CN101089247A - Method for preparing viscose staple fibre using cotton stalk - Google Patents

Abstract

The present invention relates to a method for preparing viscose staple fiber by utilizing cotton stalk. It includes two steps of preparing cotton viscose pulp and preparing viscose staple fiber by utilizing said viscose pulp. The technological process for preparing cotton viscose pulp successively includes the following steps: preparing material, prehydrolysis, digestion, rinsing, pulping, refining, dechlorination and acid treatment. The quality of said pulp finished product is as follows: alpha-cellulose content is 94%; cuprammonium viscosity is 16.5CP; ash content is 0.12%; and iron content is 20 mg/kg.

Description

Utilize the cotton stalk to prepare the method for viscose staple fibre

Technical field

The present invention relates to utilize the cotton stalk to produce cellulose viscose pulp, and the technology of further spinning production viscose.

Background technology

Viscose is to be base stock with the native cellulose, the consumption demand of its adaptation population's back to nature, traditional viscose is to form with the needlebush manufacturing, since global such there is lack of raw materials and the constantly bringing forth new ideas of pulping technique, some leaf woods, cotton linter etc. also are applied in the production of cellulose viscose pulp, but be thereby that raw material can relate to trees and fells and influence environment, problems such as destruction natural, ecological with needlebush and leaf wood; Therefore the application of some new raw materials will have more wide prospect.China second produces cotton big country in the world; cotton stalk 225～250kg is produced in one mu of cotton field; the cotton stalk annual production of China can reach 1,530 ten thousand tons; normally as agricultural wastes or burning; therefore made full use of the added value that cotton stalk resource can not only solve China's fiber-like raw material wretched insufficiency and increase agricultural production, and be significant for the protection environment.By retrieval, do not find the method for the cotton stalk viscose staple fibre of preparation as yet.

Summary of the invention

Technical problem to be solved by this invention provides and a kind ofly utilizes enormous amount, cheap and easy to get agricultural wastes---cotton stalk is a raw material production viscose staple fibre pulp, and the technology of further spinning manufacturing viscose staple fibre, promptly utilize the cotton stalk to prepare the method for viscose staple fibre

The technical solution adopted for the present invention to solve the technical problems:

The present invention includes preparation cotton stalk viscose glue pulp and prepare viscose staple fibre two with this pulp and go on foot greatly, its concrete technology is as follows:

One, the technology of preparation cotton stalk viscose glue pulp:

(1) get the raw materials ready: raw material is the full stalk of cotton stalk, go root slightly, remove the casting skin on bast top layer after, cut into 20～40mm, pound with machinery and split, choose assorted, washing then, soak;

(2) prehydrolysis: the prehydrolysis process conditions are: the concentration of hydrochloric acid is 1-3%, temperature 90-100 ℃, and 2 hours time;

(3) boiling, batch turning, wash material: in boiling vessel, carry out;

Technical conditions: alkali charge: 20-24% uses anthraquinone amount: 0.1-0.3%;

Sulphidity: 18-22%;

Liquor ratio: 1: 5;

Behind the 30min, intensification 35min, 135 ℃ of temperature, steam bleeding 20min for the first time, 110 ℃ of temperature, pressure 0.05MPa;

The 35min that heats up for the second time, 135 ℃ of temperature, steam bleeding 20min for the second time, 35 ℃ of temperature, pressure 0.2MPa;

The 30min that heats up for the third time, temperature 165-168 ℃;

Temperature retention time is: 90min, holding temperature 165-168 ℃;

Material is washed in batch turning after the boiling, 75 ℃ water washing;

(4) making beating:

Process conditions: slurry concentration 2%, beating time 50-60min, beating degree 〉=32 ° SR, humidity 18g;

(5) refining:

Technological process is followed successively by: float that preceding preliminary treatment, alkali treatment, clorox are floated, alkali treatment, clorox float;

The process for refining condition is shown in the following table:

