Method for screening dyeability of polyester fabric by vegetable dye

Abstract

The invention discloses a method for screening dyeability of a polyester fabric by using a vegetable dye. The method comprises the following steps: (1) calculating an inorganic-organic balance value of polyester; (2) preparing the extracted vegetable dye into a vegetable dye test solution for high performance liquid chromatography, qualitatively measuring the variety of pigment components, and quantitatively measuring the relative mass fraction ratio of each component; (3) calculating an inorganic and organic balance value of the vegetable dye; (4) preparing vegetable dye liquor; (5) wetting a polyester fabric, and putting the polyester fabric into the vegetable dye liquor at room temperature; the pH value is adjusted, and the temperature is slowly increased to the dyeing temperature in the infrared dyeing machine for dyeing; taking out the dyed object; washing with clear water, soaping and drying. According to the method disclosed by the invention, the plant dye with high dye-uptake rate, relatively good K / S value and relatively good dyeing fastness on the polyester fabric is screened out, and the plant dye dyeing chromatography of the polyester fabric is expanded.

Description

Technical Field

[0001] The invention relates to a screening method, in particular to a screening method for plant dyes for dyeing polyester fabrics, belonging to the technical field of polyester fabric dyeing and finishing. Background Art

[0002] With the development of society, polyester fiber among synthetic fibers is the most widely used fiber due to its excellent performance and is widely used in clothing, furniture and other industries. However, polyester fabrics are usually dyed with disperse dyes, which is difficult to achieve with plant dyes. There are few varieties of plant dyes that can be used for polyester dyeing, and there is a lack of methods to judge dyeability. Summary of the invention

[0003] The purpose of the present invention is to provide a method for screening the dyeability of polyester fabrics with plant dyes, screen out plant dyes with high dye uptake, good K / S value and good dyeing fastness for polyester fabrics, and expand the plant dyeing color spectrum of polyester fabrics.

[0004] In order to solve the above technical problems, the following technical solutions are adopted:

[0005] A method for screening the dyeability of polyester fabrics with plant dyes, characterized by comprising the following steps:

[0006] (1) Calculate the inorganic and organic values ​​of the repeating structural units of polyester molecules and substitute them into the formula to calculate the inorganic organic balance (IOB) of polyester;

[0007] (2) The extracted plant dyes are prepared into plant dye test solutions for high performance liquid chromatography, and the types of pigment components are qualitatively measured and the relative mass fractions of each component are quantitatively measured;

[0008] (3) Calculate the inorganic and organic values ​​of each component of the plant dye, and calculate the inorganic-organic balance value of the plant dye by weighted average according to the relative mass fraction of each component;

[0009] (4) placing the extracted plant dye powder in a mortar, adding a very small amount of water and a dispersant, and grinding it thoroughly, transferring it to a beaker, adding water, and stirring to prepare a uniformly dispersed plant dye solution;

[0010] (5) Wetting the polyester fabric, and putting it into the plant dye solution at room temperature; adjusting the pH value, and slowly raising the temperature to the dyeing temperature in an infrared dyeing machine for dyeing; and taking out the dyed material;

[0011] (6) Wash with clean water, soap and dry.

[0012] After optimization, the inorganic-organic balance value calculation method of step (1) is as follows: the inorganic value (I value) of the polyester molecule is calculated and determined by the difference in boiling points of alkane derivatives. The inorganic value increases with the average increase in boiling point of each hydroxyl compound and the corresponding parent alkane, and the inorganic value of the hydroxyl group is determined to be 100; the organic value (O value) of the polyester molecule is calculated and determined by the magnitude of the influence of the alkyl group on the boiling point of the compound. The boiling point of the straight-chain alkane compound increases gradually with each increase in carbon atom. It is stipulated that in organic compounds, no matter what atom the carbon atom is connected to or how the connection is made, the organic value of each carbon atom is 20; the ratio of the inorganic value to the organic value of the compound is the inorganic-organic balance value of the compound.

