CN101003953A

CN101003953A - Fixation crosslinking agent, and producing method

Info

Publication number: CN101003953A
Application number: CN 200610045703
Authority: CN
Inventors: 严欣宁; 周明; 刘杰; 仇凯
Original assignee: HENGXING FINE CHEMICAL INDUSTRY Co Ltd DANDONG
Current assignee: Dandong Hengxing Fine Chemical Group Co ltd; Liaoning Fixed Star Fine Chemical Co ltd; Liaoning Fixed Star Chemicals (Group) Co Ltd
Priority date: 2006-01-18
Filing date: 2006-01-18
Publication date: 2007-07-25
Anticipated expiration: 2026-01-18
Also published as: CN100487191C

Abstract

The present invention relates to a fixation coupling agent. It is made up by using trimethylamine, hydrochloric acid, epichlorohydrin, and cyanuric chloride and hexamethylene diamine through the processes of neutralization, quaternization and polymerization.

Description

Fixation crosslinking agent and production method

Technical field:

What the present invention relates to is the fabrics printing and dyeing fixation crosslinking agent, is a kind of color-fixing agent that is used for after textile dye dyes, and can be used for the modifier of pigment dyeing and the crosslinking agent of COAT PRINTING.

Background technology

Textile industry enters the 21st century people ecological and environmental issue is paid close attention to more, COLOR FASTNESS to dyeing and PRINTED FABRIC, especially the COLOR FASTNESS of exported product is had higher requirement, at present, color-fixing agent contains formaldehyde more, and aldehyde-free colour stabilizer 70-80% belongs to resin type, and this type of color-fixing agent is by combining salify or dying thing surface formation resin cation and improving dyefastness with anionic dye, and its fixation ability is relatively poor.As the aldehyde-free colour stabilizer DUR of auxiliary reagent factory, Shanghai and the nofix Exo of Switzerland vapour Bagong department,, can not reach desirable colour fixation because it is less to contain reactive group in its respond difference or the molecule.

Summary of the invention

The purpose of this invention is to provide a kind of no aldehyde, can improve calico staining fastness, crock fastness and soaping fastness, can be used for the fixation behind the dyeing, and can be used for fixation crosslinking agent and production method that the crosslinking agent of COAT PRINTING uses.

Fixation crosslinking agent of the present invention is to be raw material with trimethylamine, hydrochloric acid, epoxychloropropane, Cyanuric Chloride, sodium carbonate, acetone and hexamethylene diamine, and through neutralization, quaternized, fixation crosslinking agent that the polymerization three step process is made: proportioning raw materials is (weight):

Trimethylamine 120-150

Hydrochloric acid (37%) 38-46

Epoxychloropropane 75-80

Sodium carbonate (30%) 8-12

Acetone 22-30

Cyanuric Chloride 30-40

Hexamethylene diamine 35-45

Water 300-500

The product chemical index is as follows

Outward appearance: colourless to weak yellow liquid; PH value: 5.0-6.0; Solid content (%): 〉=33; Ionic: sun; Water-soluble: cold water solubles.

The production method of fixation crosslinking agent of the present invention is:

(1) neutralization reaction: add trimethylamine 120-150 in the stainless steel still, with hydrochloric acid (37%) 028-32 neutralization, temperature remains on 20-40 ℃, and the pH value of regulating product is 4-6;

(2) quaterisation: reactor is warming up to 45-55 ℃, slowly drips epoxychloropropane 75-80, dropwise in 1-2 hour, insulation reaction 4-5 hour;

(3) polymerisation: under 20-40 ℃ of stirring condition, slowly be added drop-wise to the mixed liquor of Cyanuric Chloride 30-40 and acetone 22-30 in the reactor, and use sodium carbonate (30%) 8-12 to regulate pH value at any time to be 6.0-7.0, till still constant after 20 minutes, to be warmed up to 65-70 ℃, stir the solution that adds hexamethylene diamine 35-45 and water 300-500, after dripping, be incubated 2-3 hour, be cooled to 20-40 ℃ then, regulating pH value with hydrochloric acid (37%) 10-14 is 6.0-7.0, gets product.The above-mentioned raw material that uses is weight ratio.

Colour fixation depends on kind and molecular weight size, the power of positive lotus property and the reactivity of reactive group of selected resin and high polymer.The present invention is cation group and the high reaction activity groups introduced on resin or high-polymer molecular more, it can be reacted with fiber and dyestuff or adsorb, thereby reach colour fixation.Owing to contain multiple reactive group and higher cation chain segments in the molecular structure of fixation crosslinking agent of the present invention, therefore, the binding ability of itself and fiber and adhesive is very strong, be used for the fixation after textile dye dyes, use with the crosslinking agent that is used for COAT PRINTING, overcome the alkyl quaternary ammonium compound that in the past adopts epoxide group need high-alkali, high temperature could with the shortcoming of fiber and dyestuff reaction, improved respond, reduced consumption, colour fixation is good.The advantage of fixation crosslinking agent of the present invention is:

(1) low, the environment-friendly type of this product price;

(2) the fixation requirement behind the dyeings such as satisfied simultaneously activity, sulfuration, acidity can obviously improve wet fastness, soaping fastness and the crock fastness of scalding, and especially can improve more than the calico staining fastness one-level;

(3) fabric coloured light and the form and aspect after the fixation do not change, and have again to increase dark effect, are convenient to control color and luster like this, can save the part dyestuff again;

(4) easy to use, this product can be dissolved in cold water and be disperseed rapidly, can guarantee to put in order the fastness uniformity of back fabric;

(5) multifunctionality because this product has higher cationic and extremely strong reactivity, therefore, can also can significantly improve the fastness of COAT PRINTING as the crosslinking agent of COAT PRINTING

The specific embodiment

Embodiment 1

(1) neutralization reaction: add trimethylamine 125KG in the stainless steel still, with hydrochloric acid (37%) 28-30KG neutralization, temperature remains on 20-40 ℃, and the pH value of regulating product is till 5.

