Cationic dye dyeing method based on polyamide-imide powder

Abstract

The invention discloses a cationic dye dyeing method based on polyamideimide powder. The cationic dye dyeing method specifically comprises the following steps: step 1, pretreating the polyamideimide powder; and step 2, putting the polyamide-imide powder treated in the step 1 into dye liquor for dyeing, putting the dyed polyamide-imide powder into soaping liquor containing a washing powder solution for soaping so as to remove residual dye and oil stains on the surface of the fabric, and drying after cleaning is completed. According to the invention, the problem that polyamide-imide powder is difficult to dye is solved, and the stability of the polyamide-imide structure can be ensured.

Description

Technical Field

[0001] The invention belongs to the technical field of dyeing and finishing of organic polymer materials, and relates to a cationic dye dyeing method based on polyamide-imide powder. Background Art

[0002] Polyamide-imide is an organic polymer material with excellent performance. It is a modified product of polyimide and has excellent heat resistance, corrosion resistance, high physical strength and low friction coefficient. It can remain stable at temperatures up to 350°C and is suitable for various harsh environments. Because of its unique properties, it has been widely used in industrial and high-tech fields such as high-temperature filtration materials, wear-resistant coatings, and electronic packaging materials. As a high-performance material, its molecular structure is very tight and its stereoregularity is very good. Because its powder itself is golden yellow and has a high glass transition temperature (about 300°C or above), it is difficult to dye under normal conditions.

[0003] There are few studies on the dyeing of polyamide-imide materials, most of which are studies on the dyeing of polyimide materials. Alkali pretreatment is an effective method for polyimide dyeing, and many studies have been conducted. After alkali treatment, anionic carboxyl groups are introduced on the surface of polyamide-imide, which can effectively increase the dye bit number of cationic dyes on polyamide-imide. However, alkali pretreatment will increase the roughness of the sample surface, destroy the original regular structure of polyamide-imide, and cause serious loss of structural strength.

[0004] Carrier dyeing is a dyeing method that uses small molecule compounds as carriers and has affinity for both dyes and fibers. During the dyeing process, the carrier small molecules will enter between the molecular chains of the dyeing target, cut off the interaction between the molecular chains, increase the distance between molecules, promote the dye to enter the fiber, and effectively increase the dye uptake rate. Summary of the invention

[0005] The object of the present invention is to provide a cationic dye dyeing method based on polyamideimide powder, which solves the problem of difficulty in dyeing polyamideimide powder and can ensure the stability of the polyamideimide structure.

[0006] The technical solution adopted by the present invention is a cationic dye dyeing method based on polyamide-imide powder, which specifically comprises the following steps: Step 1, pre-treating polyamide-imide powder; Step 2, putting the polyamide-imide powder treated in step 1 into a dyeing solution for dyeing, putting the dyed polyamide-imide powder into a soaping solution containing a washing powder solution for soaping to remove the dye and oil stains remaining on the surface of the fabric, and drying after washing.

[0007] The present invention is also characterized in that: The specific process of step 1 is: at room temperature, the polyamide-imide powder is put into a soaping liquid for soaping, and then dried after the washing is completed.

[0008] In step 1, the amount of polyamide-imide powder used is 1-20 g, the concentration of washing powder in the soaping liquid is 1-3 g / L, the soaping temperature is 50-90° C., the soaping time is 10-20 min; the drying temperature is 60-80° C., and the drying time is 8-16 h.

[0009] The specific process of step 2 is: Step 2.1, adding the polyamide-imide powder treated in step 1 into the dye solution, heating at a rate of 2°C / min during the heating process, the dyeing temperature is 80-140°C, and then keeping the temperature for 60 minutes; Step 2.2, stop heating and continue stirring, wait for the dye solution to cool to room temperature, then wash and dry, put the dyed polyamide-imide powder into soaping solution for soaping, and dry after soaping.

[0010] In step 2.1, the dye solution is prepared as follows: Add cationic dye, purified water and benzyl alcohol into a beaker, adjust the pH value of the solution to 3-6, stir evenly, and you will get the prepared dye solution.

[0011] In step 2.1, the mass ratio of polyamideimide powder to dye solution is 1:15-30; the mass of cationic dye is 1-5% of the mass of polyamideimide powder, and the concentration of benzyl alcohol is 10-60 g / L.

