CN110699991A - Acidic color fixing agent and preparation method thereof - Google Patents
Acidic color fixing agent and preparation method thereof Download PDFInfo
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- CN110699991A CN110699991A CN201911066631.2A CN201911066631A CN110699991A CN 110699991 A CN110699991 A CN 110699991A CN 201911066631 A CN201911066631 A CN 201911066631A CN 110699991 A CN110699991 A CN 110699991A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/39—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using acid dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/10—After-treatment with compounds containing metal
Abstract
The invention belongs to the field of dye fixing agents, and particularly relates to an acidic fixing agent and a preparation method thereof. Comprises the following components: polyethyleneimine, modified polyacrylic acid, sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate; the color fixing agent has a good color fixing effect, does not contain harmful substances such as formaldehyde and the like, and has a good pH value control effect.
Description
Technical Field
The invention belongs to the field of acid dye fixing agents, and particularly relates to an acid fixing agent and a preparation method thereof.
Background
The dye is one of the most important raw materials in the textile industry, the textile can not be separated from the dye in dyeing and printing, the color fastness is one of important quality indexes for measuring dyed finished products, the color fastness which is easy to fade is low, and the color fastness which is not easy to fade is high. The fastness of dyeing depends to a large extent on its chemical structure. In addition, the physical state of the dye on the fiber, the degree of dispersion, the binding of the dye to the fiber, the dyeing method and the process conditions, etc. also have a great influence. In recent years, with the development of science and technology, dyeing and finishing technology is remarkably improved, and due to the expansion of international textile trade and the improvement of living standard and environmental awareness of people, textiles are required to be comfortable, clean and safe.
The acid color fixing agent is one of important assistants in printing and dyeing industry, and can be used as an assistant for improving the color fastness of the dye on fabric to wet treatment. The insoluble color substance can be formed on the fabric with the dye, thereby improving the washing fastness and the perspiration fastness of the color and sometimes also improving the light fastness of the color.
The main problems of the existing acidic color fixing agent are as follows: on one hand, the color fixing agent used by a plurality of fabrics has more and non-ideal color fixing effect on dyed fabrics, and the color fixing effect is not durable. Secondly, the acid color fixing agent may contain harmful substances such as formaldehyde in the synthetic raw materials and the synthetic process, formaldehyde may be generated in the use, the production flow is longer, the process conditions are not easy to control, the treated silk fabric does not have a good color fixing effect, the color is easy to fade after washing, and the influence on the hand feeling is larger. In addition, after the conventional acidic color fixing agent is subjected to color fixing treatment, the pH value of the cloth surface of the fabric is too low. Poor fixation effect, large fixation color, and poor tolerance to hardness ions. At present, most of customers at home and abroad put forward pH value control ranges for different fabrics (fabrics), and most of the requirements are controlled between 4.5 and 7.5.
The Chinese patent application CN 104513349A discloses an acidic color fixing agent and a preparation method thereof, wherein the color fixing agent is a condensation product obtained by polycondensation reaction of raw materials of bisphenol S, sodium phenolsulfonate, formaldehyde and a catalyst. Has certain color fixing effect, but the pH value is not easy to control, and simultaneously, the color fixing agent contains formaldehyde, which is not beneficial to the application of the color fixing agent.
Chinese patent application CN 103497286 a discloses a preparation method of an environment-friendly acid dye fixing agent, which is prepared by mixing a dimethylamine aqueous solution with an epichlorohydrin solution and butyl acrylate, and adding a potassium persulfate solution to react under certain conditions. In addition, it is not favorable for the application because it requires the addition of an acidic substance such as acetic acid to adjust the acid during the application process.
Therefore, the technical problems to be solved urgently by the color fixing agent in the prior art are mainly that the color fixing effect is not ideal, the components are toxic and harmful and are not beneficial to being used in clothes dyes, the pH value is not easy to control, and the like. Therefore, the improvement of the fixing agent and the development of a novel fixing agent are still too heavy and far.
