Self-crosslinking color fixing agent and preparation method thereof

Abstract

The invention discloses a method for preparing a self-crosslinking color fixing agent, comprising the following steps: (1) adding 100 parts by weight of dimethyldiallylammonium chloride, 5-10 parts by weight of diallylamine and 3-6 parts by weight of a crosslinking monomer into a reaction kettle, adding a certain amount of hydrochloric acid to adjust the pH value between 4-5, releasing 70% of the above mixture and adding it into a titration funnel for titration; introducing a reactive monomer to copolymerize and modify the color fixing agent, so that the linear molecule contains a reactive group that can react with a crosslinking agent to form a crosslinked body, thereby greatly improving various properties of the color fixing agent, and improving the washing fastness of the fabric by 4-5 levels and the dry and wet rubbing fastness by 4-5 levels; at the same time, a reactive group is introduced into the reactive color fixing agent of the invention, AAEM can be copolymerized with a cationic monomer, and the acetoacetyl group, due to the conjugation effect of a dicarbonyl group, causes the H on the middle methylene group to be extremely active and highly reactive, and can react with active groups such as an amine group, thereby improving the film-forming property of the color fixing agent.

Description

Technical Field

[0001] The invention relates to a color fixing agent technology, in particular to a self-crosslinking color fixing agent and a preparation method thereof. Background Art

[0002] Fixing agent is one of the important auxiliaries in the printing and dyeing industry. It can improve the color fastness of dyes on fabrics to wet treatment. It can form insoluble colored substances with dyes on fabrics to improve the color fastness to washing and perspiration, and sometimes improve its light fastness. With the development of science and technology, dyeing and finishing technology has also been significantly improved. Due to the expansion of international textile trade and the improvement of people's living standards and environmental awareness, textiles are required to be comfortable, clean and safe. Since the 1970s, when Germany first launched the "Blue Angel" plan, some developed countries in the world (Japan, the United States, etc.) have successively passed and implemented relevant laws and regulations to stipulate various indicators for textiles.

[0003] The existing color fixing agents on the market generally have relatively small molecular weights, are not concentratedly distributed, and have no cross-linking. They have poor color fastness to washing, poor rubbing fastness, and large color change after fixing. In addition, most of the formaldehyde-free color fixing agents on the market are made of diallyldimethylammonium chloride homopolymer or diallyldimethylammonium chloride and diallylamine copolymers. This structure is a single straight-chain molecule with no reactive groups and poor film-forming properties.

[0004] Therefore, it is necessary to study a solution to solve the above problems. Summary of the invention

[0005] In view of this, the present invention aims at the deficiencies of the prior art, and its main purpose is to provide a self-crosslinking fixing agent and a preparation method thereof, which has good water fastness and dry and wet rubbing fastness and good film-forming property.

[0006] To achieve the above purpose, the present invention adopts the following technical solutions:

[0007] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0008] (1) Add 100 parts by weight of dimethyldiallylammonium chloride, 5-10 parts by weight of diallylamine, and 3-6 parts by weight of a crosslinking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to between 4 and 5, release 70% of the above mixture and add it into a titration funnel for titration;

[0009] (2) Raise the temperature to 80°C, add 1-2 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 5-7 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above;

[0010] (3) Maintain the temperature between 95-105°C and titrate for 3 hours. After the reaction is completed, add 3-5 parts by weight of a cross-linking agent, mix well, cool and discharge.

[0011] As a preferred embodiment, the mass concentration of the dimethyldiallylammonium chloride is 65%.

[0012] As a preferred embodiment, the solid content of the diallylamine is 100%.

[0013] As a preferred solution, the solid content of the cross-linking monomer is 100%.

[0014] As a preferred embodiment, the mass concentration of the hydrochloric acid is 31%.

[0015] As a preferred embodiment, the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0016] As a preferred solution, the solid content of the cross-linking agent is 100%.

[0017] A self-crosslinking color fixing agent is prepared by adopting the preparation method of the self-crosslinking color fixing agent.

[0018] Compared with the prior art, the present invention has obvious advantages and beneficial effects. Specifically, it can be seen from the above technical solution that:

[0019] By introducing reactive monomers to copolymerize and modify the color fixing agent, the linear molecule contains reactive groups that can react with the cross-linking agent to form a cross-linked compound, which greatly improves the various properties of the color fixing agent, and can improve the washing fastness of the fabric by 4-5 levels and the dry and wet friction fastness by 4-5 levels. At the same time, reactive groups are introduced into the reactive color fixing agent of the present invention, AAEM can copolymerize with the cationic monomer, and the acetoacetyl group, due to the conjugation effect of the dicarbonyl group, causes the H on the middle methylene group to be extremely active and highly reactive, and can react with active groups such as amine groups, thereby improving the film-forming performance of the color fixing agent. DETAILED DESCRIPTION

[0020] The present invention discloses a method for preparing a self-crosslinking color fixing agent, comprising the following steps:

[0021] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 5-10 parts by mass of diallylamine, and 3-6 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to between 4 and 5, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0022] (2) Raise the temperature to 80°C, add 1-2 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 5-7 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0023] (3) Maintain the temperature between 95-105°C and titrate for 3 hours. After the reaction is completed, add 3-5 parts by weight of a cross-linking agent, mix well, cool and discharge. The solid content of the cross-linking agent is 100%.

[0024] A self-crosslinking color fixing agent is prepared by adopting the preparation method of the self-crosslinking color fixing agent.