(2) quaterisation: reactor is warming up to 45-50 ℃, slowly drips epoxychloropropane 76KG, dropwise in 1.5 hours, insulation reaction 4-4.5 hour.

(3) polymerisation: under 20-40 ℃ of stirring condition, the mixed liquor of Cyanuric Chloride 30KG and acetone 24KG slowly is added drop-wise in the reactor, and (30%) 8-12KG that uses sodium carbonate at any time to regulate pH value be 6.5, till still constant after 20 minutes.Be warmed up to 65-70 ℃, under agitation to the solution that wherein progressively adds hexamethylene diamine 36KG and water 300KG, reaction temperature remains on 65-70 ℃.After dripping, be incubated 2.5 hours, and lower the temperature 25-30 ℃, regulating pH value with hydrochloric acid (37%) 12KG is 6.5, gets product.

Embodiment 2:

Proportioning raw materials: trimethylamine 140KG, hydrochloric acid (37%) 43KG, epoxychloropropane 80KG, sodium carbonate (30%) 12KG, acetone 28KG, Cyanuric Chloride 40KG, hexamethylene diamine 45KG, water 400KG, production process is with embodiment 1.

The using method of fixation crosslinking agent of the present invention

1, material dyeing back fixation is used:

Mix with water 10g/l with this product, two soak two rolls, dries.

2, making the COAT PRINTING crosslinking agent uses: add 0.5-0.8% this product in textile printing pigment, baking gets final product behind the stamp.Can obviously improve crock fastness, especially fastness to wet rubbing is more than half grade.Equally DUR and TinofixExo are done not obviously effect of COAT PRINTING crosslinking agent application.

This product (code name is FSE) compares with the aldehyde-free colour stabilizer DUR of auxiliary reagent factory, Shanghai and the nofix Exo of Switzerland vapour Bagong department,

(1) degree is measured and is pressed GB5711-5718-85, GB6511-85I mensuration.

(2) chromatic value compares colour meter (Beijing Optical Instrument Factory) mensuration by WSL-1.

(3) scale: GB250-1995 dyefastness fading sample card.

(4) scale: GB251-1995 dyefastness tinctorial pattern card.(Shanghai textile industry technical supervision institute)

FSE, DUR, TinofixEXO colour fixation and price

Dye well consumption (%) (OWF)	The color-fixing agent kind	X+Y+Z (tristimulus values sum)	Soaping fastness (level) former state is faded, calico staining		Friction jail (level) is done wet		Price (unit/kg)
Dye well consumption (%) (OWF)	The color-fixing agent kind	X+Y+Z (tristimulus values sum)			Friction jail (level) is done wet		Price (unit/kg)	Reactive yellow X-6G4.0	FSE	132.18	4-5	4	4	3-4	12
	DUR	142.70	4	3-4	3-4	3	20	Reactive yellow X-6G4.0	FSE	132.18	4-5	4	4	3-4	12
	DUR	142.70	4	3-4	3-4	3	20		TinofixEX O	140.01	4-5	3-4	4	3-4	40
Reactive Brilliant Red M-8B 3.0	FSE	56.75	4-5	3-4	4	3			TinofixEX O	140.01	4-5	3-4	4	3-4	40
Reactive Brilliant Red M-8B 3.0	FSE	56.75	4-5	3-4	4	3			DUR	60.81	3-4	2	3-4	3
	TinofixEX O	58.76	4	3-4	4	3			DUR	60.81	3-4	2	3-4	3
	TinofixEX O	58.76	4	3-4	4	3		Reactive Turquoise Blue KN-G 4.0	FSE	75.14	4	4	3-4	3
	DUR	80.82	4	3	3	2-3		Reactive Turquoise Blue KN-G 4.0	FSE	75.14	4	4	3-4	3
	DUR	80.82	4	3	3	2-3			TinofixEX O	78.95	4	3-4	3-4	3

As can be seen from the table:

FSE compares with DUR, and every application performance index all is better than DUR.And the every application index of Tinofix Exo of FSE and vapour Bagong department is close, and the application index that has also is higher than Tinofix Exo on some dyestuff.

Can find out that from the tristimulus values sum of product dyed thereby the product dyed thereby of using the FSE fixation gets color depth than using DUR, Tinofix Exo, illustrate that using the FSE fixation can save dyestuff.

From also the price of FSE is lower as can be seen in price.

Claims

1, a kind of production method of fixation crosslinking agent is characterized in that:

(1) neutralization reaction: add trimethylamine 120-150kg in the stainless steel still, with hydrochloric acid (37%) 28-32kg neutralization, temperature remains on 20-40 ℃, and the pH value of regulating product is 4-6;

(2) quaterisation: reactor is warming up to 45-55 ℃, slowly drips epoxychloropropane 75-8kg, dropwise in 1-2 hour, insulation reaction 4-5 hour;

(3) polymerisation: under 20-40 ℃ of stirring condition, slowly be added drop-wise to the mixed liquor of Cyanuric Chloride 30-40kg and acetone 22-30kg in the reactor, and to use sodium carbonate (30%) 8-12kg to regulate pH value at any time be 6.0-7.0, till still constant after 20 minutes, be warmed up to 65-70 ℃, stir the solution that adds hexamethylene diamine 35-45kg and water 300-500kg, after dripping, be incubated 2-3 hour, be cooled to 20-40 ℃ then, regulating pH value with hydrochloric acid (37%) 10-14kg is 6.0-7.0, gets product.

2, a kind of fixation crosslinking agent of producing by the described method of claim 1.