[0013] Preferably, the polyester fabric is 100g / m 2 Twill woven fabric.

[0014] After optimization, in the step (2), the plant dye test solution is prepared by accurately weighing 10 mg of the plant dye extract respectively, and adding methanol solution to each of them to prepare a plant dye test solution with a mass concentration of 0.1 mg / mL.

[0015] After optimization, the step (2) further includes the preparation of a plant dye standard solution: weighing 10 mg of each plant dye standard into a 100 mL volumetric flask, adding methanol to dissolve and dilute to the scale, shaking well, and preparing a plant dye standard solution with a mass concentration of 0.1 mg / mL.

[0016] After optimization, the chromatographic conditions for the high performance liquid chromatography detection of plant dyes in step (2) are as follows: using an LC-20ADXR high performance liquid chromatograph, the chromatographic column conditions are Shim-pack GIS (250mm×4.6mm, 5μm); PAD detector; methanol and 0.1% phosphoric acid aqueous solution are selected as the mobile phase, and the gradient elution program is that the initial methanol concentration is 20%, the methanol concentration is 20% to 60% at 0-20min, the methanol concentration is 60% to 90% at 20-60min, and the methanol concentration is 90% to 100% at 60-70min; flow rate: 1mL / min; detection wavelength: 254nm; column temperature: 25°C; injection volume: 10μL.

[0017] After optimization, in the step (4), the plant dye solution is prepared according to a bath ratio of 1:50, 2% (owf).

[0018] After optimization, the dyeing process conditions of step (5) are as follows: wet the polyester fabric, put it into a dye vat, and put it into the plant dye solution prepared in step (4) at room temperature; adjust the pH value to 5, slowly increase the dyeing temperature to 130°C at a heating rate of 1°C / min and keep it warm for 60 minutes, and then take it out after cooling it to 30°C at a rate of 2°C / min.

[0019] After optimization, the process conditions of soap washing in step (6) are: adding water at a bath ratio of 1:20, adding soap flakes at 2g / L, and soap washing at 60°C for 20min.

[0020] The above technical solution has the following beneficial effects:

[0021] The present invention calculates the IOB value of polyester as 0.68 through the inorganic-organic balance value theory, and screens out the plant dyes with the closest IOB value through calculation. The closer the IOB value of the plant dye is to the IOB value of the polyester repeating structural unit, the better the hydrophobic combination with the polyester, the higher the K / S value, and the better the color fastness.

[0022] In the present invention, plant dyes are screened through inorganic and organic theories, the plant dyeing color spectrum of polyester fabrics is expanded, and the dyeing depth of the polyester fabrics is adjusted through the dyeing process. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The present invention will be further described below in conjunction with the accompanying drawings:

[0024] Figure 1 is the HPLC chromatogram of Polygonum cuspidatum of Example 2;

[0025] Figure 2 It is the HPLC chromatogram of the yellow pigment of Example 3. DETAILED DESCRIPTION

[0026] The present invention aims to provide a method for screening plant dyes for dyeing polyester fabrics, comprising the following steps:

[0027] (1) Polyester is a type of synthetic fiber composed of linear macromolecules and is polymerized from dibasic acids and diols. Currently, large-scale industrial production of polyester fibers is mainly made from the condensation reaction of polyethylene terephthalate and ethylene glycol. The structure and composition of polyester fibers from the polyester chain are shown below.

[0028]

[0029] The inorganic value is the sum of the inorganic values ​​of two ester groups and one benzene ring, that is, the I value is 60*2+15=135; the organic value is calculated as the sum of the organic values ​​of 10 carbon atoms in the repeating structural unit, that is, the O value is 20*10=200; therefore, the IOB value of polyester is I / O=0.675.

[0030] (2) Since the types and contents of natural products vary slightly from place to place, the main components that account for the majority of the content are selected as the basis for calculation of the IOB value. The inorganic and organic values ​​of common compounds are shown in Table 1.