Disclosure of Invention
In order to overcome the technical problems, the invention provides an acidic color fixing agent which has a good color fixing effect, does not contain harmful substances such as formaldehyde and the like, has a good pH value control effect and is simple in preparation method.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
an acidic fixing agent comprises the following components: polyethyleneimine, modified polyacrylic acid, sodium citrate, sodium salicylate, sodium laureth sulfate and sodium stearate.
Preferably, the acidic color fixing agent comprises the following components in parts by weight: 10-20 parts of polyethyleneimine, 60-90 parts of modified polyacrylic acid, 10-20 parts of sodium citrate, 5-15 parts of sodium salicylate, 1-5 parts of sodium laureth sulfate, 1-10 parts of sodium stearate and 1-6 parts of sodium phenolsulfonate.
Preferably, the acidic color fixing agent comprises the following components in parts by weight: 15-18 parts of polyethyleneimine, 70-80 parts of modified polyacrylic acid, 15-20 parts of sodium citrate, 5-10 parts of sodium salicylate, 1-3 parts of sodium laureth sulfate, 3-9 parts of sodium stearate and 2-5 parts of sodium phenolsulfonate.
Preferably, the modified polyacrylamide is prepared from the following raw materials: methacrylic acid, 2-acrylamide-2-methyl sodium propyl sulfonate, sodium bisulfite, ammonium persulfate, azobisisobutyrimidazoline hydrochloride, a dispersing agent, ammonium sulfate and water.
Preferably, the modified polyacrylamide is prepared from the following raw materials in parts by weight: 10-30 parts of methacrylic acid, 1-5 parts of 2-acrylamide-2-methylpropanesulfonic acid sodium salt, 0.05-0.1 part of sodium bisulfite, 0.05-0.1 part of ammonium persulfate, 0.01-0.02 part of azobisisobutyrimidazoline hydrochloride, 5-10 parts of a dispersing agent, 30-40 parts of ammonium sulfate and 80-90 parts of water.
Preferably, the preparation raw materials of the dispersing agent comprise: methacrylic acid, water and azobisisobutyrimidazoline hydrochloride.
Preferably, the dispersant is prepared from the following raw materials in parts by weight: 5-10 parts of methacrylic acid, 90-95 parts of water and 0.02-0.05 part of azobisisobutylimidazoline hydrochloride.
Preferably, the preparation method of the dispersant is as follows: dissolving methacrylic acid in water at 40-60 ℃, adding azobisisobutyronitrile hydrochloride for reaction to prepare polymethacrylic acid, namely the dispersant.
Another object of the present invention is to provide a method for preparing the acidic fixing agent, comprising the following steps:
(1) dissolving methacrylic acid and 2-acrylamide-2-methyl sodium propanesulfonate in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, reacting, heating, adding azodiisobutyl imidazoline hydrochloride, and reacting to obtain a dispersion system of modified polyacrylic acid;
(2) dissolving sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate, and sodium phenolsulfonate in water, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and mixing the aqueous solution with the dispersion system, stirring and carrying out ultrasonic treatment to obtain the acidic color fixing agent.
Preferably, in the step (3), the total amount of the dispersion system is calculated according to the solid content of the modified polypropylene in the dispersion system of the modified polyacrylic acid in the step (1), and the mass of the modified polypropylene in the system formed by mixing the aqueous solution and the dispersion system in the step (3) is the formula amount.
Preferably, in the step (1), the reaction temperature after adding the sodium bisulfite is 5-25 ℃, preferably 10 ℃;
preferably, in the step (1), the reaction time after the sodium bisulfite is added is 1-2 h;
preferably, in the step (1), the temperature is raised to 40-60 ℃;
preferably, in the step (1), the reaction time of the reaction of adding the azobisisobutyronitrile hydrochloride is 2-4 h;
preferably, in the step (2), the mass ratio of the sodium laureth sulfate to the sodium stearate is 1: 2-3;
preferably, in the step (2), the mass of the water is 5-10 times of the total mass of the sodium citrate, the sodium salicylate, the sodium laureth sulfate, the sodium stearate and the sodium phenolsulfonate;
preferably, in step (2), the dissolving is carried out at 50-70 ℃;
preferably, in the step (3), the stirring is carried out at the rotation speed of 1000-2000rpm and the temperature of 50-70 ℃;
preferably, in the step (3), the frequency of the ultrasonic wave is 80-100KHZ, the power is 400-600W, and the ultrasonic wave is performed for 20-40 min.