[0012] In step 2.2, the concentration of washing powder in the soaping liquid is 1-3 g / L, the mass of the soaping liquid is 30 times the mass of the powder used, the soaping temperature is 50-90° C., and the soaping time is 10-20 min.

[0013] In step 2.2, after dyeing, the drying temperature is 80-120° C. and the drying time is 8-16 hours.

[0014] The invention has the beneficial effects that the carrier dyeing method provided by the invention dyes polyamide-imide powder, adopts cationic red dye X-5GN, and uses benzyl alcohol as a carrier to dye the polyamide-imide powder, so as to achieve low-temperature polyamide-imide dyeing. The method is simple to operate, has low equipment requirements, has a high dye uptake rate of the obtained product, has a low reaction cost, has excellent thermal performance, and has a good reaction effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a dyeing flow chart of the cationic dye dyeing method based on polyamide-imide powder of the present invention; Figure 2It is the ultraviolet absorbance test of the residual dye solution after dyeing in Examples 1 to 6 of the cationic dye dyeing method based on polyamide-imide powder of the present invention; Figure 3 In Example 6 of the cationic dye dyeing method based on polyamide-imide powder of the present invention, the infrared test of the dyed sample and the undyed sample using the cationic red dye and benzyl alcohol as carriers; Figure 4 Thermogravimetric test of the sample after dyeing with cationic red dye and benzyl alcohol as carrier in Example 6 of the cationic dye dyeing method based on polyamide-imide powder of the present invention; Figure 5 This is a test chart of ultraviolet absorbance of a black sample dyed by a cationic dye dyeing method based on polyamide-imide powder of the present invention; Figure 6 This is a test chart of the ultraviolet absorbance of a brown sample dyed by the cationic dye dyeing method based on polyamide-imide powder of the present invention; Figure 7 This is a test chart of ultraviolet absorbance of a green sample dyed by a cationic dye dyeing method based on polyamide-imide powder of the present invention; Figure 8 This is a test chart of ultraviolet absorbance of a blue sample dyed by a cationic dye dyeing method based on polyamide-imide powder of the present invention; Fig. 9 It is a test chart of ultraviolet absorbance of a purple sample dyed by the cationic dye dyeing method based on polyamide-imide powder of the present invention. DETAILED DESCRIPTION

[0016] The present invention is described in detail below with reference to the accompanying drawings and specific embodiments.

[0017] The cationic dye dyeing method based on polyamide-imide powder of the present invention specifically comprises the following steps: Step 1, pretreatment: at room temperature, pretreat the polyamide-imide powder to clean and remove impurities; Specifically, the polyamide-imide powder is put into a soaping liquid containing washing powder for soaping, and then dried after washing.

[0018] In step 1, the amount of polyamide-imide powder used is 1-20 g, the concentration of washing powder in the soaping liquid is 1-3 g / L, the mass of the soaping liquid is 30 times the mass of the polyamide-imide powder used, the soaping temperature is 50-90° C., the soaping time is 10-20 min; the drying temperature is 60-80° C., and the drying time is 8-16 h.

[0019] Step 2, dyeing: the polyamide-imide powder that has been washed and dried is put into the prepared dye solution for dyeing, the temperature is increased at a rate of 2°C / min, the dyeing temperature is 80-140°C, and stirring is continued, then the temperature is kept for 60 minutes, the heating is stopped and stirring is continued to wait for it to slowly cool to room temperature, after the dyeing is completed, the dyed polyamide-imide powder is put into a soaping liquid containing a washing powder solution for soaping to remove the residual dye and oil on the surface of the fabric, and after washing, it is dried, and the dyeing is completed.

[0020] The mass ratio of polyamide-imide powder to the prepared dye solution is 1:15~30; The specific preparation process of the dye solution is: add a certain amount of cationic red dye, purified water and benzyl alcohol into a beaker to make a dye solution, then add acetic acid to adjust the pH value of the dye solution to 3-6, and then stir the dye solution for 30 minutes to mix it evenly.

[0021] The mass of the cationic dye is 1-5% of the mass of the polyamide-imide powder, and the concentration of benzyl alcohol is 10-60 g / L.

[0022] The concentration of washing powder in the soaping liquid is 1-3 g / L, the mass of the soaping liquid is 30 times the mass of the powder used, the soaping temperature is 50-90° C., and the soaping time is 10-20 minutes; after the end, the drying temperature is 80-120° C. and the drying time is 8-16 hours.

