Synthesis process of color fixing agent for cotton

Abstract

The invention relates to a synthesis process of a color fixing agent for cotton, which comprises the following steps: uniformly stirring dimethyl diallyl ammonium chloride, pure water and sodium carbonate under the condition of nitrogen protection, heating to 56-59 DEG C, and adding ammonium persulfate and anhydrous sodium sulfite in batches; after the last batch of ammonium persulfate and anhydrous sodium sulfite are added, the temperature is increased to 75-78 DEG C, stirring and heat preservation reaction are performed, stirring and cooling are performed after the reaction is finished, an acidic material is added, uniform stirring is performed to obtain a color fixing agent precursor, and finally the color fixing agent precursor and a nano material are subjected to ultrasonic dispersion to obtain the color fixing agent for cotton. The nano material is a compound of nano silicon dioxide and nano aluminum oxide. The color fixing agent for cotton synthesized by the synthesis process of the color fixing agent for cotton not only can improve soaping fastness, rubbing fastness, washing fastness and perspiration fastness of cotton fabrics, but also does not affect the hand feeling of the cotton fabrics.

Description

Technical Field

[0001] The invention belongs to the technical field of color fixing agents, and particularly relates to a synthesis process of a color fixing agent for cotton. Background Art

[0002] The cotton textile processing process needs to go through desizing, refining, bleaching, dyeing, and finishing processes. Among them, the dyeing process is very important. Some cotton fabrics can obtain relatively bright colors through the action of dyes, but due to the effect of oxygen in the air or the influence of humidity, the dye in the fabric will fall off the dyed fabric, causing the fabric to fade, stain, and color transfer, etc. Therefore, in the dyeing process, it is generally necessary to add a certain amount of fixing agent to enhance the fastness of the pigment on the fabric.

[0003] Chinese patent CN201710794464.8 discloses a method for preparing a cotton fabric fixing agent, which comprises the following raw materials in parts by weight: 8-10 parts of diethylenetriamine, 5-7 parts of hydroquinone, 3-5 parts of acetic acid, 3-5 parts of triethylenetetramine, 3-5 parts of epichlorohydrin, 5-10 parts of dicyandiamide, 10-15 parts of acrylate, 3-5 parts of sodium hexametaphosphate, 3-5 parts of polyethylene glycol, and 20-30 parts of deionized water. After the cotton fabric fixing agent of the present invention is applied, the soaping fastness of the dyed fabric can reach level 4-5, and the rubbing fastness reaches level 4-5; however, its feel and perspiration fastness are not significantly improved.

[0004] Chinese patent CN201310609867.2 discloses a formaldehyde-free fabric fixing agent and its preparation method. The fixing agent comprises the following components, by weight: 15-25 parts n-butyl acrylate, 5-9 parts chitosan quaternary ammonium salt, 6-10 parts isobornyl methacrylate, 7-14 parts acryloyloxyethyltrimethylammonium chloride, 8-10 parts triallylamine, 2-5 parts organosiloxane, 3-5 parts glacial acetic acid, 0.1-1 part azobisisobutylcyanide, and 100-120 parts deionized water. The preparation process is simple, and the resulting fixing agent is formaldehyde- and APEO-free. The fixing agent electrostatically bonds between the cationic groups in the fixing agent molecules and the anionic groups in the dye, forming an insoluble color lake on the fabric surface. This in turn blocks the dye's water-soluble groups, thereby improving the dyed fabric's wash fastness. However, the fabric's hand, rubbing fastness, and perspiration fastness are not significantly improved. Summary of the Invention

[0005] The purpose of the present invention is to provide a synthesis process of a cotton color fixing agent. The synthesized cotton color fixing agent can not only improve the soaping fastness, rubbing fastness, washing fastness and perspiration fastness of cotton fabrics, but also does not affect the hand feel of the cotton fabrics.

[0006] The technical solution adopted by the present invention to solve the above-mentioned problem is: a synthesis process of a cotton color fixing agent, comprising the following steps: under nitrogen protection, dimethyldiallylammonium chloride, pure water, and soda ash are uniformly stirred, and at the same time, ammonium persulfate and anhydrous sodium sulfite are added in batches when the temperature is raised to 56°C to 59°C; after the last batch of ammonium persulfate and anhydrous sodium sulfite is added, the temperature is raised to 75°C to 78°C, stirred and kept for reaction; after the reaction is completed, the temperature is cooled with stirring, an acidic substance is added and stirred uniformly to obtain a color fixing agent precursor; and finally, the color fixing agent precursor and nanomaterial are ultrasonically dispersed to obtain the cotton color fixing agent. The nano material is a compound of nano silicon dioxide and nano aluminum oxide.

