CN1831235A

CN1831235A - Technology for dyeing ramie fiber with overcritical carbon dioxide method

Info

Publication number: CN1831235A
Application number: CN 200610041891
Authority: CN
Inventors: 刘昭铁; 张利利
Original assignee: Shaanxi Normal University
Current assignee: Shaanxi Normal University
Priority date: 2006-03-07
Filing date: 2006-03-07
Publication date: 2006-09-13
Anticipated expiration: 2026-03-07
Also published as: CN100494561C

Abstract

The invention relates to a new process of supercritical CO2 dyeing of ramie fiber, using ramie fiber as raw material, swelling by NaOH solution and modifying by benzoyl chloride, and dyeing with dispersive dye in supercritical CO2 medium by supercritical fluid technique. And its advantages: it is a clean producing process; the dyed ramie fiber has characters of bright color, short dyeing flow, dyeing uniformity, good color intensity, low synthetic cost, and remarkable economic and environmental protection benefits. And it also reveals a process device implementing the dyeing method, suitable to spread and apply in spinning and weaving, and printing and dyeing enterprises.

Description

A kind of technology for dyeing ramie fiber with overcritical carbon dioxide

One, technical field

What the present invention relates to is a kind of ramee colouring method, and this method is specially adapted to dyeing ramie fiber with overcritical carbon dioxide technology.Method provided by the invention can be avoided the processing of traditional dyeing method large amount of sewage, saves the energy, and obtains the dyeability suitable with traditional dyeing.

Two, technical background

Ramie is a kind of ancient crop, and the existing main place of production is China and some other Asian countries.Ramie product is good textile raw material, and nice and cool, ventilative, well-pressed advantage is arranged.But because its degree of crystallinity, the degree of orientation are higher, cause extensibility, poor flexibility, Color is good inadequately.On the other hand, China is weaving big country, and traditional dyeing and finishing water consumption is big, and environmental pollution is serious, the integrated cost height.How lifting along with scientific and technological progress and people realize ecological environment realizes the anhydrous medium staining technique, cleans production, is the expert's tackling key problem difficult problem in recent years of weaving both at home and abroad.Be suggested till now for the first time from supercritical fluid in 1991 dyeing, only limit to the supercritical CO 2 dyeing of chemical fibre both at home and abroad, still less relatively to the report of natural fabric especially ramie fiber with overcritical dyeing, and temperature height, pressure are big.Therefore the modification before the characteristic that the present invention is directed to ramee dyes is handled, technology to supercritical CO 2 dyeing is carried out systematic research, realized dyeing ramie fiber with overcritical carbon dioxide, and had the advantages that pressure is low, flow process short, dyeing time is short.

Three, summary of the invention

The present invention adopts sodium hydroxide solution that ramee is carried out swelling treatment, and then with chlorobenzoyl chloride it is carried out modification.Use supercritical CO 2 dyeing device, under supercriticality, dye, thoroughly eradicated the environmental pollution that traditional water dyeing is caused.

The present invention has following characteristics compared to existing technology: one, dyeing course water not, and pollution-free, realized cleaning production; Two, dyestuff can be recycled, and saves dyestuff; Three, the dyeing flow process is short; Four, dyeing pressure is little; Five, even dyeing; Six, integrated cost is low.

Method of the present invention can reach by following measure: at first put into a certain amount of DISPERSE DYES, will put into autoclave through the ramee after the chlorobenzoyl chloride modification again and can dye.

Liquid CO 2 flows out from steel cylinder, enters autoclave through high-pressure pump and begins dyeing.After dyeing reached the process time, ramee was taken out in step-down, takes out not set dyestuff again.

Four, description of drawings

Fig. 1 is a supercritical carbon dioxide ramee dyeing flow sketch of the present invention.

1.CO ₂Steel cylinder

2. valve

3. coolant pump

4. high pressure syringe pump

5. Pressure gauge

6. reactor

7. heating jacket

8. temperature controller

9. magnetic force rotor

10. swivelling pipe

11. magnetic stirring apparatus

12. Pressure gauge

13. safety valve (rupture disk)

Five, the specific embodiment

Embodiment 1:

Swelling treatment: ramee is handled through 15% sodium hydroxide solution, eliminates polarity and part hydrogen bond, and fibre crystallinity is reduced.At room temperature, handled 150 minutes.

Modification is handled: ramee is handled through chlorobenzoyl chloride, introduces hydrophobicity benzoyl group.At room temperature, handled 30 minutes.