Compared with the prior art, the invention has the technical advantages that:
(1) the acidic color fixing agent provided by the invention has good working solution pH value control capability, does not need to adjust acid, and keeps the pH value of the cloth surface of the treated fabric in a proper range; meanwhile, the color fixing effect is good, and various fastnesses such as washing fastness, perspiration fastness and seawater fastness can be obviously improved;
(2) the color change of the treated fabric has little influence, and the original color of the fabric is basically not influenced; the influence on the hand feeling of the fabric is small, and particularly, the influence on the hand feeling of the processed fabric by the sizing/pressing die is small;
(3) the use method of the acidic color fixing agent provided by the invention is simple to operate, and the risk of color fixing spots caused by acid adjustment is avoided;
(4) the product is in a liquid state, can be directly used, and does not generate the problem of color fixation spots caused by uneven material melting of a powdery color fixing agent;
(5) the sodium citrate, the sodium salicylate, the sodium laureth sulfate and the sodium stearate in the system have a good effect on regulating and controlling the pH value of the system under the synergistic effect, and the color fixing agent system can also have good performance and storage stability;
(6) according to the invention, the polyacrylic acid is modified and then is cooperated with polyethyleneimine, a film with a net structure can be formed on the surface of the fiber, the dye is coated in the film, the dissolution and the falling of the dye are reduced, the film formed on the surface of the fiber is soft and smooth, the friction coefficient of the surface is reduced, and the friction fastness is improved;
(7) on the other hand, the modified polyacrylic acid and the dye anion group promote the dye molecules to diffuse into the fiber under the action of electrostatic repulsion: the dye desorbed from the inside of the fiber is inhibited from diffusing to the outside of the fiber, pores for re-dissolving the dye are prevented, the damage of ionic bonds between the dye and the fiber is prevented, the dye is firmly attached to the fiber, and the capability of keeping the original state of the dye in the fiber under the action of external conditions is improved.
Detailed Description
Example 1
In this embodiment, the acidic color fixing agent comprises the following components in parts by weight: 15 parts of polyethyleneimine, 70 parts of modified polyacrylic acid, 15 parts of sodium citrate, 10 parts of sodium salicylate, 3 parts of sodium laureth sulfate, 9 parts of sodium stearate and 5 parts of sodium phenolsulfonate.
In this embodiment, the modified polyacrylamide comprises the following raw materials in parts by weight: 20 parts of methacrylic acid, 3 parts of 2-acrylamide-2-methyl propyl sodium sulfonate, 0.07 part of sodium bisulfite, 0.08 part of ammonium persulfate, 0.015 part of azobisisobutyrimidazoline hydrochloride, 6 parts of a dispersing agent, 35 parts of ammonium sulfate and 85 parts of water.
Preparation of the dispersant:
selecting raw materials: the dispersing agent comprises the following raw materials in parts by weight: 6 parts of methacrylic acid, 94 parts of water and 0.03 part of azobisisobutylimidazoline hydrochloride.
The preparation method of the dispersant comprises the following steps: dissolving methacrylic acid in water of 50 ℃, adding azobisisobutyrimidazoline hydrochloride to react to prepare polymethacrylic acid, namely the dispersing agent.
The preparation method of the acidic fixing agent in this embodiment includes the following steps:
(1) dissolving methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid sodium salt in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, controlling the reaction temperature to be 10 ℃, reacting for 1 hour, heating to 50 ℃, adding azodiisobutyl imidazoline hydrochloride, and reacting for 4 hours to prepare a dispersion system of modified polyacrylic acid;
(2) putting sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate into 8 times of water by mass, dissolving at 60 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and (3) mixing the aqueous solution with the dispersion system, stirring at 1500rpm and 60 ℃, and carrying out ultrasonic treatment for 30min at 80KHZ and 400W of power to obtain the acidic color fixing agent.