[0023] Example 1 The cationic dye dyeing method based on polyamide-imide powder of the present invention specifically comprises the following steps: Step 1: Under room temperature, weigh 60g of pure water and 0.18g of washing powder to prepare a soaping solution with a concentration of 3g / L. Put 2g of polyamide-imide powder into the soaping solution for soaping for 15min at a soaping temperature of 70°C. After soaping, dry in a hot air drying oven at 70°C for 12h.

[0024] Step 2, prepare the dye solution, add 0.08g of cationic red dye in a beaker, add 40g of pure water and 0.8g of benzyl alcohol, adjust the pH value of the dye solution to 3-4 with acetic acid, and then stir the dye solution for 30min to make its composition uniform, and the dye solution is prepared. The dried powder is mixed into the prepared dye solution, placed in a constant temperature magnetic stirring oil bath pot and placed with a magnetic stirring bar, slowly heated to 130°C, maintained at 130°C for 60 minutes and continuously stirred.

[0025] Step 3, stop heating and continue stirring until it slowly cools to room temperature, rinse and filter the polyamide-imide powder. Wash the filtered polyamide-imide powder in a soap solution with the same ingredients as in step 1. After washing, dry it in a hot air drying oven at 90°C for 12 hours.

[0026] Example 2 The cationic dye dyeing method based on polyamide-imide powder of the present invention specifically comprises the following steps: Step 1: Under room temperature, weigh 60g of pure water and 0.18g of washing powder to prepare a soaping solution with a concentration of 3g / L. Put 2g of polyamide-imide powder into the soaping solution for soaping for 15min at a soaping temperature of 70°C. After soaping, dry in a hot air drying oven at 70°C for 12h.

[0027] Step 2, prepare the dye solution, add 0.08g of cationic red dye in a beaker, add 40g of pure water and 1.2g of benzyl alcohol, adjust the pH value of the dye solution to 3-4 with acetic acid, and then stir the dye solution for 30min to make its components uniform, and the dye solution is prepared. The dried powder is mixed into the prepared dye solution, placed in a constant temperature magnetic stirring oil bath pot and placed with a magnetic stirring bar, slowly heated to 130°C, maintained at 130°C for 60 minutes and continuously stirred.

[0028] Step 3, stop heating and continue stirring until it slowly cools to room temperature, rinse and filter the polyamide-imide powder. Wash the filtered polyamide-imide powder in a soap solution with the same ingredients as in step 1. After washing, dry it in a hot air drying oven at 90°C for 12 hours.

[0029] Example 3 The cationic dye dyeing method based on polyamide-imide powder of the present invention specifically comprises the following steps: Step 1: Under room temperature, weigh 60g of pure water and 0.18g of washing powder to prepare a soaping solution with a concentration of 3g / L. Put 2g of polyamide-imide powder into the soaping solution for soaping for 15min at a soaping temperature of 70°C. After soaping, dry in a hot air drying oven at 70°C for 12h.

[0030] Step 2, prepare the dye solution, add 0.08g of cationic red dye in a beaker, add 40g of pure water and 1.6g of benzyl alcohol, adjust the pH value of the dye solution to 3-4 with acetic acid, and then stir the dye solution for 30min to make its components uniform, and the dye solution is prepared. The dried powder is mixed into the prepared dye solution, placed in a constant temperature magnetic stirring oil bath pot and placed with a magnetic stirring bar, slowly heated to 130°C, maintained at 130°C for 60 minutes and continuously stirred.

[0031] Step 3, stop heating and continue stirring until it slowly cools to room temperature, rinse and filter the polyamide-imide powder. Wash the filtered polyamide-imide powder in a soap solution with the same ingredients as in step 1. After washing, dry it in a hot air drying oven at 90°C for 12 hours.

[0032] Example 4 Step 1: Under room temperature, weigh 60g of pure water and 0.18g of washing powder to prepare a soaping solution with a concentration of 3g / L. Put 2g of polyamide-imide powder into the soaping solution for soaping for 15min at a soaping temperature of 70°C. After soaping, dry in a hot air drying oven at 70°C for 12h.

