CN1234923C - High-performance cellulose viscose and process for making same - Google Patents

High-performance cellulose viscose and process for making same Download PDF

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Publication number
CN1234923C
CN1234923C CN 200310110937 CN200310110937A CN1234923C CN 1234923 C CN1234923 C CN 1234923C CN 200310110937 CN200310110937 CN 200310110937 CN 200310110937 A CN200310110937 A CN 200310110937A CN 1234923 C CN1234923 C CN 1234923C
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temperature
grams per
yellow
dissolving
alkali
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CN1544726A (en
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冯涛
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Yibin Grace Co Ltd
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Yibin Grace Co Ltd
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Abstract

The present invention discloses a high performance viscose fiber which is produced by using bamboo pulp as one of raw materials, which is prepared from raw materials by the following weight percentages: 1% to 99% of bamboo pulp and 1% to 99% of cotton pulp, or 1% to 99% of bamboo pulp and 1% to 99% of wood pulp, or 1% to 99% of bamboo pulp, 1% to 99% of cotton pulp and 1% to 99% of wood pulp. The preparation method of the fiber comprises the following technologic procedures: pulp mixing, dipping, squeeze, pulverization, etiolation, solubilization, spinning, refining, drying and packing. The working procedure of etiolation comprises a wet temperature raising etiolation method and a dry constant temperature etiolation method. The raw materials of the present invention are easy to obtain and the cost is low. The prepared viscose fiber not only has favorable moisture absorption performance, chromaticity and antistatic performance, but also has natural antimicrobial and bacteriostatic performance.

Description

A kind of preparation method of viscose of bamboo-containing fiber
Technical field:
The present invention relates to a kind of preparation method of viscose, particularly relating to a kind of is the preparation method of the viscose of the bamboo-containing fiber produced of one of raw material with the bamboo pulp.
Background technology:
Viscose is as a kind of textile raw material, because of it has moisture absorption preferably, ventilative, dyeing, performance such as antistatic, extensive market prospects is arranged, it is raw material that traditional mode of production all adopts native celluloses such as cotton linter, timber, make through a series of chemical treatments, but along with the shortage of the development of China's viscose and cotton linter, timber, the price of cotton linter, timber goes up gradually, causes the production cost of viscose to raise thus; Meanwhile, though at present newly developed to have gone out a kind of be the viscose of raw material production with the natural bamboo, but with the pulp that pure bamboo fibre is made, its first fibre weight is lower, half fine content height, the reactivity worth of bamboo cellulose differs greatly, make that the degree of ripeness fluctuation of viscose glue is bigger after the yellow operation, and xanthate acid group skewness, the viscose glue muddiness, structural viscosity is big, has had a strong impact on the finished fiber quality.
Summary of the invention:
The purpose of this invention is to provide a kind of is the preparation method of the high-performance viscose fiber of raw material production with bamboo pulp, the cotton pulp dregs of rice or wood pulps, viscose obtained by this method, not only have good hygroscopicity, dyeability and antistatic behaviour, also possess natural antibiotic and bacteriostasis property simultaneously.
Technical scheme of the present invention is as follows:
A kind of high-performance viscose fiber, it is formulated by following weight percentages: bamboo pulp 1-99%, cotton pulp dregs of rice 1-99%, perhaps bamboo pulp 1-99%, wood pulps 1-99%, perhaps bamboo pulp 90%, the cotton pulp dregs of rice 5%, wood pulps 5%.
Preparation method of the present invention comprises following processing step: mix the dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, oven dry and packing, it is characterized in that: described yellow operation comprises wet method intensification yellow method and dry method constant temperature yellow method, and its concrete grammar is as follows:
A, wet method intensification yellow method are meant: in concentration is the carbon disulfide that adds relative alkali fiber weight 26-35% in the pre-alkalizing solution of NaOH of 100-130 grams per liter, and the yellow initial temperature is 12-20 ℃, and temperature is 26-34 ℃ eventually, and the yellow time is 60-110 minute.