Example 2
In this embodiment, the acidic color fixing agent comprises the following components in parts by weight: 10 parts of polyethyleneimine, 60 parts of modified polyacrylic acid, 10 parts of sodium citrate, 5 parts of sodium salicylate, 1 part of sodium laureth sulfate, 2 parts of sodium stearate and 1 part of sodium phenolsulfonate.
In this embodiment, the modified polyacrylamide comprises the following raw materials in parts by weight: 10 parts of methacrylic acid, 1 part of 2-acrylamide-2-methyl propyl sodium sulfonate, 0.1 part of sodium bisulfite, 0.1 part of ammonium persulfate, 0.01 part of azobisisobutyrimidazoline hydrochloride, 5 parts of a dispersing agent, 30 parts of ammonium sulfate and 80 parts of water.
Preparation of the dispersant:
selecting raw materials: the dispersing agent comprises the following raw materials in parts by weight: 5 parts of methacrylic acid, 95 parts of water and 0.02 part of azobisisobutylimidazoline hydrochloride.
The preparation method of the dispersant comprises the following steps: dissolving methacrylic acid in water at 60 ℃, adding azobisisobutylimidazoline hydrochloride to react to prepare the polymethacrylic acid, namely the dispersing agent.
The preparation method of the acidic fixing agent in this embodiment includes the following steps:
(1) dissolving methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid sodium salt in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, controlling the reaction temperature to be 5 ℃, reacting for 1 hour, heating to 40 ℃, adding azodiisobutyl imidazoline hydrochloride, and reacting for 4 hours to prepare a dispersion system of modified polyacrylic acid;
(2) putting sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate into 5 times of water by mass, dissolving at 50 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and (3) mixing the aqueous solution with the dispersion system, stirring at 1000rpm and 50 ℃, and carrying out ultrasonic treatment for 20min at 80KHZ and 400W of power to obtain the acidic color fixing agent.
Example 3
In this embodiment, the acidic color fixing agent comprises the following components in parts by weight: 20 parts of polyethyleneimine, 90 parts of modified polyacrylic acid, 20 parts of sodium citrate, 15 parts of sodium salicylate, 5 parts of sodium laureth sulfate, 10 parts of sodium stearate and 6 parts of sodium phenolsulfonate.
In this embodiment, the modified polyacrylamide comprises the following raw materials in parts by weight: 30 parts of methacrylic acid, 5 parts of 2-acrylamide-2-methyl propyl sodium sulfonate, 0.05 part of sodium bisulfite, 0.05 part of ammonium persulfate, 0.02 part of azobisisobutyrimidazoline hydrochloride, 10 parts of a dispersing agent, 40 parts of ammonium sulfate and 90 parts of water.
Preparation of the dispersant:
selecting raw materials: the dispersing agent comprises the following raw materials in parts by weight: 10 parts of methacrylic acid, 90 parts of water and 0.05 part of azobisisobutylimidazoline hydrochloride.
The preparation method of the dispersant comprises the following steps: dissolving methacrylic acid in water at 40 ℃, adding azobisisobutyrimidazoline hydrochloride to react to prepare polymethacrylic acid, namely the dispersing agent.
The preparation method of the acidic fixing agent in this embodiment includes the following steps:
(1) dissolving methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid sodium salt in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, controlling the reaction temperature to be 25 ℃, reacting for 1 hour, heating to 60 ℃, adding azodiisobutyl imidazoline hydrochloride, and reacting for 2 hours to prepare a dispersion system of modified polyacrylic acid;
(2) putting sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate into 5-10 times of water by mass, dissolving at 70 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and (3) mixing the aqueous solution with the dispersion system, stirring at 2000rpm and 70 ℃, and carrying out ultrasonic treatment for 40min at 100KHZ and 600W to obtain the acidic color fixing agent.