[0007] Preferably, the mass ratio of the dimethyldiallylammonium chloride, pure water and soda ash is 680-700:190-210:0.4-0.6.

[0008] Preferably, the mass ratio of dimethyldiallylammonium chloride:ammonium persulfate:anhydrous sodium sulfite is 680-700:0.8-1.6:0.4-1.2.

[0009] Preferably, the insulation reaction time is 8 to 10 hours.

[0010] Preferably, after the reaction is completed, the mixture is stirred and cooled to 45°C to 50°C.

[0011] Preferably, the acidic substance is hydrochloric acid.

[0012] Preferably, the mass ratio of the fixing agent precursor to the nanomaterial is 10:1 to 1.5.

[0013] Preferably, ammonium persulfate and anhydrous sodium sulfite are added in four batches, and the amount of ammonium persulfate and anhydrous sodium sulfite added in each batch is the same.

[0014] Preferably, the mass ratio of the nano-silicon dioxide to the nano-alumina is 1-2:1-2. The particle size of the nano-silicon dioxide is 100-300 nm, and the particle size of the nano-alumina is 50-100 nm.

[0015] Compared with the prior art, the advantages of the present invention are: (1) In the synthesis process of the cotton color fixing agent of the present invention, ammonium persulfate and anhydrous sodium sulfite are added in batches, which can not only effectively control the reaction rate and avoid excessive heat or by-products generated by violent reactions, but also form a more uniform cross-linked structure, improve the performance of the color fixing agent, increase the binding force with cotton fibers, and improve the soaping fastness, rubbing fastness, and washing fastness of cotton fabrics.

[0016] (2) A compound of nano-silica and nano-alumina is added to the synthesis process of the cotton color fixing agent of the present invention. The nanoparticles fill the tiny pores between the curing agent and the fiber to form a dense nano-composite layer, which has a good mechanical strengthening effect and can significantly improve the friction fastness, water washing fastness and soaping fastness without significantly affecting the hand feel. Among them, the hydroxyl groups on the surface of nano-silica can form hydrogen bonds or covalent bonds with the hydroxyl groups in the cotton fiber, thereby enhancing the wear resistance of the fiber. Nano-alumina can enhance the wear resistance and tear resistance of cotton fiber. Nano-alumina has a strong adsorption capacity and can form a stable composite structure with the active sites in the cotton fiber. DETAILED DESCRIPTION

[0017] The present invention is described in further detail below with reference to the examples. Example 1

[0018] A process for synthesizing a cotton color fixing agent comprises the following steps: Under nitrogen protection, 690 grams of dimethyldiallylammonium chloride, 200 grams of pure water, and 0.5 grams of soda ash were stirred evenly. At the same time, when the temperature was raised to 58°C, ammonium persulfate and anhydrous sodium sulfite were added in four batches, with the addition amounts of ammonium persulfate and anhydrous sodium sulfite in each batch being 0.3 grams and 0.2 grams, respectively. After the last batch of ammonium persulfate and anhydrous sodium sulfite were added, the temperature was raised to 78°C, stirred and kept warm for 8 hours. After the reaction was completed, the temperature was stirred and cooled to 45°C. 0.6 grams of hydrochloric acid was added and stirred evenly to obtain a fixing agent precursor. Finally, the fixing agent precursor and the nanomaterial were ultrasonically dispersed to obtain a cotton fixing agent, wherein the mass ratio of the fixing agent precursor to the nanomaterial was 10:1, and the nanomaterial was nano-silica (particle size of 100 nm) and nano-alumina (particle size of 100 nm) with a mass ratio of 1:1. Example 2

[0019] A process for synthesizing a cotton color fixing agent comprises the following steps: Under nitrogen protection, 690 grams of dimethyldiallylammonium chloride, 200 grams of pure water, and 0.5 grams of soda ash were stirred evenly. At the same time, when the temperature was raised to 59°C, ammonium persulfate and anhydrous sodium sulfite were added in four batches, with the addition amounts of ammonium persulfate and anhydrous sodium sulfite in each batch being 0.3 grams and 0.2 grams, respectively. After the last batch of ammonium persulfate and anhydrous sodium sulfite were added, the temperature was raised to 77°C, stirred and kept warm for 9 hours, and after the reaction was completed, the temperature was stirred and cooled to 48°C. 0.6 grams of hydrochloric acid was added and stirred evenly to obtain a fixing agent precursor. Finally, the fixing agent precursor and the nanomaterial were ultrasonically dispersed to obtain a cotton fixing agent, wherein the mass ratio of the fixing agent precursor to the nanomaterial was 10:1.2, and the nanomaterial was nano-silica (particle size of 100 nm) and nano-alumina (particle size of 100 nm) with a mass ratio of 1:2.

