CN101413218A

CN101413218A - Method for preparing terylene environment protection type dye carrier

Info

Publication number: CN101413218A
Application number: CNA200810202881XA
Authority: CN
Inventors: 孔令红; 朱泉; 郭玉良; 刘元美; 刘玉勇; 卓文明; 高琴文
Original assignee: Donghua University
Current assignee: Donghua University
Priority date: 2008-11-18
Filing date: 2008-11-18
Publication date: 2009-04-22
Anticipated expiration: 2028-11-18
Also published as: CN101413218B

Abstract

The invention relates to a method for preparing a terylene environmental protection type dyeing carrier, which comprises the following steps: (1) alkylamine, dimethylformamide, phthalic anhydride and triethylamine are added into a three-neck flask with the volume of 500mL under the condition of ice bath and are subject to thermal insulation reaction for one hour; then the temperature is increased to 120 DEG C to perform a reflux reaction for four hours; the mixture is dumped into ice water after the reaction is finished; and white crystals are precipitated; (2) according to the mass proportion of 4 to 1, a carrier precursor is added into an emulsifying agent, heated and stirred; and (3) the process formulation is a dispersion dye, 1 to 3 percent owf of carrier, and 0.3g to 0.5g.L<-1> of glacial acetic acid; the bath ratio is 1 to 20; the dyeing temperature is between 85 and 100 DEG C; the thermal insulation time is between 60 and 100 minutes; and the dyeing carrier is washed and aired. The method is suitable for terylene boiling dyeing processes of dyeing and finishing plants, can reduce production cost, and shorten dyeing period. The textile after the dyeing has bright color, pure chromatic light, high brightness, no toxicity, no smell, and low COD value, so the dyeing carrier is an environment-frinedly green auxiliary.

Description

A kind of preparation method of terylene environment protection type dye carrier

Technical field

The invention belongs to the preparation field of dyeing terylene carrier, particularly relate to a kind of preparation method of terylene environment protection type dye carrier.

Background technology

Polyster fibre has the degree of crystallinity height, structure is tight, elasticity is better and the ABRASION RESISTANCE advantages of higher, but lack the active group that can combine in its structure with dyestuff, dyeing is difficulty comparatively, adopts methods such as high temperature and high pressure method, hot melt, organic solvent method or support methods that it is dyeed usually.In recent years, along with continuing to bring out of new type functional fiber, people pursue clothes personalization, variation, functionalization, and the application of numerous multi-component fibre composite fabrics is more extensive, as wool, silk, vinegar fibre, spandex etc. and extremely consumer's the favor of polyster fibre BLENDED FABRIC.Therefore but the characteristics of fiber non-refractories such as wool, silk, vinegar fibre, spandex make the application of high-temperature and high pressure dyeing process and thermosol dyeing method be restricted, and how to be implemented under the cryogenic conditions focus that to polyster fibre dyeing becomes relevant scholar's research.

In order to realize the polyster fibre low temperature dyeing, can be by improving the physical arrangement of polyster fibre.For example, after the employing gas ions is handled dacron, can dye under cryogenic conditions, it is bright-coloured to dye the thing Dry Sack, and has reached the purpose that energy-saving and water-saving, reduction are polluted; Under the atmospheric low-temperature condition, just dying rate and balance dye-uptake all has low the raising with the dacron of ultrasonic Treatment; Supercritical CO ₂The character that presents OOS, can infiltrated fiber inside, improve the mobility of polymer molecule, fiber is had the plasticising swelling action, can reduce the fibrous glass temperature, dyeing can be carried out being lower than under the water-bath dyeing temperature; Magnetized drinking water has invigoration effect to the fixing and adsorption process of disperse dyeing, can improve the dyeing dye-uptake, is a kind of saving dyestuff, reduces cost, and saves energy resource consumption, reduces environmental pollution, the new technology approach of cleaning.But these methods only limit to conceptual phase at present, fail to realize suitability for industrialized production.