[0031] Table 1 Inorganic and organic values ​​of some groups

[0032]

[0033] The remaining steps of the screening method are further described by specific embodiments:

[0034] Embodiment 1:

[0035] (1) Natural indigo is mainly derived from the indigo plant and is obtained through biological fermentation. Its main components are 97% indigo and 3% indigotine. Use a reducing agent to treat indigo dye. Add a small amount of water to the weighed indigo dye and grind it in a mortar. Then add water to make a dye solution. Add 15g / L sodium hydroxide and stir it. Then add 20g / L hydrosulfite. Heat it and keep it warm at 55℃ for 20min. When the dye solution becomes a yellow transparent solution, the reduction is complete. Use citric acid to adjust the pH to 7, add polyester fabric at a bath ratio of 1:50, dye the polyester according to the process conditions in 2.3.1, soap it, and then place it in a cool and ventilated environment for natural oxidation.

[0036] The structure of indigo acid is shown below.

[0037]

[0038] The calculated IOB value of indigo leuco acid is 1.168. The effect of indigo leuco acid dye concentration on the K / S value and soap fastness of polyester dyeing is shown in Table 2.

[0039] Table 2 Effect of indigo leuco acid dye concentration on dyeing K / S value and soap fastness

[0040]

[0041] Embodiment 2:

[0042] (1) Polygonum cuspidatum is a plant of the Polygonaceae family. Its main components are anthraquinone pigments, namely rhubarb (C 15 H 10 O5), Chrysophanol (C 15 H 10 O4) and physaccharin methyl ether (C 16 H 12 O5), the structure is shown below.

[0043]

[0044] (2) The high performance liquid chromatography analysis of the Polygonum cuspidatum extract was compared with the standard sample. Figure 1 shown.

[0045] Depend on Figure 1(b) It can be seen that the retention times of chrysophanol, chrysophanol and physophanol methyl ether in the self-extracted knotweed plant dye are 51.988min, 56.076min and 62.113min respectively; Figure 1 (a) The retention times of the standard samples were 51.972 min, 56.105 min and 62.139 min, and the peak times were consistent, with the deviations within the standard allowable range of ±2.5%. It can be determined that the main components of the Polygonum cuspidatum sample are rhamnosin, chrysophanol and rhamnosin methyl ether.

[0046] The calculated IOB value of rhubarb was 1.35, the IOB value of chrysophanol was 1.02, and the IOB value of physophanol methyl ether was 0.95. Calculated by area normalization method, the total anthraquinone content was 1.7%, and the relative content ratios of rhubarb, chrysophanol and physophanol methyl ether were 77.233%, 3.331% and 19.435% respectively. The IOB value of Polygonum cuspidatum calculated by weighted average of the relative contents of the components was 1.2612.

[0047] (3) The dyeing process conditions are as follows: 1 g of polyester fabric is wetted and placed in a dye vat, and then immersed in the prepared knotweed plant dye solution at room temperature; the pH value is adjusted to 5, and the dyeing temperature is slowly increased to 130°C at a heating rate of 1°C / min and kept at this temperature for 60 min, and then the fabric is taken out for soap washing after being cooled to 30°C at a rate of 2°C / min.

[0048] The effect of knotweed dye concentration on the K / S value and soap fastness of polyester dyeing is shown in Table 3.

[0049] Table 3 Effect of Polygonum cuspidatum dye concentration on dyeing K / S value and soap fastness

[0050]

[0051] Embodiment 3:

[0052] (1) Rhubarb is a plant of the Polygonaceae family. Its main components are anthraquinone pigments, namely rhein (C 15 H8O6), Rhein (C 15 H 10 O5), Chrysophanol (C 15 H 10 O4) and physaccharin methyl ether (C 16 H 12 O5), whose molecular structure is shown below.

[0053]

[0054] (2) The effective components of rhubarb were extracted using ethanol solvent and the extract was analyzed by high performance liquid chromatography. The results were compared with those of the standard. Figure 2 shown.