Processing step	Slurry concentration	Chemicals and consumption	Temperature	Processing time
					Prebleaching	5％	Chlorine 7% (to brown stock)	45℃	30min
Chlorination	10％	Chlorine 10%	Normal temperature	40min
					Alkali treatment	10％	NaOH 5.5%	65℃	150min
Clorox floats	10％	Clorox 7%	45℃	150min
					Alkali treatment	10％	NaOH 2.5%	95℃	90min
Clorox floats	10％	Clorox 3%	45℃	90min

(6) dechlorination: remove residual chlorine with sodium thiosulfate;

(7) acid treatment: with acid amount 2-3%, normal temperature 60min;

End product quality: alpha cellulose: 94.0%

Cuprammonium viscosity: 16.5CP

Ash content: 0.12%

Iron-holder: 20mg/kg;

Two, the technology with cotton bar viscose glue pulp production viscose staple fibre is as follows:

(1) feed the dregs of rice:

Cotton stalk viscose glue pulp is added in hello the dregs of rice machine, and by output folding speed;

(2) dipping:

In treating tank, carry out, dipping concentration: 23 ± 1g/l, alkali concn 240g/l temperature: 54 ± 1 ℃, the time:

2 ± 0.5 hours, squeezing half fine content :≤18g/l;

(3) squeezing:

In network chain formula squeezer, carry out squeezing multiple: 3.0-3.5;

(4) experienced:

In experienced drum, carry out temperature: 40-60 ℃, time: 35-60 minute, material amount: 60-80%; Full-page proof first fibre: 30.5 ± 0.5%, full-page proof contains alkali: 16.5 ± 0.5%;

(5) cooling: be cooled to 30-35 ℃;

(6) yellow:

In xanthating machine, carry out, add CS ₂Yellow, concentration: dosage is decided on technology; Carbonization: 34-35%, true chamber degree :≤-0.08Mpa, yellow initial temperature: 19-20 ℃, yellow is temperature eventually: 27-28 ℃, yellow time: 90-120 minute;

(7) back dissolving:

Carry out in blender, lytic agent is a dilute solution of sodium hydroxide, dissolution time: 2 hours, and warm 19-20 ℃ eventually:

Dissolving glue leading indicator is as follows: first fibre: 8.80-9.20% contains alkali: 5.4-6.0%, viscosity: 36-48Pas, net value: 〉=80ml;

(8) mix:

Carry out in the viscose glue tempering tank, the leading indicator of epoxy glue is as follows: first fibre: 8.80-9.00% contains alkali: 5.4-5.8%, viscosity: 34-38Pas, degree of ripeness: 4.2-4.5ml (20%NH ₄Cl), net value: 〉=10ml;

(9) filter:

First filtration machine IF: the polypropylene fibre felt, filter pressure :≤0.4Mpa,

Two road filter IIF: single-side pile+Polypropylene, filter pressure :≤0.4Mpa;

(10) maturation:

In viscose ripening tank, carry out temperature: 20-22 ℃, time: 8-10 hour;

(11) deaeration:

In the continuous deaerator of viscose glue, carry out vacuum :≤-0.098Mpa, liquid value :≤80%;

(12) filter:

KK filter IIIF: single-side pile+Polypropylene, filter pressure :≤0.6Mpa;

(13) spinning:

In the viscose short-thread spinning machine, carry out, by metering, spray silk, solidify continuous process and finish;

Acid bath is composed as follows: H ₂SO ₄: 125-128g/l, ZnSO ₄: 10-11g/l, Na ₂SO ₄: 330-340g/l, bathe temperature: 50 ± 1 ℃;

Mouth gold: decide on spinning specification; Total draft: 2.10-2.20 doubly;

Spin speed: decide on output;

(14) boundling drawing-off:

Carry out in the boundling drawing machine, the boundling draw conditions is: I boundling temperature: 〉=85 ℃, II boundling temperature: 〉=98 ℃, two baths contain acid: 8-13g/l;