B, dry method constant temperature yellow method are meant: add the carbon disulfide of relative alkali fiber weight 26-35% in the alkali fiber after concentration is the pre-alkalization of NaOH of 100-130 grams per liter, the yellow temperature constant is at 30-32 ℃, and the yellow time is 30-100 minute.
The mixed dregs of rice of the present invention, dipping, squeezing, pulverizing process are meant: with bamboo pulp and the cotton pulp dregs of rice or bamboo pulp and wood pulps or bamboo pulp and the cotton pulp dregs of rice, wood pulps mixed according to the above ratio after, under 40-55 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is the 220-250 grams per liter, again after squeezing squeezing just, pulverizing, reaching the fine content of the fine first of alkali is 26-32%, alkali content is 15-18%, and density is 150-200 kilogram/rice 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of dissolution process of the present invention divided, and the dissolving alkali liquid temperature is lower than 10 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 8-25 ℃, dissolution time is 50-150 minute.
Spinning process of the present invention is meant: will carry out spinning with spinning machine through the viscose glue of dissolving, deaeration, filtration, make spinning cake or staple fibre, wherein the temperature of acid bath is 44-56 ℃, and containing sulfuric acid 70-140 grams per liter, sodium sulphate 190-330 grams per liter, zinc sulfate 6-15 grams per liter, total stretch ratio in the acid bath is 1.8-2.3.
Refining procedure of the present invention is meant: in concise equipment spinning cake or staple fibre are carried out desulfurization, chlorohydric acid pickling and oil, wherein: desulfurization temperature is 30-80 ℃, and alkali concn is the 2-8 grams per liter, and pickling temperature is 20-50 ℃, concentration 1-5 grams per liter, last oil concentration are the 2-8 grams per liter.
Oven dry of the present invention, packing process are meant: with dryer with spinning cake or staple fibre dry to temperature be 70-130 ℃, containing and wetly be lower than at 10% o'clock and promptly carry out long filament winder packing or staple fibre weighing packing.
Raw material of the present invention is easy to get, and cost is low, and the viscose that makes not only has good hygroscopicity, dyeability and antistatic behaviour, also possesses natural antibiotic and bacteriostasis property simultaneously.
The specific embodiment:
Embodiment 1
A kind of high performance sticking short glue fiber, it is formulated by following weight percentages: bamboo pulp 99%, the cotton pulp dregs of rice 1%.
Described preparation method comprises the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, the step of drying and pack, wherein said yellow operation adopts wet method intensification yellow method, be the carbon disulfide that adds relative alkali fiber weight 26% in the pre-alkalizing solution of NaOH of 110 grams per liters promptly in concentration, the yellow initial temperature is 15 ℃, whole temperature is 30 ℃, and the yellow time is 90 minutes.
The described mixed dregs of rice, dipping, squeezing, pulverizing process be with bamboo pulp and the cotton pulp dregs of rice mixed according to the above ratio after, under 50 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is 220 grams per liters, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 26%, alkali content is 15%, and density is 150 kilograms/meter 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolution process divided, and the dissolving alkali liquid temperature is 8 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 20 ℃, dissolution time is 100 minutes.
Described spinning process is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, makes staple fibre, and the temperature of wherein carrying out acid bath is 45 ℃, contain sulfuric acid 70 grams per liters in the acid bath, sodium sulphate 330 grams per liters, zinc sulfate 6 grams per liters, total stretch ratio are 2.0.
Described refining procedure is in concise equipment fiber to be carried out desulfurization, chlorohydric acid pickling and oil, and wherein: desulfurization temperature is 50 ℃, and alkali concn is 5g/L, and pickling temperature is 30 ℃, and concentration is 5 grams per liters, and last oil concentration is 5 grams per liters.
Described oven dry, packing process be with dryer with fiber dry to temperature be 90 ℃, containing and wet be lower than at 10% o'clock and promptly carry out the weighing packing.
Embodiment 2
A kind of high performance viscose staple fibre, it is formulated by following weight percentages: bamboo pulp 1%, wood pulps 99%.