[0055] Depend on Figure 2 (b) It can be seen that the retention times of rhein, rhein, chrysophanol and physophanol methyl ether in the self-extracted rhubarb plant dye are 44.406min, 51.984min, 56.112min and 62.151min respectively; Figure 2 (a) The retention times of the standard samples were 44.382min, 51.972min, 56.105min and 62.139min, and the peak times were consistent, with the deviations within the standard allowable range of ±2.5%. It can be determined that the main components of the rhubarb sample are rhein, rhein, chrysophanol and physophanol methyl ether.

[0056] The calculated IOB value of rhein is 1.51, the IOB value of rhein is 1.35, the IOB value of chrysophanol is 1.02, and the IOB value of physophanol methyl ether is 0.95. The total anthraquinone content of rhubarb is 3.9%, and the relative content ratios of rhein, rhein, chrysophanol and physophanol methyl ether are 23.935%, 47.383%, 34.940% and 3.742%, respectively. The IOB value of rhubarb calculated by weighted average of the relative content of the components is 1.43.

[0057] (3) The dyeing process conditions are as follows: 1 g of polyester fabric is wetted and placed in a dye vat, and then immersed in the prepared rhubarb plant dye solution at room temperature; the pH value is adjusted to 5, and the dyeing temperature is slowly increased to 130°C at a heating rate of 1°C / min and kept warm for 60 min, and then the fabric is taken out for soap washing after being cooled to 30°C at a rate of 2°C / min.

[0058] The effect of rhubarb dye concentration on the K / S value and soap fastness of polyester dyeing is shown in Table 4.

[0059] Table 4 Effect of rhubarb dye concentration on K / S value and soap fastness of polyester dyeing

[0060]

[0061]

[0062] The preferred rhubarb plant dye concentration is 2.0% (owf).

[0063] Comparative Example 1:

[0064] (1) Shellac, the main components are shellac acid A, B, and C. The relative contents of shellac acid A, B, and C are 57.95%, 31.33%, and 6.12%, respectively. The molecular structure is shown below.

[0065]

[0066] (2) The IOB value of lac acid A was calculated to be 2.15, the IOB value of lac acid B was 2.12, and the IOB value of lac acid C was 2.28. The IOB value of lac calculated by weighted average of the relative contents of the components was 2.157.

[0067] (3) The dyeing process conditions are as follows: 1 g of polyester fabric is wetted and placed in a dye vat, and then immersed in the prepared lac plant dye solution at room temperature; the pH value is adjusted to 5, and the dyeing temperature is slowly increased to 130°C at a heating rate of 1°C / min and kept at this temperature for 60 min, and then the fabric is taken out for soap washing after being cooled to 30°C at a rate of 2°C / min.

[0068] The effect of lac dye concentration on the K / S value and soap fastness of polyester dyeing is shown in Table 5.

[0069] Table 5 Effect of lac dye concentration on K / S value and soap fastness of polyester dyeing

[0070]

[0071] Lac vegetable dyes cannot effectively dye polyester.

[0072] Comparative Example 2:

[0073] (1) Carmine comes from cochineal clusters in cactus leaves. Its main component is carminic acid, which has a relative molecular weight of 492.39 and is a glucosylated anthraquinone, accounting for about 95% of the total coloring compounds. The structure of carminic acid is shown below.

[0074]

[0075] The calculated IOB value of carminic acid is 2.80.

[0076] (3) The dyeing process conditions are as follows: 1 g of polyester fabric is wetted and placed in a dye vat, and then immersed in the prepared cochineal red plant dye solution at room temperature; the pH value is adjusted to 5, and the dyeing temperature is slowly increased to 130°C at a heating rate of 1°C / min and kept at this temperature for 60 min, and then the fabric is taken out for soap washing after being cooled to 30°C at a rate of 2°C / min.

[0077] The effect of cochineal red dye concentration on the K / S value and soap fastness of polyester dyeing is shown in Table 6.

[0078] Table 6 Effect of cochineal red dye concentration on K / S value and soap fastness of polyester dyeing

[0079]

[0080] Cochineal vegetable dye cannot effectively dye polyester.