(15) post processing:

Post processing include washing, concise, oil, cut-out, desulfurization;

One washing: normal temperature, two washings: 50-55 ℃, three washings: 50-55 ℃,

Desulfurization bath temperature: 70-75 ℃, desulfurization bath concentration: 7.0-8.0g/l,

Hydrogen peroxide concentration: 0.10-0.18%, last oil concentration: 4-6g/l,

It is moisture that high pressure is pricked car: 45-55%;

(16) garden net, oven dry;

In the net dryer of garden, carry out district's temperature :≤120 ℃, two district's temperature :≤110 ℃, three district's temperature :≤110 ℃, four district's temperature :≤100 ℃;

(17) packing:

Bao Chong: 150-180kg.

The invention has the beneficial effects as follows that raw material resources are abundant, production cost is low, and fiber quality is good, does that wet strength is higher, color and luster good, sucting wet air permeability good, antibacterial mildew-resistant, soft smooth, characteristic such as drapability is good, can be used for doing textile raw material etc.

Concrete embodiment

Embodiment 1:

Get 4 tons of cotton stalks, operate, can produce the finished product of cotton stalk viscose staple fibre by described processing step of the technical scheme in the foregoing invention content part and process conditions.

Claims (1)

1. utilize the cotton stalk to prepare the method for viscose staple fibre, it is characterized in that it includes preparation cotton stalk viscose glue pulp and prepares viscose staple fibre two with this pulp to go on foot greatly that its concrete technology is as follows:

One, the technology of preparation cotton stalk viscose glue pulp:

(1) get the raw materials ready: raw material is the full stalk of cotton stalk, go root slightly, remove the casting skin on bast top layer after, cut into 20～40mm, pound with machinery and split, choose assorted, washing then, soak;

(2) prehydrolysis: the prehydrolysis process conditions are: the concentration of hydrochloric acid is 1-3%, temperature 90-100 ℃, and 2 hours time;

(3) boiling, batch turning, wash material: in boiling vessel, carry out;

Technical conditions: alkali charge: 20-24% uses anthraquinone amount: 0.1-0.3%;

Sulphidity: 18-22%;

Liquor ratio: 1: 5;

Behind the 30min, intensification 35min, 135 ℃ of temperature, steam bleeding 20min for the first time, 110 ℃ of temperature, pressure 0.05MPa;

The 35min that heats up for the second time, 135 ℃ of temperature, steam bleeding 20min for the second time, 35 ℃ of temperature, pressure 0.2MPa;

The 30min that heats up for the third time, temperature 165-168 ℃;

Temperature retention time is: 90min, holding temperature 165-168 ℃;

Material is washed in batch turning after the boiling, 75 ℃ water washing;

(4) making beating:

Process conditions: slurry concentration 2%, beating time 50-60min, beating degree 〉=32 ° SR, humidity 18g;

(5) refining:

Technological process is followed successively by: float that preceding preliminary treatment, alkali treatment, clorox are floated, alkali treatment, clorox float;

The process for refining condition is shown in the following table:

Processing step Slurry concentration Chemicals and consumption Temperature Processing time Prebleaching 5％ Chlorine 7% (to brown stock) 45℃ 30min Chlorination 10％ Chlorine 10% Normal temperature 40min Alkali treatment 10％ NaOH 5.5% 65℃ 150min

Clorox floats 10％ Clorox 7% 45℃ 150min Alkali treatment 10％ NaOH 2.5% 95℃ 90min Clorox floats 10％ Clorox 3% 45℃ 90min

(6) dechlorination: remove residual chlorine with sodium thiosulfate;

(7) acid treatment: with acid amount 2-3%, normal temperature 60min;

End product quality: alpha cellulose: 94.0%

Cuprammonium viscosity: 16.5CP

Ash content: 0.12%

Iron-holder: 20mg/kg;