Described preparation method comprises the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, the step of drying and pack, wherein said yellow operation adopts dry method constant temperature yellow method, its concrete grammar is: the carbon disulfide that adds relative alkali fiber weight 35% in the alkali fiber after concentration is the pre-alkalization of NaOH of 130 grams per liters, the yellow temperature constant is at 32 ℃, and the yellow time is 100 minutes.
The described mixed dregs of rice, dipping, squeezing, pulverizing process be with bamboo pulp and wood pulps mixed according to the above ratio after, under 55 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is 250 grams per liters, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 32%, alkali content is 18%, and density is 200 kilograms/meter 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolution process divided, and the dissolving alkali liquid temperature is 5 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 25 ℃, dissolution time is 50 minutes.
Described spinning process is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, makes staple fibre, and the temperature of wherein carrying out acid bath is 50 ℃, contain sulfuric acid 140 grams per liters in the acid bath, sodium sulphate 190 grams per liters, zinc sulfate 15 grams per liters, total stretch ratio are 1.8.
Described refining procedure is in concise equipment fiber to be carried out desulfurization, chlorohydric acid pickling and oil, and wherein: desulfurization temperature is 80 ℃, and alkali concn is 8 grams per liters, and pickling temperature is 50 ℃, and concentration 1 grams per liter, last oil concentration are 2 grams per liters.
Described oven dry, packing process be with dryer with fiber dry to temperature be 95 ℃, containing and wet be lower than at 10% o'clock and carry out the weighing packing.
Embodiment 3
A kind of high performance viscose staple fibre, it is formulated by following weight percentages: bamboo pulp 90%, the cotton pulp dregs of rice 5%, wood pulps 5%.
Described preparation method comprises the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, the step of drying and pack, wherein said yellow operation adopts wet method intensification yellow method, its concrete grammar is: in concentration is the carbon disulfide that adds relative alkali fiber weight 30% in the pre-alkalizing solution of NaOH of 120 grams per liters, the yellow initial temperature is 20 ℃, whole temperature is 34 ℃, and the yellow time is 100 minutes.
The described mixed dregs of rice, dipping, squeezing, pulverizing process are after bamboo pulp, the cotton pulp dregs of rice and wood pulps are mixed according to the above ratio, under 40 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is 240 grams per liters, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 32%, alkali content is 17%, and density is 180 kilograms/meter 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolution process divided, and the dissolving alkali liquid temperature is 3 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 10 ℃, dissolution time is 80 minutes.
Described spinning process is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, makes staple fibre, and the temperature of wherein carrying out acid bath is 50 ℃, contain sulfuric acid 140 grams per liters in the acid bath, sodium sulphate 190 grams per liters, zinc sulfate 15 grams per liters, total stretch ratio are 1.8.
Described refining procedure is in concise equipment fiber to be carried out desulfurization, chlorohydric acid pickling and oil, and wherein: desulfurization temperature is 80 ℃, and alkali concn is 8 grams per liters, and pickling temperature is 50 ℃, and concentration 1 grams per liter, last oil concentration are 2 grams per liters.
Described oven dry, packing process be with dryer with fiber dry to temperature be 95 ℃, containing and wet be not more than at 10% o'clock and carry out the weighing packing.
Embodiment 4
A kind of high performance viscose filament yarn, it is formulated by following weight percentages: bamboo pulp 99%, the cotton pulp dregs of rice 1%.
Described preparation method comprises the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, oven dry, becomes tube, classification packing step, wherein said yellow operation adopts wet method intensification yellow method, its concrete grammar is: concentration be add in the pre-alkalizing solution of NaOH of 120 grams per liters relative alkali fiber weigh 26% carbon disulfide, the yellow initial temperature is 15 ℃, whole temperature is 30 ℃, and the yellow time is 90 minutes.