Comparatively speaking, carrier dyeing process becomes the terylene atmospheric low-temperature dyeing method the most easily that realizes because of technology is simple, easy to operate, low for equipment requirements.But the early stage normal carrier that uses, as: wintergreen, methyl naphthalene, phenylphenol, chlorobenzene etc., toxicity is big, smell is heavy, biological degradability is poor, difficulty is taken off and carried, and makes DYED FABRICS have certain peculiar smell, on using, be very restricted, so the novel environment friendly carrier is demanded exploitation urgently.

Summary of the invention

Technical problem to be solved by this invention provides a kind of preparation method of terylene environment protection type dye carrier, and this preparing carriers is convenient, and technique for applying is simple, and is low to the dyeing installation requirement, can reduce energy consumption, reduces production costs.

The preparation method of a kind of terylene environment protection type dye carrier of the present invention comprises:

(1) precursor carrier is synthetic

In the 500mL there-necked flask, add alkylamine, dimethyl formamide, triethylamine and phthalic anhydride under the condition of ice bath, its mol ratio is 1.3:1.25:0.1:1, is warmed up to 120 ℃ of back flow reaction 4h behind the insulation reaction 1h, after reaction finishes the mixture thing is poured in the frozen water, separate out white crystal, promptly;

(2) emulsification of precursor carrier

By mass ratio is that 4:1 is added to precursor carrier in the emulsifying agent, be heated to 50 ℃-60 ℃ stir light yellow transparency liquid;

(3) dyeing

Technical recipe: DISPERSE DYES 0.5%-6%owf, carrier 1-3%owf, glacial acetic acid are 0.3gL ^-1-0.5gL ^-1, bath raio is 1:20, dyeing temperature is 85 ℃-100 ℃, temperature retention time is 60min-100min.

The dyeing post processing: cold wash 3 times, reduction cleaning (70 ℃ * 10min, NaOH 2-5g/L, sodium hydrosulfite (NaS ₂O ₃)) 2gL ^-1-5g/L,, bath raio 1:100), cold wash is then dried.

Alkylamine is one or several in ethamine, isopropylamine, n-butylamine, amylamine, the n-octyl amine in the described step (1).

Emulsifying agent is that its mass ratio of compound of surfactants such as neopelex, castor oil macrogol ester, aliphatic amine polyoxyethylene ether is 2.6:3.3:1 in the described step (2).

Precursor carrier is one or more in N-ethyl phthalimide, N-isopropyl phthalimide, N-normal-butyl base phthalimide, N-amyl group phthalimide, the N-n-octyl phthalimide in the described step (2).

DISPERSE DYES in the described step (3) is disperse red FB, disperse yellow E-3G or Disperse Blue 2BLN.

This preparation method does not contain APEO etc. and is banned, forbids the chemical composition used by international environmental protection organization.

This terylene environment protection type dye carrier can be realized terylene in 85-100 ℃ of dyeing, reduces 30-45 ℃ than high temperature and high pressure method, need not to use other auxiliary agents such as levelling agent, retarding agents.

Beneficial effect:

(1) preparing carriers method of the present invention is simple, and raw material sources are convenient, is suitable for the dyeing and finishing factory terylene dyeing technique that boils, and is convenient to suitability for industrialized production;

(2) carrier is low to the dyeing installation requirement, but energy savings reduces energy consumption, shortens the production cycle;

(3) Zhi Bei carrier does not influence the DYED FABRICS COLOR FASTNESS, and nontoxic, tasteless, low COD value, is a kind of environmental protection auxiliary agent;

(4) with fabric is bright in luster after this carrier dyeing, coloured light is pure, brightness is high.

Description of drawings

Fig. 1 is the cross section (amplifying 1000 times) of dyeing back polyster fibre, (a) carrier-free dyeing, (b) carrier dyeing;

Fig. 2 is that the PET fiber surface stereoscan photograph amplifies (10000 accompany), (a) after distilled water is handled, (b) after vehicle treated;

Fig. 3 dyeing temperature control curve.

The specific embodiment

Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.