With DISPERSE DYES (dye dosage be fiber heavy 5.0%) autoclave of packing into, again ramee is fixed in the still.Open refrigeration compressor, liquid CO 2 is flowed out from steel cylinder, enter autoclave through high-pressure pump.Be forced into 3-4MPa, be warmed up to 90 ℃, be pressurized to predetermined pressure 15MPa again, open and stir, dyeed 120 minutes.

After dyeing time arrived, the discharging carbon dioxide when pressure is kept to normal pressure, took out the ramee of dyeing.Reclaim remaining dyestuff.

Embodiment 2:

Swelling treatment: ramee 20% is handled through sodium hydroxide solution, eliminates polarity and part hydrogen bond, and fibre crystallinity is reduced.At room temperature, handled 90 minutes.

Modification is handled: ramee is handled through chlorobenzoyl chloride, introduces hydrophobicity benzoyl group.At room temperature, handled 20 minutes.

With DISPERSE DYES (dye dosage be fiber heavy 3.0%) autoclave of packing into, again ramee is fixed in the still.Open refrigeration compressor, liquid CO 2 is flowed out from steel cylinder, enter autoclave through high-pressure pump.Be forced into 3-4MPa, be warmed up to 110 ℃, be pressurized to predetermined pressure 18MPa again, open and stir, dyeed 150 minutes.

Embodiment 3:

Swelling treatment: ramee 25% is handled through sodium hydroxide solution, eliminates polarity and part hydrogen bond, and fibre crystallinity is reduced.At room temperature, handled 60 minutes.

Modification is handled: ramee is handled through chlorobenzoyl chloride, introduces hydrophobicity benzoyl group.At room temperature, handled 10 minutes.

With DISPERSE DYES (dye dosage be fiber heavy 2.5%) autoclave of packing into, again ramee is fixed in the still.Open refrigeration compressor, liquid CO 2 is flowed out from steel cylinder, enter autoclave through high-pressure pump.Be forced into 3-4MPa, be warmed up to 130 ℃, be pressurized to predetermined pressure 20MPa again, open and stir, dyeed 90 minutes.

Embodiment 4:

Swelling treatment: ramee 30% is handled through sodium hydroxide solution, eliminates polarity and part hydrogen bond, and fibre crystallinity is reduced.At room temperature, handled 30 minutes.

Modification is handled: ramee is handled through chlorobenzoyl chloride, introduces hydrophobicity benzoyl group.At room temperature, handled 5 minutes.

With DISPERSE DYES (dye dosage be fiber heavy 2.0%) autoclave of packing into, again ramee is fixed in the still.Open refrigeration compressor, liquid CO 2 is flowed out from steel cylinder, enter autoclave through high-pressure pump.Be forced into 3-4MPa, be warmed up to 100 ℃, be pressurized to predetermined pressure 17MPa again, open and stir, dyeed 60 minutes.

Advantage of the present invention is: no waste liquid, remove expensive liquid waste processing expense from. Need not drying, remove energy consumption cost from. The dyeing ramee is bright-colored, and is suitable for the flaxen fiber of various kinds.

Claims

1. technology for dyeing ramie fiber with overcritical carbon dioxide; it is characterized in that: be that sweller is handled ramee with the sodium hydroxide solution; eliminate part hydrogen bond, Van der Waals force etc. in the fiber and be unfavorable for the factor that dyes; and further modification; introduce hydrophobicity benzoyl group, increase compatibility and the adsorptivity of fiber dyestuff.Make it realize dyeing under the supercritical carbon dioxide state, excess dye is reusable.

2. according to the described method of claim 1, it is characterized in that: with 5-30% sodium hydroxide solution swelling ramee.Its temperature: 0-50 ℃, time: 10-180 minute.

3. according to the described method of claim 1, it is characterized in that: be that modifier carries out the modification processing to ramee with the chlorobenzoyl chloride.Its temperature: 15-30 ℃, time: 5-60 minute.

4. according to the described method of claim 1, it is characterized in that: the supercritical dyeing used medium is a carbon dioxide, critical-temperature T _c=31.3 ℃, critical pressure P _c=7.3MPa.

5. according to the described method of claim 1, it is characterized in that: supercritical CO 2 dyeing reaction process condition, pressure are 12-20MPa, and temperature is 70-130 ℃, and the time is 10-180 minute.

6. according to the described method of claim 1, it is characterized in that: the used dyestuff of supercritical dyeing is a DISPERSE DYES, makes to dye on it evenly, and COLOR FASTNESS is good.

7. according to the described method of claim 1, it is characterized in that: the DISPERSE DYES consumption that supercritical dyeing adopted is the 0.5%-5% of ramee quality.

8. according to the described method of claim 1, it is characterized in that: according to needs of production, realize that dyestuff reclaims, reusable.