Example 4
In this embodiment, the acidic color fixing agent comprises the following components in parts by weight: 18 parts of polyethyleneimine, 80 parts of modified polyacrylic acid, 20 parts of sodium citrate, 5 parts of sodium salicylate, 1 part of sodium laureth sulfate, 3 parts of sodium stearate and 2 parts of sodium phenolsulfonate.
In this embodiment, the modified polyacrylamide comprises the following raw materials in parts by weight: 10 parts of methacrylic acid, 5 parts of 2-acrylamide-2-methyl propyl sodium sulfonate, 0.1 part of sodium bisulfite, 0.1 part of ammonium persulfate, 0.01 part of azobisisobutyrimidazoline hydrochloride, 5 parts of a dispersing agent, 40 parts of ammonium sulfate and 90 parts of water.
Preparation of the dispersant:
selecting raw materials: the dispersing agent comprises the following raw materials in parts by weight: 10 parts of methacrylic acid, 90 parts of water and 0.02 part of azobisisobutylimidazoline hydrochloride.
The preparation method of the dispersant comprises the following steps: dissolving methacrylic acid in water at 60 ℃, adding azobisisobutylimidazoline hydrochloride to react to prepare the polymethacrylic acid, namely the dispersing agent.
The preparation method of the acidic fixing agent in this embodiment includes the following steps:
(1) dissolving methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid sodium salt in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, controlling the reaction temperature to be 5 ℃, reacting for 2 hours, heating to 40 ℃, adding azodiisobutyl imidazoline hydrochloride, and reacting for 4 hours to prepare a dispersion system of modified polyacrylic acid;
(2) putting sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate into 5 times of water by mass, dissolving at 50 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and (3) mixing the aqueous solution with the dispersion system, stirring at 2000rpm and 70 ℃, and carrying out ultrasonic treatment for 40min at 100KHZ and 400W of power to obtain the acidic color fixing agent.
Comparative example 1
The difference compared to example 1 is that only polyacrylic acid is commercially available polyacrylic acid (Changzhou source spring red light chemical Co., Ltd.);
in this embodiment, the acidic color fixing agent comprises the following components in parts by weight: 15 parts of polyethyleneimine, 70 parts of polyacrylic acid, 15 parts of sodium citrate, 10 parts of sodium salicylate, 3 parts of sodium laureth sulfate, 9 parts of sodium stearate and 5 parts of sodium phenolsulfonate.
The preparation method of the acidic fixing agent in this embodiment includes the following steps:
(1) dissolving polyacrylic acid in water to prepare a polyacrylic acid dispersion system;
(2) putting sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate into 8 times of water by mass, dissolving at 60 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and (3) mixing the aqueous solution with the dispersion system, stirring at 1500rpm and 60 ℃, and carrying out ultrasonic treatment for 30min at 80KHZ and 400W of power to obtain the acidic color fixing agent.
Comparative example 2
The difference compared with example 1 is that sodium laureth sulfate is not contained.
The acidic color fixing agent in the embodiment comprises the following components in parts by weight: 15 parts of polyethyleneimine, 70 parts of modified polyacrylic acid, 15 parts of sodium citrate, 10 parts of sodium salicylate, 9 parts of sodium stearate and 5 parts of sodium phenolsulfonate.
In this example, the preparation raw materials of the modified polyacrylamide are the same as those in example 1.
The dispersant was prepared as in example 1:
the preparation method of the acidic color fixing agent comprises the following steps:
(1) the same as example 1;
(2) putting sodium citrate, sodium salicylate, sodium stearate and sodium phenolsulfonate into water with the mass of 8 times of that of the sodium citrate, dissolving at 60 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) the same as in example 1.
Comparative example 3
The difference compared to example 1 is that sodium citrate is not present.
The acidic color fixing agent in the embodiment comprises the following components in parts by weight: 15 parts of polyethyleneimine, 70 parts of modified polyacrylic acid, 10 parts of sodium salicylate, 3 parts of sodium laureth sulfate, 9 parts of sodium stearate and 5 parts of sodium phenolsulfonate.
In this example, the modified polyacrylamide was prepared according to the same method as in example 1.
