comparative example 2
							Residual gum content S (%)	2.91	2.97	3.01	2.89	3.32	3.41
Dry fracture strength (CN/dtex)	2.54	2.48	2.39	2.50	2.04	2.17
							Dry elongation at break (%)	20.4	21.1	20.7	21.3	18.9	19.1
Regain (%)	11.4	11.6	11.0	11.3	10.3	10.0
							Whiteness	77.4	77.6	78.2	78.9	76.1	75.8

From data shown in table 1, can find out, compared with traditional chemical degumming technique, the residual gum content of biological-chemical combination degumming method gained loofah sponge viscose fibers of the present invention, dry fracture strength, dry elongation at break, regain and whiteness are better than the former.

Claims (2)

1. the preparation method of a loofah sponge viscose fibers, comprise slagging-off, pulverize, come unstuck, boiling, bleaching, acid treatment, manufacture paper with pulp, squeeze, pulverizing, experienced, sulfonation, grinding, dissolving, filtration, deaeration, filtration, spinning, drawing-off, cut-out, post processing, dry and packing, it is characterized in that, what described degumming tech adopted is biological-chemical combination degumming method:

(1) biological degumming: add biology enzyme in the luffa adopting after the pre-poach-pickling-washing of common process, carry out biological degumming, control biology enzyme concentration 4-15g/l in the process of coming unstuck, pH value 3.5-5.5, temperature 40-60 ℃, time 3-10 hour, bath raio 1: 10-1: 30;

(2) chemical Degumming: step (1) gained luffa is washed-beaten after fibre, carry out soda boiling, soda boiling condition is NaOH 5-20g/l, Na ₂sO ₃1-10g/l, Na ₅p ₃o ₁₀1-5g/l, bath raio 1: 10-1: 30, time 2-5h.

2. the preparation method of loofah sponge viscose fibers as claimed in claim 1, is characterized in that, described biology enzyme is pectase or hemicellulase.