[0081] Comparative Example 3:

[0082] The main component of the ethanol extract of grape seeds is 95.0% oligomeric proanthocyanidins, the structure of which is shown below.

[0083]

[0084] The calculated IOB value of proanthocyanidins is 1.87.

[0085] (3) The dyeing process conditions are as follows: 1 g of polyester fabric is wetted and placed in a dye vat, and then immersed in the prepared grape seed plant dye solution at room temperature; the pH value is adjusted to 5, and the dyeing temperature is slowly increased to 130°C at a heating rate of 1°C / min and kept at this temperature for 60 min, and then the fabric is taken out for soap washing after being cooled to 30°C at a rate of 2°C / min.

[0086] The effect of grape seed dye concentration on the K / S value and soap fastness of polyester dyeing is shown in Table 7.

[0087] Table 7 Effect of grape seed dye concentration on K / S value and soap fastness of polyester dyeing

[0088]

[0089] Grape seed dye does not dye polyester effectively.

[0090] The polyester fabrics dyed with plant dyes described in Examples 1, 2, 3 and Comparative Examples 1, 2, 3 were tested.

[0091] K / S value: SF600X Datacolor colorimetric spectrometer was used to test the K / S value of the fabric under D65 light source.

[0092] Fastness test: Determine the light fastness of dyed samples according to GB / T 8427-2008 "Textiles - Tests for colour fastness - Colour fastness to artificial light: Xenon arc fading lamp". Refer to GB / T 3921-2008 "Textiles - Tests for colour fastness - Colour fastness to washing with soap" and use the grey scale to assess the colour change of samples and the staining fastness to adjacent fabrics.

[0093] The influence of plant dye IOB value on polyester dyeing K / S value, soap fastness and light fastness is shown in Table 8.

[0094] Table 8 Effect of plant dye IOB value on polyester dyeing K / S value, soap fastness and light fastness

[0095]

[0096]

[0097] According to the data in Table 8, it can be seen that the polyester fabrics dyed with plant dyes under the process conditions described in Examples 1, 2, and 3 all have good dye uptake, K / S value, and soap fastness, among which the wearing properties of Example 2 under the preferred process conditions are the best.

[0098] By comparing Example 1 with Control Example 1, it can be seen that when the dye concentration is 2% owf and the IOB value of the plant dye is 2.157, the K / S value of the polyester fabric is too low and the plant dye cannot be effectively dyed. When the IOB value of the plant dye is 1.168, the polyester fabric has a K / S value of 11.89, and the plant dye dyeing effect is good. By comparing Example 1 with Example 3, it can be seen that the structure-activity relationship between the dyeing rate of the plant dye on the polyester fabric, the K / S value and the IOB value of the plant dye is that the closer the IOB value is to 0.675 of polyester, the higher the dyeing rate of the plant dye on the polyester fabric and the larger the K / S value.

[0099] By comparing Examples 1 and 2 with Example 3, it can be seen that when the IOB value of the plant dye is 1.236, the soap fastness of the dyeing of polyester fabric is 3 to 4, and the sunlight fastness is 2 to 3; when the IOB value of the plant dye is 1.115, the soap fastness of the dyeing of polyester fabric is 4 to 5, and the sunlight fastness is 4. The closer to the IOB value of polyester 0.675, the better the soap fastness and sunlight fastness of the plant dye to the polyester fabric. The fastness of the plant dye within the IOB value of 1.2 can meet the wear performance requirements.

[0100] According to the plant dye screening method for dyeing polyester fabrics of the present invention, the IOB value of the plant dye is calculated, and the IOB value of the polyester repeating structure unit is compared to screen out the plant dye with a larger K / S value, and the plant dye with better soap fastness can be screened out by comparing the IOB values ​​of multiple plant dyes. Therefore, the polyester fabric dyeing and finishing technology of the present invention has broad application prospects.

[0101] The above are only specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent replacements or modifications made based on the present invention to solve basically the same technical problems and achieve basically the same technical effects are all included in the protection scope of the present invention.