Two, the technology with cotton bar viscose glue pulp production viscose staple fibre is as follows:

(1) feed the dregs of rice:

Cotton stalk viscose glue pulp is added in hello the dregs of rice machine, and by output folding speed;

(2) dipping:

In treating tank, carry out, dipping concentration: 23 ± 1g/l, alkali concn 240g/l temperature: 54 ± 1 ℃, the time:

2 ± 0.5 hours, squeezing half fine content :≤18g/l;

(3) squeezing:

In network chain formula squeezer, carry out squeezing multiple: 3.0-3.5;

(4) experienced:

In experienced drum, carry out temperature: 40-60 ℃, time: 35-60 minute, material amount: 60-80%; Full-page proof first fibre: 30.5 ± 0.5%, full-page proof contains alkali: 16.5 ± 0.5%;

(5) cooling: be cooled to 30-35 ℃;

(6) yellow:

In xanthating machine, carry out, add CS ₂Yellow, concentration: dosage is decided on technology; Carbonization: 34-35%, true chamber degree :≤-0.08Mpa, yellow initial temperature: 19-20 ℃, yellow is temperature eventually: 27-28 ℃, yellow time: 90-120 minute;

(7) back dissolving:

Carry out in blender, lytic agent is a dilute solution of sodium hydroxide, dissolution time: 2 hours, and warm 19-20 ℃ eventually;

Dissolving glue leading indicator is as follows: first fibre: 8.80-9.20% contains alkali: 5.4-6.0%, viscosity: 36-48Pas, net value: 〉=80ml;

(8) mix:

Carry out in the viscose glue tempering tank, the leading indicator of epoxy glue is as follows: first fibre: 8.80-9.00% contains alkali: 5.4-5.8%, viscosity: 34-38Pas, degree of ripeness: 4.2-4.5ml (20%NH ₄Cl), net value: 〉=10ml;

(9) filter:

First filtration machine IF: the polypropylene fibre felt, filter pressure :≤0.4Mpa,

Two road filter IIF: single-side pile+Polypropylene, filter pressure :≤0.4Mpa;

(10) maturation:

In viscose ripening tank, carry out temperature: 20-22 ℃, time: 8-10 hour;

(11) deaeration:

In the continuous deaerator of viscose glue, carry out vacuum :≤-0.098Mpa, liquid value :≤80%;

(12) filter:

KK filter IIIF: single-side pile+Polypropylene, filter pressure :≤0.6Mpa;

(13) spinning:

In the viscose short-thread spinning machine, carry out, by metering, spray silk, solidify continuous process and finish;

Acid bath is composed as follows: H ₂SO ₄: 125-128g/l, ZnSO ₄: 10-11g/l, Na ₂SO ₄: 330-340g/l, bathe temperature: 50 ± 1 ℃;

Mouth gold: decide on spinning specification; Total draft: 2.10-2.20 doubly;

Spin speed: decide on output;

(14) boundling drawing-off:

Carry out in the boundling drawing machine, the boundling draw conditions is: I boundling temperature: 〉=85 ℃, II boundling temperature: 〉=98 ℃, two baths contain acid: 8-13g/l;

(15) post processing:

Post processing include washing, concise, oil, cut-out, desulfurization;

One washing: normal temperature, two washings: 50-55 ℃, three washings: 50-55 ℃,

Desulfurization bath temperature: 70-75 ℃, desulfurization bath concentration: 7.0-8.0g/l,

Hydrogen peroxide concentration: 0.10-0.18%, last oil concentration: 4-6g/l,

It is moisture that high pressure is pricked car: 45-55%;

(16) garden net, oven dry;

In the net dryer of garden, carry out district's temperature :≤120 ℃, two district's temperature :≤110 ℃, three district's temperature :≤110 ℃, four district's temperature :≤100 ℃;

(17) packing:

Bao Chong: 150-180kg.