The dispersant was prepared as in example 1:
the preparation method of the acidic color fixing agent comprises the following steps:
(1) dissolving methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid sodium salt in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, controlling the reaction temperature to be 10 ℃, reacting for 1 hour, heating to 50 ℃, adding azodiisobutyl imidazoline hydrochloride, and reacting for 4 hours to prepare a dispersion system of modified polyacrylic acid;
(2) putting sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate into 8 times of water by mass, dissolving at 60 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and (3) mixing the aqueous solution with the dispersion system, stirring at 1500rpm and 60 ℃, and carrying out ultrasonic treatment for 30min at 80KHZ and 400W of power to obtain the acidic color fixing agent.
Comparative example 4
Compared with the example 1, the difference is that the sodium laureth sulfate and the sodium citrate are not contained at the same time.
The acidic color fixing agent in the embodiment comprises the following components in parts by weight: 15 parts of polyethyleneimine, 70 parts of modified polyacrylic acid, 10 parts of sodium salicylate, 9 parts of sodium stearate and 5 parts of sodium phenolsulfonate.
In this example, the preparation raw materials of the modified polyacrylamide are the same as those in example 1.
The dispersant was prepared as in example 1:
the preparation method of the acidic color fixing agent comprises the following steps:
(1) the same as example 1;
(2) putting sodium salicylate, sodium stearate and sodium phenolsulfonate into water with the mass of 8 times of that of the sodium salicylate, the sodium stearate and the sodium phenolsulfonate, dissolving at 60 ℃, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) the same as in example 1.
Examples of effects
1. Color fastness test
The test method comprises the following steps: dipping treatment is carried out on black superfine brocade/ammonia for 20min under the condition of 80 ℃ by respectively using 3 percent (o.w.f) of different color fixing agents. After the treated fabrics are washed by cold water and dried at 105 ℃, the color change condition, the washing fastness (AATCC-61-2A) and the cloth cover pH value (GB/T-7573-.
The formula is as follows: 3% of a color fixing agent; fabric: black ultra-fine nylon/polyurethane cloth; the process comprises the following steps: 80 ℃ for 20min, wherein the standard sample is a fabric which is not subjected to fixation treatment.
TABLE 1 color change, washing fastness and cloth cover pH value of brocade/ammonia fabric with different colors after color fixation
It can be seen from this that: the acidic color fixing agent prepared by the invention has good color fixing effect, and the treated fabric has no color change and no risk of low pH value.
2. Hand feeling test
After the acid fixing agents prepared in examples 1-4 and comparative examples 1-4 were fixed to different fabrics, 10 consumers were randomly selected and rated for different fabrics after being fixed with different fixing agents, 100 being the best (not hard as standard), and 0 being the worst (hardest). The average was taken to obtain the score results, see table 2.
Table 2 the effect on feel of different fabrics after fixation with different fixing agents was scored as follows:
as can be seen from the above table: the acidic color fixing agent prepared by the invention has small influence on the hand feeling of the fabric after color fixing, and the prepared raw materials have large influence on the performance of the fabric.
3. Hardness ion resistance profiles of the fixing agents prepared in examples 1-4 and comparative examples 1-4:
the test method comprises the following steps: using working solution of dyeing residual liquid (acid dye 1% (o.w.f)), preparing color fixing working solution with different acid color fixing agents of 2% (o.w.f) +400 and 600ppm hardness, adding white nylon-ammonia cloth with the same weight, and treating for 20min at 80 ℃ in a sample dyeing machine. And (3) washing the treated fabric with cold water, and drying at 105 ℃, and observing the color fixing spot condition of the cloth surface of the treated fabric.