Claims

1. A method for screening the dyeability of polyester fabrics with plant dyes, characterized in that The steps include: (1) Calculate the inorganic and organic values ​​of the repeating structural units of polyester molecules, and substitute them into the formula to calculate the inorganic-organic balance value of polyester; (2) The extracted plant dyes are prepared into plant dye test solutions for high performance liquid chromatography, and the types of pigment components are qualitatively measured and the relative mass fractions of each component are quantitatively measured; (3) Calculate the inorganic and organic values ​​of each component of the plant dye, and calculate the inorganic-organic balance value of the plant dye by weighted average according to the relative mass fraction of each component; (4) placing the extracted plant dye powder in a mortar, adding water and a dispersant, and grinding it thoroughly, transferring it to a beaker, adding water, and stirring to prepare a uniformly dispersed plant dye solution; (5) Wetting the polyester fabric, and putting it into the plant dye solution at room temperature; adjusting the pH value, and slowly raising the temperature to the dyeing temperature in an infrared dyeing machine for dyeing; and taking out the dyed material; (6) Wash with clean water, soap and dry.

2. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: In the step (1), the inorganic-organic balance value calculation method is as follows: the inorganic value of the polyester molecule is calculated and determined by the difference in boiling points of alkane derivatives. The inorganic value increases with the average increase in boiling point of each hydroxyl compound and the corresponding parent alkane, and the inorganic value of the hydroxyl group is determined to be 100; the organic value of the polyester molecule is calculated and determined by the magnitude of the influence of the alkyl group on the boiling point of the compound. The boiling point of the straight-chain alkane compound increases with each increase in carbon atom. It is stipulated that in organic compounds, no matter what atom the carbon atom is connected to or how the connection is made, the organic value of each carbon atom is 20; the ratio of the inorganic value to the organic value of the compound is taken as the inorganic-organic balance value of the compound.

3. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: The polyester fabric is 100g / m 2 Twill woven fabric.

4. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: The step (2) is to prepare a plant dye test solution: 10 mg of the plant dye extract is weighed respectively, and methanol solution is added to each of the plant dye extracts to prepare a plant dye test solution with a mass concentration of 0.1 mg / mL.

5. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: The step (2) also includes preparing a plant dye standard solution: weighing 10 mg of each plant dye standard, adding methanol to dissolve and dilute to the scale, shaking well, and preparing a plant dye standard solution with a mass concentration of 0.1 mg / mL.

6. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: The chromatographic conditions for the high performance liquid chromatography detection of plant dyes in step (2) are as follows: using an LC-20ADXR high performance liquid chromatograph, the chromatographic column condition is Shim-pack GIS (250mm×4.6mm, 5μm); PAD detector; the mobile phase is selected from methanol and 0.1% phosphoric acid aqueous solution, and the gradient elution program is that the initial methanol concentration is 20%, the methanol concentration is 20% to 60% at 0-20min, the methanol concentration is 60% to 90% at 20-60min, and the methanol concentration is 90% to 100% at 60-70min; flow rate: 1mL / min; detection wavelength: 254nm; column temperature: 25°C; injection volume: 10μL.

7. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: In the step (4), a plant dye liquor is prepared according to a bath ratio of 1:50, 2% (owf).

8. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: In the step (5), the dyeing process conditions are as follows: wet the polyester fabric, put it into a dye vat, and put it into the plant dye solution prepared in step (4) at room temperature; adjust the pH value to 5, slowly increase the dyeing temperature to 130° C. at a heating rate of 1° C. / min and keep it warm for 60 minutes, and then take it out after cooling it to 30° C. at a heating rate of 2° C. / min.

9. The method for screening the dyeability of polyester fabrics by plant dyes according to claim 1, characterized in that: The process conditions for soap washing in step (6) are as follows: water is introduced at a bath ratio of 1:20, 2 g / L of soap flakes are added, and soap washing is performed at 60° C. for 20 min.

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