[0025] The present invention is further described in detail with multiple embodiments below:

[0026] Embodiment 1:

[0027] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0028] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 7 parts by mass of diallylamine and 4 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to 4, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0029] (2) Raise the temperature to 80°C, add 1.5 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 6 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0030] (3) The temperature was maintained at 101°C and titrated for 3 hours. After the reaction was completed, 4 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

[0031] When the self-crosslinking color fixing agent prepared in this example is used for dyeing fabrics with dyes, the washing fastness is grade 5 and the dry and wet rubbing fastness is grade 5 after testing.

[0032] Embodiment 2:

[0033] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0034] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 8 parts by mass of diallylamine and 3 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to 5, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0035] (2) Raise the temperature to 80°C, add 1 part by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 5 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0036] (3) The temperature was maintained at 95°C and titrated for 3 hours. After the reaction was completed, 3 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

[0037] When the self-crosslinking color fixing agent prepared in this example is used for dyeing fabrics, the washing fastness is grade 4 and the dry and wet rubbing fastness is grade 4 after testing.

[0038] Embodiment 3:

[0039] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0040] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 5 parts by mass of diallylamine, and 5 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to 4.3, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0041] (2) Raise the temperature to 80°C, add 2 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 7 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0042] (3) The temperature was maintained at 99°C and titrated for 3 hours. After the reaction was completed, 3.5 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

[0043] When the self-crosslinking color fixing agent prepared in this example is used for dyeing fabrics, the washing fastness is grade 4 and the dry and wet rubbing fastness is grade 5 after testing.

[0044] Embodiment 4:

[0045] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0046] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 6 parts by mass of diallylamine, and 6 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to 4.5, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0047] (2) Raise the temperature to 80°C, add 1.3 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 5.5 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0048] (3) The temperature was maintained at 97°C and titrated for 3 hours. After the reaction was completed, 4.5 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

[0049] When the self-crosslinking color fixing agent prepared in this example is used for dyeing fabrics, the washing fastness is grade 5 and the dry and wet rubbing fastness is grade 4 after testing.

[0050] Embodiment 5:

[0051] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0052] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 9 parts by mass of diallylamine, and 3 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to 4.7, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0053] (2) Raise the temperature to 80°C, add 1.4 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 6.5 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0054] (3) The temperature was maintained at 104°C and titrated for 3 hours. After the reaction was completed, 5 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

[0055] When the self-crosslinking color fixing agent prepared in this example is used for dyeing fabrics, the washing fastness is grade 4 and the dry and wet rubbing fastness is grade 5 after testing.

[0056] Embodiment 6:

[0057] A method for preparing a self-crosslinking color fixing agent comprises the following steps:

[0058] (1) Add 100 parts by mass of dimethyldiallylammonium chloride, 10 parts by mass of diallylamine and 4 parts by mass of a cross-linking monomer into a reaction kettle, add a certain amount of hydrochloric acid to adjust the pH value to 4.4, release 70% of the above mixture and add it into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the cross-linking monomer is 100%, and the mass concentration of hydrochloric acid is 31%.

[0059] (2) Raise the temperature to 80°C, add 1.7 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 5.8 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate simultaneously with the 70% monomer mixture taken out above; the mass concentration of the ammonium persulfate aqueous solution is 20%.

[0060] (3) The temperature was maintained at 105°C and titrated for 3 hours. After the reaction was completed, 3.3 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

[0061] When the self-crosslinking color fixing agent prepared in this example is used for dyeing fabrics, the washing fastness is grade 5 and the dry and wet rubbing fastness is grade 4 after testing.

[0062] The design focus of the present invention is that the reactive monomer copolymerization-modified color fixing agent is introduced to make the linear molecule contain reactive groups that can react with the cross-linking agent to form a cross-linked body, thereby greatly improving various properties of the color fixing agent, and can improve the washing fastness of the fabric by 4-5 levels and the dry and wet friction fastness by 4-5 levels. At the same time, the reactive groups are introduced into the reactive color fixing agent of the present invention, AAEM can be copolymerized with the cationic monomer, and the acetoacetyl group, due to the conjugation effect of the dicarbonyl group, causes the H on the middle methylene group to be extremely active and highly reactive, and can react with active groups such as amine groups, thereby improving the film-forming performance of the color fixing agent.

[0063] The above description is only a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any slight modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a self-crosslinking fixing agent, characterized in that The method comprises the following steps: (1) adding 100 parts by weight of dimethyldiallylammonium chloride, 7 parts by weight of diallylamine, and 4 parts by weight of AAEM crosslinking monomer into a reaction kettle, adding a certain amount of hydrochloric acid to adjust the pH value to 4, and discharging 70% of the above mixture into a titration funnel for titration; the mass concentration of dimethyldiallylammonium chloride is 65%, the solid content of diallylamine is 100%, the solid content of the crosslinking monomer is 100%, and the mass concentration of hydrochloric acid is 31%; (2) Raise the temperature to 80°C, add 1.5 parts by weight of ammonium persulfate aqueous solution, and start polymerization. The temperature will rise to 110°C. After cooling to 90°C, add 6 parts by weight of ammonium persulfate aqueous solution into the titration funnel and titrate with the 70% monomer mixture taken out above. The mass concentration of the ammonium persulfate aqueous solution is 20%. (3) The temperature was maintained at 101° C. and titrated for 3 hours. After the reaction was completed, 4 parts by weight of a cross-linking agent was added, mixed evenly, and then cooled and discharged. The solid content of the cross-linking agent was 100%.

2. A self-crosslinking fixing agent, characterized in that : Prepared by the preparation method of the self-crosslinking fixing agent as claimed in claim 1.