The described mixed dregs of rice, dipping, squeezing, pulverizing process be with bamboo pulp and the cotton pulp dregs of rice mixed according to the above ratio after, under 50 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is 220 grams per liters, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 26%, alkali content is 15%, and density is 150 kilograms/meter 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolution process divided, and the dissolving alkali liquid temperature is 8 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 20 ℃, dissolution time is 100 minute hands.
Described spinning process is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, make spinning cake, the temperature of wherein carrying out acid bath is 45 ℃, contains sulfuric acid 70 grams per liters, sodium sulphate 330 grams per liters, zinc sulfate 6 grams per liters in the acid bath, and total stretch ratio is 2.0.
Described refining procedure is in concise equipment spinning cake to be carried out desulfurization, pickling alkali cleaning, bleach and oils, and wherein: desulfurization temperature is 50 ℃, and alkali concn is 5 grams per liters, and pickling temperature is 30 ℃, and concentration 5 grams per liters, last oil concentration are 5 grams per liters.
Described oven dry, become tube, classification packing be with dryer with spinning cake dry to temperature be 90 ℃, contain and be carried out to tube, classification packing after temperature is lower than 10%.
Embodiment 5
A kind of high performance viscose filament yarn, it is formulated by following weight percentages: bamboo pulp 1%, wood pulps 99%.
Described preparation method comprises the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, the step of drying and pack, wherein said yellow operation adopts dry method constant temperature yellow method, its concrete grammar is: the carbon disulfide that adds relative alkali fiber weight 35% in the alkali fiber after concentration is the pre-alkalization of NaOH of 100 grams per liters, the yellow temperature constant is at 32 ℃, and the yellow time is 100 minutes.
The described mixed dregs of rice, dipping, squeezing, pulverizing process be with bamboo pulp and the cotton pulp dregs of rice or bamboo pulp and wood pulps or bamboo pulp and the cotton pulp dregs of rice, wood pulps mixed according to the above ratio after, under 55 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is 250 grams per liters, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 32%, alkali content is 18%, and density is 200 kilograms/meter 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolution process divided, and the dissolving alkali liquid temperature is 5 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 25 ℃, dissolution time is 50 minutes.
Described spinning process is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, make spinning cake, the temperature of wherein carrying out acid bath is 50 ℃, contains sulfuric acid 140 grams per liters, sodium sulphate 190 grams per liters, zinc sulfate 15 grams per liters in the acid bath, and total draft is than 1.8.
Described refining procedure is in concise equipment spinning cake to be carried out desulfurization, pickling alkali cleaning, bleach and oils, and wherein: desulfurization temperature is 50 ℃, and alkali concn is 8 grams per liters, and pickling temperature is 50 ℃, and concentration is 5 grams per liters, and last oil concentration is 2 grams per liters.
Described oven dry, become tube, classification packing be with dryer with spinning cake dry to temperature be 95 ℃, containing and wetly be carried out to tube, classification packing after being not more than 10%.
Embodiment 6
A kind of high performance viscose filament yarn, it is formulated by following weight percentages: bamboo pulp 90%, the cotton pulp dregs of rice 5%, wood pulps 5%.
Described preparation method comprises the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, the step of drying and pack, wherein said yellow operation adopts wet method intensification yellow method, its concrete grammar is: in concentration is the carbon disulfide that adds relative alkali fiber weight 30% in the pre-alkalizing solution of NaOH of 120 grams per liters, the yellow initial temperature is 20 ℃, whole temperature is 34 ℃, and the yellow time is 100 minutes.
The described mixed dregs of rice, dipping, squeezing, pulverizing process be with bamboo pulp and the cotton pulp dregs of rice or bamboo pulp and wood pulps or bamboo pulp and the cotton pulp dregs of rice, wood pulps mixed according to the above ratio after, under 40 ℃ temperature conditions, be immersed in the sodium hydroxide lye that concentration is 240 grams per liters, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 32%, alkali content is 17%, and density is 180 kilograms/meter 3
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolution process divided, and the dissolving alkali liquid temperature is 3 ℃, after be dissolved in the dissolving machine and carry out, back concentration of ordinary dissolution is 10 ℃, dissolution time is 80 minutes.