[0033] Step 2, prepare the dye solution, add 0.08g of cationic red dye in a beaker, add 40g of pure water and 2g of benzyl alcohol, adjust the pH value of the dye solution to 3-4 with acetic acid, and then stir the dye solution for 30min to make its components uniform, and the dye solution is prepared. The dried powder is mixed into the prepared dye solution, placed in a constant temperature magnetic stirring oil bath pot and placed with a magnetic stirring bar, slowly heated to 130°C, maintained at 130°C for 60 minutes and continuously stirred.

[0034] Step 3, stop heating and continue stirring until it slowly cools to room temperature, rinse and filter the polyamide-imide powder. Wash the filtered polyamide-imide powder in a soap solution with the same ingredients as in step 1. After washing, dry it in a hot air drying oven at 90°C for 12 hours.

[0035] Example 5 Step 1: Under room temperature, weigh 60g of pure water and 0.18g of washing powder to prepare a soaping solution with a concentration of 3g / L. Put 2g of polyamide-imide powder into the soaping solution for soaping for 15min at a soaping temperature of 70°C. After soaping, dry in a hot air drying oven at 70°C for 12h.

[0036] Step 2, prepare the dye solution, add 0.08g of cationic red dye in a beaker, add 40g of pure water and 1.6g of benzyl alcohol, adjust the pH value of the dye solution to 5-6 with acetic acid, and then stir the dye solution for 30min to make its components uniform, and the dye solution is prepared. The dried powder is mixed into the prepared dye solution, placed in a constant temperature magnetic stirring oil bath pot and placed with a magnetic stirring bar, slowly heated to 130°C, maintained at 130°C for 60 minutes and continuously stirred.

[0037] Step 3, stop heating and continue stirring until it slowly cools to room temperature, rinse and filter the polyamide-imide powder. Wash the filtered polyamide-imide powder in a soap solution with the same ingredients as in step 1. After washing, dry it in a hot air drying oven at 90°C for 12 hours.

[0038] Example 6 Step 1: Under room temperature, weigh 60g of pure water and 0.18g of washing powder to prepare a soaping solution with a concentration of 3g / L. Put 2g of polyamide-imide powder into the soaping solution for soaping for 15min at a soaping temperature of 70°C. After soaping, dry in a hot air drying oven at 70°C for 12h.

[0039] Step 2, prepare the dye solution, add 0.08g of cationic red dye in a beaker, add 60g of pure water and 1.6g of benzyl alcohol, adjust the pH value of the dye solution to 4-5 with acetic acid, and then stir the dye solution for 30 minutes to make its components uniform, and the dye solution is prepared. The dried powder is mixed into the prepared dye solution, placed in a constant temperature magnetic stirring oil bath pot and placed with a magnetic stirring bar, slowly heated to 130°C, maintained at 130°C for 60 minutes and continuously stirred.

[0040] Step 3, stop heating and continue stirring until it slowly cools to room temperature, rinse and filter the polyamide-imide powder. Wash the filtered polyamide-imide powder in a soap solution with the same ingredients as in step 1. After washing, dry it in a hot air drying oven at 90°C for 12 hours.

[0041] The dyeing rates of the samples after dyeing in the above-mentioned Examples 1 to 6 are shown in Table 1: Table 1 Dyeing rate of different examples

[0042] Figure 2 The UV absorption diagrams of the original dye solution and the dye solution after dyeing in Examples 1 to 6 at 400nm-600nm after dilution are shown in Figure 1. The dilution ratio is 115 times. According to the formula The dye uptake was calculated respectively (where A0 is the absorbance at the maximum absorption wavelength after the dye solution was diluted n times before dyeing, and A1 is the absorbance at the maximum absorption wavelength after the dye solution was diluted m times after dyeing), and the results are shown in Table 1. From the UV test results of the series of experiments from Example 1 to Example 6, it can be seen that the increase in the content of benzyl alcohol can greatly affect the dye uptake (other conditions being the same, the dye uptake is about 40% without using a dyeing carrier), indicating that the addition of benzyl alcohol carrier can increase the dye uptake of polyamide-imide powder, combine with more dyes, and achieve the purpose of dyeing. At the same time, different pH values ​​also have a certain effect on the dye uptake, and the dyeing effect is best when the pH value is 4-5.