The formula is as follows: 2% of color fixing agent and 1% of dye; fabric: white nylon ammonia cloth; the process comprises the following steps: at 80 deg.C for 20min
TABLE 3 hardness ion tolerance of the fixing Agents
| Test group | Number of fixation spots of 400ppm | Number of fixation spots of 600ppm |
| Standard sample | No color fixing spot | Fixing color spot in minute amount |
| Example 1 | No color fixing spot | Fixing color spot in minute amount |
| Example 2 | No color fixing spot | Fixing color spot in minute amount |
| Example 3 | No color fixing spot | Fixing color spot in minute amount |
| Example 4 | No color fixing spot | Fixing color spot in minute amount |
| Comparative example 1 | Little fixed color spot | A large number of fixation spots |
| Comparative example 2 | Little fixed color spot | A large number of fixation spots |
| Comparative example 3 | Little fixed color spot | A large number of fixation spots |
| Comparative example 4 | A large number of fixation spots | A large number of fixation spots |
As can be seen from the above table: the acidic color fixing agent prepared by the invention has a good shielding effect on color fixing spots caused by hardness ions.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
1. An acidic fixing agent comprises the following components: polyethyleneimine, modified polyacrylic acid, sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate and sodium phenolsulfonate.
2. The acidic fixing agent according to claim 1, comprising the following components in parts by weight: 10-20 parts of polyethyleneimine, 60-90 parts of modified polyacrylic acid, 10-20 parts of sodium citrate, 5-15 parts of sodium salicylate, 1-5 parts of sodium laureth sulfate, 1-10 parts of sodium stearate and 1-6 parts of sodium phenolsulfonate.
3. The acidic fixing agent according to any one of claims 1 or 2, wherein the modified polyacrylamide is prepared from the following raw materials: methacrylic acid, 2-acrylamide-2-methyl sodium propyl sulfonate, sodium bisulfite, ammonium persulfate, azobisisobutyrimidazoline hydrochloride, a dispersing agent, ammonium sulfate and water.
4. The acidic color fixing agent of claim 3, wherein the modified polyacrylamide is prepared from the following raw materials in parts by weight: 10-30 parts of methacrylic acid, 1-5 parts of 2-acrylamide-2-methylpropanesulfonic acid sodium salt, 0.05-0.1 part of sodium bisulfite, 0.05-0.1 part of ammonium persulfate, 0.01-0.02 part of azobisisobutyrimidazoline hydrochloride, 5-10 parts of a dispersing agent, 30-40 parts of ammonium sulfate and 80-90 parts of water.
5. The acidic fixing agent of claim 4, wherein the dispersant is prepared from the following raw materials: methacrylic acid, water and azobisisobutyrimidazoline hydrochloride.
6. The acidic fixing agent according to claim 5, wherein the dispersant is prepared by: dissolving methacrylic acid in water at 40-60 ℃, adding azobisisobutyronitrile hydrochloride for reaction to prepare polymethacrylic acid, namely the dispersant.
7. A process for the preparation of an acidic fixing agent according to any of claims 3 to 6 comprising the steps of:
(1) dissolving methacrylic acid and 2-acrylamide-2-methyl sodium propanesulfonate in water, adding ammonium persulfate, a dispersing agent, introducing nitrogen, adding sodium bisulfite, reacting, heating, adding azodiisobutyl imidazoline hydrochloride, and reacting to obtain a dispersion system of modified polyacrylic acid;
(2) dissolving sodium citrate, sodium salicylate, sodium laureth sulfate, sodium stearate, and sodium phenolsulfonate in water, and adding polyethyleneimine under stirring; preparing an aqueous solution;
(3) and mixing the aqueous solution with the dispersion system, stirring and carrying out ultrasonic treatment to obtain the acidic color fixing agent.
8. The method for preparing the acidic fixing agent according to claim 7, wherein in the step (3), the total amount of the dispersion system is calculated according to the solid content of the modified polypropylene in the dispersion system of the modified polyacrylic acid in the step (1), and the mass of the modified polypropylene in the system obtained by mixing the aqueous solution in the step (3) with the dispersion system is the formula amount.
9. The process for preparing an acidic fixing agent according to claim 7, wherein in step (1), the reaction temperature after the addition of sodium bisulfite is 5 to 25 ℃.
10. The method for preparing the acidic color fixing agent according to claim 7, wherein in the step (2), the mass ratio of the sodium laureth sulfate to the sodium stearate is 1: 2-3.
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