Described spinning process is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, makes spinning cake.The temperature of wherein carrying out acid bath is 52 ℃, contains sulfuric acid 130 grams per liters, sodium sulphate 230 grams per liters, zinc sulfate 12 grams per liters in the acid bath, and total stretch ratio is 1.8.
Described refining procedure is in concise equipment spinning cake to be carried out desulfurization, pickling alkali cleaning, bleach and oils, and wherein: desulfurization temperature is 80 ℃, and alkali concn is 8 grams per liters, and pickling temperature is 50 ℃, and concentration is 1 grams per liter, and last oil concentration is 3 grams per liters.
Described oven dry, become tube, classification packing be with dryer with spinning cake dry to temperature be 95 ℃, containing and wetly be carried out to tube, classification packing after being not more than 10%.
With the high performance viscose of method preparation of the present invention, its dried fracture strength 〉=1.00cN/dtex, wet breaking strength 〉=0.5cN/dtex, dried elongation at break 10-25%, residual sulfur content 20 milligrams/100 grams.

Claims (2)

1, a kind of preparation method of viscose of bamboo-containing fiber is characterized in that comprising the mixed dregs of rice, dipping, squeezing, pulverizing, yellow, dissolving, spinning, concise, the step of drying and pack, wherein:
The described mixed dregs of rice, dipping, squeezing and pulverising step are that 90% bamboo pulp, 5% the cotton pulp dregs of rice and 5% the mixed evenly back of wood pulps are immersed under 40-55 ℃ temperature conditions in the sodium hydroxide lye that concentration is the 220-250 grams per liter, again after the squeezer squeezing, pulverizing, reaching the fine content of the fine first of alkali is 26-32%, alkali content is 15-18%, and density is 150-200 kilogram/rice 3
Described yellow step adopts wet method intensification yellow method, in concentration is the carbon disulfide that adds relative alkali fiber weight 26-35% in the pre-alkalizing solution of NaOH of 100-130 grams per liter, the yellow initial temperature is 12-20 ℃, and temperature is 26-34 ℃ eventually, and the yellow time is 60-110 minute;
Dissolving and back two stages of dissolving just were dissolved in the xanthating machine and carry out at the beginning of described dissolving step divided, and the dissolving alkali liquid temperature is lower than 10 ℃, after be dissolved in the dissolving machine and carry out, back solution temperature is 8-25 ℃, dissolution time is 50-150 minute;
Described spinning step is that the viscose glue through dissolving, deaeration, filtration is carried out spinning with spinning machine, make spinning cake or staple fibre, wherein the temperature of acid bath is 44-56 ℃, contain sulfuric acid 70-140 grams per liter in the acid bath, sodium sulphate 190-330 grams per liter, zinc sulfate 6-15 grams per liter, total draft are 1.8-2.3;
Described refinement step is in refining equipment spinning cake or staple fibre to be carried out desulfurization, and with chlorohydric acid pickling and oiling, wherein: desulfurization temperature is 30-80 ℃, alkali concn is the 2-8 grams per liter, pickling temperature is 20-50 ℃, and concentration 1-5 grams per liter, last oil concentration are the 2-8 grams per liter;
Described oven dry and packing step process be with dryer with spinning cake or staple fibre dry to temperature be 70-130 ℃, containing and wetly be lower than at 10% o'clock and promptly carry out long filament winder packing or staple fibre weighing packing.
2, the preparation method of the viscose of bamboo-containing fiber according to claim 1, it is characterized in that described yellow step also can adopt dry method constant temperature yellow method, the carbon disulfide that adds relative alkali fiber weight 26-35% in the alkali fiber after concentration is the pre-alkalization of NaOH of 100-130 grams per liter, the yellow temperature constant is at 30-32 ℃, and the yellow time is 30-100 minute.
CN 200310110937 2003-11-17 2003-11-17 High-performance cellulose viscose and process for making same Expired - Fee Related CN1234923C (en)

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