[0043] The infrared test results of the undyed polyamide-imide powder and the powder after dyeing in Example 6 are as follows: Figure 3 As shown in the figure, they all have structures such as imide, amide, methylene and benzene ring. The intensity of the benzene ring skeleton vibration absorption peak after dyeing was observed to change, and at 1780 -1 , 1660 -1 The characteristic peak at 1375 -1 and 1720 -1 The peak at gradually moves to 1373 -1 and 1718 -1The results showed that after dyeing, the surface of the PAI structure was slightly hydrolyzed, but the molecular structure of polyamide-imide was not affected.

[0044] Example 6 Thermogravimetric test after dyeing Figure 4 As shown, from Figure 4 It can be seen that the polyamide-imide powder treated with 130°C carrier dyeing can remain stable before 400°C (the weight loss corresponding to 170°C is the incompletely dried water and aprotic polar solvent). When the gas temperature reaches about 527°C, the weight loss is obvious. When the temperature reaches the set maximum temperature of 800°C, the weight loss rate reaches 44.18%. The figure shows that the thermal stability of polyamide-imide itself is not greatly affected after dyeing by this method, and it can still maintain excellent thermal stability.

[0045] Five different colors of polyamide-imide powders were synthesized using the dyeing method proposed in Example 6 and different cationic dyes. The ultraviolet absorption graphs of the dye solutions of the five color samples at 400nm-600nm after being diluted by the same multiple are as follows: Figures 5 to 9 As shown ( Figures 5 to 9 The best dye uptake parameter obtained by the cationic dye dyeing method based on polyamide-imide powder of the present invention, using benzyl alcohol as a carrier, and using the ultraviolet absorbance test of samples dyed with different types of cationic dyes), the dye uptake is above 70%. Figure 5 For black samples, use cationic black CX-2GL; Figure 6 For brown samples, use cationic black XO; Figure 7 For green samples, use Cationic Blue X-BL and Cationic Yellow X-8GL; Figure 8 For blue samples, use Cationic Blue X-BL; Fig. 9 For the purple sample, use Cationic Brilliant Violet X-5BLH.

Claims

1. A cationic dye dyeing method based on polyamide-imide powder, characterized in that: The specific steps include: Step 1, pre-treating polyamide-imide powder; Step 2, putting the polyamide-imide powder treated in step 1 into a dyeing solution for dyeing, putting the dyed polyamide-imide powder into a soaping solution containing a washing powder solution for soaping to remove the dye and oil stains remaining on the surface of the fabric, and drying after washing.

2. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 1, characterized in that: The specific process of step 1 is: putting the polyamide-imide powder into a soaping liquid for soaping, and drying after the washing is completed.

3. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 2, characterized in that: In the step 1, the amount of polyamide-imide powder used is 1-20 g, the concentration of washing powder in the soaping liquid is 1-3 g / L, the soaping temperature is 50-90° C., the soaping time is 10-20 min; the drying temperature is 60-80° C., and the drying time is 8-16 h.

4. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 2, characterized in that: The specific process of step 2 is: Step 2.1, adding the polyamide-imide powder treated in step 1 into the dye solution, heating at a rate of 2°C / min during the heating process, the dyeing temperature is 80-140°C, and then keeping the temperature for 60 minutes; Step 2.2, stop heating and continue stirring, wait for the dye solution to cool to room temperature, then wash and dry, put the dyed polyamide-imide powder into soaping solution for soaping, and dry after soaping.

5. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 4, characterized in that: In step 2.1, the dye solution is prepared as follows: Add cationic dye, purified water and benzyl alcohol into a beaker, adjust the pH value of the solution to 3-6, stir evenly, and you will get the prepared dye solution.

6. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 5, characterized in that: In the step 2.1, the mass ratio of polyamideimide powder to dye solution is 1:15-30; the mass of cationic dye is 1-5% of the mass of polyamideimide powder; and the concentration of benzyl alcohol is 10-60 g / L.

7. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 6, characterized in that: In the step 2.2, the concentration of washing powder in the soaping liquid is 1-3 g / L, the mass of the soaping liquid is 30 times the mass of the powder used, the soaping temperature is 50-90° C., and the soaping time is 10-20 min.

8. The method for dyeing with a cationic dye based on polyamide-imide powder according to claim 7, characterized in that: In the step 2.2, after dyeing, the drying temperature is 80-120° C. and the drying time is 8-16 hours.

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