[0020] Comparative Example 1 The only difference from Example 1 is that no nanomaterial is added.

[0021] Comparative Example 2 The only difference from Example 1 is that all the nanomaterials are nano-silicon dioxide, that is, nano-aluminum oxide is replaced by nano-silicon dioxide.

[0022] Comparative Example 3 The only difference from Example 1 is that all the nanomaterials are nano-alumina, that is, nano-silicon dioxide is replaced by nano-alumina.

[0023] Comparative Example 4 The only difference from Example 1 is that the nanomaterials are nano-silicon dioxide and nano-aluminum oxide in a mass ratio of 1:5.

[0024] The performance tests of Examples 1-2 and Comparative Examples 1-4 were carried out, as shown below: Pure cotton fabric: The pure cotton fabric dyed with acid dye (red, dye concentration is 8%) was twice dipped and twice rolled. The amount of fixing agent used was 40g / L, the rolling rate was 85%, and the fabric was pre-baked for 2 minutes at a pre-baking temperature of 85°C. The fabric was baked 3 times at a baking temperature of 160°C for 2 minutes.

[0025] (1) Washing fastness: Determined according to GB / T3921-2008 "Textiles - Tests for colour fastness: Washing fastness"; (2) Rubbing fastness: Determined according to GB / T3920-2008 "Textiles - Tests for colour fastness: Rubbing fastness"; (3) Perspiration fastness: tested according to GB / T3922-1995; (4) Washing fastness: tested according to ISO 105-C03-1989, specifically: formula: ECE 4g / L + Na2CO3 1g / L; process: 60℃×30min; (5) Hand feel test: Touch the finished fabric with eyes closed, and grade it in groups of 10. The printed fabric will be graded based on different hand feels. The specific evaluation method is: grade the hand feel based on softness and smoothness, with a total of 5 levels. Level 1 is the worst, the fabric feels hard and has a poor smoothness, and level 5 is the best, the fabric feels soft and smooth.

[0026] The performance test results of Examples 1-2 and Comparative Examples 1-4 are shown in Table 1: Table 1 Performance test results of Examples 1-2 and Comparative Examples 1-4

[0027] In addition to the above embodiments, the present invention also includes other implementation methods. Any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of protection of the claims of the present invention.

Claims

1. A synthesis process of a cotton fixing agent, characterized in that: The following steps are involved: Under the protection of nitrogen, dimethyldiallylammonium chloride, pure water and soda ash are stirred evenly, and when the temperature is raised to 56°C-59°C, ammonium persulfate and anhydrous sodium sulfite are added in batches; after the last batch of ammonium persulfate and anhydrous sodium sulfite are added, the temperature is raised to 75°C-78°C, stirred and kept warm for reaction, stirred and cooled after the reaction is completed, an acidic substance is added and stirred evenly to obtain a color fixing agent precursor, and finally the color fixing agent precursor and the nanomaterial are ultrasonically dispersed to obtain a color fixing agent for cotton; The nano material is a compound of nano silicon dioxide and nano aluminum oxide.

2. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: The mass ratio of the dimethyldiallylammonium chloride, pure water and soda ash is 680-700:190-210:0.4-0.

6.

3. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: The mass ratio of the dimethyldiallylammonium chloride:ammonium persulfate:anhydrous sodium sulfite is 680-700:0.8-1.6:0.4-1.

2.

4. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: The heat preservation reaction time is 8 to 10 hours.

5. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: The acidic substance is hydrochloric acid.

6. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: Ammonium persulfate and anhydrous sodium sulfite were added in four batches, and the amount of ammonium persulfate and anhydrous sodium sulfite added in each batch was the same.

7. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: The mass ratio of the color fixing agent precursor to the nano material is 10:1-1.

5.

8. The synthesis process of the cotton color fixing agent according to claim 1, characterized in that: The mass ratio of the nano silicon dioxide to the nano aluminum oxide is 1-2:1-2.

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