Embodiment 1

With disperse red FB2% (owf), carrier 3% (owf), glacial acetic acid 0.3gL ^-1, bath raio 1:20,100 ℃ are dyed 60min.Dye complete after washing, reduction cleaning, the washing oven dry, coloration result sees Table 1

Table 1

	K/S	L*	a*	b*	C*	H*
	K/S	L*	a*	b*	C*	H*	Blank	4，18	57.29	58.88	-4.69	59.07	355.45
Carrier dyeing	10.12	48.77	64.33	3.92	64.45	3.49	Blank	4，18	57.29	58.88	-4.69	59.07	355.45

Embodiment 2

With disperse yellow E-3G2% (owf), carrier 3% (owf), glacial acetic acid 0.3gL ^-1, bath raio 1:20,100 ℃ are dyed 60min.Dye complete after washing, reduction cleaning, the washing oven dry, coloration result sees Table 2

Table 2

	K/S	L*	a*	b*	C*	H*
	K/S	L*	a*	b*	C*	H*	Blank	8.88	86.9	-1.62	80.14	80.15	91.16
Carrier dyeing	13.95	83.2	4.78	86.61	86.74	86.84	Blank	8.88	86.9	-1.62	80.14	80.15	91.16

Embodiment 3

With Disperse Blue 2BLN 2% (owf), carrier 3% (owf), glacial acetic acid 0.3gL ^-1, bath raio 1:20,100 ℃ are dyed 60min.Dye complete after washing, reduction cleaning, the washing oven dry, coloration result sees Table 3

Table 3

	K/S	L*	a*	b*	C*	H*
	K/S	L*	a*	b*	C*	H*	Blank	9.36	41.35	2.8	-43.09	43.18	273.72
Carrier dyeing	11.11	39.32	2.15	-42.22	42.88	272.92	Blank	9.36	41.35	2.8	-43.09	43.18	273.72

Claims

1. the preparation method of a terylene environment protection type dye carrier comprises:

(1) precursor carrier is synthetic

(2) emulsification of precursor carrier

(3) dyeing

Technical recipe: DISPERSE DYES 0.5%-6%owf, carrier 1%-3%owf, glacial acetic acid are 0.3gL ^-1-0.5gL ^-1, bath raio is 1:20, dyeing temperature is 85 ℃-100 ℃, temperature retention time is 60min-100min; Cold wash 3 times, reduction cleaning, cold wash is then dried.

2. the preparation method of a kind of terylene environment protection type dye carrier according to claim 1 is characterized in that: alkylamine is one or more in ethamine, isopropylamine, n-butylamine, amylamine, the n-octyl amine in the described step (1).

3. the preparation method of a kind of terylene environment protection type dye carrier according to claim 1, it is characterized in that: emulsifying agent is the compound of neopelex, castor oil macrogol ester, aliphatic amine polyoxyethylene ether surfactant in the described step (2), and its mass ratio is 2.6:3.3:1.

4. the preparation method of a kind of terylene environment protection type dye carrier according to claim 1 is characterized in that: precursor carrier is one or more in N-ethyl phthalimide, N-isopropyl phthalimide, N-normal-butyl base phthalimide, N-amyl group phthalimide, the N-n-octyl phthalimide in the described step (2).

5. the preparation method of a kind of terylene environment protection type dye carrier according to claim 1, it is characterized in that: the DISPERSE DYES in the described step (3) is disperse red FB, disperse yellow E-3G or Disperse Blue 2BLN.

6. the preparation method of a kind of terylene environment protection type dye carrier according to claim 1, it is characterized in that: described step (3) reducing condition is 70 ℃ * 10min, NaOH 2gL ^-1-5g/L, sodium hydrosulfite NaS ₂O ₃₎2gL ^-1-5g/L, bath raio 1:100.

7. the preparation method of a kind of terylene environment protection type dye carrier according to claim 1, it is characterized in that: this terylene environment protection type dye carrier can realize that terylene is in 85-100 ℃ of dyeing, reduce 30-45 ℃ than high temperature and high pressure method, need not to use levelling agent, other auxiliary agent of retarding agents.